METALLOGRAPH

Y
Dr. Vika Rizkia
Mechanichal Engineering
Jakarta State Polythechnic
METALLOGRAPHY… is the scientific discipline of examining and
determining the constitution and the
underlying structure of (or spatial relationships
between) the constituents in metals, alloys and
materials (sometimes called materialography).
the science and art of preparing a
metal surface for analysis by grinding,
polishing, and etching to show
microstructual component

The mechanical properties of the materials are strongly affected by their microstructures

Metallography is one of the most used methods in metallurgy in order to characterize the
microstructures of the materials

This method allows the study and characterization of metals, ceramics and polymers

Optical and electronic microscopy are the major techniques used to obtain images of the
characteristic microstructures of the materials

Introduction
Microstructure:
is the geometric arrangement of grains and the different phases
present in a material

Grain Boundaries
is the interface between two grains in a polycrystalline material
where the crystal is disordered due to rapid change in
crystallographic directions.

Most engineering alloys are polycrystalline this means that each piece of a metal is made
up of a great number of single crystals, or grains, each having a regular crystal structure
(for example, FCC, BCC, or HCP).

Materials specialists are interested to see the grain boundaries in order to estimate the
grain sizes. The average grain size in metals is usually in the order of several to tens of
micrometers, which can be measured only by the use of an optical or light microscope

Introduction
 Application
Study and characterization of materials
Ensure that the associations between properties and structure are
properly understood
Predict properties of materials
Design alloys with new properties
Check if the material has been correctly heat treated

Applications
SAMPLE PREPARATION
Sectioning
Is the removal of a conveniently sized and representative specimen from a larger piece, is
the first major operation in the preparation of metallographic specimens

Metallurgical sectioning is important and critical when preparing specimens for physical or
microscopic analysis
the unproper cutting technique may alter the real microstructure of the
Note: material and provide a unreal information

The sample damage caused during the cutting process depends on :

• Type of material
• Type of technique employed for cutting
• Cutting speed
• Amount and type of coolant used for cooling process

Material surface damages can easily be removed by

polishing
The damage depth varies with both the type of material and
the employed cutting method
Sectioning
Sawing is perhaps the oldest met lab method of sectioning that is still used today. It can
be accomplished with a hand-held hacksaw, but it can alter the microstructure

Abrasive Wheel Sectioning is The most popular method

of sectioning is with abrasive cut-off wheels.

Wheels made of silicon carbide, aluminum oxide, and

diamonds are used in the sectioning process.

With this type of sectioning, the metallographer has

more control over the conditions used
Sectioning
Sectioning
Sample Cleaning
Physical cleaning: removal of particles, dust, grease and other
types of residues;

Chemical cleaning: used to eliminate any contaminant on the

surface of the sample

Note:
In order to analyse oxide layers the cleaning process must
be limited to simple treatments avoiding the loosening of
the oxide layer details
The ultra-sound bath is the most effective method for
cleaning

Cleaning times may vary between 2-5 minutes

Soft materials may suffer cavitation during large cleaning

times
Sample Mounting
Small samples can be difficult to hold safely during grinding and polishing operations, and
their shape may not be suitable for observation on a flat surface.

AFTER a metallographic specimen is cut to an appropriate size, mounting of the

specimen is often desirable or necessary for subsequent handling and
metallographic polishing

Mounting may done by encapsulating the specimen in a polymeric material or by

clamping with a mechanical device.

In some cases, specimens are not mounted. For example, large-sized specimens
may not be mounted

Cold mounting can be done using two components Hot-mounting the sample is
resins (epoxies) which are liquid to start with but surrounded by an organic polymeric
which set solid shortly after mixing. it requires very powder which melts under the
simple equipment consisting of a cylindrical ring influence of heat (about 200 C).
which serves as a mould and a flat piece which Pressure is also applied by a piston,
serves as the base of the mould. the sample is ensuring a high quality mould free of
placed on the flat piece within the mould and the porosity and with intimate contact
mixture poured in and allowed to set. Cold between the sample and the
mounting takes few hours to complete polymer.
Sample Mounting
ADVANTAGES..
Edge retention of mounted specimens is markedly superior to that of
unmounted specimens
Easier handling of specimens that are too small, fragile, or awkwardly shaped

Containment of sharp edges or corners that may damage the papers and cloths used in
polishing equipment or pose a hazard during handling

Convenient and uniform configuration for either manual or automatic grinding and polishing
machines

Specimen identification of unmounted specimens is difficult and nonpermanent. More details

can be listed on the back of a mount, and this information is not easily degraded with time

Standard size for ease of storage in desiccator cabinets

Sample Mounting
It allows the proper handling of the sample during the polishing and microstructure
examination

It increases the personal security and decreases the risk of damage of the SiC paper and
cloths

For thin films the resin provides the mechanical retention of the
film

Resin thickness Too thin causes a hard handling of the sample

Too thicker decreases the contact between the sample surface and
the SiC papers and cloths

Depends on the material characteristics the heating during the mounting may alter its
microstructure
Sample Mounting
Sample Mounting
Sample Mounting
INVESTIGATIONS OF THE STRUCTURES of metals are generally carried out on sections that
have been cut from a bulk specimen. Frequently, only a single section surface is prepared,
and the structural features exposed on this surface may be investigated using various
techniques
Grinding: Papers covered by abrasive particles such as SiC. The particle size varies
according the desired finishing

The finishing of the sample surface is done by decreasing the

abrasive particle size

There are a number of grades of paper. For example 180, 240, 400,
1200, grains of silicon carbide per square inch. 180 grade therefore
represents the coarsest particles and this is the grade to begin the
grinding operation. Always use light pressure applied at the centre
of the sample.

Wash the sample in water and move to the next grade, orienting
the scratches from the previous grade normal to the rotation
direction. This makes it easy to see when the coarser scratches have
all been removed

Grinding
Grinding
The polishers consist of rotating discs covered with soft cloth impregnated with a pre-
prepared slurry of hard powdery alumina particles (Al2O3, the size ranges from 0.5 to 0.03
µm).

Begin with the coarse slurry and continue polishing until the grinding scratches have been
removed.

It is of vital importance that the sample is thoroughly cleaned using soapy water, followed
by alcohol, and dried before moving onto the final stage. Any contamination of the final
polishing disc will make it impossible to achieve a satisfactory polish.

Examining the specimen in the microscope after polishing should reveal mirror like surface

Polishing
ETCHING is used in metallography primarily to reveal the microstructure of a specimen
under the optical (light) microscope

A proper sample to applying etching must present a smooth surface carefully polished,
without scratches or deformation

A well-polished surface do not exhibit its microstructure since light is homogeneously

reflected along it

Usually the microstructure of the material is visible after acid etching

The different grains and orientations of the crystallographic structure of the material
cause a difference in light reflection which allows the visualization of the microstructure

attacks the surface with preference for those sites with the highest energy, leading to
surface relief which allows different crystal orientations, grain boundaries, precipitates,
phases and defects to be distinguished in reflected light microscopy as demonstrated in
Figure

Etching
Etching
Etching should always be done in stages, beginning with light attack, an examination in the
microscope and further etching only if required.

If you overetch a sample on the first step then the polishing procedure will have to be repeated.

ETCHING PARAMETERS
Exposition time: The times may vary from a few seconds to hours
Acid temperature: The acid temperature and exposition time
are closely linked. Usually the greater the acid temperature
the lesser the etching time
The quality of etching may be affected according the etching
times
Usually the etching procedure is performed in ambient
temperature

Etching
Etching
Colour Etching
Color etching, also commonly referred to as tint etching, has been used to color many metals and
alloys, such as cast irons, steels, stainless steels, nickel-base alloys, copper-base alloys, molybdenum,
tungsten, lead, tin, and zinc. Satisfactory color, or tint, etchants are balanced chemically to produce a
stable film on the specimen surface.

This is contrary to ordinary chemical etching (discussed in the section “Etching” of this article), when
the corrosion products produced during etching are redissolved into the etchant

Color etchants work by immersion, never by swabbing

Externally applied potentials are not used

Color etchants have been classified as anodic, cathodic, or complex systems, depending on the
nature of the film precipitation

Color etchants are usually acidic solutions, using water or alcohol as the solvent

They have been developed to deposit a 0.04 to 0.5 μm (1.6 to 19.7 μin.) thick film of an oxide,
sulfide, complex molybdate, elemental selenium, or chromate on the specimen surface.
Colour Etching

Fe-1C alloy etched with Fe-1.86C alloy color Aluminum bronze (ASTM B
acidified 1 g Na2MoO4 in 100 etched with 2% nital to 148, grade 9C) heat treated
mL H2O to color the cathodic
reveal plate martensite to form Al4Cu9. Pre-etched
cementite.
The cementite in the pearlite is within austenite grains with aqueous 10%
blue; grain-boundary cementite and ledeburite in the grain (NH4)2S2O8 and color
is violet. 500×. (G.F. Vander boundaries. 500×. (A.O. etched with Beraha's lead
Voort) Benscoter) sulfide reagent. 500×. (G.F.
Vander Voort)
Colour Etching

Alpha brass (Cu-30Zn) cold Recrystallized Ti-6Al-4V alloy Equiaxed α structure of pure
worked and annealed. with a crack resulting from titanium. The white surface
Color etching with creep-rupture testing. Attack layer is oxygen-stabilized α.
Klemm's I reagent, which polished The green at the top is
required approximately 1 and color etched in 100 mL mounting resin. Color
h, revealed all the grains distilled H2O, 4 mL HCl, and 3 etched with 100 mL distilled
and annealing twins. 100×. g NH4HF2. Polarized light H2O and 5 g NH4HF2. 50×.
(G.F. Vander Voort) illumination. 100×. (G. Müller)
(G. Müller)
Colour Etching

Ductile iron (3.63 to 3.69% C,

Armco iron friction welded Chromized sheet steel (Fe- 2.74% Si, 0.26% Mn, 0.084%
to carbon steel. Structure is 0.06C-0.35Mn-0.04Si- S, 0.13% Cu, 0.060% Mg) as-
ferrite (smaller grains) and 0.40Ti) color etched to cast
pearlite plus ferrite (large delineate ferrite alloy. Structure consists of
grains). Color etched with structure. 3 g K2S2O5, 10 g graphite nodules in
Klemm's I reagent. 200×. (G. Na2S2O3, and 100 mL H2O. envelopes of free ferrite in a
Müller) 100×. (A.O. Benscoter) pearlite matrix. Color etched
with Klemm's I reagent.
200×. (G. Müller)
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