IZMIR KATIP CELEBI UNIVERSITY

Department of Materials Science and Engineering

MSE315
MATERIALS CHARACTERIZATION TECHNIQUES I

Materials preperation methods

and Optical microscopy

2.week Prof.Dr. Mücahit SÜTÇÜ

 Optical microscopy
2

 Optical microscope is one of the most important inventions.

 It has a widely usage area in the science and industrial
applications such as biology, medicine, mineralogy and also
materials science.
 Especially, optical microscope is used to observe internal
structure of materials in materials science.
 Nevertheless, it is widely used in the manufacturing
industry for process control.
 It is one of the most important instruments for the
microstructural characterization of the materials.
 It provides detail information about the properties of
material.
 Optical microscopy
3

 The most familiar tool of metallography is the light

microscope.
 Reflected light microscopes is widely used in the
manufacturing industry as a tool for process control.
 The upper limit to the magnification possible with an
optical microscope is approximately from 50X to 2000X
times and the ability to resolve microstructural features of
~0.2 μm or larger.
 For example, in the casting of engine blocks the
microstructures of cast iron samples are routinely
inspected to make sure there is no "cementite" in the
engine block.
 Cementite (or iron carbide) is a compound of iron and
carbon, more precisely an intermediate transition metal
carbide with the formula Fe3C.
 «Cementite» makes the engine block brittle. Therefore, its
presence must be minimized during manufacturing.
Minimizing is accomplished via microstructural analysis.
 Microstructure of metal alloys
4

 In metal alloys, microstructure is characterized by the

number of phases present, their proportions, and the
manner in which they are distributed or arranged.
 The microstructure of an alloy depends on such variables
as the alloying elements present, their concentrations, and
the heat treatment of the alloy (i.e., the temperature, the
heating time at temperature, and the rate of cooling to
room temperature).

A cast dentritic structure in bronze

 Optical microscopy
5

After appropriate polishing

and etching, the different
phases may be
distinguished by their
appearance.

For example,
• for a two-phase alloy,
one phase may appear
light and the other
phase dark.
• When only a single
phase or solid solution
is present, the texture
will be uniform, except
Back reflected light for grain boundaries
Scattered light
that may be revealed.
 Optical microscopy
6

grains

OM image of polycrystalline
brass
 Scanning electron microscope (SEM)
7

 The other major examination tool

in metallography is the scanning
electron microscope (SEM).
 SEM is a microscope that is
capable of very high magnifications
(up to about 1,000,000x) and
resolution (up to 1nm) which
enables fracture surface imaging.

 The power of the SEM lies in its

ability to provide chemical
information about the surface of
the materials along with very
good depth of focus.
 Contrast in microscopy
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 Sometimes the contrast in a microstructure is inadequate with a SEM under

500×, while it is highly visible with a basic light microscope.
 Contrast between microstructural constituents in light microscopy is very
dependent on specimen preparation.
 Light microscopes also have various types of special illumination modes
that can increase the information gained from the image.
For example,
 polarized-light illumination can improve phase contrast,
 the differential interference contrast (DIC) method can be used to identify
topological height differences on a sample surface that are smaller than 0.2 μm.
 Materialography/Metallography
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 Materialography (metallography): the

Ni-Cr metal super-alloy
microstructural investigation method of the
most materials.
 Metallography is the study of the physical
structure and components of metals and
alloys, typically using microscopy.
 Ceramic and polymeric materials may also be
prepared using metallographic techniques,
hence the terms ceramography, plastography
and, collectively, materialography. Cr2O3-MgO refractory
 The term materialography includes
 ceramography (ceramics)
 metallography (metals)
 plastography (polymers)
 mineralogy (minerals)
 Materialography/Metallography
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 Metallography/materialography includes a wide field in material investigation; it bridges the gap

between science and materials engineering using the materials in modern technology.
 It covers the examination of parts from the cm and m range to atomic dimensions in the nm and
sub-nm range.
 Types of optical microscopes
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 There are mainly two types of optical

microscopes due to their terms of the
light path used:
 Reflected Light (RL) microscope

 Transmitted Light (TL) microscope

 While the former is used for the

study of opaque materials such as
metals and ceramics, the latter is
generally used by geologist for the
study of transparent materials such
as minerals.
 In RL-Microscope, the light is
reflected from the surface of the
sample while in TL-Microscope the
light passes through it.
 Therefore the surface of the sample
should be mirror-like polished and
etched with a suitable etching
solution.
 Sample preparation treatments
12

 In order to have «a mirror finish» the sample goes

through a number of sample preparation
treatments:
surface
1. sectioning and cutting
2. mounting
3. grinding
4. polishing
5. etching
 1. Sectioning and Cutting
13

 Most metallographic samples need to

be sectioned to the area of interest and
for easier handling.
 Depending on the material, the
sectioning operation can be obtained by
 abrasive cutting (metals and metal matrix
composites),
 diamond wafer cutting (ceramics,
electronics, biomaterials, minerals),
 thin sectioning with a microtome (plastics).
 Proper sectioning is required to
minimize damage, which may alter the
microstructure and produce false Figure: Creep, An aircraft part (F-110
inner liner) that was used at T>700oC
metallographic characterization. for long periods. This service abuse led
to creep cracks in the microstructure.
 It is important that the sample must be Notice that the grain boundaries are
representative. opening up under the stress.
 1. Sectioning and Cutting:
14

 Specimen should be cut to <3 cm with a hacksaw or a disc saw.

 During the cutting process the blade and the sample must be
cooled with water in order to avoid the effect of heat that might
change the microstructure.

Abrasive cutting machine

Precision cutting machine

 The most common type of abrasive blades used for metallographic sectioning
and cutting parameters for diamond wafer cutting

15

 Proper cutting
requires the correct
selection of
 abrasive type,
 bonding and size,
 cutting speed,
 load,
 and coolant.
 Cutting discs
 Resin bonded (with
Al2O3 or SiC)
 Metal bonded (with
diamond)
 2. Mounting:
16

 The mounting operation accomplishes three important

functions
 it protects the sample edge and maintains the integrity of a
materials surface features
 fills voids in porous materials
 improves handling of irregular shaped samples.
 The metallographic sample mounting is done by
encapsulating the sample into a mounting polymer
compound as hot or cold mounting depend on the material.
 2. Mounting:
17

 Hot mounting in a press w/phenolic resin, epoxy,

thermosets, acrylics
 Cold mounting in epoxy, acrylic and polyester resins.
 Hot mounting is faster and more generally used for metals
 Moulding pressure (15-40MPa) and temperature (150-
180C), curing time (2-4 min.)
 Cold mounting is favored for ceramic samples.
 Utilized with hardener for polymerization
 Curing time (1-12h) and temperature (25-100C)
 Mounting
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 Samples are embedded in

the polymer resin.
 3. Grinding:
19

 Silicon carbide (SiC) is an excellent abrasive

for grinding because it is very hard.
 Successively sized SiC grinding papers (180-
320-600-1200 Grit) are rotated on a wheel
(~50-250 rpm) and the sample is pushed face
down while watercooling.
 Small SiC particles are glued to the grinding
paper so these are also sometimes called fixed
abrasives. grinding machine
 These particles slowly remove chips from
specimen surface.

Back of grinding paper Front of grinding paper SiC particles on the paper
 3. Grinding:
20

 SiC abrasives are

typically listed by the
grit size (180-320-600-
1200 Grit).
 Abrasive papers
typically contain SiC or
alumina particles.
 Grit size increases, the
grain size of SiC
particles decreases.

Grit size: the number of wires per inch in a screen mesh

 3. Grinding:
21

 When we cut the sample, there is a cutting traces on the sample surface.
 The basic idea is to remove all of the previous specimen damage before
continuing to the next step (polishing) while maintaining planar specimens.
 The planar grinding step is accomplished by decreasing the abrasive particle
size sequentially to obtain surface finishes that are ready for polishing.

After cutting After grinding

120 grit 320 grit 600 grit 1200 grit

Microstructure

Cross-section of the sample after cutting and grinding steps

 3. Grinding:
22

 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.

Grinding directions; AA first grinding

direction, BB second grinding
direction.
 3. Grinding:
23

 The machine parameters, which effect the preparation of metallographic specimens,

include
 grinding/polishing pressure,
 relative velocity distribution,
 the direction of grinding/polishing.
 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 reduce the life of the SiC paper.
 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.
 4. Polishing:
24

 The purpose of the polishing step is to

remove the damage produced during
cutting and planar grinding.
 Polishing is accomplished with
diamond or alumina suspensions
having particles ranging from 9
micron down to 0.05 micron diameter
on polishing cloths.
 Same as grinding except the abrasive
particles are loose and no
watercooling is performed.
 4. Polishing:
25
 Polishing cloths (SEM images)
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Napless, hard, woven nylon, silk or Napless, very hard, woven, coated
acetate cloth for fine grinding/polishing polyester cloth for fine grinding/rough
polishing

Napless, medium hard, woven wool Napless, hard, non woven, synthetic
cloth for polishing cloth for fine grinding/rough polishing
 5. Etching:
27

 The purpose of etching is selectively to removal of certain microstructural

features to reveal the internal structure.
 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.

After etching, formation of pit in the grain microstructure after

boundaries etching
 5. Etching:
28

 The two most common techniques are

chemical and electrochemical etching.
 Chemical etching is typically a
combination of either an acid or
base with an oxidizing or reducing
agent in a solute such as an alcohol.
 Electrochemical etching is a
combination of chemical etching
with an electrical voltage/current.
 5. Etching
29

In multi-phase alloys, when the sample is contacted with the reagent, there is
a potential difference between the phases.
 The phase with high potency behaves
anodically relative to the low-potency
phase and begins to dissolve during
the etching.
 Since the low-potency phase acts
cathodically, it is insoluble during
etching and does not undergo any
decomposition.
 During the etching process, a certain
amount of pitting on the surface as a
result of dissolution of the anodic
phase, and also insoluble flat regions
occurs.
 This allows the acquisition of
meaningful images under the
microscope.
 Etchants
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Chemical Etching: selectively attacks specific microstructural features. It generally

consists of a mixture of acids or bases with oxidizing or reducing agents.
 Use a hood and do not inhale acid vapor.
 Wash the specimen thoroughly to avoid damage on objective lenses.

Click for other etchants: http://www.metallographic.com/Technical/Etching.htm

 OM images of sample surface after sample preparation
steps
31

1) Cutting surface 3) Polished surface

sonrası

2) Ground surface - 220 grit 4) Etched surface