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1. Introduction:

Metallography, this word mean the study of the structure and constitution and components of
metals and alloys, using microscopy and magnifications.
Using microscopy gives the experimenter a lot of critical information like size and shape of the
grains, presence of micro defects (such as segregation, hair cracks, and nonmetallic inclusions),
and distribution of secondary phases.
And the metallographic examination used in quality control to predict and explain the mechanical
properties.
Grains, known as crystallite region separated regularly. Boundary grain is an interface between
two grains, or crystallites. And tend to decrease the electrical and thermal conductivity of the
material. See Fig (1) grains and boundary grain.


At first place the experimenter should prepare a specimen to
determine the grains. Using some machine to do a processes on the
specimen, at the beginning sectioning (cutting), and passing through
mounting, course grinding, fine grinding, and polishing, etching and
finally microscopic examination. See Fig (2)




Fig (1): Grains & Boundary Grain
FIG (2): Preparation Steps

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2. Objective:

To prepare the specimens surfaces to be examined by the microscope.
To learn and to gain experience in the preparation of metallographic specimens.
To be able to prepare my future specimen.
To become familiar with machines using to prepare the specimen.
To make sense with relation between number of grains and mechanical properties.


3. Equipment:

The experiment has been done step by step in sequence using a lot of machines listed below:
1. Minitom: Small, automatic precision cut-off machine for sectioning all material graphic
and ceramic specimens. This machine cuts the specimen slowly to produce fine surface
without heavy inclusions. See Fig(3)

2. Metason: Ultrasonic Cleaning for effective ultrasonic cleaning of metallographic,
ceramic, and mineralogical specimens. See Fig (4)

Principle of work:
The ultrasound which is transferred to the liquid causes the propagation of pressure waves
in the tank. These pressure waves involve a continuous change of the pressure in the liquid
so that, as a result of sub-pressure, innumerable microscopic evacuated bubbles are formed
which will soon expand and implode (capitation).
These implosions give the cleaning liquid a high speed locally so that dirt and loose
particles are removed from the specimens which are immersed into the liquid.

3. LaboPress-3: Semi-automatic mounting press for hot mounting of all materials. See
Fig(5)








FIG (5): LaboPress-3
FIG (4): Metason FIG (3): Minitom

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4. LaboPol (grinding and polishing machine): Machines for grinding, lapping and polishing
for 200 or 230 mm discs. See Fig(6)







5. LaboForce: Specimen movers for semi-automatic preparation of materialographic
specimens on LaboPol grinding and polishing machines. See Fig (7)
6. LectroPol-5: Automatic, microprocessor controlled electrolytic polishing and etching of
metallographic specimens. See Fig (8)







MD-System Consumables:
a. MD-Disc
TM
is the supporting disc for all preparation surfaces. See FIG (9)

b. MD-Primo
TM
is a SiC embedded disc designed for plane grinding materials in the HV 40-
150 hardness range. See FIG (10)





FIG (6): LaboPol
FIG (10): MD-Primo FIG (9): MD-Disc
Fig (7): LaboForce
Fig (8): LectroPol-5

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c. MD-Allegro
TM
Fine grinding of materials harder than HV150 is carried out in one step on
MD-Allegro using DP-Suspension or DP-Spray. See Fig (11)

d. MD-Largo
TM
Fine grinding of soft materials in the HV 40-150 hardness range is carried
out in one step on MD-Largo using DP-Suspension or DP-Spray. See Fig (12)






And there another type of MD-System Consumables, like MD-Cloths
TM
, MD-Pian and MD-
Fuga.
4. Procedure:

1. At first choose the material to test, then apply the sectioning process using Minitom
machine which gives a specimen with smooth surface by slowly sectioning.

a. Adjust the position of the cut by turning the micrometer screw.
b. Push weights of the specimen holder arm back.
c. Adjust the cutting pressure with the front weight.
d. Set the adjustable knob, CUTTING SPEED, to the lowest speed.
e. Press the button, START.
f. Adjust the speed of the cut off wheel on the adjustable knob, CUTTING speed, (for
127 mm (5'') cut-off wheels the speed should be not exceed 300 rpm).

2. Clean the specimen from smooth inclusions, by using ultrasonic cleaning machine
Metason (cleaning machine)
g. Start cleaning, set the timer for the amount of time you wish the specimen to be
cleaned.

3. Take the specimen to hot mounting using LaboPress-3 to add surrounding by an organic
polymeric powder which melts under the influence of heat _about 200 _ and high
pressure applied by a piston, to give a high quality mold with intimate contact between the
sample and the polymer.
FIG (12): MD-Largo FIG (11): MD-Allegro

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Using table (1&2) and the equation below, the experimenter know the amount of polymer which
should use, time heating and cooling processes and the forces and temperature of the last two. And
this is important to avoid something wrong as shown in Fig (10)



Min no. of Spoons =
1.2Hcght o] sumpIc
Hcght o] onc spoon o] csn

And the factor 1.2 is multiplied to eliminate variation in the resin densities and the measuring
during mounting, height of 1 Spoon (15 ml) of Resin after Mounting in an Empty Cylinder.
To apply this equation we have to know that cylinder Dia. 30 mm and sample height in Polyfast
process 11.3 mm (0.44 in.) and in Multifast process 8.9 mm (0.55in.)
We use the Polyfast process, then height of sample 11.3 mm,
Then, Min number of spoons =
1.211.3 mm
15 mm
= u.9u4 1

Cylinder dia: 30 mm
Resin: mm inch
PolyFast 11.3 0.44
MultiFast (black) 8.9 0.35
Cylinder dia. Resin heating Cooling
30 mm
Type Quantity Time Temp. Force Time Rate
[spoons] [ml] [min] [
o
C] [kN] [min]
PolyFast 1.5 23 4-6 180 20 2-3 HIGH
MultiFast
(block)
2 30 4-6 180 20 2-3 HIGH
Fig (10): Errors
Table (2): Mounting Process
Table (1) Resin Height

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a. Placing the specimen
1- Press the hold RAM UP to raise the lower ram to its upper limit.
2- Apply "Mould Release Agent" to the surface of the lower arm.
3- Place the specimen on the ram. The specimen must be clean, dry, and free from
grease. 5the distance between the specimen and the cylinder wall must be minimum
3 mm to avoid cracks in the resin.
b. Pouring resin over the specimen
1- Press and hold RAM DOWN to the lower the ram to its lower limit.
2- Fill a suitable amount of resin into the cylinder by means of the enclosed funnel.
c. Installing the top closure.
1- Remove the resin from the upper part of the mounting cylinder.
2- Clean cylindrical surface of the upper ram. Cured resin can easily be removed
without damage to the surface of the ram using the scraper.
3- Apply "Mould Release Agent" to all accessible surfaces of the upper ram.
4- Place the top closure with upper ram on the mounting cylinder.
5- Press the closure straight down, turning it counterclockwise until you hear a stick.
6- Press the top closure down and turn it clockwise until its lower limit.
7- Turn the top closure quarter of a turn back.
b) Starting the mounting process
1- Set the force.
2- Set the heating time (5 minutes).
3- Set the heating temperature (180/150
o
C).
4- Set the cooling time (2.5 minutes).
5- Press start, and the process will run automatically.
c) Stopping the mounting process
The machine automatically stops and relieves the pressure when the cooling time has
elapsed.
d) removing the top closure
1- Turn the top closure counter clockwise until released from the thread.
2- Press Ram up to raise the lower ram to its upper limit.
3- Place the top closure in the top closure holder.

4. The fourth step is to clean the specimen surface from impurity, scratches, flaws, stains,
inclusions and other imperfections which make the surface of specimen more difficult to
test, be free from all traces of disturbed metal, and reveal no evidence of chipping due to
brittle intermetallic compounds and phases and to retain non-metallic inclusions. And to
achieve last objective, the specimen must pass through grinding and polishing using
LaboPol machine.

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Firstly insert the suit grinding disc into machine, then put the specimen on grinding disc
and adjust the force applied on the specimen. As shown in Table (3)
















In grinding and polishing process, there is three types of grinding disc and used according to the
surface and other articles. In this experiment the MD-Largo and MD-Primo used for grinding
process. And MD-Dac and MD-Nap used for polishing process, and there is a disc to make the
final surface smooth. And see table (4) for grinding and table (5) polishing processes.









Indication
Force
(N)
0 0
1 2.5
2 5
3 7.5
4 10
5 12.5
6 15
7 17.5
8 20


Surface MD-Primo 220 MD-Largo
Abrasive SiC DP-Suspension
Lubricant Water Green/Blue
rpm 300 150
Force(N) 120 180
Time (min) Until Plane 5
Table (3): Applied Force
Table (4): Grinding processes

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5. Electrolytes(Etching): LectroPol-5

Electrolytes:
1- Electrolyte E5-I, E5-II and E5-III: for electrolytic polishing of steel with disturbing
impurities, low carbon steel, cast iron and copper alloys.
2- Mix E5-I, E5-II and E5-III just before use. For etching surfaces for material graphic
preparations
3- Electrolyte D2: for electro polishing of copper and copper alloys.

In this experiment the External Etching method was used, and J
2
as an Electrolyte, by the steps
listed below:
1- Connect the plug for the unit for the external etching to the back of the control unit.
2- Fill the bowl with the required electrolyte.
3- Seize the specimen with the pair of pliers.
4- Dip the specimen face down into the electrolyte.
5- As soon as the specimen is immersed in the electrolyte, countdown of the pre-set time
starts.
6- When the time has expired the voltage is switched off and the etching process is stopped.

Note: Avoid contact between the etching bowl and specimen or the pair of pliers. This will
result in a short circuit and the specimen not being etched correctly.



Surface MD-Dac MD-Nap or MD-Chem
Abrasive DP-Suspension OP-S or OP-U
Grit / Grain size 3m -
Lubricant Green/Blue -
rpm 150 150
Force(N) 190 60
Time (min) 5
Table (5): Polishing Process

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6. Results:

After these processes, the specimen is prepared to test in microscope and get a picture which show
the grains. And use a picture to determine the ASTM of copper alloy. See Fig (11)

Sample
material
Etchant Composition Remarks
Carbon
steel
(Usually 2%)
(nitric acid)
HNO3 1-5 ml
Ethyl alcohol 100ml
Immersion. Time ranges
from a few seconds to a minute
Carbon
steel
Picral (picric
acid)
Picric acid 4g
Ethyl alcohol 100ml
Immersion. Time ranges
from a few seconds to
Over a minute.
Aluminum
Hydrofluoric
acid
HF (concen) 0.5ml
H2O 99.5ml
Swab for 15 sec.
Table (6): Electrolytes (Etching).
Fig (11): Grains of Copper Alloy

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1
Why should the specimen be roughly washed after each stage during either grinding or
polishing?
As soon as the process finishes the sample must be washed and cleaned to avoid any further attack
of the surface

2
Why is fine grinding performed wet?
Because it has higher capacity per unit mill volume, it makes possible the use of wet screening or
classification for close product control, it eliminates the dust problem, and it makes possible the
use of simple handling and transport methods such as pumps, and pips

3
What is the purpose of etching metallographic samples?
Etching metallographic samples uses to determine the ASTM which used to indicate the ductility
of the substance, and other mechanical properties. The purpose of etching is tw0-fold. Grinding
and polishing operation produce a highly deformed, thin layer on the surface which is removed
chemically during etching.

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What are the advantages of electrolytic polishing?
High speed.
Can be reproducible.
No mechanical deformation.
Can produce excellent surfaces for examination.

7. Determination the ASTM:

Metals, except in a few instances, are crystalline in nature and, except for single crystals; they
contain internal boundaries known as grain boundaries. When a new grain is nucleated during
processing (as in solidification or annealing after cold working), the atoms within each growing
grain are lined up in a specific pattern that depends upon the crystal structure of the metal or alloy.
With growth, each grain will eventually impinge on others and form an interface where the atomic
orientations are different.
The number of grains per square inch at 100x magnification is:
n100 = nm * [M / 100]
2
Where: n100 is the number of grains per square inch at 100x magnification.
nm is the number of grains per square inch at the magnification M of the photomicrograph.

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The ASTM grain size number N is calculated from the following equation:
N = _
lnn
ln2
_ + 1
And this a example to calculate the grain size,













From Fig (12),
M = 200,
A =
8
2.54

8
2.54
= 9.92 in.
2

nm = 36 grain /9.92 inch
2
= 3.63 grain / in
2

n100 = nm * [M / 100]
2

n100 = 3.63*(200/100) ^2 = 14.52 grain / in
N = [ln (n) / ln (2)] + 1
N = [ln (14.52) / ln (2)] + 1 = 4.86 grain / in.
2


Fig (12): Approximate Grains

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8. Comments & Recommendations:

The experiment was useful and very long, and gain experience in the preparation of metallographic
specimens.



9. References:

http://en.wikipedia.org/wiki/Grain_boundary
http://en.wikipedia.org/wiki/Metallography
http://www.struers.com/default.asp?doc_id=262
http://www.eng-tips.com/viewthread.cfm?qid=141206