Recovery, Recrystallization and Grain Growth

Abstract:
We want to examine how heat treatment of cold worked 70/30 weight percent
Cu/Zn (brass) affects microstructure, subsequently affecting mechanical properties.
Specific materials are often picked for a project but sometimes do not meet the
mechanical criteria. By annealing the material, bringing it to a high temperature and
allowed to cool slowly, we can optimize specific mechanical properties desired for the
project.
We will be using the tensile test to compute the stress versus strain graphs. Using
the stress versus strain graphs we will be calculating mechanical properties, analyzing the
trends they form with increase annealing temperature. We will find the point of
recrystallization and examine the meaning.
We find as annealing temperature increases, hardness goes down while ductility
and toughness goes up. We found annealing temperature does not have an affect on
elastic modulus. With the increase of annealing temperature comes change in
microstructure. Recrystallization and grain growth changes mechanical properties.
Larger grains form after recrystallization at higher temperatures during the annealing
process. Larger grains means the material has less high-energy interfaces increasing the
stability of the system.

Introduction:
Engineers have a wide range of materials to choose from. Sometimes the material
needed to the project is known but the mechanical properties of it are not adequate for the
task. Engineers process these materials to maximize their performance, strengthening the
specific mechanical properties needed for the project. A material can have the same
composition with varying properties such was ductility, ultimate tensile strength,
toughness etc. One way to changes these mechanical properties and extensively studied
in this lab is the process of heat treatment.
The heat treatment process examined in the lab is called annealing. In the
annealing process cold worked metal is heated to a relatively high temperature (making
sure not to exceed its melting point), kept constants for a period of time and allowed to be
slow cooled back to room temperature. Cold worked metals consist of altering the shape,
putting the metal through rollers or working on it with a hammer, by plastic deformation
to increase the hardness and tensile strength, see Figure 1.

A0 Af
Figure 1
Cold Working

Initial: Random
Final: Organized Grain Structure
Grain Order
(Elongated in direction of rolling)
 The annealing process is performed to remove stresses, soften the metal, and
improve its machinability. Heating must reach about the recrystallization temperature but
below the melting point to create an effective change. During recrystallization grains
boundaries are replaces with new un-deformed grains. The new larger and less deformed
grains usually reduce the strength and hardness but increasing its ductility. Figure 2
shows the different grain structures as annealing temperature gets higher.

Figure 2

We are to compare the results of increasing annealing temperature versus

mechanical properties. Two samples are given to each group and asked to perform the
tensile test. Samples given to the groups consisted of brass, 70/30 weight percent Cu/Zn
annealed for one hour at room temperature, 250, 350, 450, 550, and 750oC. Mechanical
properties examined in this lab are elastic modulus, yield strength, ultimate tensile
strength, ductility and toughness. A Glossary is provided at the end of the report for the
six mechanical properties.
We are also to compare how annealing effects the microstructure of each sample
provided. We will be comparing the grain boundaries and pointing to where
recrystallization occurs.

Procedures:
For this lab we were to split into groups of four. We reach the lab station finding
two samples of 70/30 weight percent Cu/Zn with different annealed temperatures. We
collected each specimen and measured its width and thickness using a caliper, Figure 3.
The gauge length for each specimen is uniform at 25.4mm. After measurements had
been taken, they were written on the class board to be individually recorded for further
reference needed in calculations. Table 1 in the Results section has the dimensions of
each specimen. All values must be accurate as for they are to be entered in the computer
to help with calibration efforts.

Figure 3 – Caliper
 After all the measurements have been taken it is time to use the tensile test
machine. We load the material to the tensile test machine, clamping the top half first then
the bottom, refer to Figure 4. It is important to stay consistent in our experiment to
reduce the amount of error.
We then had to make simple adjustments to
the programming of the tensile test machine. For
Figure 4 each test we pressed the ‘LOADCAL’ button then
Tensile Test ‘ENTER.’ After pressing ‘ENTER’ we pressed
Machine the “GL RESET” button then hit the ‘jog up’
button twice quickly. The 'jog up’ button is to
make sure there is some stress already applied at
the beginning as to which to computer takes into
account. The last step in preparing the tensile test
machine was making sure the connection between
the computer and the machine was established by
pressing the ‘IEE’ button.
Once the computer and the tensile test had
been synchronized we set up the program to the
specific material. We used the INSTRON
SERIES IX program to aid us with out testing.
After the application was opened we clicked on
‘test’ then named the file making sure it was
saved in the correct folder for easy access after the experiment. We saved the file then
clicked on the test method ‘45 Tensile Test…’ Again we had to save our file in the
correct folder. We hit the ‘start’ button but before we could begin we were asked for the
dimensions of the material being inserted, which was collected earlier in the lab. After
the dimensions were entered we ran the test and watched as the material stretched and
ultimately separated. We clicked ‘end sample,’ ‘continue,’ ‘Report to File,’ and ‘ok’ to
get us to the file naming stage. We named the file and placed it in the correct folder were
it is to be retrieved and imported into Excel.
We are done using the tensile testing machine and ready for analysis using Excel
and its plotting abilities. The data collected in Excel gave us elongation versus force.
This data will be manipulated and turned into a stress versus strain curve. Further
explanation of how we did this will be in the Results section. We emailed the Excel files
to each member of our group.

Figure 5: The next test performed was the Rockwell Hardness Test.
Hardness Tester After the sample form the tensile test breaks we take it to the
hardness tester, Figure 5 and test its dimensionless hardness.
We find a clean part of the sample and place it on the tray
provided. We crank the lever (towards the bottom)
clockwise until the ready button lights up. When the ready
light is on the green button labeled Start is pressed. The
 operation only takes a few second and a number is displayed. We repeated this process
five times for each sample and took an average. All six values were written on the class
board and recorded. The average of each sample will be displayed in Table 1.

Results:
Table 1 gives the dimensions and the average hardness of each sample.
Annealing temperature is graphed versus average hardness in Figure 6. We are setting
the “As Received” sample at 20oC because it was not annealed therefore set at room
temperature.

Annealed (oC) Width (mm) Thickness (mm) Average Hardness

Table 1
As Received 6.3 1.6 99.08
250 5.8 1.2 97.04
350 5.92 1.19 94.14
450 6.3 1.6 57.44
550 5.7 1.1 62.98
750 5.89 1.2 36.28

Figure 6

Annealing Temperature V. Hardness

120

100

80
Hardness

60

40

20

0
0 100 200 300 400 500 600 700 800
Annealing Temperature (C)

Figure 7 is a graph of all six samples on one stress versus strain plot. Table 2 was
formed through a series of calculations using the stress versus strain curves found in
Appendix A. Using Figure 8 an explanation of each mechanical property: elastic
modulus, yield strength, ultimate tensile strength, ductility, and toughness will be
explained.
 Figure 7

Table 2
Sample E. Modulus Yield Strength Toughness
(oC) (MPa) (MPa) UTS (Mpa) Ductility (%) (MJ/m^3) Hardness
20 15059.34 381.90 442.46 33.00 0.13 99.08
250 14999.62 428.90 602.01 38.00 0.22 97.04
350 15511.30 451.29 592.33 42.50 0.22 94.14
450 15262.77 131.23 347.12 70.00 0.22 51.44
550 14605.26 172.97 550.86 78.00 0.39 62.98
750 15085.94 85.50 394.06 83.20 0.4 36.28

Referring to the figure 8 we will be able to calculate elastic modulus, yield

strength, ultimate tensile strength, ductility, and toughness. We will start with elastic
modulus. Elastic modulus is the slope of the linear elastic region in the stress versus train
graph. We do not take into consideration the curve part, plastic region, of the graph. We
can take two points from the graph and use the rise-over-run analysis to find the slope.
(Y(2)-Y(1))/(X(2)-X(1))
 Figure 8
Typical Stress vs. Strain
Curve

We will then need to use the same slope in finding yield strength. When finding
yield strength we add 2% to stress versus strain linear portion of the graph. We will find
that it is the same slope of elastic modulus because the only shift is in the positive x-
direction (+.002.) Graphing the line, we are looking for the point of intersection with the
stress vs. strain curve. At the point of intersection the stress is recorded giving us yield
strength in megapascals.

15600.00

15400.00
Youngs Modulus (MPa)

15200.00

15000.00

14800.00

14600.00

14400.00
0 100 200 300 400 500 600 700 800
Annealing Temperature

Graph of Y. Modulus vs. Annealing Temperature

Ultimate tensile strength is determined where the slope of the stress versus strain
graph equals zero. This gives us the max of the curve (maximum stress). The INSTRON
SERIES IX program told us where the maximum load is. Using this information we can
find the value mathematically. Taking the maximum load dividing it by the cross
sectional area and multiplying by 1000 gives us the stress in megapascal.
((Max load)/(Cross Sectional Area))*1000
 Ultimate tensile strength and yield strength are both measure in megapascal. For
this reason they are graphed on the same plot given in Figure 9. They are plotted against
increasing annealing temperature.

Figure 9

700.00

600.00

500.00
Stress (MPa)

400.00 Yield Strength

300.00 UTS

200.00

100.00

0.00
0 100 200 300 400 500 600 700 800
Anneasling Temperature (C)

When finding ductility a physical print out the graphs in Appendix A had to be
made. The same slope found for elastic modulus has to be transferred to the point of
rupture of the sample. Tracing the slope from the rupture point we seek where is hits the
x-axis. We record the strain not before multiplying it by 100 to give us the value in a
percent. Strain is the measurement of the change in length (elongation) divided by initial
length. This already gives us a ratio; by multiplying it by 100 we get a percent. We have
graphed ductility versus annealing temperature in Figure 11. To find toughness we had
to think back to calculus to find the area under the curve. Using the right trapezoidal rule
we were about to give a close approximation to the actual area under the curve. The
formula used goes as followed:
(1/2)( (X(2)-X(1))/(Y(2)-Y(1)) = (1/2)*Base*Height
We are looking for the area of each trapezoidal section and adding them all to get
area under the curve Figure 10.
Figure 11
Figure 10
90.00
80.00
70.00
Ductility (%)

60.00
50.00
40.00
Figure 12 shows us the Toughness
30.00 versus annealing temperature.
20.00
10.00
0.00
0 100 200 300 400 500 600 700 800
Annealing Temperature
 Figure 12: Graph of Toughness versus Annealing Temperature

0.45
0.40
Toughness (MJ/m^3)

0.35
0.30
0.25
0.20
0.15
0.10
0.05
0.00
0 100 200 300 400 500 600 700 800
Annealing Temperature (C)

The annealing process changes crystal grain structure only visible in the
microscopic stage. To the eye the crystal structure has no difference and looks the same
for each sample. Changing the microstructure changes its mechanical properties as seen
in our data.
Microstructure Grain boundaries

As Receive – 20oC 250oC Sample

Similar to that of the “As Received” sample,

Cold worked brass with an uneven deformed
with uniformity occuring. Larger grain
crystal structure.
boundaries are starting to form.
350oC Sample 450oC Sample

Full recrystallization occurring. Grain

Not much of a difference between 250oC,
boundaries are very small indicating
recrystalization and new grain appearing.
reformation

550oC Sample 750oC Sample

Fully new grains have grown; as a result

Substantial grain growth has occurred.
hardness has been lowered.
Discussion:
The 6 graphs of mechanical properties versus annealing temperature look on par
with those of theoretical records. Figure 12 shows the theoretical curve for ductility and
tensile strength.

Figure 12

Our ductility curve shows to have the same curve as that of published results.
Ultimate tensile strength had similar results with only one odd value. The 550oC sample
is recorded and shown to be a bit high compared to the publish results. Referring to
Appendix A, taking a closer look at the 550oC annealed brass, we see a slight but sudden
transition from the elastic to the plastic region. It resembles such properties for steel and
can change the peak of the curve ultimately affecting the ultimate tensile strength
We can take a look at Figure 6, the hardness versus annealing curve and compare
it to our knowledge of heat treatment. A published result was not able to be found.
Knowing through the annealing processes hardness decreases it is a reasonable figure
approximation. Further investigation of the elastic modulus versus annealing temperature
reviled that they are independent of each other. Our data has elastic modulus fluctuating
at 15,000 megapascals. Published results have led the value to be closer to 11,000
megapascals. Our data showed the independence of annealing temperature as it should.
Calibration error could have made a shift in the data, increasing the slope of the elastic
region.
The Annealing process cannot say if it “worsen” or “betters” a mechanical
property. Projects ask for different needs. The annealing process is a way to maximize
Figure 13

performance of the material. Comparing Figure 7 to Figure 13 we can see the changes in
mechanical properties due to the annealing process.
With change in the microstructure comes change in mechanical properties. We
can use Figure 12 and the pictures of the microstructures to aide us in finding the
recrystallization of brass. Using published data, that of Figure 12, we can see the
recrystallization occurs between 200 – 500oC. Examining our data we can narrow the
window down saying most-to-all recrystallization occurs at 450oC. We can say this with
certainty looking at the grain boundaries of each sample. We see in the 450oC sample the
grain boundaries become very fine with which they are reorganizing each other and
relieving unwanted residual stress.
Data was shifted in some of our stress versus strain curves creating some error
when analyzing. The stress versus strain graphs found in Appendix A didn’t always start
at the origin. They sometimes started with negative values in which young’s modulus
could have been affected. We took class data resulting in some inconsistencies. Each
group has a method they follow with group members doing different task. Data is then
collected according to the specifications of each group.

Conclusion:
Our findings gave us trend lines similar to those of published data. We found
recrystallization to happen in the 750oC region. This comes from using the knowledge of
published data and the microscopic pictures provided to us. We find that hardness is
reduced with increasing annealing temperature. Using our data and resources, we come
to the conclusion that elastic modulus is independent of annealing temperature. With this
in mind we were able to find an accurate range of slopes giving us better results in
finding ductility for each sample. This experiment gave insides as to what mechanical
and microstructure changes occur with the process of annealing.
Glossary:

Elastic Modulus (E) – The measurement of stiffness in a particular uniform elastic

material. To find Young’s Modulus we take the ratio of stress over strain. We must keep
Hook’s Law in mind telling us force is proportional to elongations. Simply, the more
force excreted on an oject the longer the material gets. Graphing stress vs. strain and
taking the slope gives us the ratio, thus giving us Young’s Modulus.
E = stress/ strain
Yield strength – The stress point of a material when deformation begins to be non
reversible. This value can be determined from a tensile test, graphing stress vs. strain.
When the slope is no longer linear of we reach the yield strength ( point (2) from figure
1.) Prior of the yield strength the material can be described as elastic deformation in
which is can return to its original state. We gain the knowledge of the maximum stress
that can be applied without harming the function of the material

Figure 1

Ultimate Tensile Strength (U.T.S.) – This value can be determined using the
stress vs. strain graph. It is the maximum of the graph (Figure 1, points (4)) in which
necking occurs. Figure 2 shows the physical property of necking as where UTS is
measured. This value is proportional to the material and not the size of it.

Necking

Figure 2
 Ductility – A unit less number of how a material can be deformed without
fracture. Tensile stress is applied to the material; at the point of deformation ductility is
measured. The more ductile a material is the more stress and strain is needed to break it.

Figure 3

Ductility increases to the

right, needing more stress to
break the material

Toughness – The resistance of fracture when stress is applied. It can be related to

energy in the amount that is stored in the material before breaking. Calculated by finding
the area under a stress vs. strain curve for any given material. A simple integral can be
applied here.
εf = strain upon failure

Hardness – the resistance to various kinds of shape change when force is applied.
It is a unitless number used universally in the mechanical field.
 Appendix A:

Brass as Received

500
450
400
350
Stress (MPa)

300
250
200
150
100
50
0
0 0.05 0.1 0.15 0.2 0.25 0.3 0.35 0.4
Strain
y = 15059.34x - 162.30

Brass 250C

700
600
500
Stress (Mpa)

400
300
200
100
0
-100 0 0.05 0.1 0.15 0.2 0.25 0.3 0.35 0.4 0.45

Strain
y = 14999.62x - 77.56
 Brass 350

700
600
500
Stress (MPa)

400
300
200
100
0
-100 0 0.05 0.1 0.15 0.2 0.25 0.3 0.35 0.4 0.45 0.5

y = 15511.30x - 60.18 Strain

Brass 450C

400
350
300
Stress (MPa)

250
200
150
100
50
0
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8
Strain
y = 15262.77x - 206.61
 Brass 550C

600

500

400
Stress (MPa)

300

200

100

0
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9
-100
y = 14605.26x - 67.31 Strain

Brass 750C

450
400
350
300
Stress (MPa)

250
200
150
100
50
0
-50 0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1
Strain
y = 15084.94x - 128.28
Resources:

"Full Annealing." eFunda - Engineering Fundamentals n. pag. Web. 3 Mar

2010. http://www.efunda.com/processes/heat_treat/softening/annealing.cfm.

J.F.Shackelford, Introduction to Materials Science for Engineers, 4th edition, Prentice-

Hall, Inc., New Jersey, pp.305-345 (1996).

Schoenung, Dr. Julie Schoenung. "Annealing and Recrystallization." Wellman 106.

Davis, CA, 08 Feb. 2010.

Klink, Ian. “Recovery, Recrystallization and Grain Growth.” Eng45 Lab. Davis, CA, 13
Feb, 2010