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Table of Contents

A-Differential Thermal Analysis

Objectives . . . . . . . . . . . . . . . . . . . . . . . A-1

Introduction . . . . . . . . . . . . . . . . . . . . . A-1

Differential Thermal Analysis(DTA) . . . . . . . . . . . A-1

Use of DTA to Characterize Clay . . . . . . . . . . . . . A-4

Sample, and Object of this DTA Experiment . . . . . . . A-6

Procedure for DTA Run . . . . . . . . . . . . . . . A-6

Analysis of DTA Run . . . . . . . . . . . . . . . . . . . A-10

Modern DTA Measurements . . . . . . . . . . . . . . . A-10

Writeup . . . . . . . . . . . . . . . . . . . . . . . . . . A-11

B-Temperature Measurement and


Objectives . . . . . . . . . . . . . . . . . . . . . . . B-1

Introduction. . . . . . . . . . . . . . . . . . . . . . B-1

Introduction to Experimental Procedures. . . . . . . . . B-2

Ceramic Cones Experiment . . . . . . . . . . . . . B-2

Procedure . . . . . . . . . . . . . . . . . . . . . . . . . . B-4

Writeup . . . . . . . . . . . . . . . . . . . . . . . . . . . B-5

Temperature Transient Experiment. . . . . . . . . B-5

Procedure . . . . . . . . . . . . . . . . . . . . . . . . . . B-5

Writeup . . . . . . . . . . . . . . . . . . . . . . . . . . . B-5

Thermocouple Experiment . . . . . . . . . . . . . . B-6

Procedure . . . . . . . . . . . . . . . . . . . . . . . . . . B-6


Writeup . . . . . . . . . . . . . . . . . . . . . . . . . . . B-7

Temperature Distribution in a Furnace . . . . . . . B-7

Procedure . . . . . . . . . . . . . . . . . . . . . . . . . . B-8

Writeup . . . . . . . . . . . . . . . . . . . . . . . . . . . B-9

Non-contact Temperature Measurement . . . . . . B-9

Infrared Temperature Measurement . . . . . . . . . . B-10

Procedure . . . . . . . . . . . . . . . . . . . . . . . . . B-10

Writeup . . . . . . . . . . . . . . . . . . . . . . . . . . B-11

C-Measurement of Force and Strain

Using Gauges

Objectives . . . . . . . . . . . . . . . . . . . . . . C-1

Introduction to Measurement of Forces . . . . . . . C-1

Resistance Strain Gauges . . . . . . . . . . . . . . . . . C-2

Types of Strain Gauges . . . . . . . . . . . . . . . . . . C-3

Wheatstone Bridges . . . . . . . . . . . . . . . . . . . . C-4

Experimental Setup . . . . . . . . . . . . . . . . . C-6

Procedure . . . . . . . . . . . . . . . . . . . . . . . . . . C-6

Writeup . . . . . . . . . . . . . . . . . . . . . . . . . . C-9

D-Measurement of Length and


Objectives . . . . . . . . . . . . . . . . . . . . . . . D-1

Measurement of Length (part A) . . . . . . . . . . D-1

Procedure for Part A . . . . . . . . . . . . . . . . . . . . D-2

Write-Up for Part A . . . . . . . . . . . . . . . . . . . . D-2


Measurement of Displacement (part B) . . . . . . . D-3

Procedure for the LVDT . . . . . . . . . . . . . . . . . . D-6

Writeup for Part B . . . . . . . . . . . . . . . . . . . . . D-7

E-Chemical Analysis by Reaction


Chemical Analysis . . . . . . . . . . . . . . . . . . E-1

Objectives . . . . . . . . . . . . . . . . . . . . . . E-1

Introduction . . . . . . . . . . . . . . . . . . . . . E-2

Carbon and Sulfur Analysis . . . . . . . . . . . . . . . . E-2

Theory of Operation . . . . . . . . . . . . . . . . . . . . E-2

Experimental Procedure . . . . . . . . . . . . . . . E-4

Write-up for Carbon and Sulfur Analysis . . . . . . . . E-4

F-Metallographic Observation

Objectives . . . . . . . . . . . . . . . . . . . . . . . F-1

Introduction . . . . . . . . . . . . . . . . . . . . . . F-1

Experimental Procedure . . . . . . . . . . . . . . . F-2

Write up . . . . . . . . . . . . . . . . . . . . . . . . . . F-2

Description of Metallographic Polishing Samples . . . . F-3

G-Datalogging of Quenching Curves

Objectives . . . . . . . . . . . . . . . . . . . . . . G-1

Introduction . . . . . . . . . . . . . . . . . . . . . G-1

Quenching Curves . . . . . . . . . . . . . . . . . . . . . G-1

Details of Experiment . . . . . . . . . . . . . . . . . . . G-3


Procedure . . . . . . . . . . . . . . . . . . . . . . G-5

Acquiring the Data . . . . . . . . . . . . . . . . . . . . G-5

Program . . . . . . . . . . . . . . . . . . . . . . . . . . G-5

Plots . . . . . . . . . . . . . . . . . . . . . . . . . . . . G-6

H-Electrical Properties

Objectives . . . . . . . . . . . . . . . . . . . . . . . H-1

Introduction . . . . . . . . . . . . . . . . . . . . H-1

Electrical Conduction . . . . . . . . . . . . . . . . . . . H-1

The Hall Effect . . . . . . . . . . . . . . . . . . . . . . . H-4

Thermoelectric Effect . . . . . . . . . . . . . . . . . . . H-6

Non-ohmic devices . . . . . . . . . . . . . . . . . . . . . H-6

Integrated Circuits. . . . . . . . . . . . . . . . . . . . . H-8

Procedure for the First Afternoon . . . . . . . . . . H-9

Electrical Conductivity Measurements . . . . . . . . . H-9

Measurement of Electrical resistivity . . . . . . . . . . H-11

Hall Effect . . . . . . . . . . . . . . . . . . . . . . . . H-12

Procedure for the Second Afternoon . . . . . . . . H-12

Using the Thermoelectic Effect . . . . . . . . . . . . . H-12

Current-Voltage of a p-n Junction . . . . . . . . . . . . H-13

Metallographic Observation of a p-n Junction . . . . . H-13

C-V Characteristics and Microstructures of MOV . . . H-14

Observation of an Integrated Circuit . . . . . . . . . . H-14

Resistivity and Hall Voltage . . . . . . . . . . . . H-15

Resistivity measured by current . . . . . . . . . . . . . H-15


Carrier density, n . . . . . . . . . . . . . . . . . . . . . H-15

Calculate mobility, u . . . . . . . . . . . . . . . . . . . H-15

I-Mass Transport by Diffusion

Objectives . . . . . . . . . . . . . . . . . . . . . . . I-1

Introduction . . . . . . . . . . . . . . . . . . . . . . I-1

Procedure for the first afternoon . . . . . . . . . . . I-4

Diffusion in Gels . . . . . . . . . . . . . . . . . . . . . . I-5

Decarburization of steel . . . . . . . . . . . . . . . . . . I-6

Procedure for the Second Afternoon . . . . . . . . . I-6

Heat by Conduction . . . . . . . . . . . . . . . . . . . . . I-6

Carburization of Steel . . . . . . . . . . . . . . . . . . . I-7

J-Mechanical Properties

Objectives . . . . . . . . . . . . . . . . . . . . . . . J-1

Introduction . . . . . . . . . . . . . . . . . . . . . J-1

Tensile Test . . . . . . . . . . . . . . . . . . . . . . . . . J-1

Impact Test . . . . . . . . . . . . . . . . . . . . . . . . . J-3

Testing Brittle Materials . . . . . . . . . . . . . . . . . J-6

Linear Intersection Method . . . . . . . . . . . . . . . . J-7

Procedures for the First Afternoon . . . . . . . . . . J-9

Tensile Test . . . . . . . . . . . . . . . . . . . . . . . . . J-9

Microstructures. . . . . . . . . . . . . . . . . . . . . . . J-9

Compression Testing . . . . . . . . . . . . . . . . . . . J-10

Procedure for the Second Afternoon . . . . . . . . J-10

Microstructure to Mechanical properties . . . . . . . . J-10


Impact Testing . . . . . . . . . . . . . . . . . . . . . . J-10

Bend Testing of Glass . . . . . . . . . . . . . . . . . . . J-11

Write up . . . . . . . . . . . . . . . . . . . . . . . J-11

K-Sintering and Density

Objectives . . . . . . . . . . . . . . . . . . . . . . K-1

Introduction . . . . . . . . . . . . . . . . . . . . . K-1

First Afternoon . . . . . . . . . . . . . . . . . . . . K-4

Calibration of the Gradient Furnace . . . . . . . . . . . K-4

Overnight Sintering . . . . . . . . . . . . . . . . . . . . K-6

Second Afternoon . . . . . . . . . . . . . . . . . . K-6

Procedure for Measuring the Density of Clay Samples. . K-6

Density using the boiling method . . . . . . . . . . . . . K-7

Sintered Ceramic Microstructure . . . . . . . . . . . . . K-8

Writeup . . . . . . . . . . . . . . . . . . . . . . . . K-8


Objective . . . . . . . . . . . . . . . . . . . . . . . L-1

Introduction . . . . . . . . . . . . . . . . . . . . . L-1

Single Electrode Processes . . . . . . . . . . . . . . . . L-1

Galvanic Cells . . . . . . . . . . . . . . . . . . . . . . . L-3

Concentration Polarization . . . . . . . . . . . . . . . . L-4

Inhibitors and Passivation . . . . . . . . . . . . . . . . . L-5

Non-uniform "pitting" and "crevice" corrosion . . . . . . L-6

Procedure for the First Afternoon . . . . . . . . . . L-6

Galvanic couples . . . . . . . . . . . . . . . . . . . . . . L-6


Concentration polarization . . . . . . . . . . . . . . . . L-7

Anodes and cathodes . . . . . . . . . . . . . . . . . . . L-7

Sacrificial Anode . . . . . . . . . . . . . . . . . . . . . . L-9

Procedure for the Second Afternoon . . . . . . . . L-10

Polarization Curve . . . . . . . . . . . . . . . . . . . . L-10

Writeup . . . . . . . . . . . . . . . . . . . . . . . L-12

M-Magnetic Materials

Objectives. . . . . . . . . . . . . . . . . . . . . . . M-1

Introduction . . . . . . . . . . . . . . . . . . . . . M-1

Magnetic Moments and Domains . . . . . . . . . . . . . M-1

Magnetization and B-H Curves . . . . . . . . . . . . . M-3

Metal for a Transformer Core . . . . . . . . . . . . . . M-4

The Role of Sample Shape in Measuring B-H Curves . . M-6

Oscilloscopes for B-H Curves . . . . . . . . . . . . . . . M-6

Procedure for First Afternoon . . . . . . . . . . . . M-9

Observation of Domains in Orthoferrite Crystals . . . M-12

Application of an External Magnetic Field . . . . . . . M-12

Writeup for First Afternoon . . . . . . . . . . . . . . . M-12

Procedure for Second Afternoon . . . . . . . . . . M-13

Familiarization. . . . . . . . . . . . . . . . . . . . . . M-13

Start-up . . . . . . . . . . . . . . . . . . . . . . . . . M-13

Observation of B-H Curve and Output Distortion . . . M-14

Experiments on Toroids . . . . . . . . . . . . . . . . . M-14

Toroids to be Measured . . . . . . . . . . . . . . . . . M-16


Writeup for Second Afternoon . . . . . . . . . . . . . . M-17

Reference . . . . . . . . . . . . . . . . . . . . . . M-18

II-Background Reading

Thermocouples . . . . . . . . . . . . . . . . . . . . II-1

Laws of Thermocouple Behavior . . . . . . . . . . . . . II-3

Common Thermocouples. . . . . . . . . . . . . . . . . . II-5

Accuracy . . . . . . . . . . . . . . . . . . . . . . . . . . II-8

Other Information . . . . . . . . . . . . . . . . . . . . . II-8

References . . . . . . . . . . . . . . . . . . . . . . . . . II-9

Materials 2H03 on-line Laboratory Manual
Updated: 11 May 2000

Experiment A
Differential Thermal Analysis


To gain the following knowledge and experience:

• prepare a sample for differential thermal analysis, DTA.

• run a DTA curve to determine the amount of halloysite and kaolinite in
the clay.

2. Introduction

The DTA measurement is time consuming as the furnace is heated and cooled at a
fairly slow rate. Thus, the lab will begin with this, and while it is running, the
second part of the lab will be done.

2.a: Differential Thermal Analysis(DTA)

A cooling curve is obtained by measuring the temperature of the sample Ts as it

cools with time. If only the sample is present, and an exothermic reaction (such as

Differential Thermal Analysis(DTA) 1

A-Differential Thermal Analysis

solidification) occurs, the cooling curve will have a flat section as can be seen in
curve (a).

This is a direct result of the Gibbs phase rule, which states that if a system
containing C components and P phases is in equilibrium, the number of degrees of
freedom F is given by:

P+F = C+2

where, a degree of freedom is an intensive variable such as temperature, pressure,

mole fractions of the components, etc., that can be varied independently while still
maintaining equilibrium. For constant pressure, the phase rule becomes:

P+F = C+1

So, a sample of one component will have an extra phase present upon solidification
(i.e. solid in equilibrium with liquid), resulting in the loss of a degree of freedom.
This means that the temperature must remain constant during solidification,
leading to the flat section in the cooling curve. The heat emitted is (dH)Nm where
Nm is the number of moles and dH is the heat of reaction per mole.

If the sample is contained in a metal block, such as the nickel block in the top figure,
the heat emitted by the sample must diffuse through the nickel to the surface.

Introduction A-2
A-Differential Thermal Analysis

Thus, measuring the temperature difference between the sample and the nickel
block will give curve (b).

Better still, is to have a standard that is similar in all respects to the sample except
that it has no transformation, and measure the difference between the sample
temperature and it. This will give curve (c)

which has low background and can therefore be amplified to get a sensitive signal.
It is an excellent example of using a comparison measurement to achieve greater
sensitivity. Often the curve is plotted (Ts-Tstd) = dT against the temperature of the
standard, as in curve (d).

Since the temperature of the standard would otherwise decrease at a constant rate,
the peak gives a measure of the heat emitted by the sample during the

Differential Thermal Analysis(DTA) A-3

A-Differential Thermal Analysis

transformation. That is, the area under the peak gives a measure of (dH)Nm, after
the appropriate correction for amplification.

2.b: Use of DTA to Characterize Clay

Since commercial clays are dug out of the ground, they have many components. A
DTA curve is often used to indicate which type of clay and "accessory minerals"
such as SiO2 from sand or carbonate from limestone, are present. Three simple
types of clay are the following:

Kaolinite Al2Si2O5(OH)4 - is a layered structure with a sheet of silicate tetrahedra

on one side of the layer and OH ions on the other. These OH are part of the crystal
lattice, but on heating in the range 620 to 750ºC are emitted as steam. The release
of this "structural water" is an endothermic reaction requiring 30 kCal/mole of
kaolinite (this is the first peak of curves a and b Fig. 1, at a temperature of
approximately 600ºC). This DTA peak could be used to determine the amount of
kaolinite present, but is usually complicated by impurities.

Removing the structural water leaves behind Al2O32SiO2, which on heating to

980ºC forms mullite (2SiO23Al2O3) and excess SiO2. The transformation of this
SiO2 from its amorphous to quartz form produces a sharp exothermic peak of 9
kCal/mole SiO2 (this is the second peak of curves A and B Fig.1), which can be used
to determine the amount of this excess SiO2 present.

On cooling, the SiO2 changes from ß to alpha quartz, an exothermic reaction at

570°C with 0.27 kCal/mole. This can be used to determine the total amount of SiO2
then present.

Halloysite Al2Si2O5(OH)4- 2H2O - is the same as kaolinite but has excess water
between the layers. This weakly bonded "molecular water" is released around
120ºC with approximately 12 kCal/mole of halloysite (the first peak of curve c
Fig.1). Thus, this DTA peak is a measure of the amount of halloysite present.

Montmorillonite or "bentonite" Al2Si4O10(OH)2 - is similar to kaolinite but has

silicate tetrahedra on both sides of each layer. It has half the number of OH ions as
kaolinite but twice the silica. Thus, each mole will have half the structural water
DTA peak, but 2.5 times the silica peaks of kaolinite. Curve d in Fig.2 is most
typical, but it can be seen that all samples of Montmorillonite (i.e. A to F) contain a
large number of impurities as indicated by the presence of extra peaks.

Effect of Particle Size: the size of particles from which the clay is composed does not
affect the position of the DTA peaks (i.e. at which temperature they occur), but the
smaller the particle size, the smaller and broader the peaks become.

Introduction A-4
A-Differential Thermal Analysis


Differential thermal curves:

(A) Kaolinite, Georgia; well crystallized
(B) Kaolinite, Illinois; poorly crystallized
(C) Hydrated halloysite, Indiana
(D) Anauxite
(E) Allophane


Differential thermal curves:

(A) Montmorillonite, California
(B) Montmorillonite, Mexico

Use of DTA to Characterize Clay A-5

A-Differential Thermal Analysis

(C) Montmorillonite, Wyoming

(D) Montmorillonite, Arizona
(E) Montmorillonite, Mississippi
(F) Montmorillonite, Arkansas
(G) Nontronite, Arkansas
(H) Hectorite, California

Effect of Heating Rate: the heating rate does not affect the position of the DTA
peaks, but the faster the heating rate, the sharper the peaks become (i.e. narrower
and higher).

2.c: Sample, and Object of this DTA Experiment

In nature, the clays are seldom found together, so a quick DTA run determines
whether halloysite, kaolinite, or Montmorillonite are present, and also how much
sand, limestone, or other "accessory minerals" are present. As can be seen from the
actual DTA curves, the number of auxiliary peaks indicates that these clays are
rarely found in pure form. In this lab, we want to do a more quantitative
measurement, which DTA is often used for, and samples have been prepared for
this purpose. The demonstrator will provide you with a value for the silica content.
The clay will be a mixture of pure halloysite and kaolinite. We wish to determine
the ratio of the amount of halloysite to the amount of kaolinite using the area of the
120 and 680°C peaks on heating, with their known values of dH. The known
amount of silica and the measured area of the 570°C peak on cooling can be used to
calibrate the DTA apparatus. In commercial practice, the 680°C peak is not used for
quantitative calculations as in this experiment. Its H is too variable and a higher
temperature peak is used. However, the time limits us for this particular

To assist your appreciation for the function and operation of thermocouples, see
the Background Reading.

3. Procedure for DTA Run

Weigh an amount of sample powder (about 1.5g) that is more than enough to fill the
silica sample cup of the DTA apparatus, when tapped. Pick the thermocouple

Procedure for DTA Run A-6

A-Differential Thermal Analysis

marked "sample". Put its "hot junction" in the silica sample cup 1/3 filled with
powder, and tap sample powder around it using a glass rod. Put the cup in the
nickel block of the DTA apparatus at the hole marked S. Reweigh the excess sample
powder to determine the weight of the sample. This will only work if you have not
spilled any sample powder. Pick the thermocouple marked "standard". Place it in
the other silica cup exactly as done for the sample and tap dry alumina powder
(unweighed) around it exactly as for the sample. This is the "standard" and the heat
flow from this should be as nearly equal to that of the sample as possible, so they
must be prepared the same way.

These two thermocouples from the sample and the standard are already wired in
series opposition, so the difference between their voltages is amplified by a factor
100. The amplified signal is fed to the input of the data logging equipment.

Pick the thermocouple attached to the "reference" of the data-logger. Place its hot
junction in the third silica cup, and tap in alumina powder exactly as for the

With the samples and nickel block in the furnace, turn on the furnace power and
record the DTA curve on heating to 750°C and on cooling. The furnace has no
controller as it heats at a reasonable rate under full power. An extra thermocouple
near the furnace windings is used to stop it at some fixed maximum temperature.

° Open DASTC Graph Version Test program

° The setup file should read C:\DASTC\2H3-A.INI
° Check the parameters by using the down arrow and enter to select
Define Acquisition Parameters from the Main Screen and choose A/D
DASTC Card. The correct settings for this experiment should be as

Gain °C|V/Read Channels Synced

CH ON Thermocouple Time/Read(s)
-2.5V to 10V (°C|V/mV) to this one

-6.25 to 25 m
0 K:Chromel/Al 0 0.000000 0

1 X K:Chromel/Al -6.25 to 25 m 0 4.000000 100

2 X V: Volts see -6.25 to 25 m 0 0.010000 10

3 K:Chromel/Al -6.25 to 25 m 0 0.000000 0

4 K:Chromel/Al -6.25 to 25 m 0 0.000000 0

Sample, and Object of this DTA Experiment A-7

A-Differential Thermal Analysis


° Go back to menu screen and use the arrow and enter to highlight
Perform Data Acquisition.
° A green table will appear asking for a filename (this should include the
group name and the distinction between the cooling and heating curve
to a maximum of 8 characters and have the extension .dat). A blue
screen should then open titled Data Acquisition. The numbers
indicated in the upper right corner will be the timer for the
experiment; the number in the lower right corner indicate the number
of reading taken by the program (ie: 000239:0 has taken 239 readings).
The CJC is the cold junction compensation reading (the temperature of
the blue box) and this number is recorded but no actively used in this
experiment. The first column is labeled CHN and shows the active
channels (should be 1 and 2 for current experiment). The next column
shows the current temperature (in °C) in the CHN 1 row, and the
differential (chosen in mV here) in the CHN 2 row. The record(s)
column will show the time the last reading was taken. The record
ΰC/V shows the last temp (in row 1) and differential (in row 2)
readings that were stored. If the program is paused when opened, be
sure to start acquisition by pressing P.
° To view the graph of the data points being taken by the program, type
° When finished taking enough points to about 750°C, quit (Q), adding
notes when prompted, and switch to cool and repeat the process for the
cooling cycle and then quit the program.
° In Excel: open the file, which should be recognized in delineated
format by Excel.
° Sort by channel and then by time as readings were taken of both the
temperature and the differential at their respective conditions (set in
the parameters of the DASTC Graph Version Test program).
° Organize the data in such a way that the temperature can be plotted
on the X-axis, and the differential on the Y-axis of an XY scatter
° Note that the correct units must be used when data is put into the

Procedure for DTA Run A-8

A-Differential Thermal Analysis

The heating curve will look like this (Figure 3):

where dT = (Tsample-Tstd) and T is Tstd. The first peak is due to molecular water
in halloysite and the second is due to structural water in both kaolinite and

The program must be re-set for the cooling cycle!

At 750°C, shut off the furnace power. Measure the cooling rate in the region of the
silica peak (at about 570°C).

The cooling curve will look like this (Figure 4):

where the peak is due to the β→α transformation in the quartz.

Sample, and Object of this DTA Experiment A-9

A-Differential Thermal Analysis

3.a: Analysis of DTA Run

Measure the area of each "peak" in cm2 after correcting for the background. The
area can be measured by counting the squares on the graph paper.

The heat of reaction (H) is given by the following equation:

dH = EA(dTs)(Ts)(aNm)...(1)

where: A is the peak area (cm2); dTs is the scale on the Y-axis of the plot (°C/cm); Ts
is the scale on the X-axis (°C/cm); "a" is the cooling/heating rate (°C/min); Nm is the
number of moles in the sample that produces the reaction with dH; and E is a
constant that depends on the sample geometry.

In order to calibrate our apparatus, the constant E must be calculated. This is done
by using the area of the silica peak at 570°C on cooling. Given the initial weight of
silica, and the known heat of reaction dH=0.27 kCal/mole silica, E can be calculated
using equation (1).

Calculate the number of moles of halloysite, Nm, using equation (1), and the area of
the 120°C peak on heating, dH for this reaction is 12 kCal/mole of halloysite. The
value of E is obtained from the silica peak. Calculate the number of moles of
kaolinite using the area of the 680°C peak on heating (dH = 30 kCal/mole of
kaolinite plus halloysite), E is obtained from the silica peak as before, and the
number of moles of halloysite is calculated from the 120°C peak. Finally, convert
the number of moles to grams, and compare the result with the initial weight.

3.b: Modern DTA Measurements

The simple apparatus provided you for this experiment is nothing like a real
commercial DTA instrument! The demonstrator will take you to see such an
instrument in a research laboratory, describe its operation and provide a sample

Procedure for DTA Run A-10

A-Differential Thermal Analysis

plot from the commercial instrument. Here is such a sample from a DTA
measurement on the type of sample used in this experiment:

3.c: Writeup

The writeup should include the following (and nothing more).

1. A copy of the DTA curve with the axes drawn and labeled
properly, i.e. what is plotted, units used and values along the
2. The recorded sensitivity values for each part of the DTA
curve. The measured heating and cooling rates with their
estimated errors. These sensitivity values will be needed for
the scales in part 1, but experimental data should always be
given so that a possible error could be traced later.
3. The measured area of each of the three peaks and the
uncertainty in each of these measured areas, with a sentence
commenting on how you deduced this uncertainty.
4. The value of E and its uncertainty deduced from the silica
peak. State clearly how you deduced this uncertainty. In
order to reduce the amount of calculating, assume dH, dTs, Ts
and a, have zero error.
5. The number of moles of halloysite and kaolinite in the
sample, showing the values used in the equation from which
they are calculated.

Writeup A-11
A-Differential Thermal Analysis

6. The uncertainty in the number of moles of halloysite and

kaolinite in the sample, showing clearly how you deduced this

Procedure for DTA Run A-12

Materials 2H03 on-line Laboratory Manual
Updated: 11 May 2000

Experiment B
Temperature Measurement and
1. Objectives

• To determine the pyrometric cone temperature of two classes of cones,

and the effect of heating rate.
• To measure a furnace temperature with a thermocouple and examine the
errors introduced by different cold junctions.
• To determine the length of the hot zone within 5ºC of the peak
temperature in a tube furnace, using one thermocouple and using a
differential thermocouple; and examine the errors in each determination.
• To use a thermocouple for measuring the temperature rise when a
sample is put in the furnace.
• To examine how thermocouples are used in temperature controllers.
• To determine the accuracy and repeatability of the measurement of a
high temperature using an (infrared) optical pyrometer.

2. Introduction

The ability to measure temperatures accurately is of great importance in many

refining, fabricating, and heat treating operations. Since the temperature is not
necessarily uniform, and in particular drops near any region of heat loss, a
representative temperature is sometimes difficult to achieve. However, local values
can usually be measured accurately.

There are many ways to measure temperature. Some use a change in dimensions
such as thermometers with liquids or gas, or bimetallic strips. However, the most
common industrial way is the thermocouple, that produces a voltage (emf) which
depends on the temperature difference between the ends of two dissimilar wires.
Since the range is limited by the melting temperature of the metals, at very high
temperatures an optical pyrometer is used.

Firing of ceramics involves both time and temperature. Since they must be slowly
heated and cooled, the total effect summed over all the temperatures must be
included, which is achieved using "pyrometric cones".

B-Temperature Measurement and Control

The following table summarizes the temperature range and sensitivity of some of
these methods.

Device Range Used (°C) Normal Sensitivity (°C)


glass- mercury -40 to 350 0.5

-40 to 70
glass-alcohol 0.5


base metal -200 to 1200 0.1 to1.0

platinum type 0 to 1500 0.1 to 3.0

W-5RhW-25 Rh 0 to 2000 0.1 to 2.0

-273 to 1300 0.1 to 2.0

above 700 about 10

-60 to 3000 2 to 30

2.a: Introduction to Experimental Procedures

This experiment is divided into four parts, so that each student can do the parts
individually, spending up to 45 minutes on each part. The instructions should be
self explanatory. Read them and do the experiment, calling on the demonstrator if
in trouble.

The ceramic cones will take most of the period and are simple observations, so each
student should take a turn observing them for 45 minutes. Because it has long
waiting periods the experiment on the temperature transient is done at the same

3. Ceramic Cones Experiment

This part should be done simultaneously with Part 2A, as the cone
observation is very simple.

Ceramic Cones Experiment B-2

B-Temperature Measurement and Control

Ceramic cones

These are used to monitor firing cycles in which both temperature and time are
important. When firing ceramics, an appreciable amount of the reaction is
occurring during the heating and cooling, since these must be done very slowly. The
ceramic ware is often moved continuously through a kiln with a temperature
distribution something like this:

Thus, a monitoring system is needed to include the effect of the whole thermal
cycle. A very practical one is used that is directly related to the firing process in the
ceramic ware. (This is an example of an important principle in engineering
measurement. When the process is complex, use a measuring device that is a direct
indicator of the thing you are interested in).

Many ceramics are fabricated by mixing powders of various types, compressing

them to produce the final shape, and then firing. This sintering process involves
diffusion so depends on both temperature and time. In some cases, some of the
powder, called a "flux", has a lower melting point. During the firing process, it forms
a viscous liquid, whose amount of flow depends on both temperature and time. On
cooling it becomes rigid of course. The industry has developed compressed

Introduction to Experimental Procedures B-3

B-Temperature Measurement and Control

asymmetric cones of a variety of mixed powders, which will bend over as their flux
becomes more liquid.

In practice, that firing cycle is used that gives the optimum final properties of the
ware (often wear resistance). The firing cycle is determined experimentally and is
then monitored by a cone that has just bent over to touch its base at the end of
firing. Usually, cones that bend over both more slowly and more rapidly are
included to continually assess the condition during the firing cycle as the ware
moves through the furnace.

3.a: Procedure

Since this is such an empirical measurement there is no analysis. However, it is

useful to see these cones in operation and to compare two similar cones with
different heating rates. Thus there are two experiments:
1. Heat two cones of different composition at or near the
standard rate of 150 °C/hour and note the temperature at
which they bend to touch their plaque. This experiment will
be begun by the lab demonstrator so that the critical
temperature (in the range 550 °C to 750 °C) is reached during
the lab period.
2. Heat a cone that is equivalent to one of those in part one, at a
much faster rate, say 300 °C/hour, and compare its critical
bend temperature with that of the similar cone heated at 150
°C/ hour.

These experiments are run simultaneously in two furnaces. Sketch the appearance
of the cones every 10 minutes. Ditto marks can be used where appropriate. Each
student should make a note of the complete data, not just the part observed during
his/her turn.

Ceramic Cones Experiment B-4

B-Temperature Measurement and Control

3.b: Writeup

Include the results of all observations in a simple table. What was the temperature
and its uncertainty at which each cone touched its plaque? How did you estimate
this uncertainty? Why did the cone heated at 300°C/hour bend over at a
higher/lower temperature than that heated at the standard 150 °C/hour?

4. Temperature Transient Experiment

A change in temperature of a sample with time (Transients) is simple to measure,

by putting the output voltage of a thermocouple onto a recorder. This part of this
laboratory is designed to illustrate this when placing samples into a furnace for
heat treatment. It also gives you some idea of the heating and cooling times
involved, and the behavior of different metals and alloys.

4.a: Procedure

Two samples are available, copper and brass (a substitutional solution of 30% Zn in
Cu). Preheat the furnace to temperature (the black arrow should match up with the
red indicator). Attached to each sample is a chromel-alumel thermocouple. Each
sample should have a glass insulating tube around it. Plug the copper sample into
the recorder inputs, turn on the recorder, place the sample in the furnace block hole
and record the temperature rise. After reaching equilibrium or near it, remove the
sample from the furnace and place it in the copper block. From the plot on the
recorder, determine the time to reach half the final temperature change for both
heating and cooling. Repeat for the brass sample.

4.b: Writeup

Writeup should include the recorder graphs, a table listing the times required for
half the temperature change in each case, the uncertainty in this value, and a brief
statement describing how you estimated this uncertainty.

Why should the times be so much longer for brass than for copper? Check your
answer by looking up the values for the appropriate property in the ASM
Handbook, vol. 1, in the reference section of the science library, item TA459 A51M.

Writeup B-5
B-Temperature Measurement and Control

In this heating and cooling experiment, considerable care was taken to ensure the
heat transfer was mainly by thermal conduction from the samples to the block of
brass or copper. If the samples had been placed on a poor conducting surface in air,
the heat transfer would mainly be by radiation and convection. Both copper and
brass would lose heat at the same rate. Under these conditions, which one would
cool faster and why?

5. Thermocouple Experiment

This part is designed to give you a more detailed appreciation for the application
and function of thermocouples.

5.a: Procedure
•Use the thermometer to measure room temperature. Estimate the error.
•Use the digital voltmeter for all thermocouple measurements.
•Fill the 500 ml beaker with water and allow it to stabilize to room
• Put the thermocouple in the furnace to achieve a reading of approx.
• Measure the emf of the chromel-alumel thermocouple with the hot
junction in the furnace and the cold junction in each of the following
three locations:
1. by the thermometer in water at room temperature.
2. one inch below the surface in the ice bath. Do not stir the ice
3. at the bottom of the ice bath.

Convert all readings to °C.

Thermocouple Experiment B-6

B-Temperature Measurement and Control

• Use the ice bath readings to estimate the error in furnace temperature
due to
° uncertainty in reading the emf;
° manufacturer's specified uncertainty of ± 0.75% of total emf measured.

5.b: Writeup
• List the assumptions made in determining the furnace temperature
using the ice bath (cold junction) measurements.
• How do you account for the difference in millivolt readings from one
position to another?
• Calculate the temperature at the bottom of the ice bath.
• Calculate the furnace temperature and uncertainty in measurement
using the room temperature (cold junction) reading (include uncertainty
in room temperature read from the thermometer).
• Some furnace controllers put the cold junction in a little heater held at
40ºC. How much would this reduce the milii-voltage from that with the
cold junction at room temperature = 20ºC?
• For writeup: give data and other information requested.

6. Temperature Distribution in a Furnace

Use of a Thermocouple and Differential Thermocouple to Measure the

Temperature Distribution in a Tube Furnace. The object of a tube furnace is to
produce the maximum length of hot zone with uniform temperature. Since much of
the heat is lost out of the ends, a uniform electrical winding on the tube produces a
hot zone of uniform temperature that is at most one third the length of the furnace.

This part of the lab involves a determination of the length of hot zone in a tube
furnace, first using one thermocouple, and then repeat it with improved accuracy
using a differential thermocouple. One of the arms of the differential thermocouple
is kept at the hottest spot so that the temperature difference between it and the
moving one is very small in the region of interest. Thus, since their emfs are hooked
up in series opposition, a more sensitive scale of the millivoltmeter can be used.

Writeup B-7
B-Temperature Measurement and Control

6.a: Procedure

One chromel-alumel thermocouple is firmly located with its end at the centre of the
furnace. Do not move it. The second thermocouple moves along the axis of the
furnace. You are to move it in steps of 20 mm so that its "hot" end moves from one
end of the furnace to the furnace centre. After each movement of 20 mm, wait two
minutes for the thermocouple temperature to reach that of the new position in the
furnace, and record

a. the mV output from the thermocouple you moved, using the most sensitive
scale possible,
b. the mV output from the pair of thermocouples (the moved one and the
stationary one) connected in series opposition as shown. Be sure to use the
most sensitive mV scale possible. This will give greater sensitivity for
method when the moving thermocouple is near the centre of the furnace.

Write the data in the form of a table as you take it.

Temperature Distribution in a Furnace B-8

B-Temperature Measurement and Control

6.b: Writeup

The writeup on this part should include your page of original data, which should not
be rewritten (it doesn't need to be neat), and a graph showing the curves of
temperature vs. distance, with points plotted including error bars your
measured points. Describe in detail how you estimated the error for a
measurement. Over what length is the hot zone of the furnace within 5 °C of the
peak temperature? What is your estimated error in this length for each of your two
curves, and how did you deduce this error?

7. Non-contact Temperature Measurement

This technique has widespread applications in industrial processing and research

for measuring the temperature of objects when thermocouples or probe sensors
cannot be used or do not produce accurate results. In this lab, an infrared
thermometer or pyrometer will be used for this purpose.

Designs for infrared thermometers have existed since at least the late nineteenth
century. Nevertheless, it was not until the 1930's that the technology was available
to put these ideas into practical measuring devices. Since then, the infrared
thermometer design has changed significantly and considerable of expertise in
their use now exists.

Infrared or IR radiation is the long wavelength radiation just beyond visible light.
Infrared radiation is present between 0.75 X 10-6 and 1.0 X 10-3 metres.
Wavelengths between 0.7 and 20 X 10-6 metres are the practical range for
measurement due to the current sensitivity of IR detectors.

The manner in which infrared radiation behaves is best understood by considering

it like visible light. Infrared radiation is not visible. However, it travels in straight
lines and can be reflected or absorbed by material surfaces in its path. Objects that
are opaque to the eye will absorb and reflect infrared energy and part of this energy

Writeup B-9
B-Temperature Measurement and Control

will be re-emitted and a portion reflected internally. This also applies to objects
that are transparent to the eye but some infrared will also pass through the object.

To measure the intensity of the heat radiated from a hot surface, "black body"
conditions must prevail at the radiating surface. A "black body" is a material that
absorbs all radiations falling upon it without loss by reflection. Additionally, a
"black body" surface will radiate heat in the same manner. The fraction of heat
energy radiated by a hot surface as compared with an equivalent "black body"
surface at the same temperature is called emissivity. This emissivity depends on
the temperature and surface characteristics of a material not just its colour. For
materials like aluminum, its emissivity varies with temperature. Matte surfaces
are closer to "black body" surfaces than are smooth surfaces. Shiny materials like
gold and silver reflect most of infrared radiation striking them and have very low
emissivities. The temperature of the atmosphere surrounding a hot surface will
also affect the IR temperature measurement and must be taken into account.

7.a: Infrared Temperature Measurement

In this section of the lab, the heat radiated by a black oxide will be measured using
an infrared pyrometer and compared with a physical temperature measurement
method, a type K thermocouple on the surface of the black oxide.

7.b: Procedure

Heat the hot plate/black oxide with the thermocouple up to 300°C. Read and follow
the instruction sheet for the infrared pyrometer. Use 0.50 as a starting emissivity

Measure the temperature of the black oxide with the infrared pyrometer and at the
same time measure the temperature of the thermocouple. Increase the emissivity
by 0.01 and continue the temperature readings until an emissivity of 0.85 is
reached. You may need to make multiple readings

Non-contact Temperature Measurement B-10

B-Temperature Measurement and Control

7.c: Writeup

What is the emissivity of the black oxide at 300°C?

Is there a difference between the thermocouple temperature and the IR Pyrometer

temperature when measuring the temperature of the black oxide? Why?

What are some possible applications for infrared temperature measurement?

Your writeup should include a table with all your values including their average
and standard deviation. Compare your average value with the thermocouple
temperature and the average values measured by the other students in your group.
Comment on the difference. It may be quite large. This is an example of a
measurement that may be fairly reproducible but can also have a large systematic

Writeup B-11
Materials 2H03 on-line Laboratory Manual
Updated: 11 May 2000

Experiment C
Measurement of Force and Strain
Using Gauges
1. Objectives

• To use a Wheatstone bridge as a comparative resistance measurement

with application to strain gauges, their temperature compensation and
• To determine the strain in the surface of a cantilever beam using strain
• To examine the causes of non-linearity in a system that measures a force
by the output of a Wheatstone bridge.
• To construct scales to weigh people using strain gauges on a car spring,
including the calibration and examination of linearity and hysteresis in
the scales.

2. Introduction to Measurement of Forces

A weight, of course, is a force acting in the "downward" direction. The oldest method
of measuring weight was to use a balance arm with a pivot in the middle. Known
weights were applied on the opposite side until the arm returned to its original

This method is essential if the force changes with position in space (as in some
magnetic measurements since the force on a body depends on the local value of the
magnetic field gradient). Measuring the voltage with a potentiometer was another
null-type measurement.

More recently we have spring balances, where the weight is determined by the
deflection of a spring. Thus, any force whose magnitude doesn't change with
position in space, can be measured by one of the sensitive displacement
measurements considered in other experiments. Sometimes both are used.
Chemical balances commonly apply known weights down to one gram and then
measure a deflection to get 0.0001 gram.

Instead of measuring the deflection of a spring, we can measure the strain on its
surface. A weighted cantilever has the top surface in tension and the bottom surface
in compression. Their magnitude depends linearly on the weight applied, provided
the stresses are in the elastic region. Thus the weight, i.e. force applied, can be
measured by measuring the surface strain.

C-Measurement of Force and Strain Using Gauges

2.a: Resistance Strain Gauges

Consider a thin conducting wire of uniform cross-sectional area A, and length L,

made of a material with resistivity . The resistance of such a conductor is given by:

R= ...(1)

If the conductor is glued to the surface along the length of a cantilever beam, and
the cantilever is then loaded (see below),

the conductor on the top surface will elastically increase its length and decrease its
width. The resistance of the wire changes due to these dimensional changes, and
also because of a fundamental property of materials called piezoresistance (i.e. the
dependence of resistivity, on mechanical strain). If equation (1) is differentiated,
the change R in R is found to be:

∆R ∆ρ ∆L ∆A
= + − ...(2)
R ρ L A

Using Poisson's ratio , we obtain:

∆R ∆ρ ∆L
= + (1 + 2v )
R ρ L

The so called "gauge factor" (K) is defined as:

∆R ∆L ( ∆ρρ )
( )( ) = 1 + 2v + ≡ K ...(3)
R L ( ∆LL )

Introduction to Measurement of Forces C-2

C-Measurement of Force and Strain Using Gauges

where the first term, 1, is the resistance change due to a change in length, 2v is the
change in resistance due to a change in area, and (∆ρ/ρ)/(∆L/L) is the resistance
change due to the piezoresistance effect. Equation (3) becomes:

∆R ∆L
= K( ) ≡ Kε (4)

The gauge factor is usually specified by the manufacturer. Therefore, a

measurement of ∆R/R, and a knowledge of K allows a measurement of strain in the
wire, ε, and thus a measurement of strain in the surface of the cantilever beam, or
whatever part the gauge is cemented to.

If the wire is a metal (commonly an alloy "constantan"), then K≅2, which is 80% due
to the elastic change in shape and 20% due to the ∆ρ/ρ term which depends on the
volume change of the wire. (The volume change is zero only if v = 0.5 and for most
metals v ≅ 0.3). For metals, the linear relation is not perfect, but is quite good. For
semiconductors, K can be as high as 180 or as low as -100 due to the term. This gives
much higher sensitivity in measurement but linearity is much poorer.

2.b: Types of Strain Gauges

There are two main types of metallic gauges, unbonded and bonded strain gauges.
Unbonded strain gauges are used mainly as elements of force and pressure
transducers and accelerometers rather than directly as displacement pickups, and
are not considered in this experiment. Bonded gauges are usually cemented down
on the surface of the part whose strain is to be measured with a suitable cement for
the environmental conditions. Once cemented down, they effectively become part
of the surface they are fastened to, and undergo essentially the same strain as that
surface. Most bonded gauges are not one wire, but are in a parallel array in order to
increase sensitivity and directionality. They must be cemented down in the

Types of Strain Gauges C-3

C-Measurement of Force and Strain Using Gauges

appropriate direction, with the parallel wires in line with the strain to be measured.
Typical types of strain gauges are below:

From E.O. Doebelin, "Measurement Systems - Application and Design",

McGrawHill Book Co., New York, 1975, p. 228.

2.c: Wheatstone Bridges

The resistance change of a strain gauge can be detected very sensitively by a direct
comparison with a known resistor using a Wheatstone bridge circuit. If the strain
gauge and comparison resistor are the same value there is no output signal. If the
resistance changes slightly due to strain, the small output signal can be amplified
to achieve a very high sensitivity. A simple Wheatstone bridge circuit using direct
current is shown below.

The battery applies a fixed voltage Vo between points C and D. This causes a
current I1 to flow via CAD and I2 to flow via CBD. A voltmeter, shown V, measures
the voltage difference between points A and B. The bridge is "balanced" when V

Introduction to Measurement of Forces C-4

C-Measurement of Force and Strain Using Gauges

reads zero. This requires that I1R1 = I 2R2 and I1R4 = I 2R3. Therefore, we have at

R1 R3
R4 R2

Thus, if we know R2, R 3 and R4 then the unknown R1 can be calculated. A common
way to measure a resistor R1, is to vary the value of a known resistor until the
voltmeter reads zero. This would be a nullpoint measurement.

When these are applied to strain gauges, the gauge resistance is used for R1 and the
bridge is balanced by adjusting an internal resistor that alters R4. The sample is
then loaded, which alters R1. This puts the bridge out of balance, giving an output
signal of

∆V 1 ∆R1 1
= ( )( )
V0 4 R1 1 − 2∆RR1

for a voltmeter of infinite resistance. We see this is linear, i.e., V is proportional to

R1. Since R1 .01R1 for typical cases, the linearity of the Wheatstone bridge is quite
good. This only varied one resistor R1 (one "active arm" in the bridge) and is
commonly called a "quarter bridge".

If we vary two resistors in the bridge, say R1 and R2, then ignoring the nonlinear

∆V 1  ∆R1 ∆R2 
=  −
V0 4  R1 R2 

Note: if R1 = R2 the bridge is still in balance. We use this to remove the effect of
temperature on strain gauge R1. Thermal expansion of the sample will increase R1.
We can remove this effect by choosing R2 as a "dummy" strain gauge that is
fastened to the same type of material as the sample and located beside the sample
(so their temperatures are the same). We also use two strain gauges as two "active
arms" in the bridge for a bent cantilever, where R1 is in tension on the top side of
the cantilever and R2 is in compression on the underneath side. This obviously
doubles the sensitivity of the bridge.

Similarly, we can use "four active" arms in the bridge, giving

∆V 1  ∆R1 ∆R2 ∆R3 ∆R4 

=  − + −
V0 4  R1 R2 R3 R4 

The bridge we use is an AC bridge at 3 kHz, which works in a very similar way to
the DC bridge described above. AC is more convenient, and can detect strain

Wheatstone Bridges C-5

C-Measurement of Force and Strain Using Gauges

changes in the sample (oscillations) up to 400 kHz. In practice, the voltage is

amplified by an amount set by the "sensitivity" control on the bridge. This then
must be calibrated.

3. Experimental Setup

The four strain gauges, A, B, C, D are attached to the cantilever arms, as shown
below. Another strain gauge, we call gauge X, is attached to a piece of aluminum as
a reference resistor. They all have wire leads that can be connected to the
Wheatstone bridge. Another strain gauge is attached to the underside and near the
centre of the car spring. Try not to mangle it when you pick up the spring. Two of
these strain gauges are used as resistors R 1 and R 2. If only one gauge R 1 is active,
i.e. being strained, gauge X is used as R2.

3.a: Procedure

The demonstrator will show you how to use the strain gauge amplifier indicator.
The manufacturer gives a gauge factor of 2.05 ± .01 for this set of strain gauges. The
indicator should have bridge volts set at 10, bridge mode set a ½, and the gauge
factor adjusted to the given value (2.05).

Experimental Setup C-6

C-Measurement of Force and Strain Using Gauges

a. To Make a One-Active Arm Bridge Using the Top Strain Gauge

° start with no connections on the junction box.
° connect strain gauge A as R1 and gauge X (on loose piece of aluminum)
as R2.
° connect jumpers from P1 to P3 and P2 to P4.
° balance the Wheatstone bridge by turning the nob to the zero position.
° deflect cantilever with A on it by a reproducible amount by applying a
weight to the end of the arm.
° record meter reading in µ in/in and uncertainty in the reading. Remove
deflection, rezeroing if necessary, replace deflection and make a
reading. Repeat the whole procedure several times to determine the
reproducibility so that comparison with later cases can be made
b. To Make a One-Active Arm Bridge Using Bottom Strain Gauge
° replace A by strain gauge B (from underside of cantilever) as R1.
° balance the Wheatstone bridge.
° deflect cantilever the same as in previous case.
° record meter reading etc. as in (a). They should be the same and of
opposite sign if the gauges are precisely the same distance from the
end of the cantilever, and have the same gauge factor. Compare the
difference of your readings (a) and (b) with that possible due to the
uncertainty of the gauge factor among gauges of this set.
c. To Make a Two-Active Arm Bridge Using Top & Bottom of Cantilever
° put A as R1 and B as R2
° balance the Wheatstone bridge.
° deflect cantilever the same as in previous case.
° record meter reading in µ in/in. Why is it double the previous case?
d. Sensitivity of Gauges to Strain Perpendicular to Their Axis
° put gauge D as R1 and aluminum gauge X as R2.
° balance the Wheatstone bridge.
° deflect cantilever in standard way as before.
° record strain in µm and compare to procedure (a) above. It is much
less. However, some gauges are designed so that this value is almost

Looking at the strain gauge, what factor in its design could affect this reading the
most? This anisotropy is very useful as patterns of gauges can be put on a body to
determine where the principal strains are and thus get the principal stresses.

e. To Check Effect of Temperature Rise and How to Reduce Its Effect

• With no temperature compensation.

Procedure C-7
C-Measurement of Force and Strain Using Gauges

° put gauge A on R1 and gauge X on R2 and balance the Wheatstone

° do not deflect cantilever.
° put heat lamp 8" above cantilevers. Turn it on and read strain at 0, 15,
30, 45 seconds. Turn off heat.
• With temperature compensated using another strain gauge.
° put strain gauge C as R2 and re-balance the bridge.
° turn the lamp on and take readings as before.
° explain difference between this and previous case.
f. Making Your Very Own (but not to be taken away) Scales

A strain gauge is already on the car spring (MG midget)

• use it as R1 with aluminum gauge X as R2 and add bridges between P1

and P3, as well as P2 and P4.
• deflect the spring by standing on it a few times until reproducible. (The
heaviest one should do this). It turns out that reproducibility is better if
it is not rezeroed each time. Therefore, do not rezero.
• calibrate the scales by adding weights in increments of 20 pounds to
beyond the weight of the heaviest person and removing them
progressively to zero. Make readings after altering each weight. Do not
rezero. There will be a huge hysteresis producing different readings in
loading and unloading.
• repeat this calibration to check its reproducibility even when the
hysteresis is large. Do not re-zero.
• what are the possible reasons for the large hysteresis and how could you
reduce the hysteresis?
• weigh yourselves, recording clearly on the calibration curve how you
determined your weight from the measured deflection.

Experimental Setup C-8

C-Measurement of Force and Strain Using Gauges



3.b: Writeup

From Procedures (a) through (f) above, include all readings made, answers to
questions written in the procedure, and the calibration curve with comments from
your weighing machine. Show both the loading and unloading curve, and the
reproducibility on the repeat run. Read your weight directly off the graph, clearly
showing how you got it from the curve.

In addition, list and explain three possible sources of non-linearity in determining a

force when using a Wheatstone bridge to measure a strain gauge fastened to a

Writeup C-9
Materials 2H03 on-line Laboratory Manual
Updated: 17 May 2000

Experiment D
Measurement of Length and


1. Objectives

• To gain experience in using Vernier calipers and micrometers.

• To examine the mechanism of a mechanical dial gauge and assess the
sources of error in its use.
• To learn how an LVDT (Linear Variable Differential Transformer) works
and calibrate one for use in a dilatometer or profilometer.

If there are four students, two will start working on part A and two on part B. Then
they will interchange. If there are three students, one may start on B alone and
then interchange, if she or he wishes.

2. Measurement of Length (part A)

Lengths are measured most simply with a ruler. A Vernier scale improves the
sensitivity. For greater sensitivity, a screw micrometer can be used in which one
rotation extends the rod by one thread, or by a mechanical dial gauge in which a
linear motion is translated with a large gear multiplication to an angular change of
the resulting gear. All these devices are calibrated with blocks of metal of standard
lengths. This part of the experiment uses all these measurements. Another way,
which is very good for small samples which cannot be touched, is to use a traveling

D-Measurement of Length and Displacement

2.a: Procedure for Part A

Each student should this part of the experiment themselves unless help is needed.

Obtain one of the three machined brass cylinders supplied, making sure to record
the letter (A, B or C) on its end.

Measure all four diameters of your cylinder using:

° the Vernier caliper

° the Vernier screw micrometer
° the mechanical dial gauge.

The sequence does not matter. Estimate the reading error in each case. (Note:
Estimation of the error should not be considered trivial.) If you are unfamiliar with
how to use any of these instruments or read their scales, the demonstrator will

2.b: Write-Up for Part A

a. Present your measurements obtained with all three instruments in one
table giving the values and the reading error in each measurement. Below
the table, write an explanation justifying the value you chose for the reading
error and how your choice relates to the instrument and its scale. The
values should be recorded in the same system they were taken (i.e. metric or
imperial), but you should do your own conversions to satisfy that all the
values agree with each other.
b. Answer the following questions:
1. By how much would your measured diameter change if the
brass block and micrometer were all at 100EC? The thermal
expansion coefficient per EC is 19.6H10-6 for brass and
17.2H10-6 for stainless steel (Metals Handbook, Vol. 1).
2. Examine the inner workings of the dial micrometer. List the
sources of non-linearity and hysteresis.
3. The main coil spring of the dial micrometer obviously returns
the plunger, but it also serves another very important
function. The flat coil spring serves the same function. What
is this function (see below)?

Measurement of Length (part A) D-2

D-Measurement of Length and Displacement

4. Gears usually have backlash. When the bottom gear is

moving to the right, it contacts the upper gear teeth as shown:

When you reverse its motion, the bottom gear moves a short distance before
contacting the top gear. For a brief travel, the bottom gear moves and the top gear
does not. This is called "backlash".

3. Measurement of Displacement (part B)

Often we are only interested in the change in length of a sample, so if one end is
fixed, the other end is displaced by a small amount equal to the increase in length.
Under carefully controlled conditions of temperature and lack of vibration, a
displacement can be measured to 2 µm. or better. The table below summarizes
several methods. We will be only concerned with the Linear Variable Differential
Transformer (LVDT) in the remainder of the lab.

Measurement of Displacement With an LVDT

The LVDT is used in many applications, and is based upon a simple transformer
pick-up. The AC current through the primary coil (obtained using Ohm's law with
the sinusoidal input voltage Vin, and the resistance of the input coil) produces a
magnetic field. This induces a current (and thus a voltage) with the same frequency
as Vin in the two secondary windings via the iron core, which is free to move along
the transformer axis. However, the amplitude in each secondary coil varies with the
position of the iron core. When the secondary coils are connected in series
opposition (as shown on the next page), a null position exists (x0) at which the net

Write-Up for Part A D-3

D-Measurement of Length and Displacement

output, Vo, is essentially zero (i.e. the output in each secondary winding is 180° out
of phase, which sums to zero).

If the iron core is now displaced axially, more signal is picked up by one of the
secondary windings, and their sum is linearly dependent on the core displacement
from symmetry. The LVDT and its signal processor used in this experiment are

Measurement of Displacement (part B) D-4

D-Measurement of Length and Displacement

drawn schematically below. Note: for large displacements, non-linearity occurs as

shown in the graph of output voltage as a function of core displacement. LVDT's can
be purchased with various sensitivities and linear ranges.

Write-Up for Part A D-5

D-Measurement of Length and Displacement

3.a: Procedure for the LVDT

• adjust the dial gauge to the chosen zero position (i.e.: 0.4 inches, which is
read as 4000 on the panel meter)

• after this is completed, a couple values in the range should be checked for

Measurement of linear range

The object is to plot the curve of meter reading (called Vout in the introductory
remarks) vs. position of the core to determine for how large a core displacement the
meter gives the correct value, (i.e. is linear). Because the meter will not go beyond
the linear range, connect the "recorder output" socket on back of instrument to the
± 99.9 mV digital voltmeter scale. This output is in parallel with the instruments

Measurement of Displacement (part B) D-6

D-Measurement of Length and Displacement

° with range selector at 100, and meter polarity on "reverse", screw out
the micrometer a distance beyond the linear range (if unsure, ask the
T.A. how far). Read the digital voltmeter, and estimate uncertainties
in both these readings.
° screw in the micrometer by 0.025" (25 thou), and record the voltage
reading from the digital voltmeter.
° repeat successively in 25 thou increments to the "mechanical zero
adjustment" previously determined.

Ignore the instruments meter, which will sometimes be off scale. Return the
micrometer to 0.70 black scale for the next lab group.

3.b: Writeup for Part B

a. Include the original data and a plotted curve of these measurements. On the
graph, indicate the range of the micrometer readings over which the curve is
b. If it is assumed that the core displacement is proportional to the millivolt
reading for all possible displacements (i.e. completely linear), the so-called
"linearity" error is introduced for readings beyond the true linear range.
Choose a particular spot on the curve beyond the linear region and calculate
the value of the linearity error at this spot. Show how you did it by reference
to the graph.

Writeup for Part B D-7

Materials 2H03 on-line Laboratory Manual
Updated: 17 May 2000

Experiment E
Chemical Analysis by Reaction

1. Chemical Analysis

The need for accurate, quick, cheap, quantitative chemical analysis is always
present in materials work, whether controlling your raw materials, your
processing, or your final product. For convenience, we have divided methods of
analysis into two groups:

a. those that involve measuring the amount of final product in a chemical

reaction that uses up your sample.
b. those that involve exciting the electrons to empty levels in the atom or
molecule, thus producing an absorption or emission spectrum characteristic
of each element in the sample.

This lab concerns the first method, but not in a traditional way . As a consequence of
new technology development in chemical analysis, quick and accurate
spectroscopic detectors are often used in the detection part. This lab involves the
use of computerized instrument with the combination of both chemical and spectral

2. Objectives

• to be aware of how carbon and sulfur in steel are analyzed.

E-Chemical Analysis by Reaction Product

• to be familiar with the use of the equipment to analyze the carbon and
sulfur contents in the steel sample.
• to be aware of the error sources for the equipment.

3. Introduction

3.a: Carbon and Sulfur Analysis

The amount of carbon and sulfur in steel is analyzed by reacting them with oxygen
and the resulting CO2 and SO2 are determined by IR (infrared) detector. The
reaction process begins by oxidizing the carbon and sulfur when the sample is
melted by induction heating:

Fe+S+C+O2 --> CO+CO2+SO2+FeO

where Fe, S and C are chemical components of the sample. The gas evolved is then
passed through catalyst to further oxidize the CO to CO2. The analysis of SO2 and
CO2 is done using an infrared (IR) detector. All molecules, with the exception of
dipolar species such as O2, N2, H2, etc., absorb energy in the infrared region.

Because no two compounds absorb in the same way, infrared spectrometry is an

extremely useful method for qualitative and quantitative chemical analysis. As
radiant IR energy is projected through the sample material, an infrared absorption
spectrum is produced. Since all molecules have a characteristic spectrum, the
identity and quantity of a compound can be determined. For the further
information about the principle of the spectroscopic method, readers are referred to
the general introduction part in this manual. This approach is an accurate and very
quick method, therefore can greatly reduce the analysis time.

3.b: Theory of Operation

1. The CS-444 Carbon/Sulfur system is a microprocessor based,
software driven instrument for wide-range measurement of
carbon and sulfur content of metals, ores, ceramics and other
inorganic materials. The CS-444 uses the HF-400 induction
furnace and measures carbon and sulfur by infrared
2. Analysis begins by weighing out a sample (1 gram nominal)
into a ceramic crucible on the built-in balance.

Accelerator material is added, the crucible is placed on the loading pedestal,

and the ANALYZE key is pressed.

Furnace closure is performed automatically, then the combustion chamber is

purged with oxygen to drive off residual atmospheric gases. After purging,
oxygen flow through the system is restored and induction furnace is turned on.

Introduction E-2
E-Chemical Analysis by Reaction Product

The inductive elements of the sample and accelerator couple with the high
frequency field of the furnace. The pure oxygen environment and the heat
generated by this coupling cause the sample to combust.

During combustion all elements of the sample oxidize. Carbon bearing

elements are reduced, releasing the carbon, which immediately binds with the
oxygen to form CO or CO2. In the meantime, sulfur bearing elements are also
reduced, releasing sulfur, which binds with oxygen to form SO2.
3. Sample gases are swept into the carrier stream. The sulfur
content is measured as SO2 in the first IR cell. Carbon
monoxide is converted to CO2 in the catalytic heater assembly
while SO3 is removed from the system in a cellulose filter
trap. The carbon content is then measured as CO2, in the
form of gases flow through both the low and high range IR
cells. The measurement will be made only on the range
selected. The low carbon range features a greater resolution
carbon content as a result of the longer path-length in the IR
cell. In contrast, when high range carbon is selected, sample
gases flow through an IR cell with a shorter path length. The
high carbon range provides a better resolution of high carbon
content. The difference in path length assures optimum
representation of the gases for the range selected.
4. In the infrared detector cell, energy is emitted from a
Nichrome wire heated to 850°C. Radiant energy, chopped at
85HZ, enters the cell through a calcium fluoride window and
is projected through the cell measure chamber which contains
carrier or measured gas. Gases absorb infrared energy as they
pass through the cell chamber, producing a spectrum. As
energy exits the cell chamber through a second calcium
fluoride window, a precise wavelength filter selectively
inhibits all wavelengths, except that of CO2, from passing
into a condensing cone and on to the detector. The detector
responds to energy changes between the carrier gas and
measure gas to ultimately determine the concentration of
CO2. The same process takes place for the SO2 detection.
5. The detector output, AC coupled to the preamp, is amplified,
rectified, and filtered. The analog voltage is converted to a
digital signal through the A/D card and the nominal energy at
the cell output is 8.500VDC.

Theory of Operation E-3

E-Chemical Analysis by Reaction Product

6. A baseline is established prior to every analysis. The cell

output is automatically adjusted to 8.500VDC if any drift has
occurred. As the analysis begins, the cell output decreases
proportionally with the amount of carbon (as CO2) or sulfur
(as SO2) present in the IR cell. The computer reads the cell
output 18 times per second and stores each point in memory.
These data points are compared to an ideal linearization
table, stored in memory, which contains IR cell output and
linear correction values. All linear correction as well as noise
suppression is applied to each data point and measurement is
performed. After measurement, adjustments are made for
calibration as well as weight and blank compensation. When
all adjustments and calculations are complete, the results are
displayed as percent carbon and sulfur.

4. Experimental Procedure

The demonstrator will demonstrate the use of the CS-444 Carbon/Sulfur

determinator to analyze the carbon and sulfur contents. Through the
demonstration, students will learn the principle of the instrument and the way to
operate. In order to reduce operation time, the instrument is equipped with the
automatic sample loader, autocleaner, and accelerator dispenser. However, the last
feature is not recommended in this lab.

Each group will get four standards and one unknown sample. The unknown is a
steel bar with the carbon and sulfur concentrations bracketed among those of the
standards. Three sample pieces, each around 1 gram, are cut from the steel bar
before performing the analysis. Each sample piece, standard or unknown, need run
three times. The carbon and sulfur concentration are printed out directly after the

4.a: Write-up for Carbon and Sulfur Analysis

1. List all results and calculate the average and standard
deviation of each sample. Comment on the value of your
calculated standard deviation (which is the measured
2. Build the calibration curve using the measured and the given
standard concentrations. What information can you get from
these lines?
3. List steps in the procedure which give rise to the uncertainty
in all measurements. What are origins of the uncertainty,
and how will you avoid them?

Experimental Procedure E-4

Materials 2H03 on-line Laboratory Manual
Updated: 17 May 2000

Experiment F
Metallographic Observation

Safety Note: Since this laboratory involves the use of solvents - students
are NOT to wear contact lenses to the lab period.

1. Objectives

• To learn how to cut, mount, grind, polish and etch a metallographic

• To observe your polished sample in an optical microscope and relate the
observed microstructure to that in a standard manual

2. Introduction

The optical microscope is one of the most useful tools of a metallurgist or

ceramicist. With it, the investigator can determine a wealth of information of a
sample, including its composition, manufacture, potential performance,
environment, service history and method of failure. This investigation tool
transcends all stages of a material’s life history; therefore, its usefulness is
significant for all materials professionals - from the materials researcher’s initial
development to the forensic investigator’s failure analysis.

Since the depth of focus of the optical microscope is very small when operating at
high magnification, the sample must be polished flat. However, observing a flat,
polished metal or ceramic sample under an illuminated microscope is akin to
shining a strong light on a polished mirror surface - no detail can be seen. Thus,
after polishing, the sample is usually etched in an acid to provide contrast between

F-Metallographic Observation

viewing details. If more than one phase is present, their etching rates will differ,
which allows the phases to be distinguished. The etching may also be more rapid at
grain boundaries and twin boundaries. However, if the phases naturally reflect
light differently, they might also be distinguished in the unetched condition alone.

3. Experimental Procedure
1. One of the five different metal samples will be given to you
from the demonstrator. Record your sample. Each of the five
samples is described at the end of this laboratory. Read the
2. Cut, mount, grind, and polish it, after receiving instruction
from the demonstrator.
3. Look at the unetched surface in the optical microscope.
4. Etch it using the standard procedure given for that sample as
described at the end of this laboratory.
5. Examine it again in the optical microscope. Compare the
microstructure visible in the microscope with the
microstructures in Metals Handbook, Volume 7 in order to
identify the components. The appropriate page(s) and plate
number(s) can be found in the sample’s description.
6. Explain your sample and microstructure to the other

3.a: Write up

The write up is to include ONLY the following:

1. A list of steps required for metallographic (a) mounting, (b)
grinding, (c) polishing and (d) etching of samples. Under each
of the headings above, write in sequential order each step
required to safely and diligently complete each respective
component of metallographic sample preparation, including
any special feature used in that step. If care is necessary in
any particular procedure (e.g. washing the sample and hands
thoroughly before transferring to the next polishing stage),
why this care is needed must also be explained. This is a good
practical exercise as many practicing engineers write
‘operating procedures’ for other people to use. Write this in
sufficient detail so that another student could use it as an
operating procedure with little or no other instruction.

Experimental Procedure F-2

F-Metallographic Observation

2. Include the digital image of your sample in the etched

condition. The photo should be titled with the name of the
material, the magnification of the photo and the etch used. In
addition, the distinguishing features (shape, colour, etc.) of
each phase must be described in words and referred to in the
3. A comparison of your microstructure with that shown in
Metals Handbook, Volume 7. Use this comparison to identify
what each phase is and give addition details if appropriate.
4. Answers to the following four questions (clearly given in a
separate section at the end of the report):

a. What precaution did you take in order to not transfer grit from one
polishing stage to the next?
b. What etching procedure did you use and how did you reduce the danger
from acid to you, your clothes and the lab equipment?
c. Why did you wash the sample in alcohol after the final polish?
d. Would you expect very soft materials, such as annealed pure aluminum, to
be very difficult or very easy to polish, and why?

3.b: Description of Metallographic Polishing Samples

1. A piece of a two inch pipe coupling. This is probably a white
cast iron as in Metals Handbook, Volume 7, page 95, #757.
Etch in 2% Nital by spray, wait for the sample’s shine to
disappear, and wash.
2. A nut from a two inch pipe fitting. This is probably a ferritic
cast iron as in Metals Handbook, Volume 7, page 95, #759.
Note that this structure has been achieved by heat treating
the white cast iron of sample #1. Plates 757, 758 and 759
show the three stages during this transformation. Etch in 2%
Nital by spray, wait for the sample’s shine to disappear, and
3. Cast flange from a heat exchanger. This is a pearlitic gray cast
iron that shows the graphite alone when unetched as shown
in Metals Handbook, Volume 7, page 82, #645. This is a
common material for bases on large equipment as the
graphite flakes dampen the vibrations. The engine block in
cars is often a gray cast iron. . Etch in 2% Nital by spray, wait
for the sample’s shine to disappear, and wash. Find a
structure on pages 82 to 87 of Metals Handbook, Volume 7
that matches yours.

Description of Metallographic Polishing Samples F-3

F-Metallographic Observation

4. Cooling fin from a motorcycle engine. This is an aluminum

casting alloy. Etch in 0.5 % HF in water by immersion using
tongs for a few seconds, then wash. Be very careful with
HF. Ask the lab demonstrator about this etch before using it.
Compare your structure with those on pages 256 to 260 of
Metals Handbook, Volume 7. You may not get a unique
interpretation but comment on what you consider the most

5. A brass water tap. This is a solid solution of about 30% Zn in

Cu. Etch in 5% FeCl3 in alcohol for 20 seconds to 2 minutes
by immersion using tongs. Pages 282 to 287 of Metals
Handbook, Volume 7 show brass microstructures.

Experimental Procedure F-4

Materials 2H03 on-line Laboratory Manual
Updated: 17 May 2000

Experiment G
Datalogging of Quenching Curves
1. Objectives

• To gain experience in the use of a minicomputer to:

° collect data at relatively fast rates
° evaluate the significant parameters in the data collected.
• Measure the quenching curves, i.e., the change in sample temperature
with time, when using different quenching media.
• Gain some physical insight into what controls the cooling rate during

2. Introduction

2.a: Quenching Curves

In many heat treatments of metals the sample must be cooled rapidly (quenched)
from a high temperature. The purpose of the quench is to decrease the temperature
without allowing time for the atoms to move a significant distance. This keeps the
solute atoms dissolved, prior to precipitation in aluminum and other alloys. In
steels, it inhibits the formation of ferrite and pearlite which then allows martensite
to form at the lower temperature. Unfortunately, a rapid quench also has a bad
feature. During rapid cooling, the outer layer of the sample may be at a much lower
temperature than the inner part of the sample. The outside will try to contract but
will be held out by the inside, which is still hot. This will put the outside in tension
and the inside in compression, during the quench. If either of these reach the yield
stress, then "permanent" plastic deformation occurs which distorts the sample and
leaves a residual stress after the whole sample has cooled. A more extreme stress is
built up when an appreciable fraction of the outside region converts to martensite.
For this reason, using too severe a quench is undesirable. In particular, commercial
aluminum alloys are often quenched in hot water rather than cold water, and most
steels are quenched in oil rather than water. A more recent development, which is
cheaper than oil, is the use of a dissolved polymer in water. A polymer layer forms
on the hot surface of the sample, which reduces the rate of heat transfer, and then
dissolves in the cold water. Quenching curves for all these media will be measured
in this experiment.

The cooling rate of a sample during a quench is controlled by the rate of heat loss
from the sample surface. This is very fast if the sample surface is hot enough to boil
the liquid and produce small bubbles that rapidly leave the sample surface.
Boiling requires latent heat and causes rapid local convection at the sample

Quenching Curves G-1

G-Datalogging of Quenching Curves

surface. When the sample is at higher temperatures, a continuous vapor film occurs
at the sample surface, which will markedly reduce the rate of heat loss. At lower
temperatures where no boiling occurs, heat loss is by convection which is relatively
slow. These processes are well described in the text "Transport Phenomena in
Metallurgy" TN673 G37, pages 256 to 263. Thus, the cooling curve will look as in
Figure 1 and the rate of heat loss, Q, which is proportional to the gradient of the
cooling curve, is shown in Figure 2. Because of the large range of Q, it is usually
plotted as ln Q.

Because the rate of heat loss at the sample surface during boiling is a very complex
process, it is usually treated empirically. Newton's law of cooling is assume

Q = Ah(T-T∞)

Introduction G-2
G-Datalogging of Quenching Curves

where A is the sample surface area, T the temperature of the surface of the sample,
Tinf the temperature of the liquid, and h the "heat transfer coefficient". It is
"empirical" because this equation, which is only valid with constant h for heat loss
by simple convection, is assumed, and the value of h is determined directly from
experimental results. In most cases, it will depend on the type of liquid and on the
mechanism of heat transfer, hence on T. In this experiment we want to determine
the value of the heat transfer coefficient, h, as a function of temperature for various
liquid quenchants. Then it can be used to calculate T(t) for samples with different
sizes, densities, and heat capacities.

In order to determine the value of the heat transfer coefficient from a measured
cooling curve of sample temperature vs. time t, it is necessary to know the
temperature distribution inside the sample. For samples of high thermal
conductivity, the temperature is fairly uniform and simple theory gives the
following equation:

dT Ah( T − T∞ )
dt ρCnV

which yields (1)

T − T∞
= e − mt
T 0 − T∞

where T is the sample temperature after time t, To is the sample temperature at the
start of the quench, Tinf is the final temperature after quenching, and (2)

ρC pV

where A is the sample surface area, V its volume, its density, Cp its specific heat,
and h is the heat transfer coefficient. If all these parameters are independent of T,
then m will be a constant. If not, the value of h must be found from the measured
value of m as it changes with temperature, which is the ultimate object of the
experimental part.

2.b: Details of Experiment

In this experiment a thermocouple is imbedded in an aluminum rod which is heated

in a furnace then quenched. Since the temperature changes are too fast to follow
manually, a microcomputer is used to acquire digital values which correspond to
voltages from the thermocouple. These voltages correspond to temperatures which,
with timing information, will be used to obtain heat transfer coefficients as a
function of temperature. First, the digital readings must be converted to the
voltages from the thermocouple. These voltages are usually in the range of 0 to ±20
mV which is far too low for most Analogue to Digital Converters (ADC's). An

Details of Experiment G-3

G-Datalogging of Quenching Curves

amplifying stage having a gain A is introduced between the thermocouple and the
ADC and, because no system is perfect, there will be some offset, E. So a digital
reading, Di, is related to a thermocouple voltage Vi by:

Di = AVi + E (3)

The evaluation of A and E can be made by having two points for which the
corresponding digital value and thermocouple voltage are known. In this
experiment the values were very reproducible, so have been programmed in, but a
check is made for at least one temperature.

With the digital values converted to voltages in the computer, it is necessary to

calculate temperatures from the voltages.

Within the temperature range of this experiment the temperature, Ti, can be
related to a voltage, Vi, by:

Ti = BVi2 + CVi + D (4)

where B, C and D are constants to be determined from data collected. For a

thermocouple without a special cold junction, zero potential is just the ambient
temperature at the voltage measuring end of the thermocouple. In this experiment
that will be room temperature. From equation 4 the constant D must equal the
room temperature Tr, which is determined by a solid state detector in the present
apparatus. The coefficients B and C could be determined by having two points for
which the temperature of the thermocouple and its voltage are known, but
standard values will be used.

The check at one temperature will also confirm this procedure.

The computer will acquire digital values from the ADC, record the time elapsed
during the quench, and calculate the heat transfer coefficient at each interval. How
is this done you may ask. For equation (1), it is necessary that the heat transfer
coefficient be constant with temperature. If it is not, then h(T) can be found
numerically by changing the differentials T and t to T and t, which represent
changes in temperature and time during the interval, with the temperature T at
the centre of the interval.

No programming will be necessary for this experiment (at least not for you). The
programs used in the course of the experiment are written in Basic and may be
listed if desired.

Equipment Used in Experiment

• PC Computer running DOS6.22
• Omega TC5508 Analog/Digital
• Type K Thermocouple connected to a block of Aluminum

Introduction G-4
G-Datalogging of Quenching Curves

• Hot plate
• Alcohol thermometer
• Liquid nitrogen dewar
• Micrometer

3. Procedure

3.a: Acquiring the Data

1. All equipment will be connected and on. The furnace
controller is set to 550°C.
2. Record the room temperature from the thermometer.
3. Measure the diameter and length of the rod. Calculate the
area and volume of the rod.
4. Put rod into the furnace.
5. NEVER handle the rod by the thermocouple wires they may
6. ALWAYS use the wire handle to move the rod.
7. Fill the pail with cold water.
8. Fill the 3.5 litre beaker with hot water and heat the water to
between 80°C and 90°C (this will take some time).

3.b: Program

Run the program for data acquisition by typing

1. A> Temperature <RTN> (i.e., the ENTER key)

A title screen shows up. Press ENTER key to browse the data acquisition
program. Then the Temperature Main Screen will be displayed with five

FILE ? Type 2H3.INI at the spaced provided for SETUP FILE and click
2. Click SETUP button. A message of " " will show up. Type in
"2H3" in the space provided.
3. Click ACQUISITION button. Another screen comes up asking
you to input a name for the data file. The following filenames
are suggested for the different quenches:

CW: cold water quench

HW: hot water quench

Program G-5
G-Datalogging of Quenching Curves

AQ: aquaquench

NI: liquid nitrogen quench

And finish the name with extension ".DAT".As a result, all data files will have
the following uniform (and logical) names: CW.DAT ; HW.DAT ; AQ.DAT ;
4. Hit Enter key after the filename is given. A "Data Acquisition
Screen" comes up. The first left column under "CHN"
(Channel) shows the channel to be used for temperature
measuring in this lab, which is channel 0. The second left
column under "Current °C" shows the on-line temperature
reading from the thermal couple used. This temperature
reading fluctuates as the temperature changes. However, no
data are saved into the datafile created abovementioned at
this moment. Data saving proceeds once P key is pressed.
When the quenching is finished, press Q key to save the
acquired data into your datafile and quit when saving is done.
5. The "Temperature Main Screen" will be displayed again to
allow you to run another data acquisition process as described
above. Once all the quenching tests are done, press QUIT
button on the main screen to exit to DOS.
6. The datafiles obtained can be opened in Excel or other widely
used data processing software. Be sure when you open the
files use correct Files of Type: .dat. You can then use these
data on your diskette to make a hard copy of the plot and list
the data on a printer.

The computer will then ask if you want to run the experiment again. There are
four quenches to be performed.

• 5 seconds in cold water (22°C)

• 10 seconds in hot water (80°C)
• 35 seconds in a 25% solution of AQUAQUENCH 251 (22°C)
• 6 seconds in liquid nitrogen (-196°C)

3.c: Plots

You will then be responsible to produce the following hard copy plots:
1. Temperature vs. time.
2. Log (h) vs. temperature.
3. Axes should be labeled appropriately and the plots should
have a title.
4. Questions Related to the Experiment

Procedure G-6
G-Datalogging of Quenching Curves

Choose one T vs. t graph. What can you say about the heat transfer
coefficient from it? Explain any anomalies.
Compare the different quenching graphs. What are the main differences
between them? Why?
Take a close look at the h vs. T graphs. Relate these graphs to the quench
For temperatures Ti-1, Ti, Ti+1 at times ti-1, ti, ti+1, show how to calculate
Equation 1 is valid only for slow heat transfer, that is when h < K/(10 r),
where K = 234 J/m.°C.s is the thermal conductivity, and r is the greatest
distance the heat must travel (radius). When this is not true, the inside is
hotter than the surface, which can introduce stress. Under what conditions
did this relation hold? When did it not hold?
Was the quenching curve obtained for the liquid nitrogen quench of the form
expected? If so, why? If not, what was expected and what might have
happened to change this?

Plots G-7
Materials 2H03 on-line Laboratory Manual
Updated: 18 May 2000

Experiment H
Electrical Properties

1. Objectives

• To measure the electrical resistivity of a pure metal, an alloy, and an

extrinsic semiconductor at temperatures from 77 to 300 K.
• To determine the sign of charge carriers in extrinsic Ge using the
thermoelectric effect.
• To measure the carrier density and carrier mobility in extrinsic Ge using
the Hall Effect.
• To measure the current-voltage characteristic curve of non-ohmic
materials [a (p-n) junction and a 'varistor'] and relate the behavior to
their microstructure.
• To investigate the nature of integrated circuits.

2. Introduction

2.a Electrical Conduction

Electrical Conduction in Metals and Band-Type Semiconductors. Ohm's law gives J

= V/R, where J is the current produced by a voltage V across a resistance R. For a
rod sample of length L and cross-sectional area A, we can put Ohm's law in terms of
current density J=I/A , and electric field E=V/L , i.e.,

jA = or j = RA which gives
R (L)

j≡ ≡ σE

Where ρ=RA/L is the electrical resistivity and its reciprocal is the conductivity of
the sample material. Thus by measuring V, J, L and A, we can calculate the
electrical resistivity:

ρ= .. (2)

Electrical Conduction H-1

H-Electrical Properties

The change in resistivity of a material with a change in temperature or purity can

be understood with a simple conceptual model. Free electrons in the conduction
band of metals or semiconductors are accelerated by an applied electric field E.
When they collide with an impurity atom or an atom displaced from its site by an
atomic vibration, they lose most of this accelerated energy. The period of
acceleration produces an average drift velocity of electrons, v, in the direction of
negative E. The electric current, J, is the total electric charge passing through area
A in one second.

As can be seen in the accompanying sketch, the number of electrons passing

through per second is the number of electrons in volume vA. Hence, the current
density j = J/A is

j = nvq ...(3)

where n is the number of free electrons per m3, and q= e is the charge per electron.

Simple theory gives a drift velocity which depends linearly on E, i.e.

v = uE ...(4)

where u is a constant called the "mobility" of the electron. Putting equation 4 into 3,
and comparing it with equation 1, gives the conductivity

σ = nqu …(5)

In metals, n is very large 1028/m3, since it equals the number of atoms per unit
volume, times the number of valence electrons per atom. In "intrinsic" (pure)
semiconductors, n depends on the temperature T. Usually, "extrinsic" (doped)
semiconductors are used, in which n is controlled between 1020- 1025/m3 by the
number of dopant atoms added.

If n is independent of temperature, as in metals and doped semiconductors between

77 and 300 K, then the change in resistivity depends only on the change in mobility,
u. u is decreased at higher temperature and at a higher impurity content, since the

Introduction H-2
H-Electrical Properties

drift velocity of the electrons is reduced by the shorter acceleration time between
collisions. We usually express this in a plot of ρ(T) vs T.

Charge "carriers" can be either electrons or holes. The description of conductivity by

holes in a p-type semiconductor is exactly the same as this description of electrons
in an n-type semiconductor. The above description assumed the sample was a
cylinder (uniform area).

It is used to calculate from a measured resistance, R = V/J, in the first experiments.

To remove the effect of resistance at the connection of the current leads, the
potential leads are usually located inside the current leads, so the measured
resistance is that part between the potential leads.

However, in this experiment we will use a simple two-probe technique for

conductivity measurements of samples A,B, and C.

The resistivity can also be measured for a flat sample of irregular shape, using Van
der Pauw’s method. This is often done using a commercial unit with fixed metallic
probes as lead-in "wires". In order to see things, we will use a larger sample with
special soldered connections ("special" to make them ohmic).

If there are four small contacts at peripheral points 1, 2, 3, 4 on a flat sample, as in

Electrical Conduction H-3

H-Electrical Properties

the sketch, then the resistivity ρ of the sample materials can be determined from
resistance measurements using these as current and potential connections.

2.b The Hall Effect

The Hall effect is used to measure, n, the number of conduction electrons/m3 or, p,
the number of holes/m3 in doped semiconductors. The effect is shown in the sketch.
A voltage is applied so that the right hand side of the block is positive, and the left
hand side is negative. By convention, the current due to this applied voltage is from
positive to negative (i.e., along the negative z-axis of the figure), but electrons flow
opposite to this convention (i.e., along the positive z-axis), with a net drift velocity v.
If we now apply a magnetic field B to the sample along the positive y-axis, there will
be a force on the electron (Lorentz force), given by:

F = q(v × B )

where, q is the charge on an electron. Using the right-hand rule, the resultant
vector points in the negative x-direction of the figure, but since the charge on an
electron is negative, the force vector actually points in the positive x-direction. As a
result of this argument, electrons are deflected upward until they reach the top of
the sample, where they accumulate. If the material were electrically neutral prior
to the experiment, then some positive ions near to the bottom surface will be
deprived of their compensating negative charge, leading to a net positive charge at
the bottom of the sample. There will then be an electric field generated between the
positive bottom layer and the negative top layer. After sufficient time, the upward

Introduction H-4
H-Electrical Properties

motion of electrons is prevented by this internal field. An equilibrium is established

when this transverse electric field cancels the force due to the magnetic field.

Equating the upward force to the downward force gives:

V Hall = = dRH jB ...(6)

where w = width of sample in the direction of the VHall, and where the Hall
coefficient is

RH =

Thus, by measuring RH we can determine n. A similar argument for p-type

semiconductors gives a Hall voltage of opposite sign. Thus, both the number of
charge carriers and their type (electrons or holes) can be determined from the Hall
voltage. By combining the measured Hall voltage and the measured resistivity, the
mobility u of the charge carriers can be determined.

Of course, if RH is known, then the measured Hall voltage can be used to determine
the magnetic flux density, B, which is a common way to measure the strength of
permanent magnetic fields.

An analysis of resistance and Hall voltage measurements for rectangular samples

is given in the Appendix.

It shows that:

Resistivity, ρ, can be calculated in terms of voltage, V, current, J, and all the

sample dimensions.
Mobility, u, can be calculated from r, Hall voltage, VH, J, magnetic flux
density, B, and thickness d. [Note: this does not depend on the other
dimensions of the sample.]
Carrier density, n, can be calculated from ρ and u.

For an irregular sample:

resistivity ρ can be determined by the Van der Pauw method, described


The Hall Effect H-5

H-Electrical Properties

u can be determined from the same equation as for rectangular samples,

since it only depends on the thickness direction, r, B and J, as derived for
equation A3 in the Appendix.

VH d
u= ) .... (7)

n can be determined from ρ and u

n= .... (8)

2.c Thermoelectric Effect

The type of charge carrier, electrons or holes, can be determined from the sign of the
thermoelectric voltage. If a bar of n-type semiconductor is heated at one end, the
charge carriers (electrons) will have a higher velocity, thus move toward the cold
end and charge it negatively. Holes in a p-type semiconductor behave similarly,
which charges the cold end positively. The resulting voltage between hot and cold
ends, called the thermoelectric voltage, is positive for n-type and negative p-type.
(Voltage potential energy of a unit positive charge.)

2.d Non-ohmic devices

(p-n) Junctions

If A and B are materials of two different compositions, that are joined together,
there is a "junction" between A and B. An adjustable voltage supply, indicated by
the battery symbol, passes a current through A and B as shown. The current is
measured by the ammeter, shown as J and the voltage by the voltmeter V. If the
junction is "ohmic", then Ohm’s law is satisfied, so J = V / R and the resulting J-V
curve will be the straight line shown dotted, with R = ∆V / ∆J, the slope of the curve.
If A is p-type and B is n-type, then the p-n junction at the interface of A and B is not
ohmic. Its J-V characteristic curve is the exponential curve shown as the solid line
in the sketch.

Introduction H-6
H-Electrical Properties

The p-n junction acts as a rectifier, since a positive V will produce a large current,
and a negative V, a small current. If two junctions are connected in series, e.g.
p-n-p, then it is called a transistor and is used for amplification, among many other

Commercial transistors used to be produced by alloying two beads of indium on to

an n-type Ge slice, called the base. As seen in the sketch, when the In bead is melted
(156°C), some of the Ge dissolves in the In. On cooling, it precipitates out onto the
existing Ge, but this new layer of Ge is saturated with In, hence p-type. The
remaining In solidifies and any remaining Ge in it usually forms fine precipitates.
Gold wires are added as current leads to the In beads and as an ohmic junction to
the Ge base. It will be ohmic if there are no acceptor atoms. The junction can be
made by heating to 450°C since a low melting point Ge-Au eutectic forms. This may
be achieved by a friction weld using an ultrasonic effect, or by using a solder with
added Sb or other donors so that the solidified Ge layer is strongly n-type (usually
called n+). There is a considerable amount of metallurgical "know-how" in these
junctions !

Modern technology needed junctions of a more controlled area, that can operate at
higher temperatures. Thus Al is used as acceptor instead of In, since it melts at a
higher temperature; Si is used instead of Ge, since its band gap is bigger; and
evaporation with solid state diffusion is used instead of melting, since it gives good
control of area and thus control of capacitance. Nevertheless, this experiment will
look at alloyed beads on Ge, since contacts can be made much more easily on Ge

Non-ohmic devices H-7

H-Electrical Properties

than Si the junctions are large enough to see in the optical microscope the epitaxial
regrowth of Ge onto the base Ge illustrates the epitaxial process used in other
aspects of current semiconductor technology.


Zinc oxide varistors are used for voltage stabilization or transient surge
suppression in electronic circuits and power systems due to their high-current
non-linearity and energy absorbing capability. The characteristics of these devices
depend on the distribution of additives and the oxide grain size.

2.e Integrated Circuits

Most transistors are now formed as part of increasingly complex integrated

circuits, produced on one side of a silicon wafer. First a controlled-composition p or
n layer is put on by liquid phase epitaxy, then donors or acceptors are evaporated on
locally and diffused in. Following this, an insulating silicon oxide layer is formed,
and physical (not electrical) holes put through it by localized etching. Then a
metallization layer is put on uniformly. It is selectively etched locally to produce the
conducting paths you wish. Finally an insulating oxide or nitride is put on top. In
the lab period you will observe one using the optical microscope. A sketch showing
the cross-section of a typical components is shown here.

Integrated Circuit Durability

It is instructive to think about the durability of these extremely fine-scale devices,

and their ability to continue to operate in service. Think about the corrosion
problems of these devices and the acceptable corrosion rates (often measured in
mm/year). How might corrosion be inhibited/overcome in integrated circuits?

Introduction H-8
H-Electrical Properties

3. Procedure for the First Afternoon

Read the objectives and introduction to conduction and thermoelectric effect. Make
up the dry ice-alcohol bath (about 7cm deep with 2 cubes of dry ice) after reading the
instruction sheet.

3.a Electrical Conductivity Measurements

Three samples are provided, each connected to a board with clips on the other end
for attaching alligator clamps. DO NOT ATTACH CLIPS TO TERMINALS AT

The samples are:

Nichrome wire (80 Ni 20 Cr) used for heaters.

gold wire, which is very fine so be careful.
an extrinsic piece of Ge, which is brittle so be careful.

Examine the sample board A. Note that the copper strips underneath the board
carry the current between terminals at each end of the board.

The circuit is shown below. Connect it up using sample A.

The DC supply is an HP 6284 A model

° set its current pot to 3.0

° set its voltage pot to zero
° set its range meter switch to 24 V.

The voltmeter, V, is a Keithley 179 digital model.

Electrical Conductivity Measurements H-9

H-Electrical Properties

° set it on 2 volt scale

The ammeter, J, is a Keithley 160 B digital model.

° set it on the mA range and adjust the range as you need it.
Connect up the circuit being careful with polarity and turn on all the
To measure the resistance of the sample, you need to measure the slope of
the J-V curve. The zero value is not precise in this power supply as it is
designed for higher currents. It is most convenient to measure V for a very
small value of J, then increase the current to at least three higher values
using the voltage pot on the DC power supply. The increments of J
suggested for the various samples are on the sample sheets. They need not
be precisely those values, but your values used must be known precisely.
For low resistance samples, you will need to use the reading that gives a
stable result. Do not burn out the Au wire.
• Calculate the value of for each of your three reading intervals on the J-V
curve. Average the result. This is not as good as drawing a curve and
getting the least squares fit, but is OK.
• Repeat the procedure for sample A at liquid nitrogen temperature, and a
dry ice-alcohol temperature. Measure the bath temperatures using a
thermocouple and the digital voltmeter. State the temperatures in your
lab write-up. Calculate the value of (Rroom temp/Rliq.N2temp) for
sample A, from your results.

Calculate the value of ρ for sample A using your room temperature result of R
and equation ρ = RA/l

Do not calculate ∆ρrms.

Repeat section (b) but use the Au sample.

Repeat section (b) but use the rod-shaped Ge sample.

In this case you will need to measure the effective sample length and area. Use the
traveling microscope; remember to always move in one direction to reduce the effect
of back lash. Describe carefully in your report how you did these measurements.
Use this, including the estimated errors, to calculate the ρms error in your
calculation of ρ at room temperature. This is the only rms error calculation needed
in this write-up. Do it carefully and explain what you are doing.

In your write-up, discuss why you think the ratio of (Rroom temp/Rliq.N2temp) is
different for the various samples. A ratio similar to this, but using room
temperature and 4K, is often used as a measure of purity in metals. It might help to

Procedure for the First Afternoon H-10

H-Electrical Properties

note that ρ(T) can be separated into two components, one due to the alloy solute
addition and one due to temperature (Note that the curves on the ρ - T plots in
section 2 are parallel).

3.b Measurement of Electrical resistivity

Measurement of Electrical Resistivity and Hall Voltage of a Flat Germanium


Determine the resistivity of the irregular Ge sample (sample D), using the following

(i) Pass current J13 between terminals 1 and 3. Measure voltage V42 between
terminals 4 and 2.Calculate

V 42
R42 ,13 =
J 13

(ii) Repeat using current terminals 3 and 2, and voltage terminals 1 and 4.

V 14
R14 ,32 =
J 32

(iii) Calculate ρ from

Πd R42 ,13 + R14 ,32 R

ρ= ( ) ⋅ f ( 42 ) ...(11)
ln 2 2 R14 ,32

where d is the thickness and f is obtained from the graph below. If

R42,13/R14,32<1, then use its inverse (i.e., R14,32/R42,13) for the graph since the
function is symmetrical with respect to the two measured R values.

Measurement of Electrical resistivity H-11

H-Electrical Properties

3.c Hall Effect

To examine the Hall effect, change the leads by putting the current leads on
terminals 1 and 2, and the potential leads on terminals 3 and 4 of the sample.

° set current through the sample at 2 mA using terminals 1 and 2.

° measure the voltage between terminals 3 and 4. [In the write-up,
explain why this voltage is not zero.]
° put the sample in the field between the pole pieces of the magnet with
the sample current still on.
° turn on the current in the magnet and set it at 1 amp.
° measure the change in voltage across terminals 3 and 4, when the
current in the magnet is reversed (with the switch provided, and/or by
turning the sample around). In your write-up explain why this voltage
change is twice the Hall voltage.
° calculate the value of carrier mobility, u, using equation 7, and carrier
density n using equation 8 with q = 1.6×10-19 Coulombs and B = 0.20
Wb/m2. In fact, this is a p-type sample, so what you are calculating is
p, the hole density.

(d) Equation 6 says that the Hall voltage increases linearly with the current J
through the sample. Check this out by measuring the Hall voltage with a sample
current of 1, 2, 3, and 4 mA. In the write-up, report your results and comment on

(e) Equation 6 says that the Hall voltage is proportional to B. Measure the Hall
voltage with J = 2 mA, when the current in the magnet has values of 0, 0.25, 0.5,
0.75, 1.0 and 1.25 amps. Plot a curve of magnetic flux density B as a function of
current in the magnet. This effectively uses the Hall effect to measure a magnetic
field. There is a small Hall voltage even when the magnet current is zero. Why is

4. Procedure for the Second Afternoon

(Note: You will need another alcohol/dry ice bath for the first experiment.)

4.a Using the Thermoelectic Effect

Using the Thermoelectic Effect to Determine the Type of Charge Carrier (electrons
or holes) in a Germanium Sample. The usual method of measuring the
thermoelectric effect is to put two potential leads on a sample and heat one of them.
However, since our indium connections melt at 160°C, this is too dangerous. So we
will cool one end in the alcohol/dry ice bath and measure the potential difference
between the ends. Actually we only need the sign of the potential difference, which
is good since the other end cools down quite rapidly as well.

Procedure for the Second Afternoon H-12

H-Electrical Properties

Connect the potential leads from the millivoltmeter to Ge sample C. Note which
lead (pos. or neg.) is at the top (hot end) of the sample, and which is at the bottom
(cold end). Put the bottom end of the sample in liquid nitrogen. Record the sign of
the potential change. In the writeup, describe the voltmeter polarity connections
you used, the measured polarity observed, and from this deduce whether the
sample is p-type or n-type Ge.

4.b Current-Voltage of a p-n Junction

Measuring the Current-Voltage Characteristics of a p-n Junction. A rather old

commercial transistor is supplied. Examine the duplicate one that has had its case
removed. Sketch the components and label the parts, as done in the sketch in
Section D of the Introduction. Use the central terminal, which is from its base, and
one of the other terminals to measure J vs. V of a p-n junction.

To do this, just follow the procedure used for measuring the conductivity of your
previous samples but include the case of the applied voltage from the power supply
for both positive and negative values, i.e., reverse the current leads. Go up to 7 mA
current in the "forward" direction where the current is large. (Caution: Change the
voltage slowly, to avoid overloading the device!)

Go up to 10 µA in the "reverse" direction where the current is small. (This may take
up to 24 volts). In your write-up, plot the curve of J vs. V including both negative
and positive V.

4.c Metallographic Observation of a p-n Junction

A similar transistor has been sectioned and polished for metallographic

observation. Polishing is extremely difficult for this sample because the
indium bead is extremely soft. Do not attempt to repolish it. Examine the
microstructure of the metallic bead and germanium up to a magnification of
450. Draw a sketch of what you see.
Include the sketch in your write-up and explain what you see in the

Metallographic Observation of a p-n Junction H-13

H-Electrical Properties

microstructure in terms of the In-Ge phase diagram (below) and the

solidification process described in the introduction part D.

4.d C-V Characteristics and Microstructures of MOV

C-V Characteristics and Microstructures of Metal Oxide Varistors. Use similar

techniques as in the previous parts of this experiment to investigate the
current-voltage characteristics of a zinc oxide varistor (labeled S14K11). Measure
the current as the voltage across the varistor is increased in 0.5 Volt steps. Do not
exceed 20 Volts. Start taking current measurements using the 10 micro ampere

Switching to a higher ampere scale may be necessary as the voltage is increased.

Plot the current vs voltage and determine at what voltage the properties of the
varistor change.

Examine the microstructures of the three cross-sectioned zinc oxide varistors.

Discern how the differences in each microstructure affect the operating parameters
of each varistor. A classic example of structure-property relations!

4.e Observation of an Integrated Circuit

(a) A Texas Instruments model 2516 EPROM is supplied (erasable, programmable,

read-only memory). It has 16,384 = 214 identical transistors. This corresponds to
2K 8-bit words (K = 1024 = 210 in computer notation), where each transistor stores
one bit.

Examine the EPROM in the optical microscope. Measure the width of a typical
transistor and record for your lab write up!

Procedure for the Second Afternoon H-14

H-Electrical Properties

Aluminum is often chosen as the metallization layer for silicon devices. In your
write-up list the properties that you think are required for this metallization layer.
It may help to re-read the introduction section again.

5. Resistivity and Hall Voltage

Resistivity and Hall Voltage in a Rectangular Sample of Thickness d

5.a Resistivity measured by current

Resistivity measured by current from 1 to 2

J12 = current between terminals 1 and 2

V12 = voltage between terminals 1 and 2

R12 = V12/J12

ρ= RA/L, L = L12, A = L34d, then

ρ= L34d V12 / L12 J12 ... (Al)

5.b Carrier density, n

Carrier density, n, determined from Hall voltage. For current J 12 and Hall voltage
V34, equating forces on electrons due to magnetic flux density perpendicular to
plate and due to Hall voltage

E34 = vB

V34/L34 = vB

But J12 = nqv (L34d)

Equating v in last two equations and solving for n

n = J12B / V34 qd ..... (A2)

5.c Calculate mobility, u

Calculate mobility, u, in terms of ρ and Hall measurements. Put n from equation

A2 into

u = 1 / qρn = V34d / rJ12B .... (A3)

Calculate mobility, u H-15

I-Mass Transport by Diffusion

Materials 2H03 on-line Laboratory Manual

Updated: 18 May 2000

Experiment I
Mass Transport by Diffusion
1. Objectives

• To observe in a gel a diffusion process, that confirms the validity of the

diffusion equation.
• To determine the activation energy for the diffusion of carbon in iron
from observation of the diffusion profile produced by decarburization.
• To examine the diffusion of carbon into steel using micro hardness

2. Introduction

Diffusion is the process in which atoms or molecules are transported in a medium.

In gases and liquids, the main process is usually convection. In solids, it is by atoms
jumping from one site to another. Small interstitial atoms like carbon in iron can
diffuse very quickly but substitutional atoms like nickel in iron are very much
slower. In glasses, small ions such as Li+, Na+, and K+, which are not part of the
glass molecular network, can also diffuse relatively fast. However, all these atoms
or ions need extra energy Q to jump into the next site. Thus, their jump frequency is
proportional to exp (-Q/RT).

At equilibrium, the atoms have an equal jump frequency in all directions so no net
diffusion results. However, if there is a concentration gradient then more atoms
will be jumping from the high concentration side. Hence, one expects a net flux of

J = −D( ) .... (1)

which is known as Fick's first law (this is actually the one-dimensional case of
Fick's first law, which in 3dimensions is given by J= DC). C is the concentration and
D is called the diffusion coefficient, which is proportional to the atoms normal jump

Thus, we expect

D = D 0 exp( ) .... (2)

I-Mass Transport by Diffusion

where Do is a constant independent of temperature. Do is in general a function of

the vibrational frequency of the atoms in the lattice about their equilibrium
positions (jump frequency), the distance an atom must jump to land in an
atomically identical lattice position (jump distance), and the energy required to go
from one lattice point to the next.

In many cases we want a relatively high concentration of solute near the surface of
the sample and a low concentration, perhaps even zero, further inside. In order to
get this, we begin with a block of the low concentration, place a very highly
concentrated form on the very surface layer, and wait for the atoms to diffuse from
the region of high concentration to that of low, as in Fick's law. The curve of the
concentration with penetration, X, will vary with time t = 0, t1, t2 etc. as shown in
the sketch, where Co is the surface concentration. These curves can be calculated by
solving a differential equation called Fick's second law, with the boundary
conditions C = Co at the surfaces X=0, and C=0 at X=∞. The calculated solution
shows that the distance from the surface to a point of constant composition has the
X = ( Dt ) 2 ....(3)

This is shown schematically in the above figure. The horizontal line is the
composition considered. X1 is the distance for the concentration after diffusion for
time t1, etc. Combining equations 2 and 3 shows that a given amount of diffusion is
much more rapidly achieved at high temperatures.

Three diffusion experiments will be done in this laboratory. The simplest one is
easily seen visually. A dilute acid is placed in contact with a gel containing
phenolphthalein. A gel is an amorphous semisolid, which in this case has fairly
rapid diffusion of H+ and very slow diffusion for phenophthalein. Thus, H+ from the
liquid acid will diffuse down through the gel removing the colour from the top part.

Introduction I-2
I-Mass Transport by Diffusion

Since the colour change occurs at a specific pH value (i.e. H+ concentration), the
movement of the colour interface corresponds to the movement of the position of
constant H+ concentration in the gel. Thus, by measuring the position vs. time, it is
possible to confirm equation (3). A similar case for diffusion of OH- into the gel, is
also done.

The second experiment examines equation (2) by measuring the carbon profile
caused by annealing a high carbon steel in air at different temperatures.
"Decarburization" occurs at the outer surface because the carbon atoms react with
oxygen in the air to form CO2. This sets the surface concentration at a specific low
value, Cs, throughout the anneal. After the anneal the carbon concentration, which
was initially at Co, will have the profile shown in the sketch below.

The mid-composition Cm will be at depth Xm, where Xm satisfies equation (3). If

values of Xm are measured at several different temperatures for the same time,
then the value of Q for the diffusion of carbon in iron can be determined as follows.

Putting D from equation (2) into equation (3), squaring both sides and re-arranging,

X 2 D 0 t = exp( ) ... (4)

I-Mass Transport by Diffusion

Taking the natural log of both sides gives:

ln( X 2 )ln( D 0 t ) = − .... (5)

Thus, if this experiment is done at several different temperatures, T1, T2, T 3, ..., for
the same time, then the measured mid-concentrations squared, X12, X22, X32... ,
for the representative temperatures, can be plotted as points (X12, 1/T1) etc. On
semilog paper. This results in a straight line with slope equal to -Q/k. If k =
8.61×10-5 eV/ atom·K, then Q is the activation energy for carbon diffusion in units
of electron volts (eV) per atom. In the present experiment, all anneals are done
above 900°C, so all the diffusion will be in the iron phase.

Beware! You cannot measure the slope directly from the graph. You must record the
X2 and 1/T values at two points on your graph, and then evaluate

Q/k = [ln( X22) - ln (X21)] / [ 1/T2 - 1/T1] ... (6)

Remember T has units of Kelvin !

This analysis is for a long rod with diffusion along its length and surface
concentration Cs independent of T. Your experiment will differ somewhat, but the
simple analysis can be used.

The third experiment is a carburizing treatment in which you want a high carbon
concentration in the surface region of steel and a low concentration inside. The hard
surface improves wear and inhibits the formation of fatigue cracks. The softer
inside inhibits brittle failure due to crack propagation. In our case, the surface
carbon content is achieved by packing the sample in a sealed box with cast iron
chips of high carbon content. In most commercial practices, it is achieved with a gas
of relatively high CO/CO2 ratio. In our experiment, samples are diffused for four
different times and equation (3) is examined by measuring the micro hardness
change with distance from the surface.

3. Procedure for the first afternoon

Read the introduction before the first lab period. If there are four students in the
group, divide into pairs so that each pair does all of the following gel experiment.

Procedure for the first afternoon I-4

I-Mass Transport by Diffusion

3.a: Diffusion in Gels

Two gels have been prepared:

a. a stiff water based gel containing phenolphthalein. It will be a clear colour

but will turn pink when OH- ions diffuse in.
b. a 0.01 N NaOH based gel containing phenolphthalein. It will be pink but
will turn clear when H+ ions diffuse in.

Pour 0.02N NaOH solution on top of the water based gel and 0.01N HCl solution
onto the NaOH base gel, and note time t= 0, when this is done.

Measure the motion of the colour interface as a function of time. Take frequent
readings during the first hour, then at 1/4 to 1/3 hr intervals until the end of the
afternoon. It should be possible to obtain an additional reading the following
morning and the next day as well, before the gel breaks down. As usual, record the
uncertainty in your measurements.

Record interface position (mm) versus time and plot a graph of X vs t. It obviously
decreases with time.

Theory states that the interface position is 1.7 (Dt)½, where D is the "diffusion
coefficient". Do you find this in your experiment? Demonstrate your answer by
plotting X vs. t½.

Determine the diffusion coefficients for H+ and OH- in the gel, and comment on
your answer. Include your calculation of the rms error in your answer.

What are you assuming about the diffusivity of phenolphthalein in this

experiment? What would specifically happen if your assumption was wrong?

Diffusion in Gels I-5

I-Mass Transport by Diffusion

3.b: Decarburization of steel

Four samples of a high carbon steel drill rod (1.0wt%C) have been annealed in air
for 19 hours at different temperatures; 900, 950, 1000 and 1050°C. Remove them
from the furnaces with an air cool (this is called "normalizing"). Each student will
take one sample, remove the oxide, measure its diameter to ±0.02 mm or
equivalent, cut it into two cylinders on the cut-off machine, grind the cut surface
flat, mount it, polish it and etch it in "nital". Get instruction before using the cut-off
machine and cut slowly with water cooling to avoid overheating. Also measure the
diameter of untreated rod to within ±0.02mm.

The amount of pearlite will decrease toward the edge of the cylinder. Using the
optical microscope determine the depth, X1, from the outer edge to where it is 50%
pearlite, for each polished sample. This will be difficult to do. You will need to set up
a reproducible procedure and use it for each sample. Perhaps using the video screen
will be useful, but check its uniformity at different positions on the screen (i.e. at
different positions of your sample). Determine the value of X1 and its uncertainty
DX1 for each sample.

Xm = total depth from the original metal surface to the 50% pearlite, will include
both X1 and the metal removed by oxidation. Determine Xm ± ∆Xm for each sample.
Plot the results using ± DXm as error bars.

For each point, using semilog paper, calculate the value of Q using equation (6) of
the introduction.

Estimate the uncertainty in your value of Q and describe how you do it.

4. Procedure for the Second Afternoon

4.a: Heat by Conduction

Demonstration of the Diffusion of Heat by Conduction During the induction heat

treatment of a Fe1.0%C rod. The flow of heat by conduction down a temperature
gradient follows the same equations as the flow of atoms by diffusion down a
concentration gradient. In this experiment, the surface of part of a steel bar will be
heated by induction. The initial heat is deposited to a depth of 0.03 mm below
738°C, and 0.9 mm above 738°C. This heat diffuses to cooler regions during the 40
seconds of heating.

After 40 seconds, quench the rod, section it lengthwise, polish and etch it. The
section of the rod that was not heated above 738°C will have the original
microstructure (partially spheroidized pearlite). The section heated above 738°C
(i.e., into the austenite region) will transform on cooling. If the cooling rate was
rapid, the austenite will transform to martensite. If it was slower, the austenite
forms pearlite. All three microstructures are clearly distinguishable under the

Procedure for the Second Afternoon I-6

I-Mass Transport by Diffusion

optical microscope. With this information, you should be able to explain your

Draw a sketch of your etched sample. Mark on the sketch, the region that is the
original structure, the region that is martensite, and the region that is new pearlite.
Explain the size and shape of these regions qualitatively, in terms of the flow
(diffusion) of heat during the induction heating and subsequent quenching.

Measure the Rockwell hardness of your sample at the surface and the centre.
Explain the difference in terms of the microstructure observed.

4.b: Carburization of Steel

Four samples of a low carbon steel have been carburized using pack carburization
at 950°C for different times; two, four, six and eight hours. (Pack carburization is
done by packing chips of high carbon cast iron around the sample during the
anneal, and then air cooling the sealed box). The samples have then been sectioned,
polished, and micro hardness indentations made at increasing depths from the
carburized surface.

The demonstrator will describe the micro hardness tester for you. You will read the
values on the two samples and plot a curve of hardness vs. distance from the
carburized surface. Correlate the hardness values with the observed percent
pearlite on one of your samples. Plot a curve of hardness versus percent pearlite.

The nominal diffusion distance (X) is given by equation (3). Taking the nominal
distance as that required for the increased hardness to drop to one half that of the
increase at the surface, check equation (3) by plotting the distance, X vs. t. This will
give one point for each sample.

Do not forget to include the error bars on each point and describe how you got them.

In the write-up, discuss the changes observed in the hardness versus the distance
from the surface, and how this changes with furnace holding time.

Carburization of Steel I-7

J-Mechanical Properties

Materials 2H03 on-line Laboratory Manual

Updated: 19 May 2000

Experiment J
Mechanical Properties
I. Objectives

In addition to the obvious objective of getting practical experience, there are several
objectives in examining the role of microstructure on properties, and the correlation
of results from different testing methods. These are:

• to produce a tensile curve from a typical pure metal or alloy without

interstitial solute; in this case aluminum
• to produce tensile curves from plain carbon steels and show how they are
related to carbon content, carbon distribution and grain size to show how
hardness is correlated to the tensile properties
• to show how the hardness increases with prior plastic deformation
• to illustrate the role of temperature on the ability of a steel to withstand
brittle fracture, by measuring the energy required to fracture it as a
function of temperature
• to produce a bend test curve for a brittle material and illustrate how a
residual compressive stress can improve the properties.

II. Introduction

II.1: Tensile Test

The choice of a material for a particular application is often determined by its

mechanical properties. One of the most useful mechanical tests is the tensile test. A
sample rod is gripped at each end and pulled at a steady rate. The force required to
do this is measured with a "load cell". The "engineering stress", (force divided by
the original cross-sectional area) is plotted against the "engineering strain",

Tensile Test J-1

J-Mechanical Properties

(increase in length divided by the original length). Schematic tensile curves for
aluminum and steel are shown below.

Standard procedures for the tensile test are given in specification E8 in part 3 of the
ASTM standards, which are in the reference section of the Science Library, TA 401.
Four important mechanical properties are illustrated in the tensile stress-strain

Rigidity: i.e. how much does the material deform elastically under a given load.
This is determined by the elastic modulus, E, which is defined in the elastic range
by σ = Eε. For instance, a typical plastic will extend 300 times as much as steel
under the same stress. Its elastic modulus is 1/300 that of steel. This can be
determined from the initial slope of the tensile curve, for tests on a hydraulic tensile
machine, provided it is plotted as stress vs strain.

Yield Strength: This is the stress beyond which the material will have a
permanent change in length. In many cases, it is the main design parameter for use
of the material. The schematic curve shows a sharp break here, but in practice the
non-uniformity of the sample material and the imprecise alignment of the applied
force will round it off. Thus, the stress at 0.2% strain is always used to determine
the yield stress for specimens that do not exhibit a definite yield point. Since
gripping the ends of the test sample can introduce some very high local stresses in
addition to the one measured, an accurate reproducible measurement of the yield
stress can only be made when the tensile sample has a central section which has a
reduced diameter, the so-called "gauge section". This causes the initial deformation
to mainly occur in the central region and not at the grips.

The yield stress, σ of a metal is usually related to the length of slip plane available
for a dislocation to move. In pure materials or in low carbon steels in which a

Introduction J-2
J-Mechanical Properties

majority of the structure is ferrite, the length of the slip plane available is the grain
diameter and the relation is the so-called Hall-Petch relation:

σ = σ0 + 1

where σo and k are constants and d is the grain diameter. When the steel is mainly
pearlite, d is related to the thickness of its ferrite plates within the pearlite

Ultimate Tensile Strength is often just called the "tensile strength". This is the
maximum stress attained, as shown in the tensile curve. This may at first appear to
be a useful parameter, but it is not too useful for deformable metals. Usually, we do
not want things to deform permanently, so the yield stress is more important. Also,
the ultimate tensile stress is partly controlled by the start of severe local
deformation, which introduces a thinned region called a neck in the sample. The
elongation after the maximum stress is in the locally necked region.

Ductility: is a measure of the amount of plastic deformation and is a very

important parameter. It is measured in either of two ways:
1. "elongation" is the total strain to fracture and is usually
determined by marking two points a distance Li apart in the
centre of the sample before the test and remeasuring their
separation (Lf) after putting the broken pieces together after
the test. Li is commonly two inches and is within the reduced
gauge section. The percent elongation is then 100 (Lf-Li)/Li.
2. "reduction of area to fracture" The initial cross-sectional area
Ao of the gauge section is measured. The final area at the
fracture Af is also measured. The percent reduction in area is
then 100 (Ai-Af) / Ai. Note that this includes a large local strain
if there is necking before fracture and is a true representation
of the local strain at fracture. Because the volume of the sample
is not changed during plastic deformation, the elongation and
reduction of area will be the same if there is no necking.

II.2: Impact Test

Another important mechanical property is the ability to contain a crack or other

flaws and not have it propagate to fracture when a load is applied. All materials
have flaws, especially those produced in large quantities where the control of
quality is more difficult. A crack of length C will propagate when the tensile stress ,
oriented perpendicular to the crack, is greater than a critical value c, where

B 12
σc = ( ) ....(1)

Impact Test J-3

J-Mechanical Properties

The parameter B depends on the energy required to propagate the crack in the
material. In brittle materials like glass, B is proportional to the surface energy,
since new surface is created when a crack extends. In ductile materials like metals,
the value of B is much larger since it includes the work done by plastic deformation
at the crack tip as it moves. There are many sophisticated ways to accurately
measure B. In this experiment we will not measure it precisely but will measure a
parameter with which it is correlated: the energy required to fracture a notched
sample. This very simple test, the Charpy impact test, is much quicker and
cheaper. Since the yield stress of steel rises rapidly at lower temperatures, which is
typical of metals with body-centered-cubic structure, there is less plastic
deformation during fracture so less energy is required. Thus, the curve for energy
absorbed during fracture as a function of Charpy test temperature T, will look as
shown below.

The transition temperature Tc, between brittle and ductile behavior can be a
critical parameter, especially if you live in the North. The "shelf" energy in the
ductile range is lowered by slag inclusions and MnS stringers in the steel. A low
value correlates with poor quality steel, especially for things like pipelines, which
must be able to withstand physical abuse like gouges from rocks and bulldozers
during installation.

The Hardness Test: is made by measuring the size or depth of an impression

produced by an indenter, which is a standard sharp point or small ball, with a
specified force on it. In principle, the indenter penetrates the sample surface until
the area of contact is sufficient to lower the stress (i.e. force/area) until no further
plastic deformation occurs. Thus, while a direct comparison with the more simple
stress state of a uniaxial tensile test does not exist, the value of this "indentation
hardness" roughly corresponds to the tensile properties up to ten or twenty percent
strain. The main advantage of the hardness test is its cheapness and the fact that it
does not harm the test piece. The disadvantage is that its stress complexity inhibits
direct application to the known design conditions that are required. Thus, an

Introduction J-4
J-Mechanical Properties

empirical correlation must be known that relates past experience with the
hardness values of the materials concerned.

One particularly useful version of the hardness test is the so called "micro
hardness" test. The indenter in this case is small enough that the indentation in the
workpiece has a size the order of a micrometer, allowing for very localized hardness
measurement. The most commonly used micro hardness test is the Vickers
hardness test, in which the indenter is diamond-shaped. A schematic diagram of
the indenter and impression are shown in the diagram below.

As indicated in the diagram, the diagonals of the indentation are measured, and
the Vickers Hardness Number (VHN) calculated using the following formula:

VHN = 172

where P is the load applied, and d is an average of the two diagonal measurements
(d1 and d2). The micro hardness test has a special advantage in determining the
local strain distribution in a material. This is based on previously calibrated strain
vs. hardness curves.

This method can thus be used to measure the strain distribution in a non-uniform
region of deformation, as occurs at a crack tip, at the root of a notch, in the matrix
adjacent to a particle, interface, etc. It is used primarily for metals.

Impact Test J-5

J-Mechanical Properties

II.3: Testing Brittle Materials

Brittle materials like glass have zero (or little) plastic deformation. Since they fail
by cracks nucleating and propagating from existing flaws, the fracture stress is
much higher in compression than in tension. In practice a bend test is commonly
used. It eliminates the difficulty of gripping a brittle sample for a tensile test and it
also has the advantage of producing a maximum stress at the surface, which is
where the major flaws are located. The fracture stress is usually controlled by the
depth of surface scratches as in equation(1), with C/2 the depth of the scratch. The
tensile stress in the convex surface layer of the four-point bend test is:

3F ( L2 L1 )
s= ....(2)
2bh 2

which, if you have taken a course in engineering mechanics, should be able to

derive. The geometry is sketched below:

The glass sample is a plate of thickness h, length greater than L2, and width of b.
The two rods on the top and the bottom are symmetrically located, with a vertical
force of F/2 on each (as shown), which is produced by the tensile machine. Thus a
graph of force F vs. vertical displacement of the rods is measured. The force at
fracture, put into equation 2, gives the fracture stress.

Since most of the flaws in glass are surface scratches, and since it is weakest in
tension, it is very important to remove any residual surface tensile stresses when
manufacturing glass articles. These can be reduced by annealing after fabrication.
Even better, is to introduce a residual compressive stress in the glass surface. The
tensile stress that is then required to break it will be that much higher. One means
of doing this is to replace small ions in the surface region by large ones. Since Na+
diffuses quickly in the glass, it is replaced by potassium, K+, which is a larger ion.
Replacing it by Li+, which is smaller, will leave a residual tensile stress in the
surface. The theory is discussed in Pye's book "Introduction to Glass Science",
TP845 I6. Some patents giving commercial applications, are described in "Glass
Technology Recent Developments" TP858 R64, page 190-195.

Introduction J-6
J-Mechanical Properties

Measurement of Grain Size The grain size of a material is a very basic and
important parameter in the characterization of materials. One important effect is
on the yield strength of materials, which has already been discussed, through the
Hall-Petch relation (see Introduction). There are three major ways used to
characterize and determine the grain size of a material.
1. Average grain diameter, d. The grain diameter is defined as
the diameter of a circle, which has the same area as the grain
in question. Thus, depending on the homogeneity of the
material, the area of 20 to 50 grains are measured, and the
associated equivalent diameter calculated. The average grain
diameter is then obtained. Modern image analysis techniques
can do this with ease.
2. Index Number, N. The index number is defined by the
American Society for Testing and Materials (ASTM) as

n = 2N-1

where n is the number of grains per square inch of your sample at a magnification
of 100X. Rewriting the above equation, we get:

N = 1 + 3.32 log n

We can relate n and d (grain diameter) as follows:

π A
n( ) d 2 =
4 M2

where A is 1 in2 [654.2 mm2], and M is the magnification (in this case 100X).
Solving for d, we obtain:

1 1
d = 2866
. ( )2

Therefore, the index number is related to the grain diameter by the following

N = -9.24 + 6.64 log (1/d)

II.4: Linear Intersection Method

The simplest method is the "linear intersection method". Suppose we have a

photograph of the sample, taken at magnification M. If a line of length C is drawn
across the photograph, and the number of intersections it makes with grain

Linear Intersection Method J-7

J-Mechanical Properties

boundaries, N, is recorded, then the average length between intersections is

obtained from the following relation:

L = C / N.M

The equivalent ASTM grain size number, ge can then be calculated:

ge = -10.00 + 6.64 log (1/L)

Comparing this result with the one obtained for the index number method, we see


The following table gives the relations between the various methods:

ASTM N n d (µm) L (µm)

1 1 287 220
2 2 203 156

3 4 144 110

4 8 101 78
5 16 72 55

6 32 51 39

7 64 36 27.5
8 128 25 19.5

9 256 18 13.8

10 512 13 10
11 1024 9 6.4

12 2048 6.3 4.8

13 4096 3.5 3.5

14 8198 2.5 2.5

Introduction J-8
J-Mechanical Properties

III. Procedures for the First Afternoon

III.1: Tensile Test

The TA will explain to you how to do a tensile test. You can then test the following
samples using the full scale load deflections shown. Be sure to record all
measurements in your notebook.

a. an aluminum alloy, which has previously been annealed to recrystallize it

(525°C for 10 min). Full scale 5kN. Rate 2mm/s.
b. a low carbon steel alloy, which has previously been normalized (heated to
900°C and cooled within one hour). Full scale load 25kN.
c. the same low carbon steel alloy, which has been normalized after annealing
at 1200°C
d. a high carbon steel alloy, which has previously been normalized. Full scale
load 25 kN.
e. a spheroidized high carbon steel alloy, which has been held at 680°C for 24
hours after normalizing in order to form the carbides into spheres. Full
scale load 25 kN.
f. Perspex. Full scale load 1.5kN. Rate 0.5mm/s.

Calculate the value of the

1. elastic modulus from the initial slope,
2. the yield stress at 0.2% plastic strain (where applicable),
3. the ultimate tensile strength,
4. the elongation to fracture and
5. the reduction in area at fracture, for each tensile sample.

Put your results in a table. Show clearly on your tensile plot how you determined
the load at 0.2% strain. Note: 0.2% strain means (Lf - L i) = 0.002;Li. It is not related
to the total strain to fracture.

III.2: Microstructures

An undeformed piece of each metal tensile sample has been mounted in Bakelite or
plastic, and etched. Observe them in the optical microscope. Check the phases
present, their distribution, take micrographs and use them to measure the grain
size of samples (b) and (c) to check the validity of the Hall-Petch relationship.

Sketch what you see and describe it for the write-up.

Microstructures J-9
J-Mechanical Properties

Try to determine any relationships which appear from your results, to indicate how
mechanical properties depend on microstructure. Remember such properties are
typically determined by either "composition" or "scale".

III.3: Compression Testing

Pieces of 3/8 inch rod of commercial aluminum have been cut to ½ inch lengths with
parallel ends. They were recrystallized with one hour at 525°C. Read the
instructions for compressing a sample on the Buehler press. Measure the initial
diameter of each sample, compress one to 4000 pounds force. Remove, remeasure
central diameter.

Measure its Rockwell F hardness in at least three places in the central region of the
outside surface of the cylinder.

Repeat with other samples using 5000, 6000, 8000 pounds with each student doing
one of the samples and then combine the results.

Note: read from scale marked RAM FORCE in pounds.

IV. Procedure for the Second Afternoon

Note: It would be more efficient in time if the glass samples (described

later) were prepared at the beginning of the laboratory period!

IV.1: Microstructure to Mechanical properties

Relationship of microstructure to mechanical properties. Now that you have plotted

the tensile curves and determined the mechanical properties of the steel samples
tested, it is instructive to look again at the microstructure samples, and discuss the
relationships that you conclude.

IV.2: Impact Testing

Read the description and instructions for doing a Charpy impact test.



The samples are from 3/8 inch square bar stock, which is a bit smaller than the
standard size. They are low carbon steel, as received, cut to length and notched.
Familiarize yourself with the operation of the machine.

Very carefully test the samples at the following temperatures -196°C, 0°C, room
temperature (record it), 50°C and 100°C.

Procedure for the Second Afternoon J-10

J-Mechanical Properties

The lowest temperature is achieved by putting the sample in liquid nitrogen.

Each student should do one of the tests and share the results with the other Team


IV.3: Bend Testing of Glass

The TA will instruct you in modifying the tensile machine by inserting the sample
rig for the four-point bend tests.

Prepare the following samples, and perform three tests on each. [The scatter in
your results may be appreciable as the ASTM specification C158 in the part 17
(1980) asks for 30 repeat tests unless the surface has a standard abraded finish. In
that case they ask for ten tests. However, careful work reduces the scatter

• a piece of a glass microscope slide which you have lightly abraded with
• a new glass slide etched 5 min in 5% HF. Do not scratch the surface after
• a new glass slide with KNO3 put on one surface for 45min. at 400°C,
followed by an air cool. Test with the surface down, i.e. you wanted the
treated side under tension so you want it to be the convex side.
• a new glass slide with LiNO3 put on one surface for 15 min. at 400°C
followed by an air cool. Test with the treated surface on the convex side.

V. Write up

Answer the questions posed in the "procedures" section..

Sketch the microstructures. Indicate on each sketch what the components are: e.g.,
ferrite, pearlite, etc. correlate the yield stress of these metals with their
microstructure and explain the correlation: e.g., aluminum had the lowest yield
stress, because ..... Indicate how samples b. and c. demonstrate the Hall-Petch

Correlate the steel microstructures with the Fe-C phase diagram.

Plot a curve for the hardness of the outside cylindrical surface as a function of the
force previously used to compress it.

Include error bars on both hardness and force for each point. Compare this curve
with the tensile curve for aluminum and comment on this. Was your maximum

Bend Testing of Glass J-11

J-Mechanical Properties

compressive stress higher than the ultimate tensile strength? What would happen
if it was?

Plot your Charpy results in a curve showing energy absorbed vs. test temperature,
using SI units. Why does the curve have this shape (apart from the obvious fact that
it is brittle at low temperature, i.e., explain why is it brittle?)?

From the measured sample dimensions and breaking force, calculate the fracture
stress for the glass in tension for each sample. Put the results in a table and include
the average result for each type of sample as well.

Explain very briefly the relative values measured.

The ASTM specification on measuring the fracture (rupture) stress of glass states
that tests must be at a relative humidity of (40 ± 10)%. There is no relative humidity
specified for testing metals. Can you explain this?

Write up J-12
Materials 2H03 on-line Laboratory Manual
Updated: 23 May 2000

Experiment K
Sintering and Density
I. Objectives

• To set up a procedure for measuring the density of samples with

interconnecting pores.
• To measure the change in density of extruded clay when fired in a range
of temperatures.
• To calibrate and use a gradient furnace.

II. Introduction

Sintering is a process in which a solid material is made by pressing together fine

particles and heating them below their melting point until they become more dense.
The densification is produced by the creation of vacancies at the inner voids and
their diffusion to the outer surface or other types of vacancy "sink". This is shown
schematically in the figure, for four initial particles.

The original particles may be compacted dry powders, as used for oxide magnets or
powdered metals, or they may be clay particles immersed in water. The present
experiment uses "number 3 red smooth" clay which has been extruded into a
cylinder, dried below 100°C, and fired at 600°C to facilitate handling. On heating
the clays lose their structural water at about 650°C [as observed in the DTA
Experiment "A"], and then sinter below 1050°C. Their porosity is about 50% after
drying at 100°C and usually about 5% after this incomplete sinter. Thus, their
density and dimension changes appreciably during sintering.

If this final sintered sample is ground to a fine powder, fracture will have occurred
through most of the remaining voids. Thus, the internal porosity of the powder is
almost zero and it will have the "theoretical density" for that material.

Since sintering is a process involving the transport of large numbers of vacancies,

the rate at which it occurs depends on the temperature and the time at that
temperature (a similar argument to that for the diffusion distance of atoms and

K-Sintering and Density

ions in the diffusion experiment, "I"). One quick way to determine how much time is
needed for a given temperature, is to measure the effect that is produced in samples
held in a temperature gradient for different lengths of time. The sketch below
shows a plot of the temperature distribution along the length of a gradient furnace.

A sample with marks on it at centimeter intervals is placed in the furnace.

Correlation of the position of the sample in the furnace and the measured
temperature along the furnace length, will tell you the temperature at each interval
marked on the sample.

The density of a sample is its weight in air divided by its volume, where the volume
is defined by its external dimensions. This is obvious for an impermeable solid but
not so obvious for a solid containing interconnecting pores, such as an unfired brick.
The density of an impermeable solid is easily determined using Archimedes
principle by measuring:

Wsa = weight of sample in air

Wsw = weight of sample in water

ρw = density of water

The equation for the sample density, ρ , is

W sa ρ w
ρ= ..... (1)
W sa W sw

(You use the weight in water to determine the sample volume defined by its outer

Introduction K-2
K-Sintering and Density

Several precautions must be made in this determination. These include:

the liquid chosen must not chemically interact with the


stable bubbles must not adhere to the sample surface.

[Usually some do and you must remove them by shaking or
waiting for them to dissolve, a process whose rate is often
controlled by the surface energies involved. ]

since the measurement depends critically on the density of

the liquid, which often depends relatively strongly on
temperature, the sample and liquid should be at the same

The main parameter needed is the density of the liquid. This can be determined by
measuring the weight of liquid in a standard volume, usually called a pycnometer,
but the temperature must be the same as that used for density measurements. The
obvious equation is

ρw = .... (2)

where Ww is the weight of water and Vw the volume of water in the pycnometer.
The pycnometer can also be used to determine the density of a powdered sample,
ρpdr. The equation is:

W pdr ρ w
ρ pdr = .... (3)
(W pdr + W w − W pdr + w )


Wpdr = weight of powder in pycnometer

Ww = weight of water in pycnometer when no powder present, as in equation(2).

Wpdr+w = weight of powder plus weight of water when both are in pycnometer

The density of a sample with interconnecting pores can also be measured using
Archimedes principle. This involves weighing the sample in air (Wsa), then placing
it in water and boiling for sufficient time to saturate the interconnecting pores
(about 1 hour). The sample is then weighed

K-Sintering and Density

(i) suspended in water (Wsus), and

(ii) suspended in air (Wsat), after the surface is patted dry..

Since the pores are assumed to be saturated with water during measurements (i)
and (ii), the volume of water displaced during the Wsus measurement is equivalent
to the volume of the bulk sample (i.e., the volume of actual material plus the volume
of the pores). The bulk density of the sample is then given by:

(W sa ρ w )
(W sat − W sus )

III. First Afternoon

The first afternoon is devoted to the preparation of the sample, initial dimensional
measurements, and calibration of the gradient furnace.

III.1 Calibration of the Gradient Furnace

Calibration of the gradient furnace and qualitative short-time sinter. Read the
introduction to the experiment (above) before you arrive at the laboratory!

Obtain the clay rods, handle them very carefully as they have
not yet been sintered. They are very fragile. You will need
two rods.

Take both rods and label their ends appropriately (one of the
rods will be sintered for 1 hour, the other overnight).

° Scratch lines around the samples with a 1 cm spacing between them.

° Carefully measure the distance of each line from the marked end

First Afternoon K-4

K-Sintering and Density

° Use the calipers provided to measure the sample diameter at each

scratch line. (Note: make sure you measure the diameter in at least 2
places, since the rod is most likely not round; and a reproducible
measurement is required).

For the one-hour sinter: Put one sample on the grooved brick,
placing the identified end flush with the end of the brick and
pointed toward the furnace.

Since the furnace temperature is 1070°C, it is important to

slowly push the brick with the sample into the furnace to
avoid cracking ( allow 15 to 20 minutes for complete
insertion). Insertion is complete when the entry end of the
brick is exactly 20 cm into the furnace, i.e., 30.5 cm from the
front end of the tube, since the tube protrudes 10.5 cm.

Measure the temperature profile where the sample is located.

[ Note: Much care must be taken in correlating the temperature to position in the
furnace, since the second (longer-time) sinter will be performed without remeasuring
the temperature profile of the furnace.]

Slowly remove the sample after one hour. Allow to cool.

The remaining sample should be inserted as described in

steps 4 and 5 for the one-hour sinter. This sample will be
removed the next working day (arrange an appropriate time
with the T.A. before leaving the lab).

Measure and record the diameter of the samples at all scratch

lines (one-hour sinter).

Qualitative determination of the region of open versus

closed pores:

Calibration of the Gradient Furnace K-5

K-Sintering and Density

Using the sample sintered for 1 hour. Place the end of the bar that was closest to the
furnace entrance in ink (potassium permanganate solution), and allow to steep
until the ink has stopped diffusing through the sample (i.e., the ink has reached the
boundary between open and closed pores).

Measure the distance the ink has diffused. Would you expect a sample sintered for 1
hour with a smaller initial powder size to exhibit the same behavior? Why or why

III.2 Overnight Sintering

Morning After the First Afternoon (by appointment with the TA). Remove the
second sample from the furnace. Allow to cool. Measure and record the diameter of
the sample at all the scratch lines, using the calipers. In the writeup, calculate the
percent change in diameter at the position of all scratch lines for both the
short-time and overnight sinters. Plot these results as a function of temperature in
the furnace at the position of each scratch line.

The lab demonstrator will use a diamond wheel to cut your samples with the
overnight sinter and then put them in the oven to dry.

IV. Second Afternoon

IV.1 Procedure for Measuring the Density of Clay Samples.

The problems with density measurements of clay are:

(i) If the pores are continuous and the water penetrates them, then the density
calculated using the equation for an impermeable solid will be in error (equation
(1)). In this case, the density of the unsintered sample must be calculated using
equation (4), which involves boiling the samples in water as described previously.
For a sintered sample, the same method (i.e., boiling) is also often required.

Second Afternoon K-6

K-Sintering and Density

(ii) Air bubbles trapped on the sample or on the support wire will alter its weight in

IV.2 Density using the boiling method

Attach a suspension wire to the sample so that it hangs from

the hook above the balance pan and will be at the correct
height to weigh the sample suspended in the beaker filled
with water.

Weigh it while suspended in air.

Suspend the sample in a beaker of water, and place the

beaker on a hotplate.

Bring the water to a boil, and allow to boil for 1 hour.

Remove from the hotplate and allow to cool to room
temperature. You may want to use ice to speed up the

Weigh the sample suspended in water (do not remove the

sample from the beaker in which it was boiled).

Remove the sample from the water, and allow the excess to dry.

Weigh the sample in air.

Measure the density of all your cut samples using the boiling
method, described above.

Pulverize the small slice from the hottest end. Sieve through
200 mesh and

° weigh the dry pycnometer

Density using the boiling method K-7

K-Sintering and Density

° weigh the dry pycnometer with the powder in it

° add water in the pycnometer, dry the outside and reweigh it (with
powder and water in it)
° wash pycnometer and fill with water from beaker used for the density
measurements. Dry the outside and weigh it.

Calculate the density of the powder and the density of the


IV.3 Sintered Ceramic Microstructure

While the samples are boiling, obtain the polished and etched alumina samples
from the T.A. There are three samples to look at, all of which were sintered at

Sintered alumina with a large initial powder size.

Sintered alumina with a small initial powder size.

Sintered alumina with a mixture of small and large initial

powder sizes.

Look at each sample, and sketch what you see. Make sure you use a magnification
that shows enough detail, but shows a representative region of the sample. In the
writeup, include the following:

Sketches of the three samples.

Which sample has the highest degree of porosity? The lowest? Why?

Why is the removal of porosity important in producing a strong, tough ceramic


V. Writeup

Answer all the questions and include other items specified in the procedure.

• Plot the temperature profile of the furnace.

• Using this and the measured distance of the scratch lines on your
sample, determine the temperature that the midpoint of each of your cut
samples was at during sintering. Determine clearly the rms error in this
value of temperature for a given cut sample.
• Draw on one curve: density % as function of T, % reduction in diameter
as function of T for each sample.

Writeup K-8
K-Sintering and Density

• Why is the percent reduction in diameter less than the percent increase
in density? By what fraction should it be less and why?
• Calculate the numerical value for the percent porosity remaining in the
most sintered sample (i.e., hot end). Comment on this result.

Sintered Ceramic Microstructure K-9

Materials 2H03 on-line Laboratory Manual
Updated: 24 May 2000

Experiment L
1. Objective

• To examine and understand the basic electrode processes that control the
corrosion rate of a metal.

2. Introduction

Corrosion can be defined as the deterioration of a material because of reaction with

its environment. Although the cost of such loss is extremely high each year, the
same electrochemical processes, if used under controlled conditions, can both refine
materials and provide corrosion protection. Corrosion resistance depends on many
factors. Thermodynamics indicates the direction of the reaction, electrochemical
kinetics control its rate, and microstructural features often determine its location.
This introduction describes the simple electrode processes that take place during
corrosion of metals in aqueous solutions.

2.a: Single Electrode Processes

In general, when one material is placed in contact with another, the atoms will
diffuse into the contacted material until the equilibrium solubility is reached. Thus,
when a metal plate is put in water, some of the metal atoms will dissolve in the
water. These become ionized, i.e., lose one or more electrons, and these remain on
the metal. The positive M+ ions, will be attracted back to the negatively charged
plate to produce a charged ionic layer that is near the plate. The reaction is

M → M+ + e- ....(1)

which is called an "anodic" or "oxidation" reaction, since electrons are produced. If

nothing else occurred, a negative charge would build up on the plate that would
stop the reaction. However, as the concentration of M+ builds up, some of the ions
will move back to the metal, i.e.,

M+ + e- → M ....(2)

which is called a "cathodic" or "reduction" reaction, since electrons are consumed.

An equilibrium will be reached when the flow of M+ ions from reaction (2) arriving
at the metal equals the flow from reaction (1) that leave the metal. We can
represent this flow as an electrical current, io, which flows in both directions.
Because the ions must overcome a potential barrier in the jumping process (onto or

Single Electrode Processes L-1


off the metal), io is proportional to exp(-Ej/kT). Ej is the jump energy required, k is

Boltzmann's constant, and T is degrees Kelvin.

At equilibrium, an excess number of electrons has built up on the metal plate,

which can be measured with a voltmeter whose other terminal is connected to a
reference potential. "Voltage" or "electrostatic potential" is the potential energy per
unit positive charge. Thus, the more ions that dissolve; the more excess electrons on
the plate; and the more negative its voltage. The voltages produced by different
metals are listed as the electrochemical series.

All practical corrosion situations are not as ideal as described above. The water can
have three types of "impurities" that may replace part of reaction (2). They all
produce cathodic reactions.

Excess H+, as in an acid, will cause

H+ + e - → H ....(3)

followed by the formation of hydrogen molecules

H + H → H2....(4)

Dissolved O2 in acidic solutions will cause

O2 + 4H+ +4e- → 2H2O ....(5)

and in basic solutions the predominant cathodic reaction will be

O2 + 2H2O + 4e- → 4OH- ....(6)

These "impurities" will have two effects in our previous description. Reactions 3, 5,
and 6 can replace part of reaction 2. Thus, a steady state dissolution (equation 1)
will occur as the loss of metal atoms is not canceled by reaction 2. The number of
excess electrons on the metal plate will also decrease, which will raise the voltage
on the plate to a new volume determined by an equal rate of the anodic reaction 1,
with the sum of cathodic reactions 2, 3, 5, and 6.

Introduction L-2

2.b: Galvanic Cells

An open-circuited galvanic cell is produced by putting two different metals, that are
not in electrical contact, into water as shown in the sketch. Metal M1 which
dissolves more readily than M2, will have more excess electrons and be at a lower
voltage. Thus, a positive deflection will be seen on a voltmeter if M1 is connected to
the negative terminal and M2 to the positive terminal. M2 is said to be more
"noble" than M1, because it does not dissolve as readily. By comparing different
pairs of metals, they can be arranged in a sequence of nobility, called the
Electromotive Force Series.

In the present experiments, NaCl is added to increase the conductivity of the

electrolyte solution.

In a short-circuited galvanic cell, the metals M1 and M2 are in electrical contact,

e.g. by a wire connecting them, as in the sketch of Figure 2. Before the wire is
connected (Figure 1), M1 had more excess electrons than M2. Thus, after
connection, electrons will flow from M1 to M2.

Reducing the negative charge on M1 will make it easier for its anodic reaction,

M1 → M1++ e-

to proceed. Similarly, the flow of electrons to M2 will reduce the rate of its anodic

M2 → M2++ e-.

There are some important practical applications of these processes.

Cathodic protection of metal M2 has occurred since the rate of its dissolution
reaction is reduced. Zinc plates attached to steel will protect the steel. In this case

Galvanic Cells L-3


zinc, or M1 in our example, would function as a sacrificial anode. A similar result

occurs if a metal is made cathodic by attaching it to the negative terminal of a
battery, which is sometimes done for buried pipelines.

In a wet environment, you should not have two metals, which have a large
separation in the electromotive force series, in contact with each other, e.g.,
couplings between pipes in the ground, nails holding the metal roofing, etc.

A galvanic cell shunted by a resistor is similar to the short-circuited cell, but

the current flow is limited by the value of the resistance. Before contact, there are
more excess electrons on M1 than M2. After contact, the electrons will flow through
the resistor at a rate inversely proportional to the resistance. This transfer of
electrons, enhances the anodic reaction

M1 → M1+ + e-

on M1, and the cathodic reactions on M2. Its continuation as a current depends on
both the continual supply of electrons by the anodic reaction on M1, and removal of
electrons by the cathodic reaction at M2.

A galvanic cell driven by an external voltage At open circuit, M1 and M2 have

their own equilibrium anodic and cathodic currents, io, which are equal and
opposite, and proportional to exp(-Ej/kT) as discussed previously. In order to force
M1 to have a greater anodic current requires an added voltage η , called the over
voltage. The net current will then be

 η −η 
i = i 0 exp( ) − exp( ) 
 β β 

where b depends on kT and the charge on the M1 ion. Thus, for a given net current,
i, the actual voltage needed across the cell (using only the first exponential term) is

V = V 0 + η = V 0 + βln( )

where Vo is the open-circuit voltage between M1 and M2. Therefore, a plot of V

applied vs ln i should be linear, a so-called Tafel plot. This is called "activation
polarization" and is not dependent on time.

2.c: Concentration Polarization

This type of polarization usually increases with time, because it depends on

diffusion of ions in the liquid. Dissolved ions in the liquid will be located in places

Introduction L-4

that minimize the free energy of the system. This produces an ionic concentration
that decreases exponentially with distance from the metal surface, as in the sketch.

If the arrival or removal rate of ions from the metal is slow, they have time to
redistribute by diffusion in the liquid. (D is commonly 10-5cm2 s-1 in a liquid). If the
current is too high, they either pile up near the metal surface for a net anodic
current, or are depleted near the surface for a net cathodic current. This causes the
current to drop with time if the voltage is held constant, or causes the over potential
to increase with time, if the current is held constant.

2.d: Inhibitors and Passivation

All the above arguments assumed a relatively easy transfer of ions across the
interface between the metal and liquid. If this transfer is made difficult, then the
corrosion rate is lower. One way to inhibit this transfer is to add complex molecules
that chemisorb on the metal surface. For example, an inhibitor is added to the
coolant for cars which have an engine block made from aluminum and radiator or
couplings made from other metals. Another way to reduce this transfer of ions is to
develop a chemisorbed or oxide layer during the corrosion process. This method,
called "Passivation", occurs naturally beyond a critical current density for some
metals, if there is a good supply of dissolved oxygen in the water.

A typical curve of applied voltage vs. ln i is shown here. Low voltages give the usual
straight line, which indicates a logarithmic increase in corrosion rate with applied
potential, but the current drops suddenly once a critical current is reached.

Current and hence corrosion almost cease for applied voltages within this "passive"
region. At much higher potentials oxygen evolution gives a linear rise again in the
"transpassive" region. If the very minimal current in the passive region is not
maintained, the chemisorbed oxygen or oxide on the metal slowly dissolves.

Ni, Ti, Cr, and many stainless steels containing Cr, have very low corrosion rates
due to this Passivation process. If the water or atmosphere is sufficiently oxidizing,
they will be in the passive region without an applied voltage.

Inhibitors and Passivation L-5


2.e: Non-uniform "pitting" and "crevice" corrosion

If there are non-uniformities in the chemical composition of either the material or

the environment at its surface, then both local anodes and cathodes can exist on the
same piece of metal. The region that is locally anodic will corrode forming a pit. The
inhomogeneities are frequently caused by depletion of one of the reactants. For
instance, the oxygen supply under the centre of a water droplet, or at the bottom of
the crevices is quickly used up. This slows the local cathodic reaction, which makes
it locally anodic with respect to other areas.

Reference: Jastrzebski, "The Nature and Properties of Engineering Materials", J.

Wiley, 1987.

3. Procedure for the First Afternoon

Read parts 1-5, and 7 of the introduction before the first lab period. If uncertain
about anything ask the demonstrator before you do the experiments.

3.a: Galvanic couples

Sheets of Cu, Zn, Sn and mild steel are provided for electrodes. Clean them with
abrasive paper. Place each possible combination (6 pairs) of the four electrodes into
a 3% NaCl solution that fills one third of a 600 ml beaker. Measure the peak voltage
generated and the sign of each electrode. If the voltage is still increasing after 2
minutes, take the value at 2 minutes. (A voltmeter draws very little current
because it has an extremely high resistance). Knowing the polarity, deduce the
direction of the electron flow, and decide which metal is the anode and cathode in
each pair. Which metal in each pair is corroding? Using your results, list these four
metals in a galvanic series from least noble to most noble. Note: the "electric
current" is defined as the flow of positive charge from a positive to negative voltage.
The meter reads this electric current. Electrons will be flowing in the opposite
direction, from the negative terminal to the positive terminal. For a positive reading,

Procedure for the First Afternoon L-6


the positive terminal on the voltmeter or ammeter is connected to the positive

electrode (i.e., the cathode).

3.b: Concentration polarization

Using the Cu and Zn electrodes, set up the circuit shown. Measure the open-circuit
voltage (i.e., switch not closed). Now set the resistance to 1000 ohms, close the
switch and record the current and voltage at 15 second intervals for 5 minutes.
Remeasure the open circuit voltage. If this does not agree with earlier readings, stir
the electrolyte with the electrodes and try again.

Repeat this for resistance of 500 and 200 ohms, including the remeasurement of
open circuit voltage. Add a few ml of peroxide (H2O2), which forms H2O+ ½ O2
when put in water, and repeat the experiment using 200 ohms resistance. Clean
and dry all electrodes. Throw out the electrolyte.

In your writeup, compare the results by plotting current and voltage vs. time.
Explain the results in terms of the flow of electrons, and of specific ions at the
cathode surface. Also explain why stirring the electrolyte restores the voltage.

3.c: Anodes and cathodes

At the beginning of the session, prepare the mixed indicator gel containing 7.5 g
NaCl dissolved in 250 ml distilled water. Boil it and add 5 g agar. Boil and stir until
agar dissolves. Add 5 ml potassium ferricyanide and 5 ml of 1% phenolphthalein

Pour some of the fluid gel into a petri dish and drop into it, without disturbance,

• A short piece of the steel wire.

Anodes and cathodes L-7


• A similar piece that has been bent back and forth many times to form a
sharp U shape, and
• A steel/zinc combination
• A steel/tin combination.

Clean an area 75 mm square in the centre of a piece of steel sheet with abrasive
paper. Pour into the middle of this a small pool of the indicator gel and immediately
press the convex face of the watch onto the steel surface to make contact..

Place a few drops of indicator on the cleaned surface of another steel sheet.

Observe what you see during the afternoon, and save the samples for another look
at the second session.

Note: In the presence of Fe++, the ferricyanide will turn blue. The
phenolphthalein turns pink with excess OH-.

With this knowledge, plus the observations from part (b), and considering the
crevice between the glass and steel, explain the pink, white, and blue colour
changes observed.

When your examination is complete, remember to remove the specimens,

wash and dry them, put the gel in the container provided for disposal,
wash the Petri dish !

In the next experiments, the change in potential (voltage), of the steel is measured by
comparison with a reference potential, that is produced by a Cu plate immersed in a
saturated Cu2SO4 solution, i.e., a simple reference electrode.

Procedure for the First Afternoon L-8


3.d: Sacrificial Anode

Measure the weight of the ZINC electrode.
2. Place the steel electrode into a 3% NaCl solution and set up
the Cu/Cu2SO4 reference cell and circuit as shown by solid
lines in the accompanying figure. Connect the two beakers
with the salt bridge. Measure current and voltage. Record
3. Connect an immersed piece of Cu wire to "above" the
ammeter, as shown dotted in the sketch. Remeasure current,
voltage and record polarity.
4. Connect an immersed piece of Zn sheet to "above" the
ammeter, as shown dotted in the sketch. Remeasure current,
voltage and record polarity.
5. Remove the Zn sheet. Measure the current and voltage. Add a
commercial inhibitor and remeasure the current and voltage.
6. Remove all the steel and Cu electrodes. Wash them and
measure the approximate total immersed surface area of the
steel and zinc sheet.
7. Re-Measure the weight of the ZINC electrode.

In your writeup, explain the voltage, current, and polarity changes in parts (iii)
and (iv). Which metal is corroding in part (iii) and in part (iv)? If the steel sample
represents a ship hull to be protected, what would be the weight of zinc anode per
m2 of structure consumed in a year to protect it?

According to Faraday's Law:

Sacrificial Anode L-9


(weightofzincdissolved ) it
(GAW Zn ) nF

where GAW = gramatomic weight, i = current in amps, t = seconds, n = charge on Zn

ion, and F = Faraday's constant =96,500 coulomb per mole.

If the steel is protected now by a paint layer, whose pores cover 0.1% of the area,
what would be the new consumption of zinc?

4. Procedure for the Second Afternoon

4.a: Polarization Curve

The Measurement of the Polarization Curve of 430 Stainless Steel with a

Potentiostat (HA-151)
1. Read part 6 of the introduction and the description of the
potentiostat used in this experiment (available in the lab).
2. Before connecting or disconnecting the power cable, be sure to
turn off the power switch of the potentiostat.
3. There are two pieces of 430 stainless steel to be used as
electrodes. Set them up with the straight piece connected to
the WE1 abd WE2 of the TO-CELL-OUT cable of the
potentiostat (one connection is used to measure voltage while
the other is used to measure current), and the curved piece
connected to the CE terminal.

Procedure for the Second Afternoon L-10


4. The reference electrode to be used is Cu/Cu2SO4. Connect the

piece of copper to the RE terminal of the TO-CELL-OUT cable
of the potentiostat.
5. Pour the 6% H2SO4 solution into the beaker with the two
pieces of stainless steel, and pour the Cu2SO4 solution into
the beaker with the piece of copper. Connect the two beakers
with a salt bridge.
6. Before turning on the potentiostat, make sure the
FUNCTION selector is set to ZERO ADJ. Turn on the
7. Set the P-STAT/G-STAT selector to P-STAT (potentiostat),
and set the EXT.SET selector to the OFF position. The
potentiostat is now ready to be used.

The starting value of the potential will be the equilibrium potential,

defined as the potential of the working electrode with respect to that
of the reference electrode at zero current.
8. To measure the equilibrium potential, the FUNCTION
selector should be set to REST POT, and the
POTENTIAL/CURRENT selector should be set at 2V. The
green voltage light should be on.
9. The polarity can be set at either + or - using the POLARITY
selector. A positive potential reading with the POLARITY set
to + , means that the potential of the working electrode is
higher than that of the reference electrode. The potential
value is displayed on the digital meter on the front panel of
the potentiostat.
10. Once the equilibrium potential has been measured, set the
FUNCTION selector to OPERATION. You can now maintain
the potential at any value you choose.
11. Increase the potential by 50 mV. Take readings of both
potential and current from the digital meter. To obtain the
current values, switch the POTENTIAL/CURRENT selector
to CURRENT with a suitable current range. If the current
reading is unstable, take the current reading after 30 seconds.

12. Repeat step (k) until you have obtained enough data to plot
the Passivation curve.
13. Dissolve 10 g of NaCl in the H2SO4 solution. Repeat steps (h)
through (l). The presence of Cl- is expected to diminish the
passivity range and increase the passive current density.

Once you have completed the above steps, you must close down the
system and clean the equipment:

Polarization Curve L-11


14. Set the FUNCTION selector to ZERO ADJ. Turn off the
power to the potentiostat.
15. Return the Cu2SO4 solution to the bottle. Remove the salt
bridge, and store it in a beaker filled with distilled water.
Clean the metal sheets and the beakers used.
16. Measure the approximate immersed surface area of the
straight piece of stainless steel used as the working electrode
(don’t forget to account for both sides of the steel).

5. Writeup

Plot the data obtained for both cases (i.e., with and without NaCl) as E vs log i ,
where E and i are potential and current density (A/cm2) respectively.

Answer the following questions for each curve:

1. What is the potential range corresponding to passivity?
2. What is the minimum potential necessary to preserve
3. Discuss the differences observed in the two curves.

Writeup L-12
M-Magnetic Materials

Materials 2H03 on-line Laboratory Manual

Updated: 23 January 2001

Experiment M
Magnetic Materials
1. Objectives

• To demonstrate the temperature dependence of ferromagnetism by

measuring the Curie temperature of the Nickel alloy ‘Monel’.
• To observe the domain structure in a thin film of Orthoferrite.
• To compare the magnetization curve of several steels used in motors and

2. Introduction

2.a: Magnetic Moments and Domains

Examples of ferromagnetic materials are the transition elements Fe, Co, and Ni,
rare earth elements such as Gd, and a few oxides such as CrO2 and ErO. Their
magnetic properties originate in the magnetic moments of their atoms and free
electrons. In any material there is an interaction between the electron spins of
neighboring atoms, which is known as the exchange interaction. Ferromagnetism
occurs when this exchange interaction causes a parallel arrangement of the spins,
which in turn leads to the alignment of magnetic moments of adjacent atoms or ions
in the same direction. In iron the lowest energy is achieved by the magnetic
moments aligning in the crystallographic [100] direction. This produces a
“permanent magnet” at low temperatures. As the temperature is increased the
entropy becomes more important and the free energy is reduced by increasing the
amount of randomness. Thus, some of the atoms will have their magnetic moments
not aligned with the rest. Above the Curie temperature there is no alignment at all
and the material is no longer ferromagnetic. The Curie temperature of materials
can range from well below room temperature to around room temperature, as in the
nickel alloy “Monel” used in this experiment, to 770°C for iron, and to 1127°C for

One complication to this simple picture is that in some materials, the exchange
interaction between the atoms aligns their magnetic moments not in the same
direction, but in opposite directions for alternate atoms. In some oxides, such as the
Orthoferrite sample used in the second part of this experiment, there remains a net
magnetic moment because the moment of alternate atoms is not aligned in
precisely opposite directions. Thus, it is weakly ferromagnetic, but because of the
way in which it is formed, it is called a ferromagnetic material.

Magnetic Moments and Domains M-1

M-Magnetic Materials

A second complication to our simple picture of ferromagnetism is that the effect of

the external magnetic field produced by our permanent magnet has not been taken
into account. Remember from High School your experiment examining the
distribution of iron filings on a sheet of paper placed near a permanent magnet?
This distribution is due to the magnetic field produced by the permanent magnet
and this field requires energy. Thus, the total energy of a permanent magnet is
decreased by having its atomic moments aligned, but is increased slightly by the
external magnetic field this produces. This increase can be reduced by forming two
or more “magnetic domains” in the sample as shown in the diagram below (right),
where all the atoms in each domain have the magnetic moments oriented in one
direction shown by the arrow, but the direction is opposite for the two domains.
Thus, most of the magnetic field remains inside the sample.

The total energy is reduced but the material by itself does not act as a permanent
magnet, i.e., doesn’t act as a compass needle or attract other similar pieces of iron.
The boundary between domains is called a “domain wall”. The one shown is a 180
domain wall as the magnetic moments of the atoms on opposite sides of the wall are
180 to each other. To reduce the external field even more, small “closure” domains
also occur at the ends as shown below. They form a 90 domain wall with the long
domains. Normal iron at room temperature has thousands of domains similar to
those in the sketch.

Two of the experiments in this group are to measure the Curie temperature of a
material. The first measures the force to pull a permanent magnet from the sample.
The force between the magnet and the sample is complex in this geometry but for a
simple one-dimensional case is proportional to the product of MH dH/dx, where M
is the magnetization of the sample (or magnetic moment), and H dH/dx is the
product of magnetic field and field gradient produced by the permanent magnet at
the position of the sample. The second experiment uses a transformer in which the
sample is the core. The current induced in the secondary winding is proportional to
dB/dt of its core, where B is the magnetic induction or magnetism produced in the
core material by the magnetic field H (H is produced by passing a current through
the primary winding of the transformer). The maximum value of B, which is at the
top of the hysteresis loop, will depend on the magnetization of the core material.

Introduction M-2
M-Magnetic Materials

2.b: Magnetization and B-H Curves

As described in standard texts, the plot of magnetic induction, B, of a material as a

function of applied magnetic field, H, can be divided into three components, shown
as sections A to B, B to C and C to D in the following figure (left).

The sketches on the right are schematic representations of the domain structure at
each of labeled points on the curve. The following processes occur.

• A to B movement of 90° domain walls. Internal stress, as at dissolved

carbon, affects this.
• B to C movement of 180° domain walls. Second phase particles affect
• C to D rotation of magnetization in the domain from the low energy
crystallographic direction [100] to the direction of the applied field, H.

If an alternating current I is used to produce the field H, using the primary coil, the
induced magnetization in a sample within the coil will follow the oscillations in H to
produce a B-H or “hysteresis curve” as shown in the next figure. The B-H curves 1,

Magnetization and B-H Curves M-3

M-Magnetic Materials

2, 3, 4 are those observed if the primary current has an amplitude that produces
fields H1, H2 H3 and H4 respectively.

The magnetization curve is the thick line in the above figure. It does not appear
directly in the BH hysteresis curve but obviously controls its form. In the present
experiments, curves of type 1, 2, 3, 4 are used to plot the magnetization curve. This
is a rapid method for comparing materials but is not very accurate.

2.c: Metal for a Transformer Core

The primary coil with N turns, radius r metres, and current I amps, produces an
alternating magnetic field of amplitude

H= ampere − turns − per − metre

This induces an alternating magnetic induction of amplitude B in the metal core, as

seen from the B-H curve. The output voltage from the secondary winding is
proportional to dB/dt, thus increases with B for a given frequency. To reduce
distortion of the output cosine wave due to the production of higher harmonics, the
value of B is kept as near the initial linear region of the magnetization curve as
possible. Another important quantity in the study of magnetic materials is the
magnetic permeability, defined as µ ≡ B / H . A material that is easily magnetized
will obviously have a high value of µ; that is to say that we will have large values for
B resulting from a low primary current (and thus a low value for H). Thus, a “good”
magnetic material will have a narrow but tall hysteresis curve. Looking at the
figure and description of the magnetization curve, this can be achieved by:

Introduction M-4
M-Magnetic Materials

• reducing the value of H needed to get to point B by allowing easy 90

domain wall movement, achieved by the removal of interstitial carbon.
• allowing easy 180 domain wall movement to increase the slope of the part
B to C by removing second phase particles
• raising the height of point C by having as many grains as possible with
their [100] direction parallel to the applied field. This is achieved by
producing a “grain oriented” steel using a special heat treatment to
control second phase particles, usually MnS. The steel is rolled and
recrystallized as usual. When raised to a higher temperature, an
appropriate distribution of fine particles will inhibit the growth of grains
except those with their [100] axis parallel to the rolling direction. The
resulting grain oriented steel is said to have a “preferred orientation” or
“texture”. Some very low-loss transformers are wound as a toroid so H
can always be applied in the rolling direction. For small transformers the
core is made of C or E shaped sheets, as shown below, so in part of the
magnetic loop the flux is perpendicular to the rolling direction. Our
experiment examines this effect .

The core material must also minimize the energy loss per cycle. The total “core loss”
has two contributions. The “hysteresis loss”, represented by the area of the low
frequency hysteresis curve, is the energy lost in moving domain boundaries. The
“eddy current loss” is the electrical resistance loss due to the electrical eddy
currents induced in the core. These currents are reduced by adding three or four
percent silicon dissolved in the iron (a characteristic of electrical steels), by
laminating the core with an insulating varnish between the sheets, and finally by
using oxide magnets, which are essential at high frequencies. The loss is measured
commercially using a wattmeter but this is not used in this experiment.

Metal for a Transformer Core M-5

M-Magnetic Materials

2.d: The Role of Sample Shape in Measuring B-H Curves

The analysis always assumes that the sample is uniformly magnetized. This is only
correct for an ellipsoidal sample in a uniform field or for a sample in the shape of a
toroid (donut). Transformers must use thin sheet not only to reduce the eddy
currents but also because the field penetration depth is only about 1 mm for the
material of high permeability that is used. A “toroid-type” arrangement is usually
simulated using thin strips to form an open square, with their ends clamped to
produce a continuous metallic circuit. This so-called “Epstein Frame” (ASTM Spec.
A343) has many strips 3 cm by 10 cm, with a primary and a secondary coil on each
side of the square. The one used in our experiment will be more simple, but the
principle is the same. If a straight bar is used instead of a toroid, the induced
magnetization decreases toward the end of the bar.

2.e: Oscilloscopes for B-H Curves

As you probably know an oscilloscope has a cathode ray tube (CRT) with two sets of
deflection plates. The voltage to be observed and measured is put on the “vertical”
deflection plates causing the electron beam to move vertically. The horizontal
deflection is usually a repeated time sweep that is set to initiate (trigger) at the
same point in the wave of the measured voltage. In our case, we want to use the
CRT as an x-y plotter for the BH curve of our sample. The applied magnetic field H
is represented by a voltage, which excites the horizontal deflection plates (x-axis).
Thus, provided these signals both have the correct phase the CRT will show the B-H
curves. The voltages determined from the deflection, multiplied by the scale
sensitivity (volts per cm), must be related back with appropriate calibration to
obtain the numerical values of B and H. This is not an accurate way to measure a
B-H curve, which should be done by D-C methods with incremental changes, but it
is very informative and rapid for comparison of different materials.

The sample is put into a magnetic field H, which is produced by a coil of N turns of
radius r metres with a current of I amps. The value of H is NI / r
ampere-turns-per-metre. The older non MKS units is the “Oersted”, for which
H = 0125
. NI / r Oersteds. Thus, one ampere-turn-per-metre =.0125 Oersteds. In our
experiment N ≈ 200,r =.018m, so that H = 11 . x104 V / R, where V is the voltage
measured from the CRT. In our experiment, we use a measured current up to 1.5A,
so that the maximum field is roughly H = 165. x104 amp − turns / m = 205 Oersteds.

Introduction M-6
M-Magnetic Materials

This requires some correction, since the maximum current is a highly distorted sine

The complete electrical circuit is shown in this figure. R1 is small in order to pass
the primary current. To obtain a voltage proportional to B in the sample, a
secondary coil surrounds the sample. The voltage induced in it will be

V =N
S S dt

where N S is the number of turns, and φ is the magnetic flux through it. Assuming
all the flux is through the cross-sectional area A of the sample φ = AB. Thus,

VS = NS A ,

so to get B we need to integrate this. We convert this to a current in the secondary

circuit I s = V s / Z s , where Zs is the impedance of the circuit, thus

B= ∫ I S dt ...(1)

Since an electric current is charge per unit time, we can integrate it by allowing the
current to charge up a condenser. The voltage across the condenser will then be

Q dt
Vc = = ∫ Is .
c C

Thus, the charge on the condenser will be proportional to B in the sample, as

putting this into (1) gives

 N AC 
B =  s V c ...(2)
 Zs 

Oscilloscopes for B-H Curves M-7

M-Magnetic Materials

The circuit is shown below.

A resistance Rs is added to control the response time (time constant RS C) of the

circuit. If Rs is chosen much greater than the reactance of the condenser

 1   N S AC 
X c =  then Z S = RS , so B =  V C
 Cω   RS 

can be found once the voltage VC is measured from the oscilloscope. In practice, the
time constant of the circuit has a major effect, so the proportionality constant is
found by calibration using a known mutual inductance. We will not do this

In our experiment, the time constant was chosen as 0.7 seconds, which must be
much greater than the time for one cycle. Using a time constant that is much less
than one cycle, would just give an instantaneous value of Vc proportional to dB / dt.
The only other requirement is that the impedance of the oscilloscope, in our case 10
M, must be much greater than the impedance (reactance) of the condenser.

Introduction M-8
M-Magnetic Materials

3. Procedure for First Afternoon

Three experiments will be done.

The first two measure the Curie temperature of Monel, a ferromagnetic alloy solid
solution with 65% Ni, 30% Cu, and 5% other metals. The third experiment is the
visual observation of ferromagnetic domains in Orthoferrite.

Oscilloscopes for B-H Curves M-9

M-Magnetic Materials

The first experiment determines the Curie temperature of Monel by measuring the
force that a magnet is attracted to the monel as a function of temperature. The
apparatus is shown in the next figure.

The Monel specimen is immersed in a cold dry-ice/alcohol bath. A permanent

magnet attached to one end of a spring balance is suspended over the Monel
sample, and allowed to rest on a Lucite spacer. The tension in the spring scale is
increased until the force overcomes the magnetic attraction. The tension is then
reduced slightly and the magnet is placed back on the spacer. The position on the
scale is read. The bath is allowed to warm up, and the temperature measured when
the magnet attraction is again overcome by the spring. The tension is reduced
further, and the procedure repeated.

A plot of scale reading vs. temperature should be made on graph paper. The hot
plate should only be used at temperatures above 0°C, and must never be turned
higher than “one” on the scale.

[Note: the Curie temperature is that temperature beyond which the

force on the spring is just due to the weight of the magnet. Thus, you
must determine the scale reading for this critical reference point.]

In the second method the Monel sample is the core of a simple transformer as
shown in the diagram below. The secondary voltage is recorded, as the temperature
of the alcohol bath is increased from 50°C to 35°C. Plot a graph of the secondary
voltage vs. temperature and find the Curie temperature by extrapolating the linear
region. This corrects for the curve “rounding off” near the Curie temperature due to
non-uniformity. Do not take too long at the low temperature or you will run out of
time !

The third experiment is to observe domains in an Orthoferrite. Orthoferrites are of

the general formula MFeO3, where M stands for Yttrium or a rare earth, and are
antiferromagnetic with a weak ferromagnetism caused by a slight canting of the
antiparallel spins. The unit cell is an orthorhombic cell of sides a, b and c, with the c
sides about twice the length of the a or b. At room temperature the iron sublattice is
approximately antiferromagnetic, each iron atom having six antiferromagnetic

Procedure for First Afternoon M-10

M-Magnetic Materials

nearest neighbours. The figure shows the direction of the magnetic moments on the
Fe3+ ions.

Faraday observation of magnetic domains in an


The weak ferromagnetism along the c axis is caused by canting of the spins in an
essentially antiferromagnetic crystal. It is the weak ferromagnetism in the
direction of the c-axis that results in the formation of the domains.

In thin film of a special orientation, the magnetization of the Orthoferrite is

perpendicular to the surface of the film. Thus, domains have their magnetic
moment pointed up or down when the film is horizontal.

Oscilloscopes for B-H Curves M-11

M-Magnetic Materials

3.a: Observation of Domains in Orthoferrite Crystals

The Faraday effect is utilized for observing the domains. If a polarized light beam is
passed through the crystal it will undergo a rotation. This rotation will depend
upon whether the magnetic moments of the domain are up or down. If this
transmitted light is then passed through a properly set analyzer one should be able
to distinguish the two types of domains as a result of a difference in light intensity.

This Faraday effect method is possible because orthoferrites are transparent,

especially in the red spectrum. When viewed through a microscope the patterns
appear red since in the visible range only the red portion is transmitted.

3.b: Application of an External Magnetic Field

When an external magnetic field is applied, the domains that lie parallel to this
field will increase in size. This is accomplished by a narrowing and shortening of the
domains that are antiparallel to the external magnetic field. Draw a sketch of the
domain configuration at zero, intermediate, and high fields.

The great interest directed toward orthoferrites in the 70’s was due in part to the
fact that these isolated cylindrical domains can be manipulated to perform
memory, logic and transmission functions (see Scientific American, June 1971).
More recently, other materials such as yttrium iron garnet (YIG) have been found
to have better overall properties for this application. Although millions of dollars
were spent developing these “bubble” memories, they were soon replaced by
cheaper methods.

3.c: Writeup for First Afternoon

• Describe how the measurements were made and any problems that arose
in the measurement. What do you think caused these problems and how
do they contribute to the error in measurement? What would you suggest
to improve the measurement?
• Plot the curves. Give the values for the Curie temperature obtained from
both methods and estimate the uncertainty in these values, clearly
stating how you got these estimates.
• In the second experiment, the measured output voltage will usually rise
to a maximum at about -20°C. What do you think is the error in the
procedure of this experiment that causes this rise?
• Sketch the observations on the Orthoferrite, indicating clearly the
domain changes with increasing magnetic field.
° Why do domains magnetized parallel to the magnetic field get larger
as the field increases?
° What is the mechanism by which they grow?

Procedure for First Afternoon M-12

M-Magnetic Materials

° When only small regions remain which are not magnetized parallel to
the applied field, they tend to form a circular shape (i.e. A “bubble”).
° Why should they be circular?
° Why aren’t the domains circular when there is zero applied field?

4. Procedure for Second Afternoon

4.a: Familiarization.

Examine the circuit diagram shown below. Locate each component physically on
the lab bench. The oscilloscope across the 1MΩ resistor examines the form of the
output wave for distortion from a cosine curve. Read the introduction to understand
what other components in the circuit do.

4.b: Start-up
• Turn voltage supply to zero and turn it on.
• Turn on the BK Precision 2120B oscilloscope. Adjust “intensity” knob so
the screen doesn’t burn out. When the spot moves you may have to
increase the intensity but reduce it again for a stationary spot.
Source switch should be at position “X-Y ALT”. “X-Y” button IN.
Check that the CH1-X is fed from the one ohm resistor. [If later it is

Start-up M-13
M-Magnetic Materials

found that the B-H curve is backwards, reverse the connections from the
Check that the CH2-Y is fed from the .68 microfarad capacitor.
• Check the AVO multimeter is on AC (left knob), and on 100 mA scale for
the right knob, and is lying flat on the table.
• Attach the BK Precision 2520 Storage Oscilloscope to the 1M ohm
• Connect the computer to the X-Y common output on the storage scope.
• Connect X to the ‘+’ channel 1 and Y to the ‘+’ channel 2 on the computer
input box.
• Turn on computer select [Cancel] at password prompt. Run ‘DASTC
Graph Version Test’ from desktop. Open Setup File ‘MAGNETIC.INI’.

4.c: Observation of B-H Curve and Output Distortion


• Fe-3% Si oriented. Strip thickness 0.010 inches with rolling direction

shown by a red arrow.
° oriented steel cut parallel to rolling direction
° oriented steel cut perpendicular to rolling direction
• Fe-3% Si not oriented, often called random. Strip thickness 0.018 inches
with rolling direction shown by a blue arrow.
° random steel cut parallel to rolling direction
° random steel cut perpendicular to rolling direction
• 0.1% carbon steel strip thickness 0.028 inches with rolling direction
shown by a black arrow.
° carbon steel cut parallel to rolling direction

4.d: Experiments on Toroids

The experiments will be done on simulated toroids constructed of steel strips,

overlapped at the corners to form a square. The corners of the square must be
clamped if there is a gap there, to ensure a complete metallic circuit. Unless
otherwise stated, the same type of material is used in all strips of the toroid.

The standard procedure for each material will be:

a. set voltage supply at zero

b. select strips to be used and construct the toroid by adding strips, one layer
at a time with overlapping corners. Be careful not to bend the strips. Clamp

Procedure for Second Afternoon M-14

M-Magnetic Materials

corners if a large gap is present. One side of the toroid goes through the red
primary coil and the opposite side through the black secondary coil.
c. increase voltage and watch the B-H curve on the CRT
d. adjust vernier sensitivity of CRT so the maximum height of B-H curve is a
large deflection on the CRT.
e. note the primary current at which the BH curve first reaches near its
maximum height. You should have about ten points on the curve before
reaching this point, so divide this current by about ten to get convenient
increments to read from the meter. As you increase the current watch the
distortion in the output wave shown on the Heathkit oscilloscope. (Its
frequency vernier should be set near 60).
f. reduce the variac to zero. Increase the variac to give one increment of
current. Measure the peak to peak vertical deflection on the CRT and
convert it to mV. This value divided by the corrected cross-sectional area of
the metal in your toroid, represents the value of B as shown in the figure on
page 65. (An unknown proportionality constant is also included but it will be
the same for all our measurements and is not considered further). Measure
the peak to peak horizontal deflection on the CRT. This can be done most
conveniently after shorting out the vertical signal with the short across the
condenser. This value divided by two, represents the value of H on the
magnetization curve. (You could also use the measured primary current but
the distortion of the wave at higher currents causes a large error if this
meter reading is used to represent the current amplitude.)
g. examine the output wave on the Precision Oscilloscope. As a measure of its
distortion, measure the distances D and F as shown in the sketch. We will
arbitrarily use the value D-F as a measure of the output distortion. The
distance D is too small to measure at low currents but can be measured at
higher currents.
h. Plot the distortion curve to the computer data acquisition provided.(you can
take the output of the computer and load this into a spreadsheet program to
create the graph needed).
1. Select ‘Perform Data Acquisition’
2. Enter a filename 8 character name plus 3 character extension
3. Press ‘G’ key to place the system in graph mode.
4. Press ‘STORE’ on the storage scope. Wait for armed light.
5. Press ‘Plot 1’ on scope. Computer should be collecting data at
this point.

Experiments on Toroids M-15

M-Magnetic Materials

6. Once graph is completely transferred Press ‘Q’ key on

computer to quit acquisition.
7. Do this for each sample

a. increase the primary current by one increment and determine B, H and D/F
• repeat, doing about ten measurements in the rapidly rising part of the
B-H curve and three or four after it flattens at higher currents. Sketch
the form of the final B-H curve.
• plot the magnetization curve B vs. H and the distortion curve D/F versus
• in some applications you want a high magnetic flux, which depends on B,
at the lowest possible primary current, which is represented by H. The
optimum is represented by the maximum value of permeability defined
as µ = B / H . Plot the curve for µ = B / H as a function H.

NOTE: Because of the large number of graphs involved, remember to number each
datafile using a 8-character name and 3-character extension (you may wish to
include the group letter in the name e.g. magA01.TXT, for magnetic experiment
group A test 01). To print the data file load it into a spreadsheet program (the data
file is a TAB delimited ASCII file) you can easily sort the output by the channel
numbers then transpose the Channel 1 and 2 beside each other for the creation of
an X-Y graph.

4.e: Toroids to be Measured

Toroid Strips
• Oriented 3% Si steel with strips cut parallel to the rolling direction. Use
six strips on each side of the toroid, but in calculating the area use that of
5.2 strips. [To save time, the number of strips is lower than used
commercially. A preliminary experiment indicated this correction should
be applied. ]

Procedure for Second Afternoon M-16

M-Magnetic Materials

• Oriented 3% Si steel with strips cut perpendicular to the rolling

direction. Use six strips on each side of the toroid, but in calculating the
area use that of 4.4 strips.
• Non-oriented (random) 3% Si steel with strips cut parallel to the rolling
direction. Use six strips on each side of the toroid but in calculating the
area use that of 5.2 strips.
• Nonoriented (random) 3% silicon steel with strips cut perpendicular to
the rolling direction. Use six strips on each side of the toroid, but in
calculating the area use that of 4.4 strips.

As discussed in the introduction, in C type cores cut from an oriented sheet, one side
must be perpendicular to the rolling direction. Simulate this with a toroid of six
sheets per side in which three sides use oriented 3% Si cut parallel to the rolling
direction, and the fourth side uses strips of oriented 3% Si cut perpendicular to the
rolling direction. The effective area has not been checked so estimate it as that of
five strips. The fourth side should not be in either coil. Leave this toroid for the next

To overcome part of the effect of this one side with transverse orientation, it is
commonly made up to 20% wider. Check how this affects the magnetization curve
by adding one strip of the same type to this fourth side. It will now have seven
strips. The effective area is again an estimate; leave it at five strips as in case E.

• 0.1% carbon steel with strips cut parallel to the rolling direction. Use five
strips per side but in calculating the area use that of three strips.

4.f: Writeup for Second Afternoon

a. Draw the magnetization curves B vs. H, the distortion curves D / F vs. H
and the permeability curves µ vs. H as requested in the procedure.
b. Comment on your experimental curves in terms of the materials chemical
composition, crystallographic texture and domain movement.
c. Comment on your experimental curves in terms of choosing these materials
for C and E type transformer cores.
d. The nonoriented 3% Si steel is sometimes called “random” to distinguish it
from the oriented steel. Comment on the degree of randomness of the
orientation of its grains, from your experimental results.
e. The penetration of an electromagnetic wave into a material is to a nominal
depth of δ = [2 /( ωµσ)]1/ 2 , where is the angular frequency, µ the magnetic
permeability, and σ the electrical conductivity. For the oriented silicon steel
this is about 0.01 inches. How does this relate to the size of the samples you
were using?

Writeup for Second Afternoon M-17

M-Magnetic Materials

f. The standard procedure to demagnetize a piece of steel is to put it in a coil,

increase the AC current and then decrease it to zero. The steel will then be
demagnetized, i.e. it will not act as a magnet to attract other pieces of steel.
What would happen if a DC current was used in the coil? Explain in terms
of the effect of AC on magnetic domains, why AC is more effective than DC
in demagnetizing a sample.

5. Reference

Magnetic Materials, Tebble and Craik, QC761 T44.

Reference M-18
Background Reading:

Background Reading
1. Thermocouples

All temperature measuring devices record some physical manifestation of the

increased energy of the molecules atoms in a medium, with an increase in
temperature. That is, at a higher temperature, the molecules atoms are oscillating
with greater amplitudes (thermal motion). The most useful changes include:

a. Change in physical state

b. Change in chemical state
c. Change in dimensions
d. Change in electrical properties
e. Change in radiation properties

Although none of these can give an absolute measurement of temperature, they are
calibrated to some arbitrarily chosen standard. Thermocouples measure a change
in electrical properties, specifically the change in free electron density with
temperature. If a conductor is placed in a temperature gradient, the electrons at the
hot end have a higher velocity, causing a net drift to the cold end. This builds up a
negative charge at the cold end that stops the drift. Thus, the conductor produces a
small voltage (emf) between its hot and cold ends; this emf depends upon two
independent effects:
1. the Peltier effect, which is a phenomenon whereby heat is
liberated or absorbed at a junction when current passes from
one metal to another. Or conversely, when heat is absorbed at
a junction, current is caused to flow (a function of the contact
emf between dissimilar metals), and
2. the Thomson effect, which is the emf produced by
temperature differences in a single conductor.

Of these two effects, the Peltier effect is by far the most dominant, and the Thomson
effect can usually be neglected. As a result all metals are different. If two dissimilar
metal wires are connected together, and their junction is heated, a resultant emf is
produced which is the difference between their individual emf's (like two batteries
in series opposition). The resulting voltage between their cold ends is roughly

II-Background Reading

proportional to the temperature difference between their hot and cold ends. Thus,
by keeping their cold ends at a standard temperature (often 0C), the temperature of
the hot end can be measured.

The graph above shows this schematically, but the relationship between
temperature and measured emf is not linear, and accurate expressions that relate
junction temperatures to measured emf are usually intractable. This requires that
the thermocouple be calibrated over a complete range of temperatures. As a result,
tables are always used, and are based on the cold junction being at 0°C. If the
temperature of the cold junctions change, then the output emf will change. To keep
it constant, the cold ends are usually kept at a constant temperature of 0°C, and
copper wire connects this cold junction to the millivoltmeter. Often, the cold
junction is connected directly to the millivoltmeter, and will thus be at the ambient
temperature; in this case, the emf of the thermocouple will be:

emf measured = [emf of hot junction] - [emf of cold junction]

where the emf's on the right hand side of the equation are table values for that
temperature. This result is also indicated on the graph. Therefore, it can be seen
that temperature measurement is based almost entirely on empirical calibrations
and the application of so-called thermoelectric "laws", which experience has shown
to hold.

Thermocouples II-2
II-Background Reading

1.a: Laws of Thermocouple Behavior

The thermal emf of a thermocouple with junctions at T1 and
T2 is totally unaffected by the temperature elsewhere in the
circuit, if the two metals used are homogeneous.

Results: the lead wires connecting the two junctions may be safely exposed to
an unknown and/or varying temperature environment without affecting the
voltage produced.

If a third homogeneous metal C is inserted into either metal A
or metal B, and as long as the two new thermojunctions are at
like temperatures, the net emf is unchanged irrespective of
the temperature of C away from the junctions.

Results: it is possible to insert a voltage measuring device into the circuit to

Laws of Thermocouple Behavior II-3

II-Background Reading

measure the emf (i.e. metal C represents the internal circuit between the
binding posts of the millivoltmeter or potentiometer).

If a metal C is inserted between A and B at one of the
junctions, the temperature of C at locations other than the AC
and BC junctions is immaterial. As long as the junctions AC
and BC are at T1, the net emf is the same as if C were not

Results: same as rule (2), and it also shows that thermocouple junctions may be
soldered or brazed (thereby introducing a third metal) without changing the

If the thermal emf of metals A and C is EAC, and of metals B
and C is ECB, then the thermal emf of metals A and B is


Results: all possible pairs of metals need not be calibrated, since the individual

Thermocouples II-4
II-Background Reading

metals can each be paired with one standard (usually Pt), all other
combinations can be calculated.

If a thermocouple produces an emf E1 when its junctions are
at T1 and T2, and an emf E2 when its junctions are at T2 and
T3, it will produce an emf E1+E2 when its junctions are at T1
and T3

Note: the temperature of at least one thermojunction must be known by

independent means, usually 0°C, fixed electronically or by an ice bath.

1.b: Common Thermocouples

The most common thermocouples are the alloys chromel with alumel, alloy
platinum13% rhodium with pure platinum, copper with alloy constantan, and iron
with constantan. The important properties of these common thermocouples are
shown in the following table (see next page). Each of these pairs exhibits a
combination of properties that suit it to a particular class of application.

Type Copper/Constantan Iron/Constantan

Composition, 90Ni 10Cr/ 55Cu

100Cu/ 60Cu 40Ni 100Fe/ 60Cu 40Ni
percent 45Ni

*Range of
application, -200 to +300 -200 to +1100 0 to +1100

1.75 49 10 49 70 49

Common Thermocouples II-5

II-Background Reading

coefficient of
0.0039 0.00001 0.005 0.00001 0.00035 0.0002
per oC

temperature, 1085 1190 1535 1190 1400 1190

100oC 5.28 mv
200 10.78 100oC 6.3 mv
millivolts; 100oC 4.24 mv
400 21.82 200 13.3
reference 200 9.06
600 33.16 400 28.5
junction at 300 14.42
800 45.48 600 44.3
1000 58.16

Subject to oxidation
and alteration
above 400oC due Oxidizing and
Cu, above 600oC Reducing
due constantan atmosphere have
wire. Ni-plating of little effect on Chromel attacked
Cu tube gives accuracy. Best used by sulfurous
Influence of protection in in dry atmosphere. atmosphere.
temperature acid-containing gas. Resistance to Resistance to
and gas Contamination of oxidation good to oxidation good.
temperature Cu affects 400oC. Resistance Resistance to
calibration greatly. to reducing reducing
Resistance to oxid. atmosphere good. atmosphere.
atm. good. Protect from
Resistance to oxygen, moisture,
reducing atm. good. sulfur.
Requires protection
from acid fumes.

Low temperature,
Low temperature,
industrial. Internal
industrial. Steel
combustion engine.
Particular annealing, boiler
Used as a tube
applications flues, tube stills.
element for
Used in reducing or
measurements in
neutral atmosphere.
steam line.

Thermocouples II-6
II-Background Reading

Platinum/ Platinum/
Type Chromel/ alumel platinum rhodium platinum rhodium
10 13

Composition, 190Ni 10Cr/ 94Ni

Pt/ 90Pt 10Rh Pt/ 87Pt 13Rh i
percent 2Al 3Mn 1Si
*Range of
application, -200 to +1200 0 to 1450 0 to +1450

70 29.4 10 21 10 21

coefficient of
0.00035 0.000125 0.0030 0.0018 0.0030 0.0017
per oC
temperature, 1400 1430 1755 1700 1755 1700

0.643 0.646 mv
100oC 100oC
100oC 4.1 mv mv
200 200
200 8.13 1.436 1.464
emf, 400 400
400 16.39 3.251 3.398
millivolts; 600 600
600 24.90 5.222 5.561
reference 800 800
800 33.31 7.330 7.927
junction at 1000 1000
1000 41.31 9.569 10.470
0oC 1200 1200
1200 48.85 11.924 13.181
1400 1400
1400 55.81 14.321 15.940
1600 1600
16.674 18.680

Resistance to
atmosphere very Resistance to oxidizing atmosphere very
Influence of good. Resistance to good. Resistance to reducing atmosphere
temperature reducing poor. Susceptible to chemical alteration by
and gas atmosphere poor. As, Si, P vapor in reducing gas (CO2, H2,
temperature Affected by sulfur, H2S, SO2). Pt corrodes easily above 1000o.
reducing or Used in gas-tight protecting tube.
sulfurous gas, SO2
and H2S.

Common Thermocouples II-7

II-Background Reading

Used in oxidizing
atmosphere. International Similar to Pt/ PtRh
Industrial. Ceramic Standard 630 to 10, but has higher
kilns, tube stills, 1065oC emf.
electric furnaces.

From reference (2) (see p. 17)

1.c: Accuracy

The accuracy of factory supplied thermocouple wire relies strongly on the

manufacturers quality control procedures (since the calibration tables give average
values). If higher accuracy is required, each individual thermocouple must be
calibrated for the temperature range under investigation [see Thermocouple
Calibration, Inst. Control Systems, NBS Listings, p.1663, Sept. 1961].

1.d: Other Information

Thermocouples can be connected in series or parallel to achieve some useful


Series Connection:

Connecting the thermocouple wires as shown, increases the sensitivity (i.e. for n
thermocouples, the output is n times the output of a single thermocouple), and is
commonly referred to as a thermopile.

Parallel Connection:

Connecting the thermocouples as shown, results in an output voltage

Thermocouples II-8
II-Background Reading

corresponding to the average of temperatures T1, T2, and T3, providing that the
thermocouple response is linear over the temperatures considered.

1.e: References

Ernest O. Doebelin,"Measurement Systems Application and Design" McGrawHill

Book Co., NY, 1975.

Nathan H. Cook and Ernest Rabinowicz, "Physical Measurement and Analysis",

Addison Wesley Publishing Co. Inc., Reading, Mass., 1963.


All Values in (mV)
oC 0 1 2 3 4 5 6 7 8 9
0 0.000 0.039 0.079 0.119 0.158 0.198 0.238 0.277 0.317 0.357
10 0.397 0.437 0.477 0.517 0.557 0.597 0.637 0.677 0.718 0.758
20 0.798 0.838 0.879 0.919 0.960 1.000 1.041 1.081 1.122 1.163
30 1.203 1.244 1.285 1.325 1.366 1.407 1.448 1.489 1.530 1.571
40 1.612 1.653 1.694 1.735 1.776 1.817 1.858 1.899 1.941 1.982
50 2.023 2.064 2.106 2.147 2.188 2.230 2.271 2.312 2.354 2.395
60 2.436 2.478 2.519 2.561 2.602 2.644 2.685 2.727 2.768 2.810
70 2.851 2.893 2.934 2.976 3.017 3.059 3.100 3.142 3.184 3.225
80 3.267 3.308 3.350 3.391 3.433 3.474 3.516 3.557 3.599 3.640
90 3.682 3.723 3.765 3.806 3.848 3.889 3.931 3.972 4.013 4.055
100 4.096 4.138 4.179 4.220 4.262 4.303 4.344 4.385 4.427 4.468
110 4.509 4.550 4.591 4.633 4.674 4.715 4.756 4.797 4.838 4.879
120 4.920 4.961 5.002 5.043 5.084 5.124 5.165 5.206 5.247 5.288
130 5.328 5.369 5.410 5.450 5.491 5.532 5.572 5.613 5.653 5.694
140 5.735 5.775 5.815 5.856 5.896 5.937 5.977 6.017 6.058 6.098
150 6.138 6.179 6.219 6.259 6.299 6.339 6.380 6.420 6.460 6.500
160 6.540 6.58 6.620 6.660 6.701 6.741 6.781 6.821 6.861 6.901
170 6.941 6.981 7.021 7.060 7.100 7.140 7.180 7.220 7.260 7.300
180 7.340 7.380 7.420 7.460 7.500 7.540 7.579 7.619 7.659 7.699
190 7.739 7.779 7.819 7.859 7.899 7.939 7.979 8.019 8.059 8.099
200 8.138 8.178 8.218 8.258 8.298 8.338 8.378 8.418 8.458 8.499
210 8.539 8.579 8.619 8.659 8.699 8.739 8.779 8.819 8.860 8.900
220 8.940 8.980 9.020 9.061 9.101 9.141 9.181 9.222 9.262 9.302
230 9.343 9.383 9.423 9.464 9.504 9.545 9.585 9.626 9.666 9.707
240 9.747 9.788 9.828 9.869 9.909 9.950 9.991 10.031 10.072 10.113
250 10.153 10.194 10.235 10.276 10.316 10.357 10.398 10.439 10.480 10.520
260 10.561 10.602 10.643 10.684 10.725 10.766 10.807 10.848 10.889 10.930
270 10.971 11.012 11.053 11.094 11.135 11.176 11.217 11.259 11.300 11.341
280 11.382 11.423 11.465 11.506 11.547 11.588 11.630 11.671 11.712 11.753
290 11.795 11.836 11.877 11.919 11.960 12.001 12.043 12.084 12.126 12.167
300 12.209 12.250 12.291 12.333 12.374 12.416 12.457 12.499 12.540 12.582
310 12.624 12.665 12.707 12.748 12.790 12.831 12.873 12.915 12.956 12.998

References II-9
II-Background Reading

oC 0 1 2 3 4 5 6 7 8 9
320 13.040 13.081 13.123 13.165 13.206 13.248 13.290 13.331 13.373 13.415
330 13.457 13.498 13.540 13.582 13.624 13.665 13.707 13.749 13.791 13.833
340 13.874 13.916 13.958 14.000 14.042 14.084 14.126 14.167 14.209 14.251
350 14.293 14.335 14.377 14.419 14.461 14.503 14.545 14.567 14.629 14.671
360 14.713 14.755 14.797 14.839 14.881 14.923 14.985 15.007 15.040 15.091
370 15.133 15.175 15.217 15.259 15.301 15.343 15.385 15.427 15.469 15.511
380 15.554 15.596 15.638 15.680 15.722 15.764 15.808 15.349 15.891 15.933
390 15.975 16.017 16.059 16.102 16.144 16.186 16.228 16.270 16.313 16.355
400 16.397 16.439 16.482 16.524 16.566 16.608 16.651 16.693 16.735 16.778
410 16.820 16.862 16.904 16.947 16.989 17.031 17.074 17.116 17.158 17.201
420 17.243 17.285 17.328 17.370 17.413 17.455 17.497 17.540 17.582 17.624
430 17.667 17.709 17.752 17.794 17.837 17.879 17.921 17.964 18.006 18.049
440 18.091 18.134 18.176 18.218 18.261 18.303 18.346 18.388 18.431 18.473
450 18.516 18.558 18.601 18.643 18.686 18.728 18.771 18.813 18.856 18.898
460 16.941 18.983 19.026 19.068 19.111 19.154 19.196 19.239 19.281 19.324
470 19.366 19.409 19.451 19.494 19.537 19.579 19.622 19.664 19.707 19.750
480 19.792 19.835 19.877 19.920 19.962 20.005 20.048 20.090 20.133 20.175
490 20.218 20.261 20.303 20.346 20.389 20.431 20.474 20.516 20.559 20.602
500 20.644 20.687 20.730 20.772 20.815 20.857 20.900 20.943 20.985 21.028
510 21.071 21.113 21.156 21.199 21.241 21.284 21.326 21.369 21.412 21.454
520 21.497 21.540 21.582 21.625 21.668 21.710 21.753 21.796 21.838 21.881
530 21.924 21.966 22.009 22.052 22.094 22.137 22.179 22.222 22.265 22.307
540 22.350 22.393 22.435 22.478 22.521 22.563 22.606 22.649 22.691 22.734
550 22.776 22.819 22.862 22.904 22.947 22.990 23.032 23.075 23.117 23.160
560 23.203 23.245 23.288 23.331 23.373 23.416 23.458 23.501 23.544 23.586
570 23.629 23.671 23.714 23.757 23.799 23.842 23.884 23.927 23.970 24.012
580 24.055 24.097 24.140 24.182 24.225 24.267 24.310 24.353 24.395 24.438
590 24.480 24.523 24.565 24.608 24.650 24.693 24.735 24.778 24.820 24.863
600 24.905 24.948 24.990 25.033 25.075 25.118 25.160 25.203 25.245 25.288
610 25.330 25.373 25.415 25.458 25.500 25.543 25.585 25.627 25.670 25.712
620 25.755 25.797 25.840 25.882 25.924 25.967 26.009 26.052 26.094 26.136
630 26.179 26.221 26.263 26.306 26.348 26.390 26.433 26.475 26.517 26.560
640 26.602 26.644 26.687 26.729 26.771 26.814 26.856 26.898 26.940 26.983
650 27.025 27.067 27.109 27.152 27.194 27.236 27.278 27.320 27.363 27.405
660 27.447 27.489 27.531 27.574 27.616 27.658 27.700 27.742 27.784 27.826
670 27.869 27.911 27.953 27.995 28.037 28.079 28.121 28.163 28.205 28.247
680 28.269 28.332 28.374 28.416 28.458 28.500 28.542 28.584 28.626 28.668
690 28.710 28.752 28.794 28.835 28.877 28.919 28.961 29.003 29.045 29.087
700 29.129 29.171 29.213 29.255 29.297 29.338 29.380 29.422 29.464 29.506
710 29.548 29.589 29.631 29.573 29.715 29.757 29.798 29.840 29.882 29.924
720 29.965 30.007 30.049 30.090 30.132 30.174 30.216 30.257 30.299 30.341
730 30.382 30.424 30.466 30.507 30.549 30.590 30.632 30.674 30.715 30.757
740 30.796 30.840 30.881 30.923 30.964 31.006 31.047 31.089 31.130 31.172
750 31.213 31.255 31.296 31.338 31.379 31.421 31.462 31.504 31.545 31.586
760 31.628 31.669 31.710 31.752 31.793 31.834 31.876 31.917 31.958 32.000
770 32.041 32.062 32.124 32.165 32.206 32.247 32.289 32.330 32.371 32.412
780 32.453 32.495 32.536 32.577 32.618 32.659 32.700 32.742 32.783 32.824
790 32.865 32.906 32.947 32.988 33.029 33.070 33.111 33.152 33.193 33.234
800 33.275 33.316 33.357 33.398 33.439 33.480 33.521 33.562 33.603 33.644


Thermocouples II-10