E 45 Laboratory Manual

Laboratory 4
Heat Treatment of Steel
Objectives
1. To understand the effect of thermal processing (heat treatment) on both the microstructure and properties (hardness) of steel
2. To understand the application of time-temperature-transformation (TTT) curves in ferrous metallurgy

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Overview

T (C)
1600

tural components in the construction and transporta-

1538
1495

1400 1394
1300

tion industries to specialty tools in the medical indus-

1200

try. Its properties vary widely, depending upon the

1100

thermomechanical processing cycles to which steel

1000

components are subjected, and their exposure to in-

900

Steel is one of the most versatile engineering materials, used in a wide range of applications from struc-

service conditions. This lab offers a survey of the

role of heat treatment in the development of microstructures and properties to optimize engineering
performance in ferrous alloys.

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1500

L
1227
1148
2.11

6.67

4.30

910

800

727

700 0.02 0.77

600

6.67
Cementite

500
400
300
200

Figure 1 The Fe-C phase diagram, to 6.67wt.%

C, from Metals Handbook, 8th edition, Volume 8,
ASM, Metals Park, Ohio, (1973).

Copyright 2014, Berkeley

100
0

Fe

3
4
wt % C

Fe3C

Professor Lane W. Martin

Laboratory 4: Heat Treatment of Steel

Equipment
Heat Treatment

1. ASTM 1045 (0.45 wt.% C) cold-rolled steel specimen

2. Furnace and wire for suspending specimen in hot zone
3. Thermocouple [chromel + alumel]
4. Computer data acquisition system
Metallography

5. Polishing clamp, wet belt grinder , and polishing papers (240, 320, 400, 600)
6. Electropolisher, with polishing solution consisting of 60 ml distilled water + 50 ml butyl cellulose + 350 ml ethyl
alcohol, 95%, (and just before using, add)+ 40 ml perchloric acid, 60%
7. Glass slide, specimen press
8. Optical microscope
Hardness Testing

9. Rockwell hardness tester

10. Measurement ruler

Background
Steel is an alloy of iron (Fe) and carbon (C), with concentrations of carbon from 0.1 to 2.0 weight percent. Carbon is
soluble in Fe because the C atoms are small enough to fit into interstitial locations between Fe atoms without too
much distortion of the lattice. Carbon is soluble in the FCC phase of Fe (called austenite or gamma-Fe, or ) up to
approximately 2%. However, in the BCC phase of Fe (called ferrite or alpha-Fe or ), the maximum solubility is only
about 0.02%. These phases are shown on the equilibrium phase diagram in Fig. 1.
When austenite is cooled below a critical temperature called the eutectoid temperature (727C), it becomes unstable.
Most of the Fe tends to precipitate as nearly pure ferrite and most of the C tends to aggregate in the intermetallic compound Fe3C (cementite). The transformation of austenite requires redistribution of C atoms from a random solid solution to one in which nearly all C is contained in the Fe3C precipitates.
At temperatures just below the eutectoid decomposition temperature the driving force for the transformation is low,
and nucleation of the two new phases, ferrite and cementite, is slow. It is therefore necessary to hold the specimen at
temperature for a considerable time to allow the transformation to take place in those regions of the specimen that are
just below 727C. The lower the temperature, the greater the driving force for the reaction to occur, causing a higher
nucleation rate. At temperatures below about 540C, however, the rate of transformation again becomes slower. This

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Laboratory 4: Heat Treatment of Steel

is due to the decreasing mobility of C atoms in the austenite. In order for the transformation to continue, C atoms
must diffuse away from the growing ferrite regions to the growing Fe3C regions.
If the austenite is cooled so rapidly that there is not enough time for nucleation and growth of ferrite and Fe3C, an entirely different kind of transformation takes place called the "martensitic" transformation. In this reaction the FCC
austenite changes instantly by a shear mechanism to a body-centered tetragonal structure, trapping C in the new
phase, called martensite.
These reactions are best illustrated in a figure known as a time-temperature-transformation (TTT) diagram. It portrays
the decomposition kinetics of austenite, obtained by isothermally holding a sample for different times until the reaction is complete. An example is shown in Fig. 2.

800 804
727
700

500

e 3C

400
300
200

+ Fe3C

+F

Temperature (C)

600

Ms
Mf

100
0
0.1

1 sec.
1

1 min.
10

102
Time (seconds)

1 hour
103

1 day
104

105

Figure 2 Schematic TTT curve for a hypoeutectoid plain carbon steel. The pro-eutectoid ferrite constituent
forms below 804C, and the eutectoid constituent below 727C. Both the start (Ms) and the finish (Mf) of the
athermal martensitic transformation are seen at lower temperatures. From The Making, Shaping, and Treating of Steel, H.E. McGannon (Ed.), 9th Edition, United States Steel Corporation, Pittsburgh, (1971), p. 1087.

The mechanical properties of steel depend upon the dispersion of C atoms or of cementite particles in the Fe matrix.
Since redistribution of C atoms requires diffusion and since the rate of diffusion decreases exponentially with decreasing temperature, the coarsest dispersions of Fe3C and of ferrite result from the transformation that is allowed to take
place at high temperatures, just below the critical temperature. The resulting eutectoid product is known as coarse
pearlite. If the transformation is forced to take place at lower and lower temperatures by increasing the rate of cooling, then finer and finer dispersions of the hard brittle carbon-rich phase (Fe3C) and the relatively soft ductile ferrite
are produced, known as fine pearlite. If the transformation takes place at temperatures below about 400C, the ferrite
and cementite form as extremely fine needles. This microstructure is known by another name, "bainite."

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Laboratory 4: Heat Treatment of Steel

The hardness of steel generally increases with the fineness of the dispersion of the phases in the microstructure. If the
rate of cooling is increased still further, the precipitation of carbon as Fe3C can be suppressed altogether, forming
martensite, in which the C atoms are still distributed nearly at random. This is the hardest structure possible for any
given steel. However, since martensite has low ductility, many machine parts are first rapidly cooled to produce
martensite, then tempered by holding at slightly elevated temperatures to redistribute the carbon as fine precipitates.
The resulting microstructure is known as tempered martensite and benefits from some restored ductility.

Experimental Procedures
Part I Heat Treatment

Each group will be given a sample of 1045 cold rolled steel.

The sample will first be heated uniformly in the

austenitic region of the phase diagram (Fig. 1). The sample will then be heated under conditions resulting in a temperature gradient along its length, as illustrated in Fig. 3.

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Thermocouple

Top view:
sample
aligned
with
furnace
slot

Figure 3 Schematic experimental setup.

The thermocouple tip rests in a small depression in the top of the sample, which is suspended by a Nichrome wire. Inset at left
shows crucial alignment of sample with the
rectangular slot at the bottom of the furnace.
In center frame, the entire sample is heated
to 1050C and held for 5 minutes. At right,
the sample is lowered into the water, submerged 1/8 inch, to establish temperature
gradient (900C at top) and held for 15 minutes. It may be necessary to replenish the
water supply due to evaporative losses.

1/8 inch
gap to
water
and
under
water

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Laboratory 4: Heat Treatment of Steel

1. Suspend both the steel sample on its Nichrome wire tether and the thermocouple using an adjustable lab clamp
as shown in Fig. 3. Note carefully the relative orientation of the sample and the rectangular slot through the furnace. Adjust so there is adequate clearance for the sample to pass smoothly through the furnace slot by simple
vertical motion of the lab clamp. This will be critical during the later stages of this experiment.
2. Position the sample in the center of the furnace heating coils.
3. Connect the thermocouple to the data acquisition interface box.
4. Turn on power to the furnace and start the data acquisition program to begin recording temperature data.
5. Heat to 1050C and hold at this temperature for at least 5 minutes.
6. Quickly drop the sample so that it is contacts the water with approximately " submerged, as shown in Fig. 3.
7. Adjust the power input so that the temperature at the top of the sample is 900C. If the water level decreases,
carefully add more water with the squirt bottle, avoiding any splashing of water into the furnace. Hold the temperature at 900C for 15 minutes by adjusting the power source as needed.
8. After 15 minutes, quench the sample by dropping it quickly into the water and vigorously agitating it until cool.
9. Turn off the power. When the furnace has cooled to about 50C, remove the sample and terminate data recording.
Part 2 Metallographic Polishing

Mount the sample in the holding clamp and remove the oxide scale by pressing the sample lightly on the grinder to
obtain a flat surface on one side. Do this for both sides of the sample. Then grind by hand, moving the sample in a
straight line (not a circular motion) on successively finer paper down to 600 grit. For each change of grit paper,
change the orientation of the sample by 90 and continue sanding until the orthogonal scratch marks disappear. Remember to wash the sample between paper changes to remove all remnant grit.
Part 3 Metallographic Etching

Samples must be electropolished to a specular finish as the final step in metallographic preparation, which also provides a light etch to delineate grain boundaries, dislocations that intersect the surface, and interphase boundaries. Afterwards, quickly wash the sample in running water, rinse with alcohol and dry under the hot air blower. Be careful
not to touch the polished surface at any time, or else the fine grinding and polishing steps will have to be repeated.
Part 4 Hardness Indentation Test

Take a series of Rockwell A hardness measurements (60 kg major load) at -inch intervals along the long dimension of the sample, to probe the effect of the temperature gradient on the mechanical properties of the sample. Record
the results, approximately 16 hardness values total, on the data sheet.

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Laboratory 4: Heat Treatment of Steel

Part 5 Metallography

Mount the sample on a glass slide with plasticene using the specimen press to level the surface. This will keep the
sample in focus as it is moved laterally with the microscope stage. Choose five (5) areas along the edges where the
hardness readings are different and/or where the microstructure looks different. Sketch the microstructures at each of
the five areas. Notice the difference in grain sizes, the density of defects (dislocations), and the morphology of the
microconstituents. Sketch these and record your observations in your lab notebook to support your sketches. Also,
look for the answers to the questions in the Lab Report section when examining the sample.
DataSheet 1 Hardness Measurements

Position

Major Load

Minor Load

Hardness

1
2

16

This datasheet should be set up in a spreadsheet application to facilitate the use of a graphing function as called for in
the Questions below.

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References

1. G. Krauss, Principles of Heat Treatment of Steel, American Society for Metals, Metals Park, OH, (1980).
2. W.T. Lankford, et al., Eds., The Making, Shaping, and Treating of Steel, 10th edition, Association of Iron and Steel
Engineers, Pittsburgh, PA, (1985).
3. Metals Handbook, 9th edition, Vol. 4, Heat Treating, American Society for Metals, Metals Park, OH, (1981).

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Laboratory 4: Heat Treatment of Steel

Lab Report
Precise data presentation is expected, accompanied by relevant references. Answers to the following questions are
also required.
Question 1

For each of the five (5) different microstructures evident in your results, draw a representative cooling curve on a TTT
diagram corresponding to the thermal history associated with the specific area of the sample where the microstructure
was observed. Use a separate TTT diagram for each of the five cooling curves, but show them all at the same scale.
Verify the phases present in each microstructure and compare to your cooling curves. Specify the order in which the
phases appeared, and refer to the phase diagram as necessary to validate your conclusions.
Question 2

Make a plot of hardness versus distance from the 900C end of the sample. Use your hardness data to rank martensite, ferrite, and pearlite from the hardest to the softest. Support your results by discussing the nature of the microstructure, crystal structure, and chemical bonding associated with all three phases (martensite, ferrite, and carbide).
Question 3

Does the transformation of austenite into ferrite begin at the austenite grain boundaries and propagate inward, or does
it begin inside the grains and propagate outward toward the boundaries? Include a sketch of the microstructure from
the appropriate part of the specimen illustrating the answer to this question. Explain.
Question 4

How could a structure containing only ferrite and martensite be produced in a 1045 steel specimen? Illustrate on a
TTT diagram.
Question 5

Could you heat treat a 1045 steel specimen so that it contains only ferrite? Describe how this can be achieved, or explain why it cannot be done.
Question 6

Why isn't martensite on the Fe-Fe3C phase diagram of Fig. 1? Why doesn't its absence from the phase diagram prevent it from being an important engineering material?

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