Sheikh Shahir Cold Working and Recrystallization KEM120702

TITLE

Cold Working and Recrystallization


ABSTRACT

The following experiment was conducted to apply cold working on pieces of copper metal followed to
observe any changes in their microstructure. This was followed up by annealing the said copper pieces
and determining the crystallization temperature. As a control, one piece of copper didnt undergo any cold
working while the other three were cold rolled to 10%, 30% and 50% respectively. After that, we cut each
piece into four samples and annealed them at 3 different temperatures: 200
o
C, 300
o
C and 600
o
C. The
batch that was left over didnt receive any treatment and were used as the control .Having being annealed
for a period of 30 minutes, we observed each sample using a microscope. This was followed up by testing
their hardness using a Vickers Hardness testing machine. Microstructures of each sample were drawn out
and the characteristics were observed. Also, a graph of hardness against cold-work degree for each
annealing temperature was plotted to observe the trend of the results.




INTRODUCTION

Cold working can be referred to as altering the shape or size of a metal by plastic deformation. Processes
include rolling, drawing, pressing, spinning, extruding and heading, it is carried out below the
recrystallization point usually at room temperature. Hardness and tensile strength are increased with the
degree of cold work whilst ductility and impact values are lowered. The cold rolling and cold drawing of
steel significantly improves surface finish.

Whereas hot working refers to processes where metals are plastically deformed above
their recrystallization temperature. As the material is above the recrystallization temperature, it can
recrystallize during deformation. The importance of this is that it keeps the material from strain
hardening and thus keeping the yield strength and ductility low. This is in extreme contrast to cold
working.





Sheikh Shahir Cold Working and Recrystallization KEM120702
The cold working process thats taking place in this experiment is known as cold rolling. In this process,
metal stock is passed through a single or more than one pairs of rolls in order to reduce its thickness and
make the thickness uniform. When the temperature of the metal is below its recrystallization temperature
this is known as cold rolling.



Fig 1: Example of Cold Rolling



Annealing, in metallurgy and materials science, is considered to be a process of heat treatment that can
be used to alter the properties of a material and make it more ductile and workable. It requires heating a
material above its critical temperature, maintaining a suitable temperature and then cooling it. Annealing
can induce ductility, soften material, relieve internal stresses, refine the structure by making it
homogenous and improve cold working properties.
For the metal, this process simply involves heating the material for a while until it glows and then slowly
letting it cool down to room temperature. It can also be cooled by quenching in water, unlike ferrous
metals such as steel which must be cooled slowly to anneal. Annealing prepares the metal for further
work such as shaping, stamping or forming.

Hardness give a measure of how resistant a solid matter is to various kinds of permanent shape change
when it is exposed to a force. Macroscopic hardness is generally characterized by strong intermolecular
bonds, but the behavior of solid materials under force is complex; therefore, there are different
measurements of hardness: scratch hardness, indentation hardness, and rebound hardness. In this
experiment the pieces of copper metal undergo Vickers Hardness Test.

The Vickers test can be used for all metals and has one of the widest scales among hardness tests. The
unit of hardness given by the test is known as the Vickers Pyramid Number (HV). Vickers hardness test
use a 136 pyramidal diamond indenter that creates a square indent.
Sheikh Shahir Cold Working and Recrystallization KEM120702
HV = Constant x test force / (indent diagonal)
2

The constant is a function of the indenter geometry and the units of force and diagonal. The Vickers
number, which normally ranges from HV 100 to HV1000 for metals, will be increased as the sample gets
harder. Tables are available to simplify the calculation, while all digital test equipment do it
automatically. A typical Vickers hardness is specified as follows:
212HV0.5
Where 212 is the calculated hardness and 0.5 is the test force in kg.

The biggest advantage of Vickers is its scale, which comprises the smallest and the highest
hardness values in one scale. It is thus very suitable for laboratory tests.
Most of the disadvantages of Vickers are based on the long duration of the whole procedure
because the indentation must be measured optically (with the help of a miscroscope or projector).
This, of course, also is a source for measuring errors. However, modern, automatic image
evaluation computer systems reduce this source of errors significantly.
The surface must be well prepared and the penetrator must be applied evenly. Otherwise, the
smallest inclination would cause irregularities in the indentation. Thus, the Vickers procedure is
not suitable for routine tests.
The indentation is not well readable on some materials because of the irregular distribution of the
load (more load on the edges than on the sides of the pyramid).

OBJECTIVES

There are two objectives in this experiment:
1) To do cold working on copper and observe any changes in microstructure.
2) Followed by annealing the cold worked metal and find out crystallization temperature.









Sheikh Shahir Cold Working and Recrystallization KEM120702
RESULTS

Table 1: Experimental Results
Temperature
(C)

Percentage of Cold
Working (%)
Vickers Hardness Number
(HV)
Room
Temperature
10.00 124
30.00 130
50.00 122

200
10.00 129
30.00 135
50.00 144

300
10.00 48.9
30.00 45.7
50.00 48.5
600
10.00 39.4
30.00 46.1
50.00 46.2




0
20
40
60
80
100
120
140
0 10 20 30 40 50 60
V
I
C
K
E
R
S

H
A
R
D
N
E
S
S

B
U
M
B
E
R

(
H
V
)

PERCENTAGE COLD WORKED (%)
Hardness vs Percentage Cold Worked
Room Temperature 200 oC 300 oC 600 oC
Sheikh Shahir Cold Working and Recrystallization KEM120702
DISCUSSIONS
Cold working and hardness:

1) It can be seen from the graph that, at room temperature, the hardness decreases slightly at first
before rises, as the cold worked percentage increases. This in turn shows that the metal undergoes
strain hardening when it is cold rolled.
2) Whereas when annealing at a temperature of 200
o
C, the hardness is seen to increase with
increased percentage of cold-rolling. Also, a large difference in hardness is seen between samples
of 10% and 30% cold rolled. For the temperature of 300
o
C, the hardness is fairly constant and for
600
o
C, the hardness increases and becomes constant.
3) When the copper metal is cold-worked far below its melting point, the dislocation density
increases rapidly during plastic deformation. The dislocations together with other obstacles such
as grain boundary and inter-metallic particles prevent further dislocation motion. This results in
an increase of the hardness. The greater the amount of dislocation density, the greater the effect of
work hardening.
4) The annealing process at temperatures of 200
o
C and 300
o
C causes the internal stresses to be
relieved by heating the metal. The crystal lattice is broken by plastic deformation which causes
distortions and results in the cold worked metal in being thermodynamically unstable resulting in
a decrease in hardness.
5) If we allow the temperature to be sufficiently high, the metal will try to achieve equilibrium
through three stages, namely recovery, recrystallization and grain growth. The process of
recovery is the result of dislocations interacting with each other at high dislocation densities, by
virtue of attractive and repulsive forces. The line of 200
o
C and 300
o
C in the theoretical graph
shows the process of recovery. Recovery softens a material by lowering the dislocation density.
Hence, the hardness number is decreased while the ductility goes up.



Annealing Temperature and Hardness
The general trend is that the higher the annealing temperature, the lower the hardness after
annealing. This result agrees with the theory.
This is because, when further heating is applied to the metal, nucleation and growth of new
crystals will replace all the deformed crystals of the cold worked metal. This is recrystallization
process. The hardness and strength of the metal are greatly reduced while ductility increases.

Observations under microscope
In general, grain patterns followed the theoretical predictions.
For the rolled (but not annealed) grain, the directionality of the grains increases with increasing
percentage cold work. The grains are equiaxed for 0% cold work, but gradually become more elongated
as % cold work increases. For the 50% cold worked sample, grains appear as long, thin pieces
longitudinal to rolling direction. This is because thickness of the grains decreases as the length increases.
For the samples annealed at 200
o
C, a similar pattern can be observed. As % cold work increases,
the grains show more elongation in rolling direction. However, it is also observed that for the 30% cold
worked sample, there are many small grains at the grain boundary of larger grains. For the 50% cold
Sheikh Shahir Cold Working and Recrystallization KEM120702
worked sample, this is even more obvious as many small grains are formed. This is because increasing the
amount of cold work prior to annealing increases the instability of the structure. This reduces
recrystallization temperature and speeds up recrystallization rate. Hence, the higher the degree of cold
work, the smaller, new, equiaxed grains are formed.
For the samples annealed at 300
o
C, while it is visible that some degree of elongation occurs as %
cold work increases, it is not very obvious. This is because at 300
o
C, recrystallization occurs quite fast
resulting in the elongated grains being replaced by newly formed, equiaxed grains. For the 10% cold
worked sample, several small equiaxed grains are already visible although the degree of cold work is low.
For the 30% cold worked sample, some of the equiaxed grains are growing significantly. For the 50%
cold worked sample, there are many small equiaxed grains and it is visible that many grains are non-
directional they are the grains that are formed during heat treatment and subsequently grew in size to
replace the directional grains.
For the samples annealed at 600
o
C, grains no longer appear directional even if cold worked. Even
for the 0% cold worked sample, there are signs of nucleation. For the 10%, 30% and 50% grains, there are
very few grains that are elongated. They are mostly large equiaxed grains with some newly formed small
grains at boundaries. The higher the % cold work, the smaller, equiaxed grains are formed.
There are a few special observations worth extra mentioning. The first is the appearance of some
very black spots under the microscope. Although we cannot be certain of the composition of the black
spots, they are likely to be copper oxide regions, which are formed when copper was heated in the
presence of oxygen.
The second is that some grains appear slightly darker than the others. There are two reasons for
this observation. Firstly, the amount of light reflected from the crystal grains are dependent on
crystallographic orientation some orientations more favourably reflect more light. Secondly, consistent
with our observation, highly deformed grains tend to be darker. This is because dislocations, when view
with greater magnification, appear as dark lines. On a smaller magnification, such as the degree used
during our experiment, dislocations cannot be seen but the effect remains grains that are more deformed
(more elongated) have high dislocation concentration and hence appear darker due to the light-scattering
effect of the distorted lattice caused by deformations. The same reasoning applied to the small, newly
formed equiaxed grains they appear brighter because they are less plastically deformed.
The inconsistencies of the results with the theory are caused by some possible reasons or errors
that may occur during the experiment:
1. The actual percentage of thickness reductions after cold-roll are not exactly the same with the one
desired.
2. The surfaces of the copper pieces are not perfectly smooth due to oxide layer. This will affect the
accuracy of readings measured in Vickers Hardness Test.
Thus, in this experiment, some precaution steps have to be taken to minimize the discrepancies
and to get more accurate results:
1. The thickness of copper piece is reduced slightly for every pass when rolling process of the
copper.
2. All the copper pieces are cleaned by using sand papers before the Vickers hardness test is
performed.
3. The crucibles are labeled first before putting them into the furnaces to avoid confusion.


Sheikh Shahir Cold Working and Recrystallization KEM120702

CONCLUSIONS
To conclude, it can be seen that cold working causes microstructural change in copper alloys which is the
elongation of copper grains. Generally, the higher the cold working percentage, the higher is the hardness.
In addition to that, annealing softens the copper samples. The higher is the annealing temperature, the
lower the hardness of the sample after annealing. Annealing causes smaller, equiaxed grains to replace the
elongated grains formed during cold working. Unfortunately, some of the experimental results are
inconsistent with the theory due to experimental errors.

REFERENCES
1) Wikipedia.
2) Laboratory sheet.
3) Material Science and Engineering : An Introduction by William D. Callister Jr., David G.
Rethwisch
4) http://metals.about.com/library/bldef-Cold-Working.htm
5) Howstuffworks.com