Object

Experiment: Metallography Specimen Preparation and Examination Objectives 1.

To learn and to gain experience in the preparation of metallographic specimens.
2. To examine and analyze the microstructures of metals and metallic alloys.
Abstract Proper preparation of metallographic specimens to determine
microstructure and content requires that a rigid step-by-step process be followed.
In sequence, the steps include sectioning, mounting, course grinding, fine
grinding, polishing, etching and microscopic examination. Specimens must be
kept clean and preparation procedure carefully followed in order to reveal
accurate microstructures. Each student will prepare and examine a brass, steel or
aluminium sample for metallographic examination. Additionally, a brass, steel or
aluminiumsample with different composition, a eutectoid steel sample and a
eutectoid Pb-Sn sample will be examined under the metallographic microscope.
Photographs will be taken of the samples and the ASTM grain size number
determined for each of the specimens if applicable. Background 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;
advanced examination and research laboratories often contain electron
microscopes (SEM and TEM), x-ray and electron diffractometers and possibly
other scanning devices. 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.
Hot or cold working can occur during the specimen preparation process if the
metallurgist is not careful. Expertise at the methods employed to produce high-
quality metallographic samples requires training and practice. The basic
techniques can be learned through patient persistence in a matter of hours. This
module takes the student through the metallographic sample preparation process
step-by-step with demonstrations and explanations 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.
Abrasive Cut-Off Wheels consist of abrasive grains (such as Aluminum Oxide or
Silicon Carbide), bonded together with rubber or other materials in the form of a
thin wheel. Rubber bonded wheels are most extensively used for wet operation
and resin bonds for dry cutting. When sectioning a piece of metal, the abrasive
grains on the cutoff wheel become dull, therefore, the bond must be destroyed at
the correct rate so that new grains are always at the edge and are still held firmly
by the bonding material. The rate at which the bond breaks down is affected by
several different factors, including: 1) The hardness of the bond. 2) The hardness
and workability of the metal sample. 3) The size and speed of the wheel. 4) The
power of the driving motor. 5) The type and amount of coolant and its method of
application. 6) The amount of pressure by which the wheel is applied to the
sample. 7) The amount of vibration in the machine. Cutoff wheels are indexed
from hard to soft and are referred to by "grade". As a rule of thumb, a hard
bonded wheel should be selected when sectioning soft stock, and a soft wheel for
sectioning harder material. A reasonable amount of wheel pressure must be
applied so the abrasive grains will "bite" and remove the metal ME 3701,
Materials of Engineering, LSU

in fine chips. An experienced operator can tell whether the wheel is cutting or
merely "dragging" by the feel of the control arm and monitoring of the power
consumption of the cutting equipment. Proper cutting procedures must be
followed; abrasive cut-off wheels will crack and become flying projectiles when
used improperly. Lab Procedure - Sectioning

Place the sample on the slotted Table so that it is at the center of the swing of the
head. Place the Locking Lever in the forward position to allow the Control Rod to
be moved to the furthest position. Move the Rear Vise section to contact the rear
face of the sample. Move the Front Section to a position near the front face of the
sample. Tighten the Nuts that secure the Vise sections to the Table. Push the
Control Rod in to make firm contact with the sample and pull back the Locking
Level to secure the sample. Turn on the coolant; it should flow readily to both
cool and clean the cutting area. Apply steady moderate pressure until the
specimen is sectioned; avoid jerking motions that may cause the blade to splinter.

Mounting Small samples are generally mounted in plastic for convenience in

handling and to protect the edges of the specimen being prepared. Compression-
type molding is commonly applied to encase specimens in 1 to 1.5 inch diameter
plugs of a hard polymer. Compression molding materials are classified as either
thermosetting or thermoplastic: 1) Bakelite is a low cost, relatively hard
thermosetting polymer that is commonly utilized. 2) Expensive Transoptic
Thermoplastics are utilized when transparency is required. Transoptic materials
remain molten at maximum temperature and become transparent with an
increase in pressure and a decrease in temperature. By definition, thermosetting
materials require heat and pressure during the molding cycle. During mounting,
the pressure and molding temperature are generally held constant thus time is
the only variable. The metal sample is placed in the mounting cylinder which is
then encased in a pre-measured amount of powdered polymers. The mounting
cylinder is then sealed, pressurized and heated to complete the polymerization
process necessary to solidly encase the metal sample. Although inferior in quality
to compression-type molding, cold molding (room temperature) is often used
with epoxy to mount samples by simply mixing the epoxy and pouring it over a
sample that is positioned facedown in a cold-mounting ring. When the epoxy
cures the specimen can be prepared. Caution must be exercised when cold
mounting due to relatively poor adhesion between the specimen edges and the
epoxy plug; gaps often form which can degrade the quality of the specimen. Lab
Procedure Mounting Procedure (Hot-Mounting Equipment Currently Unavailable
@ LSU!) Supplies for Cold-Mounting: - KoldMound Kit (Vernon-Benshoff Co.): Mix
2 parts powder with 1 part liquid - Plastic Mounting Ring with Removable Bottom
- 8 Ounce Paper Cup with Stirrer - Weight Scale - Liquid Soap 1. 2. 3.
Apply liquid soap to the inner walls and base of the mounting ring. Place the
specimen in the center/bottom of the plastic mounting ring base with the
examination surface facedown. Attach the mounting ring cylinder to the base by
simple pressing firmly in place.

ME 3701, Materials of Engineering, LSU

Mix the appropriate amount of KoldMount (2/1 Powder/Liquid - 15 grams of

Powder/7.5 grams of Liquid per Sample) in a paper cup. Simply pour the epoxy
mixture into the mounting ring; sample should be approximately 0.75" thick. After
one hour, remove the sample from the mounting ring and proceed with course
grinding.

Coarse Grinding In view of the perfection required in an ideally prepared

metallographic sample, it is essential that each preparation stage be carefully
performed. The specimen must:

1. Be free from scratches, stains and others imperfections which tend to mark the
surface. 2. Retain non-metallic inclusions. 3. Reveal no evidence of chipping due
to brittle intermetallic compounds and phases. 4. Be free from all traces of
disturbed metal. 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 in size and parallel to each other in any
one grinding stage. Proper grinding involves rotation of the sample by 90o
between stages while the grinding angle must be held constant during the
grinding at any one stage. The sample MUST be washed thoroughly before
proceeding from one grinding stage to the next ! ! ! Failure to follow this basic
rule will result in transferring abrasive particles between stages and will cause
timeconsuming, frustrating problems in removing unwanted scratches. Lab
Procedure-Coarse Grinding: *Note: Safety Glasses must be worn when operating
the Course Grinding Equipment ! ! !

1. Label the specimen with your name so that it can be easily identified. 2. Turn
the Motor On, then the water, adjust the flow to obtain a good film of water. Too
much water will cause a spray when it contacts the sample. 3.

Beginning with the 120 grit belt and using both hands to hold the specimen,
carefully place the sample face onto the exposed area of the belt being careful
not to contact the rotating surface with a sharp edge of the specimen or your
hand.

4. Applying moderate pressure evenly, move the sample left-and-right across the
belt surface to obtain uniform grinding. Use both hands to hold the specimen;
unsecured specimens can "Catch an Edge and FLY"!

5. Lift the sample from the wheel periodically to determine the progress of
grinding but do not rotate the sample. The 120 grit stage is complete when all the
lines scratched in by the grinder are parallel on the specimen surface. If any line
or scratch is not in the same direction as the other lines, continue grinding until all
of the lines are parallel.

6. When all of the sample's scratches are parallel, carefully wash all of the debris
from sample using tap water and dry the specimen immediately using a paper
towel or pressurized air to avoid corrosion. ME 3701, Materials of Engineering,
LSU

7. Proceed to the 180 grit stage with the scratches oriented approximately
perpendicular to the intended grinding direction and repeat steps 3 thorugh 6.

8. When the 180 grit stage is complete, you're ready to move on to the
medium/fine grinding station.

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"! Wet grinding is generally applied in
medium and fine grinding to avoid possible side affects 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.

Lab Procedure-Fine Grinding "The sample MUST be washed thoroughly before

proceeding from one fine grinding stage to the next!!!"

1. Manual Fine Grinding is performed by drawing the specimens in one direction

across the surface of the water lubricated abrasive paper. (Back to front is
recommended) Use of backward and forward motion is less desirable because
there is a tendency to rock the sample, producing a curved rather than a flat
surface.

2. Begin with the lowest grade abrasive paper (240 grit) and proceed to the
highest (600 grit).
3. To monitor progress, each fine grinding step should be performed in a
direction off-angle with respect to the previous step.

4. Fine Grinding should be continued until the previous stage's scratches are gone,
using a few extra strokes to assure complete scratch removal.

5. Sufficient water must be applied to provide lubrication and flush away the
removal products. Too much water will result in a hydroplaning action where the
sample rides on a film of water, thereby reducing the effectiveness of the
abrasive. Use the valve at the top of the roll-grinder to increase and decrease the
quantity of water needed or desired.
6. The specimen should be carefully rinsed after each step of Fine Grinding; debris
from one step must not contaminate the next step! Rinse the specimen very
thoroughly before proceeding to polishing.

ME 3701, Materials of Engineering, LSU

Mechanical Polishing Polishing involves the use of abrasives, suspended in a water

solution, on a cloth-covered electrically powered wheel. Diamond abrasives
provide the best, and most expensive, compounds utilized in polishing; standard
sized aluminum oxide powders are applied for general use purposes. 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! Beginning
with 25-micron suspended aluminum oxide particles (suspended in water) on a
Nylon-cloth, the final fine-grinding surface layer resulting from the previous
grinding procedure should be completely removed with a rotation rate of 150-200
rpm. The specimen is initially held at one position on the wheel, without rotation,
until most of the previous grinding marks are removed. It can be rotated slowly,
counter to the wheel rotation, until only scratches from the 25micron aluminum
oxide are visible. During the initial polishing stage, moderate pressure can be
applied to the specimen and the entire stage should generally take 1 or 2
minutes! After carefully washing the specimen, proceed to the 5-micron stage
where a separate polishing wheel with 5micron particles; repeat the procedure
outlined above using lighter pressure and a gradual rotating motion across the
polishing cloth. The final polishing stage with 1-micron suspended aluminum
oxide particles should be carried out on a separate polishing wheel following
"Careful washing of the specimen and operator's hands" at a slower speed of 100
- 150 rpm using a napped cloth. After 1 or 2 minutes a properly polished specimen
should have a mirror-like surface free of scratches! During final polishing, minimal
pressure should be applied and time should be kept to a minimum since the
napped material will conform to the specimen shape under pressure. The wetness
of the cloth used for Final Polishing has a great influence on the end result. If the
cloth is too wet the sample will show pits; if too dry, buffing and/or smearing will
result. To determine the proper wetness, the sample should be removed from the
wheel and the time required for the polishing film to dry (five to eight seconds)
should be checked. A thin opaque film indicates that sufficient abrasive is present.
For precision work, extremely fine grades of diamond abrasives may often be
used for the final polishing sequence. Cerium Oxide is especially excellent for the
final polishing of aluminum and other soft metals and alloys. The best abrasive
types and sizes for various metals and alloys are listed in the literature; references
should be consulted for recommended practice. Generally, polishing can also be
accomplished electrochemically, using an electrolytic cell which is similar to the
ones used for electroplating, except that the polishing cell operates in reverse.
The metal atoms are thus stripped from the specimen surface. Careful control is
required for electropolishing; it is best suited to finishing a large number of
identical specimens. The following general flow sheet is included for the various
stages of steel sample preparation.

Stage Fine Grinding

Abrasive Lubricant 240, 320, 400 then 600 Water

Cloth None

Rough Polishing

5 to 25-Micron Aluminum Oxide 1-Micron Aluminum Oxide

Distilled Water

Nylon

Distilled Water

Napped Microcloth

Final Polishing
The ability to prepare a specimen is an art and the required skill is acquired only
after significant hands-on experience. Using automated equipment, an
inexperienced technician can be taught to prepare well polished specimens in a
few hours; he/she could not, however, hand polish well without further training
and experience.

ME 3701, Materials of Engineering, LSU

5
Lab Procedure - Mechanical Polishing 1.
Safety goggles must be worn when using the Polishers!

2.
Make sure your specimen and hands have been thoroughly cleaned before
Polishing!

3.
Begin with the 25-micron, nylon cloth polishing station!
4.
Turn the water on adjusting to less than one drop per second!

5.
Apply a small amount of the aluminum oxide abrasive solution to the polishing
cloth.
6.
When polishing the specimen, hold it with both hands, apply a moderate amount
of pressure, and don't let it go. The Rough Polishing Stages (5-25 microns) should
take between 1 and 2 minutes each! If you let go of the specimen it may fly, harm
you or others in the laboratory and become damaged forcing you to start over
again with coarse grinding - hold it tight and be careful!

7.

Do not contaminate the polishing wheel; cover the wheel when it's not in use!

8.

Before proceeding to the next polishing stage, wash and dry both the specimen
and your hands thoroughly then rinse the specimen.

9.

Repeat steps 4 through 8 for the 5-micron stage.

10. Proceed to the Final Polishing Station (1 micron) when all of the 25 micron
marks are removed at the 5 micron stage. 11. Hold the specimen with both hands
and apply a SMALL amount of pressure, and Don't Let Go! 12. The Final Polishing
Stage (1-micron) should take between 1/2 and 1 minute! 13. Be very careful that
you do not contaminate the polishing wheel! Cover the wheel when it's not in
use!!!

14. Before proceeding to Etching, wash and dry both the specimen and your
hands thoroughly then rinse the specimen with distilled water. DO NOT TOUCH
THE SPECIMEN SURFACE!!!

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. Even in a carefully prepared sample, a
surface layer of disturbed metal, resulting from the final polishing stage, is always
present and must be removed. 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. The etching process is usually
accomplished by merely applying the appropriate solution to the specimen
surface for several seconds to several minutes. Nital, a Nitric Acid - Alcohol
mixture, is the etchant commonly utilized with common irons and steels. Nital is
dripped onto the specimen using an eye-dropper or cotton swab. Ten seconds to
one minute is usually sufficient for proper etching depending on sample and nital
concentration. The sample is immediately washed under running water, rinsed
with alcohol and dried in an air blast. Do not touch, wipe or swab the specimen
following etching; dry off the rinsing alcohol on the specimen with the air blast
and then move on to the microscopic examination stage!

ME 3701, Materials of Engineering, LSU

6

Etchants Materials

Composition

Iron & Steel

1-5 Parts Nitric Acid 100 Parts Alcohol 1 Part Ammonium Hydroxide 1 Part 3%
Hydrogen Peroxide 1 Part Water Copper & Brass 5 g Ferric Chloride, 10 ml
Hydrocloric Acid 100 ml Water 5-10 g Ammonium Persulphate 1 ml Hydrofluoric
Acid Aluminum 99 ml Water 10 g Sodium Hydroxide, 100 ml Water 10 g Oxalic
Acid 100 ml Water Stainless Steels 5 ml Sulfuric Acid 100 ml Water

Application Procedure Immerse/Swab Swab Immerse Immerse Immerse Use

Electrolytically Use Electrolytically

Lab Procedure- Etching Steel Specimens Note: Always wear Acid Resistant gloves
when Etching! 1. 2. 3. 4. 5. 6. 7. 8.

Place the specimen on the table under the Fume Hood with the polished surface
up. Turn on the Fume Hood. Without touching the specimen surface, clean the
surface with alcohol and let it dry using the hot air gun. Do not let anything but
the alcohol touch the specimen surface! Using the Eye-Dropper, apply a few drops
of Etchant to the specimen surface covering the entire metallic surface of the
specimen. After about 20 to 30 seconds, rinse the Etchant into the sink with water
and quickly rinse the specimen with alcohol, but do not touch the surface! Use
the Hot Air Gun to dry the sample. Proceed to Microscopic Examination; if further
etching is required you may return and proceed through steps 1 through 6 varying
the time in step 5 depending on the results. If the specimen has many scratches
and marks or the microstructure cannot be seen after several etches, return to
fine grinding and go back through the necessary steps.

Microscopic Examination Initial microscopic viewing should be done utilizing a

stereomicroscope, which reveals a three-dimensional scanning of the specimen
surface. The specimen is placed on the stage of the microscope so that its surface
is perpendicular to the optical axis. Detailed viewing is done with a Metallurgical
Microscope. A metallurgical microscope has a system of lenses (objectives and
eyepiece) so that different magnifications (25X to 1000X) can be achieved. The
important characteristics of the microscope are: (1) magnification, (2) resolution
and (3) flatness of field. The resultant magnification is the product of the
magnifying power of the objective and that of the ocular. Scanning Electron
Microscopes (SEMs) are capable of magnifications up to 20,000X and
Transmission Electron Microscopes (TEMs) are utilized to view at magnifications
up to 100,000X for highly detailed microstructural study. Grain Size Calculation In
single phase specimens, the ASTM grain size of the metal can be estimated by
comparing the image at 100X with standard microstructure examples
corresponding to standard grain sizes from 1 to 10. Also, suitable eyepieces
etched with a square 0.01" x 0.01" in size can be used to calculate the number of
grains per square inch, N.

ME 3701, Materials of Engineering, LSU

7
The ASTM grain size number, n, can be calculated using the following relationship:
2
N (M/100) = 2
(n - 1)
N = number of grains per square inch at 100X n = ASTM grain size number M =
Magnification For single phase materials, ASTM grain size number is given to
denote the grain sizes. These are not the actual grain size values, but the latter
can be derived from the ASTM grain size number, n; the larger the grain size
number, the smaller the grains. If there are N grains per square inch at a
magnification M then there are (N) 1/2 length. The size of each grain at
magnification M is then 1/(N) inches.

1/2

grains along a 1 inch

1/2

The actual size of the grain is given by Actual Grain Size = 1/(N M)

Lab Procedure- Microscopic Examination 1.

Each student will examine the following four samples in the microscope: •

A metallic specimen provided by the instructor and prepared by the student;

A metallic specimen provided by the instructor and prepared by another student;

•
A Eutectoid Steel Specimen (provided by instructor); and

•
A Eutectic Pb-Sn Specimen (provided by instructor).

Initially examine the specimens through the stereomicroscope, which gives a

three-dimensional impression of the specimen surface. With a properly etched
specimen, grains can be differentiated and impurity particles can be clearly seen.
2. 3.

Use a Metallurgical Microscope to view the specimen at various magnifications

and note the microstructural aspects of the material. Take a photograph of each
specimen at the optimal magnification. (if the camera is not working then sketch
the microstructure of each specimen.) 4. Make sure that the specimen that you
prepared is clearly labeled and the specimen surface is in its final condition; it
must be submitted with your lab write-up to the laboratory instructor.

Lab Requirements
1. Prepare a metallographic brass, steel or aluminum specimen going through the
course grinding, fine grinding, polishing and etching stages of specimen
preparation. Clearly label your specimen and submit it with the lab write up; the
quality of your specimen will be graded
. 2. Examine the four requisite samples and photograph each at the optimal
magnification (if a camera is not available then sketch each of the
microstructures).
3. Determine the ASTM grain size number and the average grain size for the
single-phase brass specimen.
4. Briefly describe the salient features of the eutectoid specimens that you
examined. How many phases and constituents are present in each?
5. Based on the observed microstructure of the steel sample, can you determine
the carbon content of the steel? If yes, then briefly explain how you know the
carbon content.
6.Based on the observed microstructures, which of the two brass specimens
would you expect to be: ME 3701, Materials of Engineering, LSU

8
Strongest? Why?

Hardest? Why?

More Ductile? Why?

Stiffer (Elastic Modulus)? Why?

Homework 1. Briefly (one concise sentence each) describe the steps involved in
the preparation of a metallographic sample: Sectioning Mounting Course Grinding
Fine Grinding Polishing Etching 2. Why must metallographic samples be washed
and carefully dried before proceeding from one grinding or polishing operation to
the next? 3. What is the purpose of etching metallographic samples? 4. Why are
metallographic samples sometimes mounted in plastic? 5. What is the difference
between a Eutectoid steel and a Hypoeutectoid steel? 6. At room temperature : •

What are the phases of a eutectoid steel?

What are the constituents of a eutectoid steel?

What are the phases of a hypoeutectoid steel?

What are the constituents of a hypoeutectoid steel?

7. If the ASTM grain size number of a single phase monel alloy (nickel solvent) is
given as 5, approximate the average grain size for this alloy?(M = 100X) 8. If the
grain size of a piece of brass is 0.07 mm, what is the ASTM grain size number? (M
= 100X) For this piece of brass, how many grains will be there per square inch at a
magnification of 250X? 9. Briefly explain the effect of grain size on the strength of
a metal.

ME 3701, Materials of Engineering, LSU

Introduction
Metallography is basically the study of the structures and constitution of metals
and alloys, using metallurgical microscopes and magnifications, so that the
physical and mechanical properties of an alloy can be related to its observed
microstructure.It provides information about the specimen under investigation,
including the size and shape of the grains (crystallites), the presence of micro
defects (such as segregation, hair cracks, and nonmetallic inclusions), and the
nature and distribution of secondary phases.
The surface of a metallographic specimen is prepared by various methods
of grinding, polishing, and etching. After preparation, it is often analyzed
using optical or electron microscopy. Using only metallographic techniques, a
skilled technician can identify alloys and predict material properties.
Mechanical preparation is the most common preparation method. Successively
finer abrasive particles are used to remove material from the sample surface until
the desired surface quality is achieved. Many different machines are available for
doing this grinding and polishing, which are able to meet different demands for
quality, capacity, and reproducibility.
A systematic preparation method is the easiest way to achieve the true structure.
Sample preparation must therefore pursue rules which are suitable for most
materials. Different materials with similar properties (hardness and ductility) will
respond alike and thus require the same consumables during preparation.
Metallographic specimens are typically "mounted" using a hot
compression thermosetting resin. In the past, phenolic thermosetting resins have
been used, but modern epoxy is becoming more popular because reduced
shrinkage during curing results in a better mount with superior edge retention. A
typical mounting cycle will compress the specimen and mounting media to
4,000 psi (28 MPa) and heat to a temperature of 350 °F (177 °C). When specimens
are very sensitive to temperature, "cold mounts" may be made with a two-part
epoxy resin. Mounting a specimen provides a safe, standardized,
and ergonomic way by which to hold a sample during the grinding and polishing
operations.
A macro etched copper disc
After mounting, the specimen is wet ground to reveal the surface of the metal.
The specimen is successively ground with finer and finer abrasive media. Silicon
carbide abrasive paper was the first method of grinding and is still used today.
Many metallographers, however, prefer to use a diamond grit suspension which is
dosed onto a reusable fabric pad throughout the polishing process. Diamond grit
in suspension might start at 9 micrometres and finish at one micrometre.
Generally, polishing with diamond suspension gives finer results than using silicon
carbide papers (SiC papers), especially with revealing porosity, which silicon
carbide paper sometimes "smear" over. After grinding the specimen, polishing is
performed. Typically, a specimen is polished with a slurry of alumina, silica,
or diamond on a napless cloth to produce a scratch-free mirror finish, free from
smear, drag, or pull-outs and with minimal deformation remaining from the
preparation process.
After polishing, certain microstructural constituents can be seen with the
microscope, e.g., inclusions and nitrides. If the crystal structure is non-cubic (e.g.,
a metal with a hexagonal-closed packed crystal structure, such as Ti or Zr) the
microstructure can be revealed without etching using crossed polarized light (light
microscopy). Otherwise, the microstructural constituents of the specimen are
revealed by using a suitable chemical or electrolytic etchant.
1 METALLOGRAPHY Objective To study the structural characteristics or
constitution of a metal or an alloy in relation to its physical and mechanical
properties. Introduction There are two examination methods in metallography: I)
Macroscopy 2) Microscopy In macroscopy the examination of the structural
characteristics or chemical characteristics of a metal or an alloy is done by the
unaided eye or with the aid of a low-power microscope or binocular, usually
under l0x. In microscopy similar examination is done with the prepared metal
specimens, employing magnifications with the optical microscope of from 100x to
as high as 2000x. Specimen preparation 1. Grinding A small piece of specimen is
cut by a metal-cutting-saw. After cutting operation, burrs on the edges of the
specimen should be carefully removed by a fine file or coarse grinding paper. The
silicon carbide grinding papers are held flat in a unit containing water facility for
lubrication purpose. Each unit contains four grades of papers, starting with grade
400 (coarse) and finishing with grade 1200 (fine). Grinding of the work piece is
done by starting with the coarse papers and then continuing with the fine papers.
In each stage, grinding is done by rubbing the specimen backwards and forwards
on the grinding paper in one direction only, until the surface is completely
ground, that is, until only grinding marks due to this particular paper can be seen
to cover the whole surface. The specimen is washed thoroughly to remove coarse
silicon carbide particles before proceeding to a finer paper. The direction of
grinding is changed from paper to paper, so that the removal of previous grinding
marks is easily observed. The extra time spent on each paper should be increased
as the finer papers are used. At the end of the grinding sequence, the specimen is
washed thoroughly and dried. Now, the specimen is ready for polishing. 2.
Polishing The polishing is done on rotating wheels covered by a special cloth.
Alumina is employed as polishing agent. The 1-micron size is commonly used, but
the total polishing time shortened by starting on the 7 or 3 micron grade. The pad
should be kept well supplied with lubricant. The specimen should be held firmly in
contact with the polishing wheel, but excessive pressure should be avoided.
During polishing the specimen should be rotated or moved around the wheel so
as to give an even polish. The specimen should be thoroughly cleaned and dried
between each wheel.
2 3. Etching Before etching, it is essential to ensure that the polished surface is
grease and smear free. If the final polishing has involved the use of magnesia ( in
the form of an aqueous paste of fine magnesia) or alumina (in the form of an
aqueous suspension of fine alumina), then thorough washing followed by drying
off with acetone or alcohol will give a suitable surface, although it must not be
fingered afterwards. Etching is generally done by swabbing. Etching times will
vary from specimen to specimen, however, a good general, procedure is to
observe the surface during etching, and to remove the specimen when evidence
of the grains first appears. Microscopical examination will then reveal whether
the degree of etching is sufficient. Further etching can then follow to strengthen
up the details as required. After each etching, the specimen should be thoroughly
washed in running water, followed by drying off with acetone or alcohol. * As a
guide the following etchants are commonly used: Alcoholic Ferric Chloride
-copper alloys Mixed Acids -aluminum alloys Nital (ethyl alcohol+ 2% HN03) -iron
and steel Dilute HCI -zinc alloys A. MICROSCOPICAL EXAMINATION The
microstructural study of a material can provide information regarding the
morphology and distribution of constituent phases as well as the nature and
pattern of certain crystal imperfections. Optical metallography is a basic tool of
material scientists, since the equipment is relatively inexpensive and the images
can be obtained and interpreted easily. Distribution and morphology of the
phases can be studied and, if their properties are known, a quantitative analysis
of the micrographs provides some information about the bulk properties of the
specimen. A limited study of line and surface informations is also possible with
the optical microscope. In order to obtain reproducible results, with good
contrast in the image, the specimen surface is polished and subsequently etched
with appropriate reagents before microscopic examination. In a polished
specimen, the etching not only delineates grain boundaries, but also allows the
different phases to be distinguished by differences in brightness, shape, and color
of the grain. Differences in contrast may result from differences in light
absorption characteristics of the phases. Etching results in preferential attack or
preferential colouring of the surface. The preferential attack is electrochemical
corrosion; it is well known that different materials corrode at different rates.
Grain boundaries are often anodic to the bulk metal in the interior of the grain
and so are etched away preferentially and delineated. Staining is produced by the
deposition of solid etch product on the specimen surface. This is formed by
chemical reaction between the etchant and the specimen. Under favorable
conditions the use of a proper etchant enables the identification of constituents.
Failure analysis depends a great deal on metallographic examination.

3 Microstructural examination can provide quantitative information about the

following parameters: 1) The grain size of specimens 2) The amount of interfacial
area per unit volume 3) The dimensions of constituent phases 4) The amount and
distribution of phases. Magnifications up to 1000x can be obtained with a
resolution of 2 =. For grain size measurements, the grains along a line, circle, or
within a known area are counted. It would be useful to obtain an average value of
grain diameter from a microstructural section. In linear intercept method, the
grains intercepted by a theoretical line on the specimen surface are counted (Fig.
1). The number of grain boundaries intersected per unit length of a test line (n L )
can be noted. The average grain size is indicated by the inverse of n L, corrected
for the magnification, M, of the micrograph. In general, then, the average grain
diameter, d, is given by d= C/n L.M where C is some constant greater than 1
( Typically, a value of C=1.5 is adequate). Experimental Fig.1 Linear intercept
method for grain size determination Specimens are going to be polished and
etched as explained above. With an unmounted specimen, even if it is almost
level, it is best to fix it on a glass or metal slide by means of a piece of plasticine.
The prepared surface is made level by means of a suitable levelling device. The
correct procedure is to start with low power examination in order to obtain an
overall picture, and then successively higher magnifications are used to resolve
the fine details. In focusing, the stage is gradually moved towards the objective
and when the image appears, focusing is completed with the fine adjustment. It is
almost good practice to examine specimens first in the polished condition, as
certain features, such as the presence of inclusions, cracks, porosity, and
sometimes even the different phases, are revealed. This is followed by an
examination in the etched condition. Do not examine one or two fields only. It
should always be remembered that the structure of a given specimen exists in
three dimensions, whereas the prepared surface represents a two-dimensional
picture in the plane of the micro-section. This fact should be taken into account in
the interpretation of the geometry of any particular configuration. Results The
investigation result of the optical microscopy is going to be recorded as follows: 1.
Examine each specimen and sketch typical microstructure 2. Estimate the carbon
content of the steels. 3. Calculate the average grain diameter of the micrograph,
using linear intercept method.

4 B. MACROSCOPIC EXAMINATION OF METALS Objective To examine the nature

of inhomogenities and flow lines in a metal by unaided eye or with the aid of a
low-powered microscope or magnifying glass. Introduction Metallurgical data
obtained by a chemical and metallographic analysis of a metal or an alloy are
usually not representative of the entire piece. These data represent the
characteristics of the metal only at the particular section of the piece. The general
distribution and variation in size of nonmetallic inclusions; the uniformity of
structure; the location and extent of segregation; the presence of fabricating
defects, such as seams or hammer bursts; and residual ingot defects, such as pipe
can not be examined by microscopy. The nature of inhomogenities in a metal, and
the extent to which they exist therein, are best determined by macroetching a
representative piece and subsequently examining the conditions thereby revealed
with the unaided eye or with the aid of a low-powered microscope or magnifying
glass. Such an examination is referred to as a macroscopic, or macro,
examination. The magnification employed is usually not over 10x. Macroetching
sections may reveal conditions in the metal that are related to one or more of the
following heterogeneous circumstances: 1. Crystalline heterogeneity, the
presence and extent of which depend upon the manner of solidification and the
crystalline growth of the metal or alloy. 2. Chemical heterogeneity, owing to
impurities in the metal or alloy and to localized segregation of certain chemical
constituents. Such segregation may be intentional (the introduction of carbon into
the surface of steel during the process of case carburizing), or may be
unintentional and undesirable, as for example, the segregation of sulphur or
phosphorus that is so often found in cast steels. 3. Mechanical heterogeneity,
arising from cold-working or process that introduces permanent stresses into the
metal. Such heterogeneity seldom occurs in cast metals, but its presence is of
importance in cold-rolled metals, forging, etc. Experiment Three experiments will
be performed: 1. Sulphur Printing: Impurities may exist in steel products. It is
desirable that their amounts should be minimal and homogeneously distributed
within the product. These impurities degrade the mechanical properties of the
steel, especially sulphur content in steel makes it brittle. Sulphur may exist
chemically in steel in one of two forms, either as manganese sulphide or as iron
sulphide. Sulphur printing detects and permanently records the distribution of
sulphur in steel. The surface of interest to be tested for distribution of sulphur
should be reasonably smooth and free from foreign matter such as dirt and
grease. Grinding the surface on papers, numbers 400 to 1200 and subsequent
thorough washing will generally produce a surface satisfactory for the purpose.

5 Photographic bromide paper is soaked in a 2% aqueous solution of sulphuric

acid for approximately 3 or 4 min. The paper is removed from the acid solution
and allowed to drain free from excess solution. The emulsion side of the paper is
then placed in direct contact with the prepared specimen surface and allowed to
remain in contact under moderately applied pressure for 1 or 2 min. Care must be
taken that all entrapped air bubbles between the paper and the specimen surface
are eliminated. The reaction of the sulphuric acid with the sulphide regions of the
steel produces hydrogen sulphide gas, which reacts with the silver bromide in the
paper emulsion, forming a characteristic brown to gray-black deposit of silver
sulphide. These reactions may be expressed as follows: FeS + H2SO4 ~ FeS04 +
H2S or MnS + H2SO4 ~ MnS04 + H2S H2S + 2 AgBr ~ Ag2S + 2 HBr When the
reaction has proceeded for approximately the recommended length of time, the
photographic paper is removed from the surface of the specimen, rinsed in clear
running water, and then fixed permanently by placing it in a photographic fixing
solution for about 15 min. When fixation is completed, the print is again washed
in running water for approximately 30 min. and subsequently dried in the usual
manner. The examination of properly prepared sulphur print will disclose quite
clearly, because of the presence of darkly colored areas of silver sulphide, the
precise location of sulphur inclusions on the prepared surface of the metal. A
grouping or gathering of such silver sulphide areas indicates the presence of
sulphur segregation, whereas a random dispersion of the spots denotes a more
uniform, distribution of the sulphur inclusions. 2. Flow lines: It is sometimes
desirable to determine whether or not a finished piece has been forged, cut, or
cast into shape and to note, in the event that it was forged, the direction of metal
flow. Flow lines as revealed by macroetching in forgings are a natural
consequence of applied mechanical working. If the flow pattern shows highly
selective etching characteristics, it is likely that the material may be defective and
may contain an excessive amount of inclusions and segregated areas. A
macroetched forged-material shows a directional flow pattern consisting of
streaks and striations. The orientation of this pattern with respect to the plane of
the prepared surface indicates the direction of metal flow during deformation.
The flow lines are made visible because the elongated inclusions of impurities,
such as oxides, sulphides and other elongated heterogeneous areas are
selectively attacked by the etching reagent. 3. Welded sections: It is often
desirable, and frequently necessary, to determine the soundness of a welded
joint and to observe macroscopically over a cross section of the weldment the
various zones wherein structural changes have occurred. This is accomplished by
macroetching the prepared surface with the usual hydrocworic acid solution, or in
some cases with a milder reagent such as 2 or 3 % nital (ethyl alcohol + 2% HN03).
In ferritic welds, the specimen of interest is prepared in a manner described for
metallographic specimens and finally alternately polished and etched in saturated
picral to remove disturbed

6 metal. The prepared surface is then etched for 10 to 20 sec. in 5% nital, after
which the surface is thoroughly washed and lightly rubbed on a metallographic
polishing cloth until the columnar grains in the weld metal show distinctly. This
procedure is repeated several times to lessen the light reflectivity characteristics
of the surface and to produce some relief of the macrostructure. The specimen of
interest is then etched by immersion for about 2 min. in saturated picral, followed
by thorough washing in cold running water and swabbing with a tuft of cotton to
remove the loosely adhering reaction products formed on the surface. The
specimen is finally rinsed in alcohol and dried in a stream of warm air. Specimens
1. Sulphur printing: a piece of rail material 2. Flow lines: done without a specimen,
shown on blackboard 3.Welded sections: finding the location of weld section of a
welded-material Procedure 1. Sulphur printing: follow the instructions in the
introduction section. 2. Flow lines: 3. Welded section: follow the instructions in
the introduction section (for grinding the specimen use number 240 to 400
grinding papers then rub the specimen surface using a cotton tuft by 9g FeCl cm3
HCl cm3 H2O solution until the weld section appears). Results 1. Draw
schematically sulphur inclusions in the rail material (Specimen 1). 2. Are the
sulphur inclusions distributed homegeneously or as segregated points in the
material? Discuss their effects on the mechanical properties of the material. 3
What causes the flow lines to appear. Do flow lines exist in casted materials?
Why? 4. What do the flow lines indicate in terms of mechanical properties of the
material? 5. Draw schematically welded-section of specimen What do you find
out by examining the welded-sections? Can you talk about the weld quality,
appearance and the welded materials, etc.? By inspecting the weld section, relate
this result to the mechanical properties of the material. References 1. Kehl, G.L.,
The Principles of Metallographic Laboratory Practice, 3rd Ed., Güleç,K., Malzeme
Ders Notlan, Makina Fakültesi, LTÜ. 3. Imperial College of Science and
Technology, Department of Metallurgy and Materials Science, 2nd Year Materials
Laboratory Notes for Mechanical and Aeronautical Engineers. 4. ASTM Standards
and ASM Standards (they exist in our library, please consult with the librarian)

Theory
Metallography is the study of metals by optical and electron microscopes.
Structures, which
are coarse enough to be discernible by the naked eye or under low
magnifications, are termed
macrostructures. Useful information can often be gained by examination with
the naked eye of the
surface of metal objects or polished and etched sections. Those, which require
high magnification
to be visible, are termed microstructures. Microscopes are required for the
examination of the
microstructure of the metals. Optical microscopes are used for resolutions down
to roughly the
wavelength of light (about half a micron) and electron microscopes are used for
detail below this
level, down to atomic resolution. The most commonly used microscope is the
conventional light
microscope. In principle, optical microscopes may be used to look through
specimens ('in
transmission') as well as at them ('in reflection'). Many materials, however, do
not transmit light
and so we are restricted to looking at the surface of the specimens with an
optical microscope.
Electron microscope can be used in the transmission e.g. Transmission Electron
Microscope (TEM)
and to look at the surfaces e.g. Scanning Electron Microscope (SEM) Microscopy
can give
information concerning a material's composition, previous treatment and
properties. Particular
features of interest are
(1) Grain size (II) phases present (III) Chemical homogeneity (IV) distribution of
phases (V)
Elongated structures formed by plastic deformation

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 ofthe
material's surface. Optical microscopy is sufficient for general purpose
examination; advanced examination and research laboratories often contain
electron microscopes (SEM and TEM), X-ray and electron diffractometers and
possibly other scanning devices.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.
Hot or cold working can occur during the specimen preparation process If the
metallurgist is not careful. Expertise at the methods employed to produce high-
quality metallographic samples requires raining and practice. The basic
techniques can be learned through patient persistence in a matter of hours This
module takes the student through the metallographic sample preparation
process step-by-step w the demonstrations and explanations of sectioning,
mounting, coarse and fine grinding, polishing, etching and microscopic
examination.

Procedures

other defects can be observed in

this way, and if they are
identified before etching,
subsequent
confusion and misinterpretation
can be largely avoided. The
specimen to be etched is treated
by immersion in, or by
swabbing with, the appropriate
reagent. It is impossible to lay
down
general rules for the time of
etching. Usually the desired
effect will be produced between
ten
seconds and two minutes. The
specimen after etching should
be washed in a stream of
running water. The surface
should be dried untouched by
holding in air current. When
selecting etching times, it is
more desirable to under-etch
than to over-etch. If a
specimen, after a first attempt is
found to be insufficiently
etched, the etching process can
usually be repeated without
further preparation of the
surface. A specimen that is
over-etched
can only be corrected by
repolishing and then reetching
for a shorter time.
Etching reagents can produce
effects in several different
ways:
1. The etching of a pure metal
or a single phase alloy is a
process of chemical solution of
the
metal by the reagent wherein
the grains are attacked at rates
dependent upon their
orientations with respect to the
polished section plane. Because
the rate of solution of any one
grain differs among different
crystallographic planes, during
etching a series of well-defined
facets develop that are similarly
oriented for any one grain, but
as a group are differently
oriented from those on
neighboring grains. The
different facet orientations on
the respective
grains reflect the incident light
from the microscope in
different amounts. This gives
rise to
contrast in the reflected light
intensities and, thus, the
respective grains can readily be
identified. In general, grain
boundary regions (and twin
boundaries) are also delineated
because of their higher energies
and, correspondingly, higher
dissolution rates.
2. The mechanism of etching
multiphase alloys is essentially
electrochemical in nature.
Because of a difference in
potential between the structural
components when the specimen
is
brought into contact within the
etching reagent, one phase tends
to go into solution more
readily than the others. The
preferential dissolution causes
the phase to be somewhat
roughened and depressed,
especially at the boundaries.
When observed
microscopically,
shadow effects are seen and the
various structural features are
delineated.
3. The operative characteristics
of some reagents reveal
structural details by preferential
dissolution and selectively
discolor or stain certain phases
of the structure.
The Metallurgical Microscope
Having already described in
some detail the methods by
which a metallographic
specimen is
best prepared and subsequently
etched for microscopic
examination, it is now
appropriate to
discuss the principles of the
metallurgical microscope. A
metallurgical microscope differs
from a biological microscope in
the manner by which the
specimen is illuminated.
Because of
the inability of visible radiation
to propagate through a metal
specimen, observations are
made
using light reflected from the
polished surface. A horizontal
beam of light is deflected by a
plane glass reflector, upward
and through a microscope
objective onto the surface of the
specimen. A certain amount of
incident light will be reflected
from the specimen surface back
through the objective lens
system and then through a
second lens system, the
microscope
eyepiece.
Metallography is essentially the study of the structural characteristics or constitution of a
metal or an alloy in relation to its physical and mechanical properties. The most important
part of metallography deals with the microscopic examination of a prepared metal specimen.
The metallographic microscope is described in Appendix D, which should be read carefully at
this point. Correct preparation begins with the selection of a suitable specimen and continues
to the etching stage where the structure of the specimen is revealed. The microscopic
examination then defines clearly such structural characteristics as grain size, the size, shape
and distribution of secondary phases and non-metallic inclusions; and segregation and other
heterogeneous conditions
These characteristics profoundly influence the mechanical properties and
physical behavior of the metal. Metallographic examination can provide
quantitative information about specimengrain sizes, amount of interfacial
area per unit volume, and the amount and distribution of
phases. When these and other constitutional features are determined by
microscopicexamination and the extent to which they exist in the
microstructure is known, it is then possible to predict with considerable
accuracy the expected behavior of the metal when used for a specific
purpose. Of equal importance is the fact that, within limits, the
microstructure can provide an accurate picture of the mechanical and
thermal treatments that a metal has received.
Preparation of Specimens
The technique for preparing metal sections can be divided into two groups,
those processes
involving the use of emery papers and coarse abrasives (grinding) and the
subsequent
operations using fine abrasives (polishing treatments). Grinding must be
carried out carefully
in such a way that all microscopic constituents in the surface are preserved
and that the
grinding medium is not embedded in the sample. To achieve this, the
specimen is ground on
successively finer grades of emery (sand) paper. During grinding, the
specimen is held with
the newly formed scratches at right angles to the scratches introduced on
the preceding
paper. Undue pressure should be avoided since the disturbed layer this
produces on the
surface can extend to considerable depth. For some heat treated alloys and
in particular for
many of the soft metals, it is an advantage to use paper thoroughly wetted.
Grinding also
removes surface deformations. After grinding, the specimen is washed
thoroughly in water
and then polished. Mechanical polishing can best be carried out by holding
the specimen
against a rotating disc covered with a suitable pad that is impregnated with
either a suspension
of polishing alumina in water or diamond dust oil.

Mounting of Specimens
It is frequently convenient to mount small specimens in bakelite or acrylic to
aid specimen
preparation, grinding, polishing and etching. You will be given instructions
on the use of the
apparatus for mounting specimens. The basic idea is that bakelite powder is
thermosetting.
Therefore the specimen is placed in a tube 2/3 filled with powder. The tube
is heated while
the powder is compressed. The pressure and heat are removed when the
powder has
completely melted and the bakelite has set. To maintain orientation small
shot are sometimes
placed next to the specimen in some identifying arrangement.

Grinding and Polishing Procedure

The following instructions indicate the general method to be used in
specimen preparation.
The edges of cylindrical metal specimens must first be beveled off to avoid
damaging the
polishing cloths. For Mg and Al and their alloys, use the aluminum polishing
wheels
Stage Abrasive Lubricant Cloth
Rough Grinding Silicon Carbide Tap Water
Fine Grinding Grit 240
Grit 320
Grit 400
Grit 600
Rough Polishing Gamma Alumina 1.0µ Tap Water Rayon
Final Polishing Gamma Alumina 0.05µ Tap Water Rayon

Hypoeutectoid. Composition less than that of the eutectoid.

Metallography. Study of metallic microstructures. This can be used to

determine a number
of things including: Heat treatment, mechanical processing, material
properties and phases
present.

Phase. A material having the same composition, structure, and properties

everywhere under
equilibrium conditions.

Plastic deformation. Permanent deformation of the material when a load is

applied, then
removed.

Precipitate. A solid phase that forms from the original matrix phase when
the solubility limit
is exceeded. In most cases, we try to control the formation of the
precipitate to produce the
optimum dispersion strengthening.

Proeutectoid. Phase that forms by solid-state precipitation in a temperature

range above the
eutectoid temperature. For example Proeutectoid alpha phase in
hypoeutectoid steels.

Twin boundary. A surface defect across which there is a mirror image

misorientation of the
lattice. Twin boundaries can also move a cause deformation of the material.

Write-Up
No write up is required. Place the photographs you took in your laboratory
notebook. Be sure
they are labeled to indicate subject matter (steel, brass, aluminum) and
magnification.

other defects can be observed in

this way, and if they are
identified before etching,
subsequent
confusion and misinterpretation
can be largely avoided. The
specimen to be etched is treated
by immersion in, or by
swabbing with, the appropriate
reagent. It is impossible to lay
down
general rules for the time of
etching. Usually the desired
effect will be produced between
ten
seconds and two minutes. The
specimen after etching should
be washed in a stream of
running water. The surface
should be dried untouched by
holding in air current. When
selecting etching times, it is
more desirable to under-etch
than to over-etch. If a
specimen, after a first attempt is
found to be insufficiently
etched, the etching process can
usually be repeated without
further preparation of the
surface. A specimen that is
over-etched
can only be corrected by
repolishing and then reetching
for a shorter time.
Etching reagents can produce
effects in several different
ways:
1. The etching of a pure metal
or a single phase alloy is a
process of chemical solution of
the
metal by the reagent wherein
the grains are attacked at rates
dependent upon their
orientations with respect to the
polished section plane. Because
the rate of solution of any one
grain differs among different
crystallographic planes, during
etching a series of well-defined
facets develop that are similarly
oriented for any one grain, but
as a group are differently
oriented from those on
neighboring grains. The
different facet orientations on
the respective
grains reflect the incident light
from the microscope in
different amounts. This gives
rise to
contrast in the reflected light
intensities and, thus, the
respective grains can readily be
identified. In general, grain
boundary regions (and twin
boundaries) are also delineated
because of their higher energies
and, correspondingly, higher
dissolution rates.
2. The mechanism of etching
multiphase alloys is essentially
electrochemical in nature.
Because of a difference in
potential between the structural
components when the specimen
is
brought into contact within the
etching reagent, one phase tends
to go into solution more
readily than the others. The
preferential dissolution causes
the phase to be somewhat
roughened and depressed,
especially at the boundaries.
When observed
microscopically,
shadow effects are seen and the
various structural features are
delineated.
3. The operative characteristics
of some reagents reveal
structural details by preferential
dissolution and selectively
discolor or stain certain phases
of the structure.
The Metallurgical Microscope
Having already described in
some detail the methods by
which a metallographic
specimen is
best prepared and subsequently
etched for microscopic
examination, it is now
appropriate to
discuss the principles of the
metallurgical microscope. A
metallurgical microscope differs
from a biological microscope in
the manner by which the
specimen is illuminated.
Because of
the inability of visible radiation
to propagate through a metal
specimen, observations are
made
using light reflected from the
polished surface. A horizontal
beam of light is deflected by a
plane glass reflector, upward
and through a microscope
objective onto the surface of the
specimen. A certain amount of
incident light will be reflected
from the specimen surface back
through the objective lens
system and then through a
second lens system, the
microscope
eyepiece.

other defects can be observed in

this way, and if they are
identified before etching,
subsequent
confusion and misinterpretation
can be largely avoided. The
specimen to be etched is treated
by immersion in, or by
swabbing with, the appropriate
reagent. It is impossible to lay
down
general rules for the time of
etching. Usually the desired
effect will be produced between
ten
seconds and two minutes. The
specimen after etching should
be washed in a stream of
running water. The surface
should be dried untouched by
holding in air current. When
selecting etching times, it is
more desirable to under-etch
than to over-etch. If a
specimen, after a first attempt is
found to be insufficiently
etched, the etching process can
usually be repeated without
further preparation of the
surface. A specimen that is
over-etched
can only be corrected by
repolishing and then reetching
for a shorter time.
Etching reagents can produce
effects in several different
ways:
1. The etching of a pure metal
or a single phase alloy is a
process of chemical solution of
the
metal by the reagent wherein
the grains are attacked at rates
dependent upon their
orientations with respect to the
polished section plane. Because
the rate of solution of any one
grain differs among different
crystallographic planes, during
etching a series of well-defined
facets develop that are similarly
oriented for any one grain, but
as a group are differently
oriented from those on
neighboring grains. The
different facet orientations on
the respective
grains reflect the incident light
from the microscope in
different amounts. This gives
rise to
contrast in the reflected light
intensities and, thus, the
respective grains can readily be
identified. In general, grain
boundary regions (and twin
boundaries) are also delineated
because of their higher energies
and, correspondingly, higher
dissolution rates.
2. The mechanism of etching
multiphase alloys is essentially
electrochemical in nature.
other defects can be observed in
this way, and if they are
identified before etching,
subsequent
confusion and misinterpretation
can be largely avoided. The
specimen to be etched is treated
by immersion in, or by
swabbing with, the appropriate
reagent. It is impossible to lay
down
general rules for the time of
etching. Usually the desired
effect will be produced between
ten
seconds and two minutes. The
specimen after etching should
be washed in a stream of
running water. The surface
should be dried untouched by
holding in air current. When
selecting etching times, it is
more desirable to under-etch
than to over-etch. If a
specimen, after a first attempt is
found to be insufficiently
etched, the etching process can
usually be repeated without
further preparation of the
surface. A specimen that is
over-etched
can only be corrected by
repolishing and then reetching
for a shorter time.
Etching reagents can produce
effects in several different
ways:
1. The etching of a pure metal
or a single phase alloy is a
process of chemical solution of
the
metal by the reagent wherein
the grains are attacked at rates
dependent upon their
orientations with respect to the
polished section plane. Because
the rate of solution of any one
grain differs among different
crystallographic planes, during
etching a series of well-defined
facets develop that are similarly
oriented for any one grain, but
as a group are differently
oriented from those on
neighboring grains. The
different facet orientations on
the respective
grains reflect the incident light
from the microscope in
different amounts. This gives
rise to
contrast in the reflected light
intensities and, thus, the
respective grains can readily be
identified. In general, grain
boundary regions (and twin
boundaries) are also delineated
because of their higher energies
and, correspondingly, higher
dissolution rates.
2. The mechanism of etching
multiphase alloys is essentially
electrochemical in nature.
other defects can be observed in
this way, and if they are
identified before etching,
subsequent
confusion and misinterpretation
can be largely avoided. The
specimen to be etched is treated
by immersion in, or by
swabbing with, the appropriate
reagent. It is impossible to lay
down
general rules for the time of
etching. Usually the desired
effect will be produced between
ten
seconds and two minutes. The
specimen after etching should
be washed in a stream of
running water. The surface
should be dried untouched by
holding in air current. When
selecting etching times, it is
more desirable to under-etch
than to over-etch. If a
specimen, after a first attempt is
found to be insufficiently
etched, the etching process can
usually be repeated without
further preparation of the
surface. A specimen that is
over-etched
can only be corrected by
repolishing and then reetching
for a shorter time.
Etching reagents can produce
effects in several different
ways:
1. The etching of a pure metal
or a single phase alloy is a
process of chemical solution of
the
metal by the reagent wherein
the grains are attacked at rates
dependent upon their
orientations with respect to the
polished section plane. Because
the rate of solution of any one
grain differs among different
crystallographic planes, during
etching a series of well-defined
facets develop that are similarly
oriented for any one grain, but
as a group are differently
oriented from those on
neighboring grains. The
different facet orientations on
the respective
grains reflect the incident light
from the microscope in
different amounts. This gives
rise to
contrast in the reflected light
intensities and, thus, the
respective grains can readily be
identified. In general, grain
boundary regions (and twin
boundaries) are also delineated
because of their higher energies
and, correspondingly, higher
dissolution rates.
2. The mechanism of etching
multiphase alloys is essentially
electrochemical in nature.
other defects can be observed in
this way, and if they are
identified before etching,
subsequent
confusion and misinterpretation
can be largely avoided. The
specimen to be etched is treated
by immersion in, or by
swabbing with, the appropriate
reagent. It is impossible to lay
down
general rules for the time of
etching. Usually the desired
effect will be produced between
ten
seconds and two minutes. The
specimen after etching should
be washed in a stream of
running water. The surface
should be dried untouched by
holding in air current. When
selecting etching times, it is
more desirable to under-etch
than to over-etch. If a
specimen, after a first attempt is
found to be insufficiently
etched, the etching process can
usually be repeated without
further preparation of the
surface. A specimen that is
over-etched
can only be corrected by
repolishing and then reetching
for a shorter time.
Etching reagents can produce
effects in several different
ways:
1. The etching of a pure metal
or a single phase alloy is a
process of chemical solution of
the
metal by the reagent wherein
the grains are attacked at rates
dependent upon their
orientations with respect to the
polished section plane. Because
the rate of solution of any one
grain differs among different
crystallographic planes, during
etching a series of well-defined
facets develop that are similarly
oriented for any one grain, but
as a group are differently
oriented from those on
neighboring grains. The
different facet orientations on
the respective
grains reflect the incident light
from the microscope in
different amounts. This gives
rise to
contrast in the reflected light
intensities and, thus, the
respective grains can readily be
identified. In general, grain
boundary regions (and twin
boundaries) are also delineated
because of their higher energies
and, correspondingly, higher
dissolution rates.
2. The mechanism of etching
multiphase alloys is essentially
electrochemical in nature.
Caluclation
In single phase specimens, the ASTM grain size of the metal can be
estimated by comparing the image at
100X with standard microstructure examples corresponding to
standard grain sizes from 1 to 10. Also,
suitable eyepieces etched with a square 0.01" x 0.01" in size can be
used to calculate the number of grains
per square inch, N.
The ASTM grain size number, n, can be calculated using the following
relationship:
N (M/100)2 = 2(n - 1)
N = number of grains per square inch at 100X
n = ASTM grain size number
M = Magnification
For single phase materials, ASTM grain size number is given to denote
the grain sizes. These are not the
actual grain size values, but the latter can be derived from the ASTM
grain size number, n; the larger the
grain size number, the smaller the grains.
If there are N grains per square inch at a magnification M then there
are (N)1/2 grains along a 1 inch
length. The size of each grain at magnification M is then 1/(N)1/2
inches.
The actual size of the grain is given by Actual Grain Size = 1/(N M)1/2
Lab Procedure- Microscopic Examination
1. Each student will examine the following four samples in the
microscope:
• A metallic specimen provided by the instructor and prepared by the
student;
• A metallic specimen provided by the instructor and prepared by
another student;
• A Eutectoid Steel Specimen (provided by instructor); and
• A Eutectic Pb-Sn Specimen (provided by instructor).
Initially examine the specimens through the stereomicroscope, which
gives a three-dimensional
impression of the specimen surface. With a properly etched specimen,
grains can be differentiated and
impurity particles can be clearly seen.
2. Use a Metallurgical Microscope to view the specimen at various
magnifications and note the microstructural
aspects of the material.
3. Take a photograph of each specimen at the optimal magnification. (if
the camera is not working then sketch
the microstructure of each specimen.)
4. Make sure that the specimen that you prepared is clearly labeled and
the specimen surface is in its final
condition; it must be submitted with your lab write-up to the laboratory
instructor.

Discussion
How many steps of Metallography Examination?

 Sectioning and Cutting

 Mounting
 Grinding
 Polishing
 Final Polishing
 Etching
 Microscopic analysis
 Hardness Testing

What are grihdiving terms?

Surfaces cut by abrasive cutoff saw start with 120 to 240 grits.

Surfaces cut by EMD or diamond saw start with 320 to 400 grits.
What articles addedvtobthe rotary disk

1-in Grinding Abrasive paper (covered with silicon car bide grite ) commonly.
ascrics of abrsive paper is used. from coarse to fine one Table Ishow the
approximate meidan particle diameter for agiven sizein mi cromeler.

2-In polishing lubricant and polishing surface support is often specifie to the metal
and the object of the investigation polishing can be divided in to rough (coarse)
and fine (final) stages

What are the modem hays usede in mounting?

*Mechanical Monnting:

Strip and sheet specimen may be momted by binding or clamping several

specimens

in to apack held to gether by tow end pieces and tow boths the specimens should
be tighhy bound to gether to prevent absoption and subsequent exudation of
polishing.

*Thermal monnting:
The saple is embeddeb in thermososetting plastice at elevated temperature and
pressure as shown in fig -5

Cold mounting:

Where aliquid mixture of two or mare poly mers solidi fise at rom temperature
after being poured in to amold containing the specimen cold mounting compound
are relatively easy to mixand use and mount can by made at one time resins for
cold mounts include epoxise a crylices and poly ester

There three common types of cutting,what it is ?

1-Abrasive culting is the most common sectioning method The adradive cuoff disc
shin in

2-Electric Dischrye Mashining (EDM).

Electrically conductive materaile can be seetioned by (EDM)

3-Micro tomy:

Is usful to prepare soft material such as polymer sampare steel glass or dimond
knife ina micro tome can cat samole

What are cotton types that use from experiment ?

*1-In siscan carbide the cotton its will be Brown cbth or white cloth

2-In called Diamond the cotton its will be Black

Reference
1.  Salmon, Stuart (February 2010). "What is Abrasive
Machining?". Manufacturing Engineering. Society of Manufacturing
Engineers.  Abrasive machining is  not precision grinding. The objective is
neither super precision nor high-luster surface finishes. Abrasive machining
first and foremost generates high stock removal.
2. ^ Stephenson, David A.; Agapiou, John S. (1997).  Metal Cutting Theory and
Practice (2nd ed.). Boca Raton: CRC Press. pp.  52–60. ISBN  978-0-8247-
5888-2.
3. ^ Nadolny, Krzysztof (9 April 2012).  "The method of assessment of the
grinding wheel cutting ability in the plunge grinding".  Central European
Journal of Engineering. 2  (3): 399–409.  doi:10.2478/s13531-012-0005-
5. S2CID  136037527.
4. ^ Matthew, Sam (2016-12-17). "The basics of abrasive
cutting". tungstengrinder.net. Retrieved 17 December  2016.
5. ^ [1], T. Saleh, M. Sazedur Rahman, H.S. Lim, M. Rahman, Development and
performance evaluation of an ultra precision ELID grinding machine, Journal
of Materials Processing Technology, Volumes 192-193, Pages 287-291.
6. ^ Adithan & Gupta 2002, p. 129