Metallography and Sample

Preparation
Metallography
Metallography is the study of the microstructure of all types of metals and their
metallic alloys. It can be more precisely defined as the scientific discipline of
observing and determining the chemical and atomic structure and spatial
distribution of the constituents, inclusions or phases in metal alloys.
In other words, Metallography is a branch of materials science which relates to
the constitution and structure, and their relation to the properties, of metals
and alloys.

Pearlitic grey cast iron Ductile iron with spheroidal graphite

What is Microstructure?
The structure of a suitable prepared specimen as revealed by a microscope.

3
 Sample Preparation
In order to investigate structure we should prepare samples.
Preparation of metallographic specimens generally requires five
major operations:
1.Sectioning

2. Mounting

5. Etching 3. Grinding

4. Polishing 4
Sample Preparation

A well-prepared metallographic specimen :

 Represents sample.
 Sectioned, ground and polished so as to minimize disturbed or flowed

surface metal caused by mechanical deformation, and thus to allow the true
microstructure to be revealed by etching.
 Free from polishing scratches and pits and liquid staining.

 Flat enough to permit examination at high magnification.

5
 Sectioning

 Many metallographic specimens are used for process control.

 Important uses of metallography include examination of defects that appear in finished
or partly finished products and studies of parts that have failed in service.
 Investigations for these purposes usually require that the specimen be broken from a
large mass of material, and often involve more than one sectioning operation.
 Many metallographic studies require more than one specimen.

 Failed parts may best be studied by selecting a specimen that intersects the origin of
the failure, if the origin can be identified on the surface. Depending on the type of failure,
it may be necessary to take several specimen from that area of the failure and from
adjacent areas.

6
Osmangazi Bridge (Gulf of Izmit)

7
 Sectioning
Sectioning Methods
 Crushing
 Cutting

 Sawing

 Abrasive cutting

Cutting the Sample

 The first thing to remember when cutting samples, is to

preserve the sample axes orientation. Cut the sample in such a

manner that important sample directions, like the Rolling

Sectional
Direction, Transverse Direction and Sample Normal are not lost.

View
 The second thing to remember that the cutting process must

not damage or change the sample as this would lead to Cutting

erroneous results 8
 Wire saw with an endless loop.
Low speed dimond saw

9
 Mounting of Specimens
 The primary purpose of mounting specimens is for convenience in handling
specimens of difficult shapes or sizes during the subsequent steps of
preparation and examination.
 A secondary purpose is to protect and preserve extreme edges or surfaces
defects during preparation.
 Specimens also may require mounting to accommodate various types of
automatic devices used in laboratories or to facilitate placement on the
microscope stage.
 An added benefit of mounting is the ease with which a mounted specimen
can be identified by name, alloy number, or laboratory code number for storage
by scribing the surface of the mount without damage to the specimen.
 Small specimens generally require mounting so that the specimen is
supported in a stable medium for grinding and polishing. The medium chosen
can be either a cold curing resin or a hot mounting compound.

10
The mounting operation accomplishes three important functions:
(1) it protects the specimen 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
specimen preparation without damage to the specimen.

11
Mounting Methods
 The method of mounting should not injure the microstructure of the specimen.

 Mechanical deformation and the heat are the most likely sources of injurious

effects. The mounting medium and the specimen should be compatible with
respect to hardness and abrasion resistance. A great difference in hardness or
abrasion resistance between mounting media and specimen promotes differential
polishing characteristics, relief, and poor edge preservation.
 The mounting medium should be chemically resistant to the polishing and
etching solutions required for the development of the microstructure of the
specimen.

12
Clamp Mounting
 Clamps are used most often for mounting thin sheets of metal when preparing

metallographic cross sections.

 Several specimens can be clamped conveniently in sandwich form.

 The hardness of the clamp should be approximate or exceed the hardness of the
specimen.
 The clamp plates are cut longer and wider than specimens to be clamped.

13
Compression (Hot) Mounting
 Compression mounting involves molding around the specimen by heat and pressure

such molding materials as bakelite, diallyl phthalate resins, and acrylic resins.
 Bakelite and diallylic resins are thermosetting, and acrlyic resins are thermoplastic.

Both thermosetting and thermoplastic materials require heat and pressure during the
molding cycle.

Cold Mounting
 Materials for cold mounting are classified as polyesters, epoxides and acrylics.
Polyesters are transparent, epoxides are almost transparent and straw color; acrylics are
opaque.
 Cold mounting requires no pressure and little heat, and is a means of mounting large

numbers of specimens more rapidly than by compression mounting.

14
15
Table 1 Typical properties of thermosetting molding resins
Resin Heat Coefficient Abrasion Polishing Transparency Chemical
Molding conditions of thermal rate, rate, resistance
distortion
Temperatu temperature expansion μm/min(b) μm/min(c)
Pressure Tim in./in.
re
e, °C(a)
°C MPa MPa psi min °C °F
135- 275- 17- 2500 5-12 140 285 3.0-4.5 × 100 2.9 Opaque Attacked
Bakelite
170 340 29 - 10-5 by strong
(wood-
4200 acids and
filled)
alkalies
Diallyl 140- 285- 17- 2500 6-12 150 300 3.5 × 10-5 190 0.8 Opaque Attacked
phthalate 160 320 21 - by strong
(asbestos- 3000 acids and
filled) alkalies
Source: Ref 1 (a) Determined by method ASTM D 648. (b) Specimen 100 mm2 (0.15 in.2) in area abraded on slightly worn 600-grit
silicon carbide under load of 100 g at rubbing speed of 105 mm/min (4 × 103 in./min). (c) 25-mm (1-in.) diam mount on a wheel
rotating at 250 rpm covered with synthetic suede cloth and charged with 4 to 8 μm diamond paste.

16
Table 2 Typical properties of thermoplastic molding resins
Resin Transpare Heat Coefficient Abrasio Polishing Chemical
Molding conditions ncy distortion of thermal n rate, rate, resistance
Heating Cooling temperatu expansion, μm/mi μm/min(
re(a) in./in. °C n(b) c)
Temperatu
Pressure Tim Temperature Pressure
re Time
°C °F MPa psi e °C °F MPa psi
Not resistant
Methyl 140- 285- 17- 2500- 6 75-85 165- max ma 6-7 Water, 65 150 5-9 × 10-5 ... 7.5 to strong
methac 165 330 29 4200 185 x white to acids and
rylate clear some
solvents,
especially
ethanol
Polystyr 140- 285- 185-
17 2500 5 85 max . . . 6 ... 65 150 . . . ... ... ...
ene 165 330 212
Polyvin Light Not resistant
yl 220 430 27 4000 ... ... ... ... ... ... brown, 75 165 6-8 × 18-5 20 1.1 to strong
formal clear acids
Polyvin Resistant to
120- 250-
yl 0.7 100 nil 60 140 27 400 . . . Opaque 60 140 5-18 × 10-5 45 1.3 most acids
160 320
chloride 0 and alkalies

Source: Ref 1
(a) Determined by method ASTM D 648.
(b) Specimen 100 mm2 (0.15 in.) in area abraded on a slightly worn 600-grit silicon carbide paper under load of 100 g at rubbing speed of 105 mm/min.
(c) 25-mm (1-in.) diam mount on a wheel rotating at 250 rpm covered with a synthetic suede cloth and charged with 4-8 μm diamond paste.

17
 Grinding
Grinding is a most important operation in specimen preparation.

Grinding is accomplished by abrading the specimen surface through a sequence of

operations using progressively finer abrasive grit. Grit sizes from 40 mesh through 150
mesh are usually regarded as coarse abrasives and grit sizes from 180 mesh through
600 mesh as fine abrasives.
During grinding the operator has the opportunity of minimizing mechanical surface

damage that must be removed by subsequent polishing operations.

Even if sectioning is done in a careless manner, resulting is severe surface damage,
the damage can be elimenated by prolonged grinding.
Sectional
View

Grinding 18
Cutting
Grinding

 The purpose of grinding is to lessen the depth of deformed metal to the

point where the last vestiges of damage can be removed by series of
polishing steps.
 The scratch depth and the depth of cold worked metal underneath the
scratches decrease with decreasing particle size of abrasive.
 It is imperative that each grinding steps completely remove the deformed
metal produced by the previous step.
To ensure the complete elimination of the previous grinding scratches
found by visual inspection, the direction of grinding must be changed 45 to
90 degrees between successive grit sizes.
 In addition, microscopic examination of the various ground surfaces during
the grinding sequence may be worthwhile in evaluating the effect of grinding.
Each ground surface should have scratches that are clean-cut and uniform in
size, with no evidence of previous grinding scratches.
19
 Grinding
Most grinding of metallographic specimen is performed by manually holding the
specimen with its surface against a grinding material.
To establish and maintain a flat surface over the entire area being ground, the operator
must apply equal pressure on both sides of the specimen and avoid any rocking motion
that will produce a convex surface.
Specimens should be cleaned after each grinding steps to avoid any carryover of
abrasive particles to the next step.
The grinding abrasives commonly used in the preparation of specimens are silicon
carbide (SiC), aluminium oxide (Al2O3), emery (Al2O3 -Fe3O4), diamond particles, etc.
Usually are generally bonded to paper or cloth backing material of various weights in
the form of sheets and disks.

20
Grinding

21
 Grinding
The series of photos below shows the progression of the specimen when ground with
progressively finer paper.
Copper specimen ground with 180 grit paper Copper specimen ground with 400 grit paper

Copper specimen ground with 800 grit paper Copper specimen ground with 1200 grit paper

22
 Polishing

 Polishing is the final step in production a surface that is flat, scratch free, and mirror

like in appearance.
 Such a surface is necessary for subsequent accurate metallographic interpretation,
both qualitative and quantitative.
 Before final polishing is started, the surface condition should be at least as good that

obtained by grinding with a 1200-grit abrasive.

Sectional
View

Grinding Polishing 23
Cutting
Polishing
Copper specimen polished to 6 micron level

Copper specimen polished to 1 micron

level

24
 Etching
 Although certain information may be obtained from as-polished specimens, the
microstructure is usually visible only after etching.
 Only features which exhibit a significant difference in reflectivity (10% or greater)
can be viewed without etching.
 This is true of microstructural features with strong color differences or with large
differences in hardness. Cracks, pores, pits and nonmetallic inclusions may be observed
in the as-polished condition.
 In most cases, a polished specimen will not exhibit its microstructure because

incident light is uniformly reflected.

25
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.

26
Etching

Etched copper specimen Over etched copper specimen

27
Specimen Storage
When polished and etched specimens are need to be stored for long periods of
time, they must be protected from atmospheric corrosion. Desiccators and vacuum
desiccators are the most common means of specimen storage.

28
Materials Characterization
Depending on the nature of the material being investigated, a suite of techniques
may be utilized to assess its structure and properties. Whereas some techniques
are qualitative, such as providing an image of a surface, others yield quantitative
information such as the relative concentrations of atoms that comprise the aterial.
Recent technological advances have allowed materials scientists to accomplish
something that was once thought to be impossible: to obtain actual two-
dimensional/three dimensional images of atomic positions in a solid, in real time. It
should be noted that the sensitivity of quantitiative techniques also continues to be
improved, with techniques now being able to easily measure parts per trillion (ppt)
concentrations of impurities in a bulk sample.

29
Materials Characterization
Optical Microscopy
The microstructure of a material is related directly to its physical, chemical, and
mechanical properties as they are influenced by processing and/or the environment.
Among the numerous investigative techniques used to study materials, optical microscopy,
with its several diverse variations, is important to the researcher and/or materials
engineer for obtaining information concerning the structural state of a material.
Information gained using optical microscopy is complementary to other techniques and
provides unique information to assess the microstructure of the sample.

30
Materials Characterization
Material characterization gives information needed about the structure and
composition of materials.

Microscopy is a category of characterization techniques which probe and map the

surface and sub-surface structure of a material. These techniques can use photons,
electrons, ions or physical cantilever probes to gather data about a sample's
structure on a range of length scales.
31
Scanning Electron Microscopy

The scanning electron microscope (SEM) is a type of electron microscope that images
the sample surface by scanning it with a high-energy beam of electrons in a raster
scan pattern. The electrons interact with the atoms that make up the sample
producing signals that contain information about the sample's surface topography,
composition and other properties such as electrical conductivity.

32
SEM – X-ray Analysis (eds)

33
Scanning Tunneling Microscopy

A scanning tunneling microscope (STM) is a powerful instrument for imaging surfaces at

the atomic level. Its development in 1981 earned its inventors, Gerd Binnig and Heinrich
Rohrer (at IBM Zürich), the Nobel Prize in Physics in 1986. For an STM, good resolution is
considered to be 0.1 nm lateral resolution and 0.01 nm depth resolution. With this
Resolution, individual atoms within materials are routinely imaged and manipulated. The
STM can be used not only in ultra high vacuum but also in air, water, and various other
liquid or gas ambients.

34
Atomic Force Microscopy (AFM)

Atomic or near-atomic resolution images of topography of conductors,

semiconductors and insulators.

35
X-ray Photoelectron Spectroscopy (XPS)

X-ray photoelectron spectroscopy (XPS) is a quantitative spectroscopic technique

that measures the elemental composition, empirical formula, chemical state and
electronic state of the elements that exist within a material. XPS spectra are
obtained by irradiating a material with a beam of X-rays while simultaneously
measuring the kinetic energy and number of electrons that escape from the top 1
to 10 nm of the material being analyzed. XPS requires ultra high vacuum (UHV)
conditions.

36
X-ray Diffraction (XRD)

Powder XRD (X-ray Diffraction) is perhaps the most widely used x- ray diffraction
technique for characterizing materials. As the name suggests, the sample is usually in
a powdery form, consisting of fine grains of single crystalline material to be studied.
The technique is used also widely for studying particles in liquid suspensions or
polycrystalline solids (bulk or thin film materials).

37