Documenti di Didattica
Documenti di Professioni
Documenti di Cultura
Objectives . . . . . . . . . . . . . . . . . . . . . . . A-1
Introduction . . . . . . . . . . . . . . . . . . . . . A-1
Writeup . . . . . . . . . . . . . . . . . . . . . . . . . . A-11
Objectives . . . . . . . . . . . . . . . . . . . . . . . B-1
Introduction. . . . . . . . . . . . . . . . . . . . . . B-1
Procedure . . . . . . . . . . . . . . . . . . . . . . . . . . B-4
Writeup . . . . . . . . . . . . . . . . . . . . . . . . . . . B-5
Procedure . . . . . . . . . . . . . . . . . . . . . . . . . . B-5
Writeup . . . . . . . . . . . . . . . . . . . . . . . . . . . B-5
Procedure . . . . . . . . . . . . . . . . . . . . . . . . . . B-6
I-1
I-
Writeup . . . . . . . . . . . . . . . . . . . . . . . . . . . B-7
Procedure . . . . . . . . . . . . . . . . . . . . . . . . . . B-8
Writeup . . . . . . . . . . . . . . . . . . . . . . . . . . . B-9
Procedure . . . . . . . . . . . . . . . . . . . . . . . . . B-10
Writeup . . . . . . . . . . . . . . . . . . . . . . . . . . B-11
Objectives . . . . . . . . . . . . . . . . . . . . . . C-1
Procedure . . . . . . . . . . . . . . . . . . . . . . . . . . C-6
Writeup . . . . . . . . . . . . . . . . . . . . . . . . . . C-9
Objectives . . . . . . . . . . . . . . . . . . . . . . . D-1
I-2
I-
Objectives . . . . . . . . . . . . . . . . . . . . . . E-1
Introduction . . . . . . . . . . . . . . . . . . . . . E-2
F-Metallographic Observation
Objectives . . . . . . . . . . . . . . . . . . . . . . . F-1
Introduction . . . . . . . . . . . . . . . . . . . . . . F-1
Write up . . . . . . . . . . . . . . . . . . . . . . . . . . F-2
Objectives . . . . . . . . . . . . . . . . . . . . . . G-1
Introduction . . . . . . . . . . . . . . . . . . . . . G-1
I-3
I-
Procedure . . . . . . . . . . . . . . . . . . . . . . G-5
Program . . . . . . . . . . . . . . . . . . . . . . . . . . G-5
Plots . . . . . . . . . . . . . . . . . . . . . . . . . . . . G-6
H-Electrical Properties
Objectives . . . . . . . . . . . . . . . . . . . . . . . H-1
Introduction . . . . . . . . . . . . . . . . . . . . H-1
I-4
I-
Objectives . . . . . . . . . . . . . . . . . . . . . . . I-1
Introduction . . . . . . . . . . . . . . . . . . . . . . I-1
J-Mechanical Properties
Objectives . . . . . . . . . . . . . . . . . . . . . . . J-1
Introduction . . . . . . . . . . . . . . . . . . . . . J-1
Microstructures. . . . . . . . . . . . . . . . . . . . . . . J-9
I-5
I-
Write up . . . . . . . . . . . . . . . . . . . . . . . J-11
Objectives . . . . . . . . . . . . . . . . . . . . . . K-1
Introduction . . . . . . . . . . . . . . . . . . . . . K-1
Writeup . . . . . . . . . . . . . . . . . . . . . . . . K-8
L-Corrosion
Objective . . . . . . . . . . . . . . . . . . . . . . . L-1
Introduction . . . . . . . . . . . . . . . . . . . . . L-1
I-6
I-
Writeup . . . . . . . . . . . . . . . . . . . . . . . L-12
M-Magnetic Materials
Objectives. . . . . . . . . . . . . . . . . . . . . . . M-1
Introduction . . . . . . . . . . . . . . . . . . . . . M-1
Familiarization. . . . . . . . . . . . . . . . . . . . . . M-13
Start-up . . . . . . . . . . . . . . . . . . . . . . . . . M-13
I-7
I-
Reference . . . . . . . . . . . . . . . . . . . . . . M-18
II-Background Reading
Thermocouples . . . . . . . . . . . . . . . . . . . . II-1
Accuracy . . . . . . . . . . . . . . . . . . . . . . . . . . II-8
References . . . . . . . . . . . . . . . . . . . . . . . . . II-9
I-8
Materials 2H03 on-line Laboratory Manual
Updated: 11 May 2000
Experiment A
Differential Thermal Analysis
1.
Objectives
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.
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
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
transformation. That is, the area under the peak gives a measure of (dH)Nm, after
the appropriate correction for amplification.
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:
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.
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
Fig.1
Fig.2
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).
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
experiment.
To assist your appreciation for the function and operation of thermocouples, see
the Background Reading.
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
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
"standard".
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.
-6.25 to 25 m
0 K:Chromel/Al 0 0.000000 0
...
° 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
G.
° 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
graph.
° Note that the correct units must be used when data is put into the
equations
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
halloysite.
At 750°C, shut off the furnace power. Measure the cooling rate in the region of the
silica peak (at about 570°C).
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.
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.
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
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
Writeup A-11
A-Differential Thermal Analysis
Experiment B
Temperature Measurement and
Control
1. Objectives
2. Introduction
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-1
B-Temperature Measurement and Control
The following table summarizes the temperature range and sensitivity of some of
these methods.
-40 to 70
glass-alcohol 0.5
thermocouples
optical
above 700 about 10
pyrometer
infrared
-60 to 3000 2 to 30
pyrometer
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
time.
This part should be done simultaneously with Part 2A, as the cone
observation is very simple.
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).
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
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.
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.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
temperature.
• Put the thermocouple in the furnace to achieve a reading of approx.
23mV.
• 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
bath.
3. at the bottom of the ice bath.
• 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.
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.
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?
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.
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.
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
value.
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
7.c: Writeup
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
error.
Writeup B-11
Materials 2H03 on-line Laboratory Manual
Updated: 11 May 2000
Experiment C
Measurement of Force and Strain
Using Gauges
1. Objectives
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
position.
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-1
C-Measurement of Force and Strain Using Gauges
ρL
R= ...(1)
A
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
∆R ∆ρ ∆L
= + (1 + 2v )
R ρ L
∆R ∆L ( ∆ρρ )
( )( ) = 1 + 2v + ≡ K ...(3)
R L ( ∆LL )
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)
R L
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.
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
appropriate direction, with the parallel wires in line with the strain to be measured.
Typical types of strain gauges are below:
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
reads zero. This requires that I1R1 = I 2R2 and I1R4 = I 2R3. Therefore, we have at
balance
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
1
If we vary two resistors in the bridge, say R1 and R2, then ignoring the nonlinear
term:
∆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.
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
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).
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.
Procedure C-7
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.
Writeup C-9
Materials 2H03 on-line Laboratory Manual
Updated: 17 May 2000
Experiment D
Measurement of Length and
Displacement
1. Objectives
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.
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
microscope.
D-1
D-Measurement of Length and Displacement
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.
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
assist.
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".
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.
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
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
Calibration
• 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
accuracy
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
meter.
° 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.
Experiment E
Chemical Analysis by Reaction
Product
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:
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
methods.
2. Objectives
E-1
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
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:
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.
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.
4. Experimental Procedure
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
analysis.
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
2. Introduction
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-1
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
description.
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
students.
3.a: Write up
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?
Experiment G
Datalogging of Quenching Curves
1. Objectives
2. Introduction
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
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
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)
Ah
m=
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.
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.
Within the temperature range of this experiment the temperature, Ti, can be
related to a voltage, Vi, by:
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.
Introduction G-4
G-Datalogging of Quenching Curves
• Hot plate
• Alcohol thermometer
• Liquid nitrogen dewar
• Micrometer
3. Procedure
3.b: Program
A title screen shows up. Press ENTER key to browse the data acquisition
program. Then the Temperature Main Screen will be displayed with five
buttons: SETUP, CONFIGURATION, ACQUISITION, QUIT and SETUP
FILE ? Type 2H3.INI at the spaced provided for SETUP FILE and click
ACQUISITION button.
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:
Program G-5
G-Datalogging of Quenching Curves
AQ: aquaquench
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 ;
NI.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.
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
graphs.
For temperatures Ti-1, Ti, Ti+1 at times ti-1, ti, ti+1, show how to calculate
h(Ti).
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
2. Introduction
EL E
jA = or j = RA which gives
R (L)
E
j≡ ≡ σE
ρ
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:
VA
ρ= .. (2)
JL
j = nvq ...(3)
where n is the number of free electrons per m3, and q= e is the charge per electron.
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.
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.
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).
the sketch, then the resistivity ρ of the sample materials can be determined from
resistance measurements using these as current and potential connections.
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
wjB
V Hall = = dRH jB ...(6)
nq
where w = width of sample in the direction of the VHall, and where the Hall
coefficient is
1
RH =
nq
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.
It shows that:
VH d
u= ) .... (7)
BρJ
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.)
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
uses.
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
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.
Varistors
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.
Introduction H-8
H-Electrical Properties
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.
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 SAMPLE.
Examine the sample board A. Note that the copper strips underneath the board
carry the current between terminals at each end of the board.
° 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
instruments.
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
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
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).
Determine the resistivity of the irregular Ge sample (sample D), using the following
procedure:
(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.
Calculate
V 14
R14 ,32 =
J 32
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.
(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
them.
(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
this?
(Note: You will need another alcohol/dry ice bath for the first experiment.)
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.
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.
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.
Examine the EPROM in the optical microscope. Measure the width of a typical
transistor and record for your lab write up!
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.
R12 = V12/J12
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
Experiment I
Mass Transport by Diffusion
1. Objectives
2. Introduction
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
atoms
dc
J = −D( ) .... (1)
dx
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
rate.
Thus, we expect
−Q
D = D 0 exp( ) .... (2)
RT
I-1
I-Mass Transport by Diffusion
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
form
1
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.
Putting D from equation (2) into equation (3), squaring both sides and re-arranging,
gives:
−Q
X 2 D 0 t = exp( ) ... (4)
kT
I-3
I-Mass Transport by Diffusion
Q
ln( X 2 )ln( D 0 t ) = − .... (5)
kT
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
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.
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.
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.
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.
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
optical microscope. With this information, you should be able to explain your
microstructure.
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.
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.
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:
II. Introduction
(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
curve:
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:
k
σ = σ0 + 1
d2
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
structure.
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.
B 12
σc = ( ) ....(1)
C
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.
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:
P
VHN = 172
.
d2
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.
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
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
follows:
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
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
n
Therefore, the index number is related to the grain diameter by the following
equation:
L = C / N.M
Comparing this result with the one obtained for the index number method, we see
that:
d=1.3L
The following table gives the relations between the various methods:
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
Introduction J-8
J-Mechanical Properties
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.
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.
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".
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.
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.
Each student should do one of the tests and share the results with the other Team
members.
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
appreciably!]
• a piece of a glass microscope slide which you have lightly abraded with
sandpaper.
• a new glass slide etched 5 min in 5% HF. Do not scratch the surface after
etching.
• 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
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
relationship.
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
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.
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
II. Introduction
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.
K-1
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.
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:
ρw = density of water
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
surfaces).
Introduction K-2
K-Sintering and Density
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
Ww
ρw = .... (2)
Vw
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 )
where
Wpdr+w = weight of powder plus weight of water when both are in pycnometer
together.
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-3
K-Sintering and Density
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 )
ρ=
(W sat − W sus )
The first afternoon is devoted to the preparation of the sample, initial dimensional
measurements, and 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).
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.
[ 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.]
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
not?
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.
(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.
(ii) Air bubbles trapped on the sample or on the support wire will alter its weight in
water.
Remove the sample from the water, and allow the excess to dry.
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
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
1500°C:
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:
Which sample has the highest degree of porosity? The lowest? Why?
V. Writeup
Answer all the questions and include other items specified in the procedure.
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.
Experiment L
Corrosion
1. Objective
• To examine and understand the basic electrode processes that control the
corrosion rate of a metal.
2. Introduction
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)
M+ + e- → M ....(2)
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.
H+ + e - → H ....(3)
H + H → H2....(4)
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
L-Corrosion
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.
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
reaction
M2 → M2++ e-.
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
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.
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.
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
i
V = V 0 + η = V 0 + βln( )
i0
Introduction L-4
L-Corrosion
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.
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.
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.
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,
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.
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
solution.
Pour some of the fluid gel into a petri dish and drop into it, without disturbance,
Samples
• A short piece of the steel wire.
• 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.
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.
1.
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
polarity.
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?
(weightofzincdissolved ) it
=
(GAW Zn ) nF
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?
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:
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.
Writeup L-12
M-Magnetic Materials
Experiment M
Magnetic Materials
1. Objectives
2. Introduction
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
Co.
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.
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
The sketches on the right are schematic representations of the domain structure at
each of labeled points on the curve. The following processes occur.
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,
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.
The primary coil with N turns, radius r metres, and current I amps, produces an
alternating magnetic field of amplitude
NI
H= ampere − turns − per − metre
r
Introduction M-4
M-Magnetic Materials
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.
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.
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
wave.
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
dφ
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,
dB
VS = NS A ,
dt
NS A
B= ∫ I S dt ...(1)
ZS
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
N AC
B = s V c ...(2)
Zs
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
calibration.
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
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.
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.
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.
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 !
nearest neighbours. The figure shows the direction of the magnetic moments on the
Fe3+ ions.
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.
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.
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.
° 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.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
resistor.]
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
resistor.
• 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’.
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
(.TXT)
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.
a. increase the primary current by one increment and determine B, H and D/F
again.
• 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
H.
• 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.
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. ]
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
experiment.
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.
5. Reference
Reference M-18
Background Reading:
Background Reading
1. Thermocouples
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
1
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:
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.
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.
2.
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.
measure the emf (i.e. metal C represents the internal circuit between the
binding posts of the millivoltmeter or potentiometer).
3.
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
there.
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
readings.
4.
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
EAC+ECB.
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.
5.
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
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.
Chromel/Constanta
Type Copper/Constantan Iron/Constantan
n
*Range of
application, -200 to +300 -200 to +1100 0 to +1100
oC
Resistivity,
1.75 49 10 49 70 49
micro-ohm-cm
Temperature
coefficient of
0.0039 0.00001 0.005 0.00001 0.00035 0.0002
resistivity,
per oC
Melting
temperature, 1085 1190 1535 1190 1400 1190
oC
100oC 5.28 mv
emf,
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
0oC
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
Resistivity,
70 29.4 10 21 10 21
micro-ohm-cm
Temperature
coefficient of
0.00035 0.000125 0.0030 0.0018 0.0030 0.0017
resistivity,
per oC
Melting
temperature, 1400 1430 1755 1700 1755 1700
oC
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
oxidizing
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.
Used in oxidizing
atmosphere. International Similar to Pt/ PtRh
Particular
Industrial. Ceramic Standard 630 to 10, but has higher
applications
kilns, tube stills, 1065oC emf.
electric furnaces.
1.c: Accuracy
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:
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
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
THE END
Thermocouples II-10