Lab 3: Recovery, Recrystallization and Grain Growth

July 24, 2015

Steven Whittlesey
T.A.: Alvin Mao
Section: 2

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Abstract
A set of 70/30 brass samples annealed at 250oC, 350oC, 450oC, 550oC, 650oC, 750oC,
and one untreated sample at 25oC were put to a tensile test. The samples that were annealed
at higher temperatures stretched out more than low temperature samples. Using the tensile
test data, the youngs modulus, yield strength, ultimate tensile strength, ductility, and
toughness were measured. Using pictures of microstructures of differently heat treated
samples, a corresponding grain size was calculated. As the temperature increased, the results
showed an increase in toughness, ductility, grain size and youngs modulus and a decrease in
yield strength (YS), Ultimate Tensile Strength (UTS), and hardness. The recrystallization
temperature was determined to be 450oC. The increase in grain size brought about by the
annealing is the cause for the stated change in the mechanical properties, as a larger grain
size results in a weaker but more elastic material.
Introduction
In this experiment, heat treated samples of brass were put to a tensile test . The
purpose of this experiment is to relate properties of a material to its microstructure and
history of processing. Microstructures show grain size, which is responsible for many
properties of a material. If the grain size is large, for example, the material will be very
elastic or ductile. If a material has high ductility, it means that it has a greater ability to be
stretched. This high ductility is responsible for determining the amount of energy needed to
completely fracture a material, which is also called toughness. Larger grain size also means
that a material is of low strength. The material will stretch too easily, which means less
stress is required to deform it. Due to this, larger grain size affects yield strength, hardness,
and UTS inversely. As the material becomes more elastic, the modulus of elasticity, or
youngs modulus, increases.
Grain size itself is a product of processing. The processing dealt with in this
experiment is annealing a cold worked sample. Cold working is to heat a sample and then
immediately cool it so that there is an increase in the number of defects. The increased
number of dislocations in the sample creates a resistance to plastic deformation by raising the
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yield strength of the sample. This strengthens a material but also makes it brittle. Annealing
itself is heating a material to a temperature and letting it stay there for some specific time.
Annealing is used for making a hard material easier to shape and bend to fit given parameters
like when choosing materials suited for designing and building a machine or construction. In
this process, the material may go through three stages depending on the temperature. The
first stage is called recovery. This stage happens at a moderate temperature. During this
stage, the sample recovers grains and removes some defects. After recovery is the second
stage, recrystallization, happening at a third to a half of the melting temperature. During
recrystallization, new grains are formed at the old grain boundaries and further defects and
dislocations are removed. The last stage is grain growth, which happens at temperature
higher than during recrystallization. This stage is when the grains fuse together to form larger
grains. These stages also affect the grain size and the mechanical properties of the material.
During recovery, the material weakens, which decreases UTS, YS, and hardness. During
recrystallization, the material weakens again but does so drastically, because a significant
number of defects are removed. This results in an increase of toughness, ductility, and
youngs modulus and a decrease in UTS, YS, and hardness. The last stage of regrowth
continues this trend but at a much slower pace. This experiment aims to observe these
changes of the properties and see if they correctly correspond with the theory of how
properties change at each stage. As a result, it can be expected or predicted that the changes
described above will be the changes seen at the different temperatures in the lab data.
Methods
The experiment began with recording the measured parameters, in millimeters using
Westward digital calipers accurate to 0.01 mm, of each 70/30 brass sample which consisted
of six samples treated at 250oC, 350oC, 450oC, 550oC, 650oC, 750oC respectively and one
untreated sample at25oC . The samples were then taken to the Instron 4204 tensile tester
with Bluehill 3 software and placed between the grips. Tensile tests were run using a constant
elongation rate of 2.54 mm/min. The test parameters of the sample input into the machine
and the test began. Using measuring software to monitor the applied load as a function of
elongation, the machine converted load vs. elongation to create a graph of stress vs. strain.
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Some of the recorded data was observed to be negative. This error can be amended by adding
the magnitude of the difference between the initial value at the origin and zero to each
recorded value on the graph. Other graphical errors that were observed were the vertical
lines. Any vertical lines that appeared on the stress vs. strain graph were removed because
the lines made no physical sense.
The hardness tests were performed after the tensile tests in order to avoid compromising
mechanical properties of the samples. Using the Buehler Macromet Hardness Tester (HTM),

the hardness of each sample was measured in HRB using a load of 100kgf and a

1
16 in.

steel sphere indenter and applied to the wide part of the samples. The hardness was
measured three times and an average was taken.

Example of Stress Strain Plot at 350C

450
400
350
300
250

350 Celcius

Stress [] (MPa) 200

150
100
50
0
0

0.1

0.2

0.3

0.4

Strain [] (mm/mm)

Figure 1: Example of Stress Strain Curve

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Using each set of data, a stress vs. strain curve such as Figure 1 can be created and
used to calculate the toughness, ductility, Youngs Modulus, Yield Strength, and UTS for
each sample.
The strain, (mm/mm), was calculated using the gauge length, Lo (mm), and the
extension L (mm).
=

LoL
Lo

The stress, (MPa) was calculated using load, P (kN), and Ao (mm2).
=

P
A o /1000

A o =wt

With Ao (mm2), being cross-sectional area calculated by width, w (mm), and thickness, t
(mm).
The toughness (MJ/m3) was calculated by finding the area under the stress vs. strain curve.
This was done using the trapezoid sum.
Toughness= ( avg )

avg =

n+1 + n
2

= n+1n

Youngs Modulus,

(MPa), is simply the slope of the initial linear part of the stress vs.

strain curve.

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 =Eb

The ductility (mm/mm) is found using the strain at fracture, stress at fracture, and Youngs
Modulus.
Ductility= fracture

fracture
E

The UTS (MPa) is simply the highest stress value on the stress vs. strain curve.
The Yield Strength (MPa) is calculated by offsetting the initial linear curve by .2% and
finding the stress value at the point of intersection between the new offset line and the
original stress vs. strain curve.
Yield Strength=E( .002 )b

intersection is the strain at the point of intersection.

HRB average was calculated by
HR C Bavg =

HRC 1+ HRC 2+ HRC 3

3

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Figure 2: 250C Micrograph

In order to calculate grain size, a circle of known radius was drawn on a picture of a
microstructure like in figure 2. In this circle, the number of grains was counted using full
grains as one grain and partial grains as a half grain. The grain size was calculated using the
equation:
Average Grain

Area
N Grains

The normalized plot values were determined using the equation:

Propert y Normalized=

Propert y iPropert y minimum

Propert y maximum Propert y minimum

Results

Temp
(C)

UTS
(MPa)

YS
(MPa)

E
(/)

650

525.5
357
544.0
682
422.0
911
400.9
318
345.0
448
306.1
163

408.6
308
417.9
659
321.6
163
220.0
94
105.5
963
80.01
663

1927
4
2773
8
2655
4
2787
8
2065
0
1704
5

750

269.5
994

49.46
495

2283
3

25
250
350
450
550

Ductility(mm
/mm)

Toughn
ess
(MJ/m^
2)

0.826682

137.54
2
134.53
18
131.98
67
158.92
169
211.85
475
201.46
031

0.719235

105.00
29

0.291182
0.262195
0.334017
0.44358
0.747614

Hardne
ss
(HRB)

61.5
63.4
64.2
53.26
67
20.6
0.633
333
28.46
67

Grain
Size
(m)

11.04
6
17.28
3
18.31
4
11.13
3
19.21
3
0
82.91
67

Table 1: Properties
As the annealing temperature goes up, there is a general increase in youngs modulus,
ductility, toughness, and grain size and a general decrease in yield strength, UTS, and
hardness. Although a general increase is observed, the youngs modulus wavers in value.
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Contrarily to the trend set by previous values, the ductility and toughness of the sample
annealed at 750oC is lower than the previous sample. There is a large jump in grain size
between 550oC and 750oC. The grain size of the 450oC sample is also a trend breaker.

Temperat
ure (C)
25
250
350
450
550
650
750

UTS
(MPa)
0.9659
37

YS
(MPa)
0.9776
65

1
0.7758
05
0.7369
15
0.6341
94
0.5626
43
0.4955
25

1
0.7694
8
0.5265
84
0.2526
43
0.1914
43
0.1183
47

E (/)
0.6913
7
0.9949
78
0.9525
07
1
0.7407
27
0.6114
14
0.8190
33

Ductility(mm/m
m)
0.051351
0
0.127234

Toughne
ss
(MJ/m^
2)
0.30452
5
0.27635
4
0.25253
5
0.50461
3

Hardne
ss
(HRB)
0.9708
63
0.9913
67

1
0.90272
1

1
0.8820
15
0.5294
97
0.3140
29

0.809655

0.321327
0.859929

Grain
Size
(m)
0
0.0867
81
0.1011
26
0.0012
11
0.1136
35

Table 2: Normalized Properties

These normalized values simply reflect the values displayed in Table 2. It is easier to notice
the trends mentioned earlier.

Stress vs Strain of Brass at Different Annealing Temperatures

350

Room Temperature

300

205 Celsius

250

350 Celsius

200

450 Celsius

Stress (MPa) 150

550 Celsius

100

650 Celsius

50

750 Celsius

0
0 0.2 0.4 0.6 0.8 1
Strain (mm/mm)

Figure 3: Stress vs. Strain Curve

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As the temperature at which the sample was annealed at increases, the samples are
able to handle more strain and less stress. The most significant change occurs between 250 oC
and 350oC. The only trend breakers are the samples that were annealed at 250oC and 450oC.
The sample at 250oC is able to handle more stress than the sample before it and the sample at
750oC can handle less strain than the one before it.

Mechanical Properties vs Annealing Temperature

1.2
1
UTS

0.8
Normalized Properties

Ductility

0.6

Hardness

0.4

Grain Size

0.2
0
0 200 400 600 800
Annealing Temperature (C)

Figure 4: Normalized Properties

The normalized curves of the selected properties show a general increase in grain size
and ductility and a general decrease in UTS and hardness as the annealing temperature
increases. Most of the curves seem to intersect at around 450 oC. This is the recrystallization
temperature.
As the temperature increased, the area per grain of a microstructure increased. The
outlier is the large change in grain size at 450C compared to 350C.
Discussion
The significant decrease in hardness between the 450oC and 550oC samples, as shown
in tables 1, 2, and figure 2, is due to the stage of the annealing process the samples range
from. The lower temperature sample is in the recovery stage while the higher temperature
sample is in the recrystallization stage. In the recovery stage, the sample still maintains a
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significant number of defects from cold working. These defects, although decreasing in
number, are still of higher quantity than the number of defects found during the
recrystallization stage. These relatively high numbers of defects is responsible for the
relatively high hardness. The sample in the recrystallization stage displays a significant
decrease in the number of dislocations or defects when compared to a sample in the recovery
stage. These significantly low number of defects cause for a very large decrease in hardness.
This drop in hardness also is reflected in the general decline in the UTS values of the
samples as the temperature increases. This drop is seen clearly in table 2 and figure 2. Like
UTS and hardness, the yield strength also decreases significantly between 450 oC and 550oC.
This is because the yield strength is dependent on how hard a sample is to stretch or deform.
If the sample is able to be easily stretched, then that means there is less stress required to
deform the sample. This results in a lower yield strength value. As the temperature
increases, a material is able to deform under lower amount of stress. In relation to yield
strength, this means that as the temperature increases, the yield strength decreases. This is
supported by the lab data.
Table 2 shows the increase in youngs modulus, ductility, and toughness as the
temperature increases. This is due to the stage of annealing a sample is in. For 250 oC and
350oC, the sample is in its recovery stage. As explained earlier, this stage sees a decrease in
defects in a material. Due to this decrease, the material slightly softens and becomes slightly
more ductile. An increasing ductility means the material will be able to stretch or deform
easier. This increase in tendency to deform is, by definition, cause for an increase in youngs
modulus. Since the material is able to stretch farther than itself at a lower annealing
temperature, it will fracture after a longer amount of strain. This is a key aspect in
calculating toughness. Toughness is the area under the stress vs. strain curve. Looking at
figure 1 shows the area increasing due to the strain increasing faster than the stress
decreasing. For the recovery stage, there isnt a significant change in ductility, or strength,
which is the reason for the almost nonexistent change in toughness displayed in table 2.
During the recrystallization stage between 450oC and 550oC, the changes are significant. As
explained earlier, during this stage, the number of dislocations decreases drastically. As a
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result, the material significantly gets weaker and ductile. This significant increase in the
deformability of the material results in a large change in ductility, youngs modulus, and
toughness. Because the largest changes happen at the recrystallization temperature and the
results display the largest changes happened at around 450oC, the recrystallization
temperature is determined to be 450oC.
After the recrystallization stage is the regrowth stage. This stage happens between
550oC and 750oC. During this stage there is no significant change in most properties.
During this stage, the grains fuse together to form larger grains, which is the reason for the
large increase in grain size during this stage. The other properties continue to follow their
original trends at a much slower pace than during the recrystallization stage. This is because
most defects have been removed by the time of regrowth.
The microstructures of the different samples show an increase in grain size with an
increase in temperature. The grains gradually merge together during the recovery stage, as
the grain boundaries are blurred due to decrease in defects. During the recrystallization
stage, however, new grains are formed at the grain boundaries. This means for the same
amount of area, there are a higher number of grains, which results in a smaller grain size.
The microstructures of the samples in the regrowth stage have an enormous grain size
compared to previous stages. This is due to the grains fusing together in the regrowth stage.
Grain size determines the mechanical properties of a material. When grain size is
large, the material has a low amount of defects and vice versa. A material with low amounts
of defects is more ductile, and overall weaker than a material with high defects. This is
because defects strengthen a material. Annealing a material such as brass essentially frees
the material of its defects or dislocations, and consequently, its strength. The larger grain
size means, in simpler terms, a material has a low amount of areas at which it can break and
a higher amount of areas at which it can stretch. Its the difference between breaking a single
entity and breaking two fused entities. The single entity requires more energy to break, and
is more resistant to fracture than the set of fused entities. For this reason, larger grain size

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causes for a higher toughness, higher ductility, and a higher youngs modulus, while a set of
smaller grains are stronger but break under lower strain.
The experiment confirmed most of the initial predictions regarding the ductility,
toughness, UTS, grain size, yield strength, and hardness. Errors in the data could be due to
incorrectly choosing values to estimate in plotting, and incorrectly discarding data at the ends
of the stress vs. strain curves. Preventative measures such as determining clearer points of
fracture and determining linear portions can help bring about more accurate results.
Conclusion
The samples annealed at different temperatures did reflect the stages of annealing
they were supposed to be in. The lower temperature samples were in recovery, displaying
theorized changes in the mechanical properties. The mid temperature samples were in
recrystallization, displaying significant changes in mechanical properties compared to those
values of recovery. The samples in regrowth show a slower paced change as predicted. The
recrystallization temperature was determined to be 450 oC due to the immense change present
during that temperature. These properties were in relation to the grain size in a way that a
larger grain size resulted in smaller strength and higher elasticity, while a smaller grain size
correlated with higher strength and lower elasticity. The reasons for this are because larger
grain size is product of a smaller number of defects, which results in high elasticity and low
strength. The regrowth stage did result in a drastic increase in grain size, just as it should.
The processing history of a material and its microstructures affect the grain size, which in
turn affects the mechanical properties of a material. The small structures that make up an
entire entity and shape every facet of its properties are directly a result of processing. This
experiment only provided further evidence to such theory.
References
Shackelford, James F. Introduction to Materials Science for Engineers. 8th ed. New York:
Macmillan, 1985. Print.

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