MAE 351

Cold worked and recrystallized microstructures in brass

1. Objective

To examine the consequences of strain hardening, recovery, and recrystallization on the

microstructure of brass.

2. Introduction
Cold work (strain hardening) and its effect
Cold work is an alloy forming process that alters the shape or size of a metal by plastic
deformation. Cold work processes include rolling, drawing, pressing, spinning, extruding and
heading. They are carried out below the recrystallization point usually at room temperature. Cold
work causes increase of hardness and tensile strength and reduction of ductility and impact energy
values or strain hardening. The cold rolling and cold drawing significantly improve surface finish
too. When a polycrystalline alloy is subjected to cold working, new dislocations are introduced, and
this causes the density of dislocations to increase. In addition, as the amount of cold working
increases the distortion of the grains increase. First, they may become distorted and later it may be
hard to distinguish different grains. The increase in dislocations and the distortions of the grains
means that there is a certain amount of energy stored in the grains. As shown in Figure 1, cold
rolling will alter the equiaxied and randomly orientated grains into a directional grain orientation
along the rolling direction.

Figure 1.
a) Isotropic grains are approx. spherical, equiaxed & randomly oriented.
b) Anisotropic (directional) since rolling affects grain orientation and shape.

Percentage Cold Work – measurement

Cold work is measured with extension of the length or reduction of the area for rolled samples as
shown in Figure 2 and the measurement of cold work is given by:

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 (1)
or

(2)

Figure 2 Measurement of cold work.

Annealing
Annealing is a process where material is heated to at or above the recrystallization temperature of
the sample and then cooled down. The main purpose is to improve cold work properties by
increasing ductility and retaining most of the hardness. There are 3 steps involved with annealing:
recovery, recrystallization, and grain growth.

Recovery
The cold worked alloy is annealed in a short period of time. During recovery, some of the stored
internal strain energy is relieved through dislocation motion due to enhanced atomic diffusion at the
elevated temperatures. Recovery leads to annihilation of dislocations (Figure 3) and hence
reduction in the number of dislocations as shown in Figure 3.

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 Figure 3. Annihilation of dislocation by diffusion of atoms to the regions of tension.

Recrystallization
After recovery is complete, the grains are still in a relatively high strain energy state.
Recrystallization is the formation of a new set of strain-free and uniaxial grains that have low
dislocation densities. The driving force to produce the new grain structure is the internal energy
difference between strained and unstrained material. The new grains form as very small nuclei and
grow until they consume the parent material (Figure 4).

Figure 4. Process of recrystallization. (a) Cold worked grains, not annealed. (b) Recovery. (c)
Partial replacement of the strained and distorted grains with small nuclei of new crystals. (d)
Complete crystallization (small crystals).

Grain Growth
After recrystallization, the strain-free grains will continue to grow if the metal specimen is left at
elevated temperatures. As grains increase in size, the total boundary area decreases, as does the
total energy. Large grains will grow at the expense of smaller grains.

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Metallography
Metallography consists of the study of the constitution and structure of metals and alloys. Much can
be learned through specimen examination with the naked eye, but more refined techniques require
magnification and preparation of the material's surface. Optical microscopy is sufficient for general
purpose examination. However advanced examination and research laboratories often contain
electron microscopes (SEM and TEM), x-ray and electron diffractometers and possibly other
scanning devices.
Sample preparation is crucial. Incorrect techniques in preparing a sample may result in altering the
true microstructure and will most likely lead to erroneous conclusions. It necessarily follows that
the microstructure should not be altered. The metallographic sample preparation process include
step-by-step processes of sectioning, mounting, course & fine grinding, polishing, etching and
microscopic examination.
Sectioning
Operations such as shearing produce severe cold work, which can alter the microstructure of a
sample. Abrasive cutting (sectioning) offers the best solution to eliminate these undesirable
features; the resultant surface is smooth, and the sectioning task is quickly accomplished. Low-
speed cut-off wheels are utilized in cases where the heat created by standard abrasive cutters must
be avoided. Ample coolant and proper speed control are essential in all sectioning operations.

Mounting
Small samples are generally mounted in plastic for convenience in handling and to protect the
edges of the specimen being prepared.

Coarse Grinding
The purpose of the coarse grinding stage is to generate the initial flat surface necessary for the
subsequent grinding and polishing steps. As a result of sectioning and grinding, the material may
get cold worked to a considerable depth with a resultant transition zone of deformed material
between the surface and the undistorted metal. Course grinding can be accomplished either wet or
dry using 80 to 180 grit electrically powered disks or belts, but care must be taken to avoid
significant heating of the sample. The final objective is to obtain a flat surface free from all
previous tool marks and cold working due to specimen cutting. An important factor throughout the
Coarse Grinding and Fine Grinding Stages is that the scratches be uniform.

Medium and Fine Grinding

Medium and Fine Grinding of metallurgical samples are closely allied with the Coarse Grinding
which precedes them. Each stage of metallographic sample preparation must be carefully
performed; the entire process is designed to produce a scratch free surface by employing a series of
successively finer abrasives. Failure to be careful in any stage will result in an unsatisfactory
sample. The idea is to carefully move from one stage to the next where the abrasives become finer
at each successive stage. Movement from one stage to the next should only proceed when all of the
scratches from the preceding stage are completely removed. In general, successive steps are 240,
320, 400 and 600 grit SiC and the grinding rate should steadily decrease from one stage to the next.
Proper grinding involves the rotation of the sample between stages while the grinding angle must
be held constant during the grinding at any on stage. Recall that "The sample MUST be washed
thoroughly before proceeding from one grinding operation to the next"!

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Wet grinding is generally applied in medium and fine grinding to avoid possible side effects due to
heating such as tempering, transformation, aging, incipient melting, etc. Wet grinding also provides
a flushing action for loose particles and keeps sharp edges of the grinding medium exposed at all
times.
Repeated for Emphasis: Proper grinding involves the rotation of the sample between stages while
the grinding angle must be held constant during the grinding at any on stage.

Polishing
This final stage of polishing which involves the use of abrasives, suspended in a water solution, on
a cloth-covered electrically powered wheel. Following the final 600 grit fine-grinding stage, the
sample MUST be washed and carefully dried before proceeding to the first polishing stage! At the
polishing stages, even hard dust particles in the air which settles on the polishing cloth can cause
unwanted scratching of the specimen! Careful washing of the specimen and the operator's hands
must be carried out prior to each stage of polishing!

Etching
Microscopic examination of a properly polished, unetched specimen will reveal only a few
structural features such as inclusions and cracks or other physical imperfections. Etching is used to
highlight, and sometimes identify, microstructural features or phases present. Etchants are usually
dilute acid or dilute alkalis in a water, alcohol or some other solvent. Etching occurs when the acid
or base is placed on the specimen surface because of the difference in rate of attack of the various
phases present and their orientation. Etching will result in uneven surface. The unevenness will
reflect light in different directions (Figure 5). Under a microscope the surface of the etched sample
will show areas with different shades and details of microstructure.

Figure 5. As-polished and etched surfaces.

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Reference: See chapters 6-7 of the textbook for MEN 301- Materials Science and Engineering by
W. D. Callister, Jr., John Wiley and Sons. 1997

3. Experimental Procedure

1. You will be using the three 360 free cutting Brass (61.5 % Cu, 35.4 % Zn, 3.1 % Pb) specimens.
Specimen A is fully annealed as the reference. Use another fully annealed specimen B and apply
cold worked to about 10%CW.

Pieces A1 is cut from A. A1 will be used for metallography.

B1, B2, B3 and B4 are cut from B.

B1 will be used for metallography directly.
B2 will be annealed at 550°C for 10 minutes. B2 will be used for metallography.
B3 will be annealed at 550°C for 60 minutes. B3 will be used for metallography.
B4 will be annealed at 550°C for 4 hours. B4 will be used for metallography

2. Mount A1, B1, B2, B3, and B4 in plastic molds, grind, polish, and etch to make metallographic
samples. (The TA will give you some from previous labs)

Etchant for brass: 5 g Ferric Chloride, 10 ml Hydrochloric Acid, 5-10 g Ammonium

Persulphate, 100 ml Water.

3. Examine A1 that is without any cold working and record images. Measure the length and width
of 20 crystals.

4. Examine B1, B2, B3, and B4 and record images. Measure the length and width of 20 crystals.

4. Report

Report the micrographs of all the specimens that you observed.

If it is necessary draw cartoons of the microstructures by hand to do the following:

1. Compare the microstructures of A1 thru B4.
Evaluate the average aspect ratio (=Width/Length).
Discuss the effect of cold working on the microstructures, aspect ratio and average size of the
grains.

3. Plot aspect ratio as function of annealing time.

4. Plot average size as a function of annealing time.

What did you learn in this experiment? How can you apply this knowledge?