E 45 Laboratory Manual

Laboratory 2
Recovery, Recrystallization,
and Grain Growth
Objectives
1. To illustrate the use of thermal treatments in the restorative processing of materials that have been shaped by mechanical deformation.
2. To understand the detailed microstructural changes occurring during the three stages of annealing.

Overview
This lab explores the capacity of heat treatment to alter the microstructure, and therefore the properties, of materials.
In this case, the heat treatment is known as "annealing" and it is specifically employed to remove the damage to the
internal microstructure of materials that is caused by cold work or deformation at room temperature. No phase
transformations are involved, such as those found during your laboratory on the heat treatment of steel, but there are
microstructural changes, and these cause a marked difference in mechanical properties, as will be seen.

Equipment
Heat Treatment

1. Brass specimen (70% copper and 30% zinc)

2. Furnace, nichrome wire for suspending specimen in hot zone, and chromel + alumel thermocouple
3. Computer data acquisition system
Metallography

4. Polishing clamp, wet belt grinder, polishing papers (240, 320, 400, 600)
5. Electropolisher with polishing solution consisting of 1 part orthophosphoric acid + 1 part ethyl alcohol (95%) + 2
parts distilled water
6. Optical microscopy, glass slide, specimen press

Copyright 2014, Berkeley

Professor Lane W. Martin

Laboratory 2: Recovery, Recrystallization & Grain Growth

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Hardness Testing

8. Rockwell hardness tester

9. Measurement ruler

Background
When a material is deformed plastically, its defect density increases with the amount of deformation. The types of
defects generated during deformation include point defects (vacancies, interstitials), line defects (dislocations), planar
defects (twins, stacking faults), and possibly volumetric defects too (internal cracks or voids). The most common of
these defects in metallic materials is the dislocation, which is most commonly associated with plastic deformation.
Since each dislocation has a finite strain energy associated with it, the total free energy of the system increases with
the number of dislocations. Because the system always tends towards minimizing its free energy, it will attempt to
decrease its strain energy by either rearranging its dislocations into a more favorable configuration with a lower strain
energy, and/or nucleating undeformed strain-free grains. Although thermodynamically it is advantageous for the deformed (work-hardened) system to be in an undeformed state, the rate of transformation is limited by the kinetics of
the system, which governs the rate of change. At low temperatures the kinetics of the system is so slow that no
change can be detected. However, at high temperatures many changes in the system can be directly observed.
In this lab the processes of recovery, recrystallization, and grain growth are investigated. After a metallic material has
been work hardened, it can be softened at low temperature by recovery, a process involving the annihilation of point
defects and the migration of line defects (dislocations) into configurations with lower strain energy. At higher temperatures the material can be rapidly softened by recrystallization. This process eliminates most of the dislocations
by nucleating small strain-free (dislocation-free) grains that grow and replace the original deformed grains. Once all
the deformed grains are replaced, the recrystallization process is complete. Now the system is made up of many undeformed grains. Although these strain-free grain have very little strain energy, they still have a high surface energy associated with their numerous grain boundaries. Therefore, the system can further decrease its free energy by decreasing the amount of grain boundaries. This is accomplished by a process called grain growth where the larger
grains grow by eliminating the smaller grains, driven by the overall reduction in surface energy of the system.

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Laboratory 2: Recovery, Recrystallization & Grain Growth

Experimental Procedures
Part I Heat Treatment

Each group will be given a sample of brass that has been subjected to a mechanical deformation process known as
cold-rolling," in this case with a specimen geometry designed to induce a strain gradient across its width, as shown in
Fig. 1.

0.250 in.

0.125 in.

0.095 in.
Wedge-shaped
sample

Flat after
rolling

Figure 1
Schematic of sample
preparation to induce a gradient
in strain energy across the width
of the brass sample. One edge is
undeformed while other edge
undergoes a 50% reduction in
thickness by cold rolling. The
overall width of the sample
(transverse to rolling direction)
increases slightly after rolling,
from approximately 0.5 in. to
approximately 0.7 in. The overall
length of the sample (along the
rolling direction) remains approximately constant at 2 inches.

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Figure 2
Schematic experimental set-up. The
thermocouple tip rests in a small depression in the
top of the sample, which is suspended by a
Nichrome wire. Inset shows crucial alignment of
sample with the rectangular slot at the bottom of the
furnace. At right, the sample is lowered into the
water, submerged inch, to establish temperature
gradient (900C at top) and held for 15 minutes
before quenching. It may be necessary to replenish
the water supply due to evaporative losses.

Thermocouple

Top view:
sample aligned
with furnace slot
1/8 inch gap between
furnace and water
Sample submerged
1/8 inch

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Laboratory 2: Recovery, Recrystallization & Grain Growth

The sample will then be subjected to a thermal treatment during this laboratory exercise to induce a temperature gradient along its length, as shown in Fig. 2. Consequently the sample can be viewed as a two dimensional map of the
effects of the amount of deformation along one axis and annealing temperature along the other.
1. Attach, align, and position the deformed brass sample as shown in Fig. 2. Note that the orientation of the sample
must allow it to clear the rectangular slot in the bottom of the furnace so it can extend into the water bath and be
quenched rapidly at the end of the annealing treatment.
2. When the sample is in position, turn ON the power to the furnace. Begin at full power (maximum setting) to
ramp up to the target annealing temperature (900C) quickly.

Once the temperature reaches approximately

850C, reduce power to slow the progression to the target temperature of 900C. Care is needed to avoid large
temperature fluctuations here; the sample will melt at 920C.
3. Start the data acquisition program and begin to record data. If the water level decreases, add more water with the
squirt bottle to avoid wetting the furnace.
4. Hold the temperature at 900C for 15 minutes, adjusting the power source as needed to compensate for small
variations.
5. After 15 minutes, quench the sample by loosening the retention screw at the end of the holder to allow the brass
sample to fall completely under water.
6. Turn off the power. When the furnace has cooled, stop recording data and recover the sample from the water
bath.
Part II Metallographic Polishing

Mount the sample in the holding clamp and press the sample lightly against the grinder to obtain a flat surface on one
side. Do the same for the other side. When flatness is achieved (inspect contours of abrasions to determine this), take
the sample to the metallographic polishing papers for further surface preparation. Polish the sample carefully by
hand, moving the sample in a straight line (not a circular motion) and inspecting the surface for evidence of deep
scratches left by the prior 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. Finish with 600 grit paper.
Part III Metallographic Etching

Samples must next be electropolished to a specular finish as the final step in metallographic preparation. This also
provides a light etch to delineate microstructural features for observation in the optical microscope. After removal
from the electrolyte, 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.

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Laboratory 2: Recovery, Recrystallization & Grain Growth

Part IV Hardness Indentation Test

Make a series of Rockwell A hardness measurements at -inch intervals along the most severely worked (50% reduction) edge of your sample (approximately 15 data points) and along the edge submerged in the water (approximately 5 data points). Record the results in your data sheet.
Part V Optical Microscopy

Mount the sample on a glass slide with clay using the specimen press to level the surface. This will keep the sample
in focus as it is moved laterally on the microscope stage. Using your data from Part IV above, select five different
areas along the edges of the sample where the hardness readings are noticeably different. Sketch or photograph the
microstructures at each of these five areas and enter descriptions in your notebooks of any subtle details that might be
difficult to capture in your sketches. It is most important that your sketches have sufficient precision to reflect differences in relative grain sizes and dislocations density. Detailed descriptions in your lab notebook will of course assist
your later interpretation of your sketches when preparing your lab report.
DataSheet 5-1 Hardness Measurements

Position
1
2
3

Major Load

Minor Load

Hardness

20
This datasheet can incorporate additional columns in a spreadsheet, such as those called out in the Questions below, to
enable the use of any graphing functions (see questions requesting plots for data to be programmed in other columns)
embedded in the spreadsheet application(s).

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Laboratory 2: Recovery, Recrystallization & Grain Growth

Lab Report
Strive to be precise with your data presentation and answers to the following questions.
Question 1

Construct a plot of hardness vs percentage reduction in thickness, assuming the thickness reduction varies linearly
across the width of the sample from 0% (undeformed) to 50%. Explain why the hardness increases as the percentage
reduction (amount of cold work) increases.
Question 2

From the sketches of the microstructure, explain: (a) why the recrystallized grain size increases with increasing temperature; and (b) why the hardness decreases with increasing grain size. Assuming the temperature gradient is linear,
is there a temperature below which no recrystallization is observed? How does this temperature compare to the tabulated recrystallization temperature of brass?
Question 3

Now plot hardness vs length (which corresponds to the annealing temperature) along the most deformed edge of the
sample. Are the hardness readings consistent with the observed microstructure? Explain.

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