Metallographic Test Report
Metallography is the science and art of preparing a metal surface for analysis by
grinding, polishing, and etching to reveal microstructual constituents. After preparation, the
sample can easily be analyzed using optical or electron microscopy. A skilled technician is
able to identify alloys and predict material properties, as well as processing conditions by
metallography alone.
Metallographic and materialographic sample preparation seeks to find the true
structure of the sample. Mechanical preparation is the most common method of preparing the samples for examination. Abrasive particles are used in successively finer steps to remove material from the sample surface until the needed result is archived. A large number of preparation machines for grinding and polishing are available, meeting different demands on preparation quality, capacity, and reproducibility.
A systematic preparation method is easiest way to achieve the true structure. Sample preparation must therefore pursue rules which are suitable for most materials. Different material with similar properties (hardness and ductility) will respond alike and thus require
the same consumables during preparation.
Main aim of this examination to conduct failure analysis. Failure analysis consists of investigations to find out how and why something failed. Understanding the actual reason for failures is absolutely required to avoid recurrence and prevent failure in similar equipment. The analysis should also help with the understanding and improvement of design, materials
selection, fabrication techniques, and inspection methods.
Contents:
I.Introduction
Objective of Metalography
II.Examination Procedure
a) Specimen Preparation
1)Grinding
2)Polishing
3)Etching
b) Examination Methods:
1) Microscopical Examination
2) Macroscopic Examination
III.Theory
1)Microscopical Examination
2)Macroscopic Examination
IV.Experimental Apparatus
V.Analysis – Results
1)Microscopical Examination
Specimen No 1
Specimen No 2
Specimen No 3
Specimen No 4
2)Macroscopic Examination
I .Sulphur Printing
II. Flow Lines
III. Welded Sections
VI.Discussion
VII.Conclusion
VIII.Referances
II. Introduction
Objective of Metalography
Metallography is the imaging of topographical or microstructural features on prepared
surfaces of materials. The properties and performance of materials are controlled by the
structures studied by metallography.
In this technique, planar surfaces are prepared to obtain a polished finish. Chemical or
other etching methods are often used to delineate macrostructure and microstructure
features,which provide information on phase distribution, grain size, solidification structure,
and thermo-mechanical processing history.
Metallography is also used for characterizing the macroscopic and microscopic
configuration at planar sections of welds, brazes, and fabricated components. In failure
analysis, morphology or corrosion of cracks can be characteristic of failure mode. The
prepared samples are examined by the unaided eye, light microscopy, and/or electron
microscopy.
III. Examination Procedure
a)Specimen Preparation
A systematic preparation method is 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.
Grinding
The purpose of the grinding step is to remove damage from cutting, planarize the specimen(s),
and to remove material approaching the area of interest.
The most common metallographic abrasive used is Silicon Carbide – SiC. It is an ideal
abrasive for grinding because of its hardness and sharp edges. For metallographic preparation,
SiC abrasives are used in coated abrasive grinding papers ranging from very coarse 60 grit to
very fine 1200 grit sizes. Some of the application procedures are given below.
• Soft non-ferrous metals – Initial grinding is recommended with 320 grit SiC abrasive paper
followed by 400, 600, 800 and 1200 grit SiC paper. Because these materials are relatively soft
they do not easily break down the SiC paper. Thus initial grinding with 320 grit is generally
sufficient for minimizing initial deformation and yet maintain adequate removal rates. For
extremely soft materials such as tin, lead and zinc it is also recommended that the abrasive
paper be lightly coated with a paraffin wax. The wax reduces the tendency of the SiC abrasive
to embed into the soft specimen.
• Soft ferrous metals – are relatvely easy to grind with the depth of deformation being a major
consideration. 240 grit SiC abrasives provide a good initial start with subsequent use of 320,
400, 600, 800 and 1200 grit SiC.
• Hard ferrous metals – require more aggressive abrasives to achieve adequate material
removal. Thus coarse SiC abrasives (120 or 180 grit) are recommended for stock removal
requirements. Once planarity and the area of interest are obtained a standard 240, 320, 400
and 600 grit series is recommended.
• Super alloys – are generally of moderate hardness but have extremely stable elevated
temperature characteristics and corrosion resistance. The procedures for preparing super
alloys is very similar to that for most non-ferrous metals.
• Ceramics – are extremely hard, corrosion resistant and brittle materials. They fracture
producing both surface and subsurface damage. Proper grinding minimizes both of these
forms of damage. This requires the application of a semi-fixed abrasive which are held rigidly
for grinding but can be dislodged under high stress in order to minimize subsurface damage.
The abrasive size is also important because very coarse abrasives will remove material
quickly but can seriously damage the specimen. For ceramics, consideration of the damage
produced at each preparation step is critical to minimizing the overall preparation sequence.
• Composites – are perhaps the most difficult specimens to prepare because of the wide range
of properties for the materials used. For example, a metal matrix composite (MMC) such as
silicon carbide ceramic particles in an aluminum metal matrix is a difficult specimen to
prepare. This composite contains extremely hard/brittle ceramic particles dispersed in a
relatively soft/ductile metal matrix. As a rule of thumb, initial grinding should focus on metal
planarization and grinding to the area of interest. The secondary grinding steps require
focusing on the ceramic particles and typically requires the use of diamond abrasives.
2) Polishing
Polishing is the most important step in preparing a specimen for microstructural analysis. It is
the step which is required to completely eliminate previous damage.
Ideally the amount of damage produced during cutting and grinding was minimized through
proper blade and abrasive grinding so that polishing can be minimized.
To remove deformation from fine grinding and obtain a surface that is highly reflective, the
specimens must be polished before they can be examined under the microscope. Polishing is a
complex activity in which factors such as quality and suitability for the cloth, abrasive,
polishing pressure, polishing speed and duration need to be taken into account. The quality of
the surface obtained after the final polishing depends on all these factors and the finish of the
surface on completion of each of the previous stages.
Polishing Cloths
There are three types of polishing clothes; Woven, Non-Woven and Flocked.
- Woven cloths offer ‘hard surface’ polishing properties and guarantee flat pre-polishing,
without deterioration of the edges.
- Non-woven cloths, are used on very hard materials for high precision surface finishing such
as glass, quartz, sapphire and semi-conductors.
- The Flocked cloths, guarantee a super-polished finish. The polishing duration must be as
short as possible, to avoid inclusions from being extracted.
Diamond products
Diamond, due to its exceptional hardness and cutting capacity, has become the first choice
abrasive in metallographic polishing. Diamonds for metallographic grinding and polishing are
available in two different crystalline shapes: Polycrystalline (P) and monocrystalline (M).
Polycrystalline diamonds provide vast numbers of small cutting edges. In the metallographic
preparation process these edges result in high material removal, while producing only a
shallow scratch depth.
Monocrystalline diamonds are more block-shaped and provide few cutting edges. These
diamonds give high material removal with a more variable scratch pattern. For high
requirements, the (P)-type diamonds are chosen. The (M) type diamonds are best suited for
all-purpose polishing. Diamond products are usually available in three forms; diamond paste,
diamond suspension and diamond spray.
Polycrystalline diamond as compared to monocrystalline diamond provides better surface
finishes and higher removal rates for metallographic specimen preparation. The features and
advantages of polycrystalline diamond include the following:
• Higher cutting rates
• Very uniform surface finish
• More uniform particle size distribution
• Higher removal rates (self sharpening abrasives)
• Harder/tougher particles
• Blocky shaped
• Hexagonal microcrystallites (equally hard in all directions)
• Extremely rough surface (more cutting points)
• Surface area 300% greater than monocrystalline diamond
• No abrasion-resistant directionality
3) Etching
The purpose of etching is two-fold. Grinding and polishing operations produce a
highly deformed, thin layer on the surface which is removed chemically during etching.
Secondly, the etchant 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. There are
many tried and tested etchants available but there are mandatory safety issues associated with
the preparation and use of all of these. Consequently, you are limited to using just three preprepared
solutions (Table). Please adhere to the general safety regulations provided to you at
the beginning of the academic year.
2% Nital Ferric Chloride Sodium Hydroxide
Steel Stainless steel Aluminium & alloys
- Copper & alloys Zinc & alloys
- – Magnesium & alloys
A polished sample is etched using a cotton tip dipped in the etchant. 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 go then the polishing
procedure will have to be repeated.
b) Examination Methods:
A)Microscopical Examination
This is performed on samples either cut to size or mounted in a resin mold. The
samples are polished to a fine finish, normally one micron diamond paste, and usually etched
in an appropriate chemical solution prior to examination on a metallurgical microscope. This
is performed on samples either cut to size or mounted in a resin mold. The samples are
polished to a fine finish, normally one micron diamond paste, and usually etched in an
appropriate chemical solution prior to examination on a metallurgical microscope.
In order to obtain reproducible results,with good contrast in th image, the specimen
surface is polished and subsequently etched with reagents before microscopic
examination.Grain boundaries ares 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 speciemen surface.
B)Macroscopical Examination
Macroetching is the procedure in which a specimen is etched and evaluated macro structurally
at low magnifications. It is a frequently used technique for evaluating steel products such as
billets, bars, blooms, and forgings. There are several procedures for rating a steel specimen by
a graded series of photographs showing the incidence of certain conditions and is applicable
to carbon and low alloy steels. A number of different etching reagents may be used depending
upon the type of examination to be made. Steels react differently to etching reagents because
of variations in chemical composition, method of manufacturing, heat treatment and many
other variables.
Macro-Examinations are also performed on a polished and etched cross-section of a welded
material. During the examination, a number of features can be determined including weld run
sequence, important for weld procedure qualifications tests. As well as this, any defects on the
sample will be assessed for compliance with relevant specifications. Slag, porosity, lack of
weld penetration, lack of sidewall fusion and poor weld profile are among the features
observed in such examinations. It is normal to look for such defects either by standard visual
examination or at magnifications of up to 50X. It is also routine to photograph the section to
provide a permanent record. This is known as a photomacrograph.
IV. Theory
A)Microscopical Examination
Microstructural examination may provide various information about list below
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
For grain size measurement the grains along a line,circle, or within a known area are
counted. In lineer intercept method, the grains intercepted by a theoretical line on the
specimen surface are counted. The average grain diameter is given by:
d=C/nL.M
d= The average grain diameter
C= Some constant greater than 1 ( typically, a value of C=1,5 is adequate)
nL= per unit length of a test line
M= Corrected for the magnification
Magnifications up to 1000x can be obtained with a resolution of 2 um.
B)Macroscopical Examination
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 ~ FeSO4 + H2S
Or
MnS + H2SO4 ~ MnSO4 + H2S
H2S + 2 AgBr ~ Ag2S + 2 HBr
V. Experimental Apparatus
In Microscopy examination is done with the prepared metal specimen, employing
magnifications with the optical microscope of from 100x to as high as 2000x
In Macroscopy the examination of the structural characteristics of metal is done by
unaided eye or the aid of a low-power misroscope ,usually under 10x
VI. Anaysis – Results
1) Microscopical Examination
Specimen No 1 :
Ductile Cast Iron By adding a small amount (0.05wt %) of magnesıum to the molten
metal of the gray iron composition , spherodial graphite precipitates rather than flakes are
produced. Ductility is increased by a factor of 20 , and strength is doubled
Specimen No 2 :
Gray Cast Iron It has a grey fracture surface with finely faceted structure.A significant
silicon content ( 2 to 3 wt %) promotes graphite (C) precipitation rather than cememntite
(Fe3C) . The sharp, pointed graphide flakes contribute to the characteristic brittleness in gray
iron
Specimen No 3 :
White Cast Iron It has a characteristic white ,crystalline fracture surface: Large amounts
of Fe3C are formed during casting, giving a hard , brittle material.
Specimen No 4 :
Low Carbon Stainless Steel That steel has two constituents, which are ferrite and pearlite. The
light coloured region of the microstructure is the ferrite. The grain boundaries between the
ferrite grains can be seen quite clearly. The dark regions are the pearlite. Decreasing the size
of the grains and decreasing the amount of pearlite improves the strength, ductility and the
toughness of the steel.
2) Macroscopical Examination
I) Sulphur Printing
Impurities is desiarable 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 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.
II) Flow Lines
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.
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.
III) Welded Sections
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 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.
VII. Discussion
1)
2)In this sitiation sulphur distributed homogeneously so that this material is not brittle as
much as the material that has segratgated points.Being gather together for sulphur inclusions
maket he part more brittle.
3)Lathing makes the flow lines appear.The reason of appearing flow lines to cut and take out
the particle.When casting occuring there is not any big flow lines appear because casting
doesn’t cut the lines by the way it is done as particle is liquid.
4)It effect tensile and pressing stress of material and make pressing stres 10 multıple than
tensile stres.
5)
6) . The different light reflections of welded material and welding consolidative shows the
structure of whole section such as dispersion of welding material or air holes, that minimize
the quality of welding. It can be interpreted from the image whether the welding done
efficiently, faulty or incompletely. So, the stability of the welding section can be estimated.
VIII. Conclusion
In both macroscopical examination and the microscopical examination the fundemental
is to study the characteristic or constitution of a metal in relation to its physical and
mechanical properities.In macroscopy this procedure is more sketchy and more memorable so
that grinding , polishing and etching the three crucial preperation types should be learnt
exactly.In microscopy , microscope used and structures check and decided which belong to
sources .It is also studied that sulphur inclusions as segregated points and lathing(destroy flow
lines) make particle brittle.
IX. Referances
1) General prosedure taken from MATERIAL TESTING Laboratory Manual – 2006
Metallographic Test - Metallography Testing
Metallographic Test Report
Stress Corrosion Cracking (SCC)
Chloride Stress Corrosion Cracking
Stainless Steel Corrosion
Corrosion of Piping
Corrosion Process
Surface Coatings for Corrosion
Corrosion Resistant Material
Bi- Metallic Corrosion.Galvanic Corrosion
Intergranular Corrosion
Intergranular Corrosion of Stainless Steel Tubes
Corrosion Resistant Stainless Steel Tube
Corrosion Resistance of Stainless Steel Tubes
Seawater Resistance of Stainless Steel Tubes
Corrosion Mechanism in Stainless Steel Tube
ASTM A262 Intergranular Corrosion Test IGC
ASTM E112 Standard Test Methods for Determining Average Grain Size
Methods of minimizing chloride stress corrosion cracking
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