FACULTY OF PRODUCTION ENGINEERING AND
MANAGEMENT
DEPARMENT OF TECHNOLOGY AND MATERIAL ENGINEERING
PRACTICAL METALLOGRAPHY
30.6.2014
Pasa Yaman
Theoretical Part
What is the basics of preparation of metallographic sample?
Metallography is the study of a material’s microstructure. Analysis of a material’s
microstructure aids in determining if the material has been processed correctly and is
therefore a critical step for determining product reliability and for determining why a material
failed. The basic steps for proper metallographic sample preparation include: documentation,
sectioning and cutting, mounting, planar grinding, rough polishing, final polishing, etching,
microscopic analysis and hardness testing.
Documentation – Metallographic analysis is a valuable tool. By properly documenting the
initial sample condition and the proceeding microstructural analysis, metallography provides a
powerful quality control as well as an invaluable investigative tool.
Sectioning and Cutting – Following proper documentation, most metallographic samples
need to be sectioned to the area of interest and for easier handling. Depending upon the
material, the sectioning operation can be obtained by abrasive cutting (metals and metal
matrix composites), diamond wafer cutting (ceramics, electronics, biomaterials, minerals), or
thin sectioning with a microtome (plastics).
Proper sectioning is required to minimize damage, which may alter the microstructure and
produce false metallographic characterization. Proper cutting requires the correct selection of
abrasive type, bonding, and size; as well as proper cutting speed, load and coolant. Table I list
the most common type of abrasive blades used for metallographic sectioning and Table II lists
cutting parameters for diamond wafer cutting.
Mounting – The mounting operation accomplishes three important functions (1) it protects
the sample edge and maintains the integrity of a materials surface features (2) fills voids in
porous materials and (3) improves handling of irregular shaped samples, especially for
automated sample preparation. The majority of metallographic sample mounting is done by
encapsulating the sample into a compression mounting compound (thermosets - phenolics,
epoxies, diallyl phthalates or thermoplastics - acrylics), casting into ambient castable
mounting resins (acrylic resins, epoxy resins, and polyester resins), and gluing with a
thermoplastic glues.
Compression mounting - For metals, compression mounting is widely used. Phenolics are
popular because they are low cost, whereas the diallyl phthalates and epoxy resins find
applications where edge retention and harder mounts are required. The acrylic compression
mounting compounds are used because they have excellent clarity. Table IIIa and IIIb list the
application as well as the physical properties of the most common compression mounting
resins.
Castable Mounting Resins - Castable resins provide a convenient way to mount and orient
specimens for microstructural preparation. Castable resins are monomer resins utilizing a
catalyst or hardener for polymerization. Polymerization results in cross-linking of the polymer
to form a relatively hard mount. Castable resins are advantageous because they do not require
specialized mounting equipment. In addition, mounting high volumes of samples is faster then
by compression mounting because multiple specimens can be mounted at the same time.
Epoxy, acrylic and polyester resins are the most popular metallographic casting compounds.
Planar Grinding - or course grinding is required to planarize the specimen and to reduce the
damage created by sectioning. The planar grinding step is accomplished by decreasing the
abrasive grit/ particle size sequentially to obtain surface finishes that are ready for polishing.
Care must be taken to avoid being too abrasive in this step, and actually creating greater
specimen damage than produced during cutting (this is especially true for very brittle
materials such as silicon).
The machine parameters, which effect the preparation of metallographic specimens, include
grinding/polishing pressure, relative velocity distribution, and the direction of
grinding/polishing.
Grinding Pressure - Grinding/polishing pressure is dependent upon the applied force
(pounds or Newton's) and the area of the specimen and mounting material. Pressure is defined
as the Force/Area (psi, N/m2or Pa). For specimens significantly harder than the mounting
compound, pressure is better defined as the force divided by the specimen surface area. Thus,
for larger hard specimens higher grinding/polishing pressures increase stock removal rates,
however higher pressure also increases the amount of surface and subsurface damage. Note
that for SiC grinding papers, as the abrasive grains dull and cut rates decrease, increasing
grinding pressures can extend the life of the SiC paper. Higher grinding/polishing pressures
can also generate additional frictional heat, which may actually be beneficial for the chemical
mechanical polishing (CMP) of ceramics, minerals and composites. Likewise for extremely
friable specimens such as nodular cast iron, higher pressures and lower relative velocity
distributions can aid in retaining inclusions and secondary phases.
Grinding Direction - The orientation of the specimen can have a significant impact on the
preparation results, especially for specimens with coatings. In general, when grinding and
polishing materials with coatings the brittle component should be kept in compression. In
other words, for brittle coatings the direction of the abrasive should be through the coating
and into the substrate. Conversely, for brittle substrates with ductile coatings, the direction of
the abrasive should be through the brittle substrate into the ductile coating.
Manual Preparation - In order to insure that the previous rough grinding damage is removed
when grinding by hand, the specimen should be rotated 90 degrees and continually ground
until all the scratches from the previous grinding direction are removed. If necessary the
abrasive paper can be replace with a newer paper to increase cutting rates.
Automated Preparation - The key to successful automated preparation is to thoroughly
clean the specimens between each abrasive grit size that is used. The tracking of the
specimens should also uniformly break down the SiC paper, otherwise non-uniform grinding
will occur (especially for hard specimens in soft mounts). In other words, the specimen should
track across the entire diameter of the SiC paper.
Abrasive Selection - The most common
abrasive used for planar grinding metal and
polymer metallographic specimens is silicon
carbide (SiC). Silicon carbide is an excellent
abrasive for planar grinding because it is very
hard and maintains a sharp cutting edge as it
breaks down during cutting. SiC abrasives are
typically listed by the grit size. Table VI shows
the two most common grit size-numbering
systems, along with their respective median
diameter particle size.
Planar Grinding Recommendations –
Metallic Specimens - For metallic specimen grinding, sequential grinding with silicon
carbide (SiC) abrasive paper is the most efficient and economical rough grinding process.
Although extremely coarse grit abrasive papers can be found, it is recommended that a
properly cut specimen not be rough ground with an abrasive greater than 120 grit SiC paper.
A typical abrasive grinding procedure would consist of 120 or 240 grit SiC paper followed by
decreasing the size of the SiC paper (320, 400, and 600 grit). Finer papers are also available
for continued abrasive paper grinding (800 and 1200 grit).
In addition to the correct sequence and abrasive size selection, the grinding parameters such
as grinding direction, load and speed can affect the specimen flatness and the depth of
damage. The basic idea is to remove all of the previous specimen damage before continuing
to the next step while maintaining planar specimens.
Electronic Specimens - Grinding electronic components is very dependent upon both the
substrate (silicon, alumina, barium titanate, plastic PCB's, etc) and the metallic materials used.
In general, when grinding plated or coated materials, it is recommended that the coating be
prepared in compression to prevent the coating from separating from the substrate. Silicon
specimens should be have been sectioned with a fine grit diamond blade and cut as near as
possible to the area of interest. For rough grinding, fine abrasives such as 400 or 600 grit SiC
or a 15-micron diamond lapping film is recommended to avoid producing more damage than
created during sectioning. Hard ceramic substrates (especially porous materials) should be
rough polished with diamond lapping films to minimize edge rounding and relief between the
widely varying materials hardness'.
Plasma Spray Components - Similar to the preparation of electronic components, plasma
spray coatings should be kept in compression to minimize the possibility of delamination at
the coating/ substrate interface. For ceramic plasma spray coatings, diamond-lapping films are
recommended to minimize edge rounding or relief and to maintain the integrity of any
inclusions within the coating.
Ceramics and Ceramics Composites - Rough grinding ceramics and ceramic matrix
composites should be performed with 15 or 30 micron diamond on a metal mesh cloth in
order to obtain adequate stock removal and to minimize surface and subsurface damage.
Plastics and Plastics Composites - Plastics are generally very soft and therefore can be
planar ground with sequentially decreasing SiC abrasive paper grit sizes. When plastics are
used in conjunction with hard ceramics, planar grinding can be very tricky. For these
composite materials cutting must minimize damage as much as possible because almost all
grinding and polishing will cause relief between the soft plastic and the hard ceramic.
Following proper cutting, grinding with as small as possible a diamond (6-micron diamond)
on a metal steel mesh cloth or the use of lapping films is suggested.
Rough Polishing - The purpose of the rough polishing step is to remove the damage
produced during cutting and planar grinding. Proper rough polishing will maintain specimen
flatness and retain all inclusions or secondary phases. By eliminating the previous damage
and maintaining the microstructural integrity of the specimen at this step, a minimal amount
of time should be required to remove the cosmetic damage at the final polishing step. Rough
polishing is accomplished primarily with diamond abrasives ranging from 9 micron down to
1-micron diamond. Polycrystalline diamond because of its multiple and small cutting edges,
produces high cut rates with minimal surface damage, therefore it is the recommended
diamond abrasive for metallographic rough polishing on low napped polishing cloths.
Final Polishing - The purpose of final polishing is to remove only surface damage. It should
not be used to remove any damage remaining from cutting and planar grinding. If the damage
from these steps is not complete, the rough polishing step should be repeated or continued.
Etching - The purpose of etching is to optically enhance microstructural features such as
grain size and phase features. Etching selectively alters these microstructural features based
on composition, stress, or crystal structure. The most common technique for etching is
selective chemical etching and numerous formulations have been used over the years. Other
techniques such as molten salt, electrolytic, thermal and plasma etching have also found
specialized applications.
Chemical Etching - selectively attacks specific microstructural features. It generally consists
of a mixture of acids or bases with oxidizing or reducing agents. For more technical
information on selective chemical etching consult corrosion books which discuss the
relationship between pH and Eh (oxidation/reduction potentials), often known as Eh-pH
diagrams or Pourbaix diagrams.
Molten Salt etching is a combination of thermal and chemical etching techniques. Molten salt
etching is useful for grain size analysis for hard to etch materials such as ceramics. The
technique takes advantage of the higher internal energy associated at a materials grain
boundaries. At the elevated temperature of molten salts, the higher energy at the grain
boundaries is relieved, producing a rounded grain boundary edge, which can be observed by
optical, or electron microscope techniques.
Thermal etching is a useful etching technique for ceramic materials. Thermal etching is
technique that relieves the higher energy associated at the grain boundaries of a material. By
heating the ceramic material to temperatures below the sintering temperature of the material
and holding for a period of minutes to hours the grain boundaries will seek a level of lower
energy. The result is that the grain boundary edge will become rounded so that it can be
evaluated by optical or electron microscope techniques.
Depending upon the ceramic material, the atmospheric condition of the furnace may need to
be controlled. For example, etching silicon nitride will require either a vacuum or an inert
atmosphere of nitrogen or argon to prevent oxidation of the surface to silicon dioxide.
Plasma etching is a lesser-known technique that has been used to enhance the phase structure
of high strength ceramics such as silicon nitride. For silicon nitride, the plasma is a high
temperature fluoride gas, which reacts with the silicon nitride surface producing a silicon
fluoride gas. This etching technique reveals the intragrain microstructure of silicon nitride.
Metallographic Analysis –
Metallurgical analysis (metallography) of the microstructural provides the Material Scientist
or Metallurgist information varying from phase structure, grain size, solidification structure,
casting voids, etc. Figure 2 shows an example of two cast iron structures. Figure 2a shows a
cast iron microstructure which has graphite flakes. Over time this materials will most likely
fail under load. On the other hand by adding some solidifying agents the cast iron can be
made to form the more durable graphite nodules (Figure 2b).
Figure 3 shows the grain size of a tough pitch copper. Analysis of a materials grain size
provides valuable information regarding a materials physical hardness and ductility.
Microstructural analysis can also provide very useful information about the types of phases
that occur during cooling. Figure 4
shows the dendritic growth of the
microstructure for an aluminum-
silicon alloy which formed during
solidification. The direction and size
of these dendrites again relate to the
materials strength and durability.
Other examples of metallographic analysis include: analyzing printed circuit board (PCB)
solder hole connections, microelectronic failure analysis, steel heat treating such as surface
hardening, ceramic grain size and porosity, polymer composite fiber wetting and orientation,
etc.
Microscopic Analysis
Bright Field (B.F.) illumination is the most common illumination technique for
metallographic analysis. The light path for B.F. illumination is from the source, through the
objective, reflected off the surface and returning through the objective and back to the
eyepiece or camera. This type of illumination produces a bright background for flat surfaces
with the non-flat features (pores, edges, etched grain boundaries) being darker as light is
reflected back at an angle.
Field (D.F.) illumination is a lesser know illumination but powerful illumination technique.
The light path for D.F. illumination is from the source, down the outside of the objective,
reflected off the surface and returning through the objective and back to the eyepiece or
camera. This type of illumination produces a dark background for flat surfaces with the non-
flat features (pores, edges, etched grain boundaries) being brighter as light is reflected at an
angle back into the objective.
Differential Interference Contract (DIC) - is a very useful illumination technique for
providing enhanced specimen features. DIC uses a normarski prism along with a polarizer in
the 90° crossed positions. The two light beams are made to coincide at the focal plane of the
objective, thus rendering height differences visible as variations in color.
Optical Interferometry - is a technique that provides precise details of a materials surface
topography. The simplest interferometer employs the interference between two beams of
light. One beam is focused on the specimen and the second beam on an optically flat reference
surface. The two reflected beams are then recombined by the beam splitter and pass through
the eyepiece together. The two beams reinforce each other for those points on the specimen
for which their path lengths are either the same of differ by an integral multiple of the
wavelength, nλ. The beams cancel for path differences of nλ /2. Today's interferometers
provide quantitative 3-dimensional surface topography information.
The two most common optical interferometry techniques include - phase shifting
interferometry (PSI) which uses a PZT to shift the optical path of the objective and vertical
scanning interferometry (VSI) which changes the focus range of the objective. The main
differences between PSI and VSI are that PSI has a higher z-axis resolution, whereas VSI has
a larger scan range. PSI and VSI can also be combined to provide both high surface resolution
and a larger scan range.
Atomic Force Microscopy (AFM) - Is a non-optical technique that provides angstrom level
surface profiling information. AFM's are very powerful tools and can be provide
electrochemical, magnetic, and other surface feature information.
References:
1. http://www.lt-scientific.com/me_c_cmr.pdf
2. www.metallographic.com
3. http://www.lapmaster.com/metallographic-products/abrasive-cut-off-
wheels/default.html
4. http://dce.karabuk.edu.tr/metalografik.html
5. http://www.tse.org.tr/hizmetlerimiz/deney-hizmetleri/laboratuvarlar/makine-
laboratuvar%C4%B1-(gebze)/sertlik-ve-metalografik-analizler-
b%C3%B6l%C3%BCm%C3%BC
6. http://imechanica.org/files/handout9.pdf
Pictures from different structures
Ledeburite is a mixture of 4.3% carbon
in iron and is a eutectic mixture of
austenite and cementite. Because of
mixture, there occur some gray waves.
Gray cast iron is a kind of cast iron that
has graphitic structure. Chemical
composition of structure should be 2.5-
4.0% carbon and 1-3% silicon.
Al-Si alloy. High levels of silicon (4.0–
13%) contribute to give good casting
characteristics. Aluminium alloys are widely
used in engineering structures and
components where light weight or corrosion
resistance is required.
Cu-Zn alloy. Copper alloys are
metal alloys that have copper as their
principal component. They have high
resistance against corrosion. The most known
copper alloy is bronze and brass.
Practical Part
Day 1 (June 12th, 2014)
All the students chose their own samples to examine by pursuing metallographic traditions
step by step under supervising of Ing.Svobodova and her laboratory colleagues. Firstly, I
picked AlMg3 for my sample. Then, using the abrasive disc in the cutting machine, cut the
sample twice for having proper material shape to examine at it.
After obtaining proper shapes, it is time to put the sample in resin. But first we need to
prepare it. First, the sample has to be cleaned by water to put it in the plastic mold.
Then, in a different cup, we prepare resin casting.
The things that we use is a chemical called
Dentacryl Technicky. When we research, we find
out that it is a methylmethacrylate compound. We
add liquid and powder version of this compound
altogether and try to obtain proper concentration.
After that pour it to plastic molds that has
our sample. We need to care that the
surface we wish to examine should be
upside down to the bottom so that after taking out of sample from mold we can carry out
some procedure on it.
After pouring it down, we have to wait 24 hours so that solidification process can be
completed.
Day 2 (June 24th, 2014)
We take the sample off from the plastic mold so that we can do operations on it. So, we turn
the centrifugal machine on and put the proper disc on it. First, we place the abrasive paper
with number p280. When it starts turning, we put our sample on turning disc with the abrasive
paper. Here the grinding starts. When we need more power, we change the abrasive paper.
Respectively; p280, p800, p1500, p2500. The number of paper goes up, the size and number
of grit on the paper gets increased.
Day 3 (June 25th, 2014)
Today we start to polish our sample. For that,
we change disc and put the one provides our
needs. We prefer a disc that has some
roughness over the surface. We add AlO2 for
lubricating. The reason why we polish is to
take the damage and scratches away that
occured during cutting the material. The
surface will be flat and without scratches. In
this way, we will have more clear and specific
results over the surface. But my sample looks
quite scratchy in comparison with other
samples. It requires so much time to fix its
surface more than we do. There are a lot of
bulges and scratches. Despite of polishing hardly and repeatedly it is not bright and shiny.
After polishing, we wash and add alcohol and dry. Then, send it to microscope. But my
sample AlMg2 does not look smooth and sharp.
Day 4 (June 26th, 2014)
Today we will work on final polishing. We will use 3
different lubricants so that surface can be shiny enough
and scratch free. Firstly, we use green suspension
called 3 µm -monocrystalline diamond suspension. We
put another disc. Today we will use 3 different discs.
All of them different roughness values. And they
started to have softy surfaces. After spraying the 3 µm
suspension, we press the sample over the disc. But my
sample does not respond as usual. We check it with
microscope.
Then, we change the disc and add another suspension called 1
µm – DP-Suspension M. We press the sample over the disc but
my sample still does not respond. Its surface still same but
started to be shiny. Not so much as other samples but when we
compare its situation in respect with first polishing.
After washing, alcoholizing and drying, checked it with
microscope. It seemed worse in respect with first polishing.
Keeping polished by the disc does not work with my sample at
all.
For the last, we used some other nameless suspensions or lubricants yellow and white colored.
Of course, changed the disc for the last time. Add lubricant and put pressure over the sample.
After washing, alcoholizing and drying, checked it with microscope. It still seems bad.
Day 5 (June 27th, 2014)
Today, Ing.Svobodova is going to take
microscobic pictures using € 125.000 –
microscobe called Olympus Lext, OLS 3100.
It provides pictures in high resolution or 3D. It
depends what you will need. Its features are:
1. Ideal 3D imaging achievable with a single
click.
2. Industrial-leading resolution and
repeatability for extremely reliable measurement
data.
3. Ability to observe and analyze all types of
specimens thanks to versatile observation methods
and a variety of 3D image presentation patterns.
Here are some images of metallographic analysis.
When we look the image, we can see some
pitting corrosion. But in comparison of other
samples this corrosion is not much and harmful.
Material is highly corrosion resistant. It is a
useful property for manufacture. Scratches
occured because of grinding direction.
This part of sample is very corroded. There
scratches over the surface and dendrites. Because
of them we cannot have a good examination over
the surface. But we can learn the negative sides of
metallograhic images for how cannot we study
over a surface? It can answer this question
surroundly.
We can see a lot of dendrites all over the
surface. It is a problem for sample. Because
dendrites are uniform and solid, no way to split
them up. So it makes a big problem to solve
for whole body of sample. It occurs because of
undercooling or supercooling of molten
material.
And about the black dots, they are alpha or
betha phases which means Al solves Mg or
backwards. So that the dots occur.
Properties of AlMg3
