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CoIIege of Engineering

Decarburization in 1095 SteeI




Report Irom a laboratory experiment conducted on April 12, 2011





Group Name: Tow

April 22, 2011
MATE 370
ecarburization
Team Tow
April 2011
MatE 370

College oI Engineering




i
Abstract:
UnIavorable reduction in surIace hardness oI heat-treated steels caused by
decarburization is diIIicult to quantiIy and preventative process adjustments can subsequently be
ineIIective. QuantiIying decarburization using the interstitial-diIIusion model could prove useIul
Ior implementing countermeasures within heat treatment. ecarburization depths oI heat
treatments varying time and temperature were measured to determine the eIIective activation
energy oI carbon diIIusion in -iron. The calculated diIIusion rates Iollowed expected trends and
yielded an activation energy value oI 84.3 kJ/mol, however depth measurement sensitivity
precluded more accurate results.
ecarburization
Team Tow
April 2011
MatE 370

College oI Engineering




ii
Table oI Contents
Abstract: ...................................................................................................................................... i
1. Introduction and Background .............................................................................................. 1
2. Procedure ............................................................................................................................ 1
3. ata .................................................................................................................................... 1
4. Analysis oI ata .................................................................................................................. 4
5. iscussion oI Results .......................................................................................................... 5
6. Conclusions......................................................................................................................... 5
ecarburization
Team Tow
April 2011
MatE 370

College oI Engineering




1
1. 3troductio3 a3d Backgrou3d
$teel is a versatile alloy that has varying microstructures with diIIering heat treatments and
thus can achieve greatly diIIerent mechanical properties. uring these heat treatments diIIusion
causes atomic rearrangement, leading to microstructural changes. In this application, diIIusion is
deIined as the movement oI carbon atoms within the iron matrix across a concentration gradient.
There are many types oI diIIusion applications Ior steel, such as carburization- a heat treatment
process oIten used to increase the surIace hardness oI steel components aIter casting or Iorging.
This process is perIormed by establishing a concentration gradient between a carbon-rich
environment and the surIace oI the steel sample. When heated between 900-950C it is
energetically and kinetically Iavorable Ior the atmospheric carbon to diIIuse into the part surIace.
In carburization the chemical potential oI carbon is lower in steel than in the atmosphere oI the
Iurnace, so it is thermodynamically Iavorable Ior the carbon atoms to diIIuse into the steel.
ecarburization, in which the gradient is reversed, can sometimes occur in high carbon steels
that are being heat treated Ior other reasons. The carbon will diIIuse out into a generally oxygen
rich atmosphere because the chemical potential oI carbon is less as a gas in an oxygen-rich
atmosphere than trapped in a solid steel matrix. This Iorms carbon dioxide gas, and leaves the
steel surIace with lower carbon content, and, by extension, diIIerent mechanical properties than
desired. This is unacceptable in applications requiring uniIorm surIace properties and requires
investigation to prevent it Irom occurring.
Commercialized steel production is done using either electrical Iurnaces or natural gas Iired
Iurnaces; it is inevitable that these Iurnaces atmospheres contain oxygen and thus the
atmospheres have lower chemical potential oI carbon than the steel. Because oI this many steel
samples are being pulled oI production lines due to low surIace hardness. In this experiment the
decarburization depth oI heat treated 1095 steel was measured and the activation energy oI the
decarburization was determined.

2. !rocedure
To begin the experiment, the samples were divided into nine smaller samples so that they
could be heat treated at the varied times and temperatures; the decarburization that occurred
could be compared and used Ior data on a plot to eventually calculate the activation energy (Q)
oI our material (Table I). BeIore this heat treatment was conducted the samples were cleaned in
a mild solvent to remove any surIace contaminants or oils prior to treatment. Weight and
thickness measurements were taken in order to determine iI any mass or dimensional changes
occurred during decarburization. Micro hardness was also measured Ior each sample using a
Vickers diamond indenter.

Table I: Heat treatments varying time and temperature



Temperature (C) Time 1 (hours) Time 2 (hours) Time 3(hours)
830 1 3 5
865 1 2 3
900 0.5 1 3

These times were decided based on preliminary experiments in an eIIort to receive data that
would show a trend while minimizing room Ior error. A Fe-C phase diagram was used to help
ecarburization
Team Tow
April 2011
MatE 370

College oI Engineering




2
with the temperatures and a minimum austenitization temperature oI 830C was determined and
set as the lower heat treatment boundary at which decarburization will occur. The upper limit oI
900C was established because it is the highest temperature the heat treatment Iurnaces can
reliably reach and maintain Ior the duration oI the heat treatment. AIter austenitization, samples
were normalized to room temperature to allow grain growth.
At this point, each sample was weighed and dimensionally measured again. When the
samples reached room temperature they were cut in halI to expose the longitudinal cross-section,
and then mounted in a cold-set acrylic epoxy to expose the cross-section oI interest. Each mount
was then ground on successively Iiner abrasive media until a smooth surIace was achieved, then
polished with 6, 1, and sub-micron abrasive suspensions to a mirror Iinish. $amples were then
etched with a 2 nital solution Ior 30 seconds, rinsed with ethanol. $ome samples were re-
polished at the 1 micron level due to over-etching. Etching was repeated this time Ior less than
20 seconds, which successIully revealed the microstructure and phase boundaries at the samples'
edges. AIter rinsing with ethanol the samples were prepared Ior microscopic imaging by placing
each on a metal stage and leveling with a hand press. Images were taken at 100X magniIication
with an Olympus U-M$$P optical microscope, equipped with a digital camera. Pictures
depicting the suspected decarburization region were gathered, with a second set oI photographs
marked with layer measurements calculated by the Image Pro Express program. The layers
measured were the suspected Iull decarburization region, consisting oI alpha Ierrite (wt
C0.022), and the partially decarburized area (0.022wt C0.95).

3. Data A3alysis
In order to calculate activation energy Irom an observed decarburized depth, Fick`s second
law must be used. Given constant source and isothermal boundary conditions, Fick`s second law
yields:





Where: C(x,t) is the concentration at depth x aIter time t,
C
0
is the concentration oI the source
x is the depth (cm)
is the diIIusion coeIIicient (cm
2
/s)
t is the time (s)

When C(x,t) is halI oI C
0
, the equation simpliIies to:





Which can be approximated to:




(1)
(2)
ecarburization
Team Tow
April 2011
MatE 370

College oI Engineering




3
The decarburized layers oI each sample were measured and plotted with respect to the
time that each was in the Iurnace, each data set representing a treatment temperature (Figure 1).
The linear regression Iits to the data points were Iorced to have an intercept oI zero to correctly
model equation (2).



This slope oI each line in this graph is the diIIusion coeIIicient () oI carbon through
austenitic steel at the given temperature. The speciIic values oI are shown (Table II).

Table : iIIusion CoeIIicient () values at each temperature.

Temperature (K) (m
2
/h) (m
2
/sec)
1103 10907 3.02972E-12
1138 15922 4.42278E-12
1173 18842 5.23389E-12


Figure 1: Graph oI squared junction depth (m
2
) versus time (s) at diIIerent temperatures Ior all nine samples.
The samples (Irom leIt to right) are 900C, 865C, and 830C, with decreasing slopes in the same order.
ecarburization
Team Tow
April 2011
MatE 370

College oI Engineering




4

$ince the purpose oI this study is to Iind activation energy Q, the Arrhenius equation
must be used. The Arrhenius equation is shown in Equation 3.





This equation simpliIies to:




Activation energy was calculated using linear regression on the data set. This equation
was graphed with the diIIusion coeIIicient () values Irom Table II, temperature in Kelvin, and
R (the Ideal Gas Constant) equal to 8.314 Joules per mole-Kelvin. The slope is then equal to Q
(Figure 2).



This slope was determined to be -84,312, which corresponds to an activation energy (Q) value oI
84.312 kJ/mol.

Figure 2: Graph oI the natural log oI versus the inverse oI temperature (multiplied by the Ideal Gas Constant). The
slope oI this graph is equal to Q, which is 84,312 J/mol, or 84.312 kJ/mol.
(3)
(4)
ecarburization
Team Tow
April 2011
MatE 370

College oI Engineering




5

. Discussio3 of Results
The value oI activation energy acquired Irom the $mithells Metals ReIerence Book Ior
carbon in austenitic steel is 148 kJ/mol
1
. Given the experimental value oI 84.312 kJ/mol, there
was an experimental error oI 43. According to the A$TM standards, however, the
measurement oI the decarburization layer is an inherently errant process. It speciIically states
that there is an error oI 10-20, which can skew the results even Iurther. UnIortunately, the
microscopes used in Iinding the decarburized layer were not top oI the line by any means, so the
error in that step would likely be closer to the 20 margin. The results were also interpreted
three diIIerent ways by three diIIerent teams. This does not necessarily add to the error, but it
Iorced each team to use one set oI data, or attempt to average them all out. With all the values
averaged, a activation energy oI roughly 30 kJ/mol was calculated, which gives an 80 error.
This necessitated the use oI one data set, preventing an increase in variance Irom experiment
inconsistencies.

There were also issues with the etching. The 2 nital etchant was the correct
concentration, but some oI the samples were still over-etched, which led to slightly burned
sample surIaces. This made the decarburized layer harder to accurately distinguish.

There was also some error in that some samples were removed Irom a Iurnace while others
were still in. This means that the samples with longer time were actually in the Iurnace longer,
but they received less heat than intended. This likely resulted in a decarburization depth below a
given treatments` expectation.

Based on these Iacts, most oI the error in the project can be attributed to the diIIiculty in
determining how thick the decarburized layer actually was.

. o3clusio3s
The objective oI this experiment was to Iind the activation energy oI the decarburization oI
1095 steel. It was Iound that the activation energy was 84.312 KJ/mol however the standard
value was expected to be 148 KJ/mol. In this experiment there were many sources oI error,
which caused the results to be 43 oII Irom the expected values. A$TM standards suggest that
with a sample size oI 20, there would be an error between 10-20. This experiment had a
sample size oI 15, so it is not surprising that our error is over 20. II this experiment were to be
perIormed again it is recommended that the sample size be increased to at least 20, this will
increase the accuracy oI the results.

ecarburization
Team Tow
April 2011
MatE 370

College oI Engineering




6

orks ited
1. Brandes, E. A., & Brook, G. B. (1992). Smithells Metals Reference Book, 7th Edition. OxIord:
Buttorworth-Heinemann.

2. Cornell, R., & Bhadeshi, H. K. (n.d.). Decarburi:ation of Steel. Retrieved April 20, 2011,
Irom www.msm.cam.ac.uk/phase-trans/abstract/M.html: www.msm.cam.ac.uk/phase-
trans/abstract/M.html

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