Experiment #7

Heat Treatment and Hardness of Tool Steel

Stephen Mirdo

Performed on November 15, 2010

Report due November 22, 2010

 Table of Contents

Object ………………………………………..………………………….………….…. p. 1

Theory …………………………………………………………………………..…pp. 1 - 3

Procedure ………………………….…………………………………...……..……..... p. 4

Results …................................................................................................................ pp. 5 - 7

Discussion and Conclusion …………………….......…………………….…….....…... p. 8

Appendix ……………………………………..………………..…..….………... pp. 9 - 11

 Object
The object of this experiment was to determine the effect of heat treatment on the
hardness of tool steel.

Theory
The mechanical properties of a material, such as hardness, can be influenced by
the process of heat treatment. Heat treating a material, such as a ferrous alloy, alters the
microstructure of the material. The microstructure of the material determines the
mechanical properties of a material. Therefore, by controlling the microstructure of a
material, it can be tailored to meet specifications.

Figure 1: Iron-iron carbide phase diagram (Source: Materials Laboratory Manual, Fall
2010, University of Memphis, Department of M.E.)

The process of heat treating the ferrous alloy of tool steel begins with raising the
material’s temperature to that which is above the A3-temperature, as seen in the phase
diagram in Figure 1. The percent weight carbon composition of tool steel is between
0.7% and 1.5% carbon. The percent weight of the solute, carbon, is the horizontal axis of
the phase diagram and temperature is the vertical axis. Above the A3-temperature, the
ferrous alloy forms the microstructure of austenite, which is the γ region of the phase
diagram. This polymorphic transformation of ferrite to austenite is known as
austenitizing.

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 Once the material has been austenitized by heat treatment, the material is cooled
to allow the precipitation of a desired microstructure, thus tailoring the mechanical
properties of the ferrous alloy. The rate at which the sample is cooled determines the
microstructure that will occur. A discussion of the various microstructures that can occur
as a result of the cooling of an austenitized ferrous alloy follows.
Pearlite consists of two phases of the ferrous alloy. As seen in Figure 2, the
microstructure of pearlite is composed of alternating layers of α ferrite and cementite.
Pearlite is formed as a result of a slow cooling process of austenitized ferrous alloy, such
as a process consistent with letting a specimen cool in the furnace used to heat the
sample. The mechanical properties of pearlite, relative to other microstructures of ferrous
alloy, make it a ductile and soft material and because of its lamellar structure, it has high
wear resistance.

Figure 2: Photomicrograph of the pearlite microstructure of a ferrous alloy.

Bainite is the ferrous alloy microstructure that consists of the phases cementite,
ferrite and martensite present in a non-lamellar manner. The grain of bainite in Figure 2
below passes from the lower left of the image to the upper right corner. Bainite is formed
by a cooling process that is moderately more rapid relative to the cooling process that
forms pearlite. An example of a moderate cooling process would be to allow an
austenitized specimen to cool in room temperature air. Relative to pearlite, bainite is a
harder and less ductile material.

Figure 2: Transmission electromicrograph of the bainite microstructure of a ferrous

alloy.

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 Martensite, unlike the previous microstructures discussed, is a nonequilibrium
single phase microstructure that results from the rapid cooling, or quenching, of
austenitized ferrous allow. The quenching process is the plunging of the heat treated
material into a fluid that is at or below the ambient temperature of the forging
environment. The needle-like structures of martensite can be seen in Figure 3 below.
The lighter shaded region around the needle-like structures is retained austenite that did
not transform due to the rapid cooling process. Relative to pearlite and bainite,
martensite is a very hard material, yet very brittle.

Figure 3: Photomicrograph of the martensitic microstructure of a ferrous alloy.

Figure 4: Flowchart demonstrating the formation of microstructures as a function of the

rate of cooling. (Adapted from: Fundamentals of Material Science and Engineering: An
Integrated Approach, W.D. Callister, Jr and D.G. Rethwish, 2008)

A method employed to determine the hardness of materials is the Rockwell

hardness test. To perform the test, a pointed instrument called an indenter is applied
normal the surface of the test specimen at an initial minor load, and then again at an
increased load. The difference in the depth of the indentation equates to a Rockwell
hardness value, which is a unitless number. There are a variety of Rockwell hardness
tests. The test type that will be the focus of this experiment is the Rockwell C hardness
test. The indenter of the C test is a 120o conical diamond. The initial, minor load is 10
kg and the subsequent load is 150 kg.

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 Procedure
Equipment
Furnace
Wilson Instruments Rockwell Hardness Tester Series B2000 (SN: RB2000R4831)
Four (4) small (approximately 2 in. x 2 in.) polished alloy steel specimens

Experiment
1) Polish the four alloy steel specimens very carefully
2) Heat three of the four steel specimens in the furnace (Figure 1) to a
temperature of 1550 oF for one and a half hours.
3) Upon completion of Step 2:
a. Leave one specimen to cool in the furnace overnight
b. Let one specimen cool in room temperature air overnight
c. Quench one specimen in tap water that is approximately 55 oF
4) Calibrate the Rockwell hardness tester apparatus by measuring the hardness of
a specimen that has a known hardness. Compare the indicated hardness of the
calibration sample to the accepted hardness value of the material. If the
values are in agreement, proceed to Step 5.
5) Obtain the hardness of all specimens using the Rockwell hardness tester
(Figure 2) using the Rockwell C-Scale. Obtain three test values for each
specimen.

Figure 5: Furnace used for heat treatment
of steel specimens. (Source: Materials
Laboratory Manual, Fall 2010, University
of Memphis, Department of M.E.)
Figure 6: Photograph of the Rockwell
hardness testing apparatus.
(Source: Materials Laboratory
Manual, Fall 2010, University
of Memphis, Department of M.E.)

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 Results

Table 1: Rockwell C-Scale hardness of the control tool steel specimen (untreated).
Trial # HRC
1 8.2
2 9.9
3 10
Avg. HRC 9.4

Table 2: Rockwell C-Scale hardness of the furnace cooled tool steel specimen
Trial # HRC
1 21.3
2 17.2
3 18.2
Avg. HRC 18.9

Table 3: Rockwell C-Scale hardness of the air cooled tool steel specimen
Trial # HRC
1 53.7
2 53.7
3 53.6
Avg. HRC 53.7

Table 4: Rockwell C-Scale hardness of the quenched tool steel specimen

Trial # HRC
1 58.4
2 58.3
3 58.9
Avg. HRC 58.5

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 Table 5: T-test for the control specimen and the furnace cooled specimen
t-Test Control Furnace Cooled
Mean 9.4 18.9
σ 1.0 2.1

df = 4
t stat = 6.982
t crit = 2.776

The calculated tstat is greater than tcrit, therefore the null hypothesis is rejected and it is
determined that the hardness values of the control specimen and furnace cooled specimen
are statistically significant.

Table 6: T-test for the control specimen and the air cooled specimen
t-Test Control Air Cooled
Mean 9.4 53.7
σ 1.0 0.1

df = 4
t stat = 75.727
t crit = 2.776

The calculated tstat is greater than tcrit, therefore the null hypothesis is rejected and it is
determined that the hardness values of the control specimen and air cooled specimen are
statistically significant.

Table 7: T-test for the control specimen and the quenched specimen
t-Test Control Quenched
Mean 9.4 58.5
σ 1.0 0.3

df = 4
t stat = 80.229
t crit = 2.776

The calculated tstat is greater than tcrit, therefore the null hypothesis is rejected and it is
determined that the hardness values of the control specimen and quenched specimen are
statistically significant.

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 Table 8: T-test for the furnace cooled specimen and the air cooled specimen
t-Test Furnace Cooled Air Cooled
Mean 18.9 53.7
σ 2.1 0.1

df = 4
t stat = 28.158
t crit = 2.776

The calculated tstat is greater than tcrit, therefore the null hypothesis is rejected and it is
determined that the hardness values of the furnace cooled specimen and air cooled
specimen are statistically significant.

Table 9: T-test for the furnace cooled specimen and the quenched specimen
t-Test Furnace Cooled Quenched
Mean 18.9 58.5
σ 2.1 0.3

df = 4
t stat = 31.755
t crit = 2.776

The calculated tstat is greater than tcrit, therefore the null hypothesis is rejected and it is
determined that the hardness values of the furnace cooled and quenched specimen are
statistically significant.

Table 10: T-test for the air cooled specimen and the quenched specimen
t-Test Air Cooled Quenched
Mean 53.7 58.5
σ 0.1 0.3

df = 4
t stat = 25.809
t crit = 2.776

The calculated tstat is greater than tcrit, therefore the null hypothesis is rejected and it is
determined that the hardness values of the air cooled specimen and quenched specimen
are statistically significant.

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 Discussion & Conclusion
The Rockwell C hardness test indicates that heat treatment and the cooling
process have an affect on the hardness of the tool steel specimens. Excluding the control
sample, all specimens underwent the same heat treatment at a temperature of 1550 oF.
The difference in the hardness values, HRC, is due to the cooling process selected for
each specimen.
The specimen that was allowed to cool slowly inside the furnace yielded the least
amount of increase in its hardness. The HRC value for this specimen was 18.9, double
the control specimen’s HRC of 9.4. The air cooled specimen had an HRC of 53.7, which
was a large increase compared to the control sample. The quenched specimen had an
HRC of 58.5, which is slightly higher than the air cooled sample. The quenched sample
would have yielded a higher hardness value if it had been quenched in ice water.
However, due to availability, tap water was used for the quenching process. It can
therefore be concluded that for the ferrous alloy used in this experiment, a more
expedient cooling process yields a harder end product.
There were few sources of error in this experiment. Due to an inconsistent
microstructure of each specimen used in the hardness test, vary HRC values were
recorded. To compensate for this discrepancy, an average of three trials was used to
determine the hardness of each sample.
It would be difficult to improve the effectiveness of this experiment. However, a
few modifications to the technique are in order. One such improvement would be to
quench one of the test specimens in ice water and another specimen in water at ambient
temperature for an identical time interval. This would allow for a more direct
demonstration of the time and temperature constraints pertaining to material hardness.
Another improvement would be to use more than one type of material. Having a control
and a heat treated specimen for each type of material would demonstrate heat treatments’
affect on different materials.

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 Appendix
Data Usage

Sample calculation of the mean of the HRC values of the control specimen:

(8.2 + 9.9 + 10.0) / 3 = 9.4

Sample calculation of the standard deviation of the HRC values of the control
specimen:
________________________________
√ [(8.2 – 9.4)2 + (9.9-9.4)2 + (10-9.4)2] / 3 = 1.0

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Bibliography

Fundamentals of Material Science and Engineering: An Integrated Approach

W.D. Callister, Jr and D.G. Rethwish (2008)

Materials Laboratory Manual, Fall 2010

University of Memphis, Department of Mechanical Engineering

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