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Training Module - Quality Assurance & Control

MATERIAL TESTING

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OBJECTIVE

Objective of this Module to understand the Importance and Procedure of Various Material Testing which are done in house for Mechanical Properties, Chemical Properties & for Microstructure evaluation of Steel. In this Module a brief discussion is done on the Mechanical properties of Steel.

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MATERIAL TESTING
To know the Properties of material we do the Material Testing. In Steel we do the following Testing to know the Material Properties:

1. Mechanical Properties i.e., Strength, Hardness, Toughness, fatigue etc. 2. Microstructure i.e., structure, grain size, inclusion etc. 3. Chemical Properties i.e., % of alloying elements presents in steel.

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MATERIAL TESTING MECHANICAL PROPERTIES

Strength Tensile Yield Shear Creep Flexural Stress rupture etc.

Formability % elongation % reduction in area Bending radius etc.

Rigidity Modulus of elasticity Modulus of rigidity Bulk modulus Flexural Modulus etc.

Toughness Impact strength Notch sensitivity etc

Durability Hardness Wear resistance Fatigue Strength etc.

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MECHANICAL PROPERTIES

1. ELASTICITY 2. PLASTICITY 3. STRENGTH 4. DUCTILITY 5. HARDNESS 6. BRITTLENESS

7. TOUGHNESS 8. STIFFNESS 9. RESILIENCE 10. MALLEABILITY 11. FATIGUE 12. CREEP

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MECHANICAL PROPERTIES
1. ELASTICITY: It is defined as non-permanent deformation. It is ability of material to resume its original size and shape, after the force is removed. It is defined as permanent deformation. It is the ability of material to be permanently deformed without fracture even after the removal of force. Strength may defined as the capacity of metal to withstand load. It is the ability of material to be permanently deformed without breaking when a force is applied. Hardness of material is defined as the resistance of material to scratch, wear or penetration of its surface by harder bodies. The property fracturing a material without warning or appreciable deformation is called brittleness.

2. PLASTICITY:

3. STRENGTH:

4. DUCTILITY:

5. HARDNESS:

6. BRITTLENESS:

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MECHANICAL PROPERTIES
7. TOUGHNESS: Toughness is the property of material which enables material to be twisted, bent or stretched under a high stress before rupture. Stiffness is the property of material which enables material to resist deformation. Resilience is the capacity of a material to absorb or store energy , or to resist shock and impact. Malleability is the property of material of getting permanently deformed by compression without rupture. The failure of metal under alternating stresses is known as fatigue failure. A time dependent, permanent deformation at high temperatures, occurring at constant load or constant stress.

8. STIFFNESS:

9. RESILIENCE:

10. MALLEABILITY:

11. FATIGUE:

12. CREEP:

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MATERIAL TESTING
To know the Mechanical Properties of steel we do the following Testing: 1. Tensile testing 2. Hardness Testing 3. Impact Testing 4. Drop-Weight Wear and Tear Test 5. Bend Test

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LIST OF TESTING EQUIPMENTS AT PLATE & COIL MILL


S. N.
1 2 3

NAME OF FACILITY/MACHINE
UNIVERSAL TENSILE TESTING MACHINE WITH ROBOT IMPACT TESTING MACHINE MICRO & MACRO VICKERS HARDNESS TESTER

MAKE
ZWICK ROELL, GERMANY TINUS OLSEN, USA ZWICK ROELL, UK

CAPACITY
1200 KN 542 JOULES Test Forces : 0.1, 0.5, 1, 3, 5, 10, 30 kgf Test Scales : HV0.1, HV0.5, HV1, HV3, HV5, HV10, HV30 and Knoop scales MAGNIFICATION : 10X & 50X XY RANGE : 50x50 MM ANGLE RANGE : 0 to 360 80000 JOULES 150 TON 28 Analytical Channels with Low Nitrogen Channel OXYGEN & HYDROGEN DETECTION MAGNIFICATION : 1500X GRAIN SIZE, INCLUSION RATING, MICRO STRUCTURE ANALYSIS

4 5 6 7 8

PROFILE PROJECTOR DROP WEIGHT TEAR TESTER BEND TEST MACHINE OPTICAL EMISSION SPECTROMETER OXYGEN/HYDROGEN DETECTOR METALLURGICAL MICROSCOPE

MITUTOYO, JAPAN ZWICK ROELL, GERMANY MICRO CONTROL SYSTEM SHIMADZU, JAPAN LECO CORP., USA OLYMPUS, JAPAN

9 ANALYZER & CAMERA STERIO ZOOM MICROSCOPE WITH ILLUMUNATION & SWIVAL

10

OLYMPUS, JAPAN

SURFACE INSPECTION & MACRO PHOTOGRAPHY

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1. TENSILE TESTING
UNIVERSAL TENSILE TESTING MACHINE WITH ROBOT,MAKE-ZWICK ROELL, GERMANY, CAPACITY-1200 KN

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1. TENSILE TESTING
RECTANGULAR TENSION TEST SPECIMEN

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1. TENSILE TESTING
Terminology
Ultimate Tensile Strength The ultimate tensile strength (UTS) is the maximum resistance to fracture. It is equivalent to the maximum load that can be carried by one square inch of crosscross-sectional area when the load is applied as simple tension Elongation A measurement of ductility expressed in terms of the stretch having occurred over a given length on a standard tensile specimen at time of fracture, usually based upon an original length of 2 inches. Yield Strength The stress beyond which stainless steel undergoes important permanent flow commonly specified as that stress producing a 0.2% offset from the linear portion of the stress-strain curve. stressYield Point Load at which a material deforms permanently without increase in the load.
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1. TENSILE TESTING
The Strength of a material when it is called upon to withstand loads which produce a tensile stress in it, is defined as the tensile strength of material.

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1. TENSILE TESTING
The Tensile Strength or ultimate tensile strength (UTS) is the maximum load divided by the original cross-sectional area of the specimen.

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2. HARDNESS TESTING
Hardness is the property of a material that enables it to resist plastic deformation, penetration, indentation and scratching. These tests are commonly used in industry and research work because they provide an easy and reliable method for evaluating the effect of hot and cold working processes and heat treatments, upon the basic properties of metals. There are number of arbitrary definitions of hardness, on the basis of which hardness testing method is selected. Some of these are: 1. Resistance to permanent indentation under static or dynamic loads Indentation Hardness. 2. Energy absorption under impact load Rebound hardness. 3. Resistance of scratching Scratch Hardness. 4. Resistance to abrasion - Wear Hardness. In the Industry, the Indentation Hardness is most commonly used. In the metallurgical sense, it has become a practice to understand hardness as the indentation hardness only, unless otherwise specified.

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INDENTATION HARDNESS
The amount of resistance offered by a metal for indentation or penetration is defined as the Indentation Hardness. In Industry, some hardness test are used as described under: 1. Brinell Hardness Test. 2. Rockwell Hardness Test. 3. Vicker Hardness Test.

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1. BRINELL HARDNESS TEST


Brinell hardness testing machine uses a hardened steel ball of diameter 10mm+/-0.0045mm and the load is 3000kg for hard material, 1500kg for intermediate hardness and 500kg for soft materials. Applying the load on the steel bal for 15 seconds, the load is removed and the indentation made is measured. The surface area of the indentation id dependent upon the depth of penetration. The load applied (in kgf) divided by the spherical area of indentation (in square millimeter) is taken as the Brinell Hardness Number.

Brinell Hardness Test is best for measuring hardness of gray iron casting consisting of soft flake graphite, iron and hard iron carbide.
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2. ROCKWELL HARDNESS TEST


Rockwell Hardness tester is developed with the depth of penetration as the criterion for the hardness of the metal. The machine is a direct type. The dial consists of two pointers. The small pointer which is situated in the top left quarter of the dial proper indicates the application of the minor load of 10 kgf. The anvil with the specimen placed on it is turned slowly so as to lift it upward. The small pointer starts to move once the specimen touches the indenter. The anvil is lifted up until the pointer comes to the stipulated position. Viz., until it comes up to the black dot. Thos indicates that the minor load of 10kgfs is acting upon the indenter. The dial is then turned to the required position i.e., the zero on the C-scale. The major load is applied by pressing the hand lever. The major load of 60,100 and 150kg are used. The common indenters employed in the Rockwell hardness tester are a 1/16 hardened steel ball and a diamond cone. When the former is employed, the major load is maintained at 100kgf and the hardness value read on the B-scale. The B-scale is suitable to test plain carbon steels and common non-ferrous metals and alloys like copper, brasses, bronze etc. For testing very hard materials like hardened steel, diamond indenter is employed. The major load consists of 1540kgf. The hardness is read on C-scale.
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2. ROCKWELL HARDNESS TEST


Advantages of the process: The process is relatively fast. The hardness is directly read on the dial. There is greater latitude for soft to hard materials. A small indentation is left on the objects. Use of initial minor loads avoids the errors arising out of the uneven surface of the metal, and machine and table errors. Disadvantages of the process: The scale range is contracted. The use of more than one scale to express the hardness. Difficulty to readily convert the Rockwell hardness values either into Brinell or Vickers. Errors are likely to be induced when the work is large and overhangs.

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3. VICKER HRADNESS TEST


MICRO & MACRO VICKERS HARDNESS TESTER , ZWICK ROELL, UK

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3. VICKER HRADNESS TEST


The Vickers hardness test uses a square-base diamond pyramid as the indenter. The included angle between opposite faces of the pyramid is 136 . Because of the shape of the indentation diameter, this is frequently called the diamond-pyramid hardness test. The diamond-pyramid hardness number (DPH), or Vickers hardness number (VHN, or VPH) is defined as the load divided by the surface area of the indentation. In practice, this area is calculated from microscopic measurements of the length of the diagonals of the impression. The DPH may be determined from the following equation:

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3. VICKER HRADNESS TEST

The Vickers hardness test has received fairly wide for research work because it provides a continuous scale of hardness, for a given load, from very soft metals with a DPH of 5 to extremely hard materials with a DPH of 1500. The loads ordinarily used with this test range from 1 to 120kg, depending upon hardness of metal to be tested. In spite of these advantages, the Vickers hardness test has not been widely accepted for routine testing because it is slow, requires careful surface preparation of the specimen, and allows greater chance for personal error in the determination of the diagonal length.

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IMPACT TEST
IMPACT TESTING MACHINE , TINUS OLSEN, USA , 542 JOULES

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IMPACT TEST
A simple tensile test does not reveal the brittle nature of the metals, and if only the tensile test data are relied upon the and the object put into use, failure is certain. It is therefore, necessary to test the specimen under shock or sudden loading condition. Strength data are mostly academic. In actual use and practice, we rarely come across the ideal case of gradually applied loads. When we sit on chair, our weight of few kilograms is applied to the chair, suddenly. When an electric motor is put on, the shaft takes a sudden torque of the full r.p.m., being at zero r.p.m. just before. Many instances can be cited when loads at=re borne by engineering components suddenly. There are four types of impact tests. They are: 1. Izod 2. Charpy 3. Fremont,and 4. Amsler. Of the above, the first and second are commonly employed. These machines are standardized in all respects, including the specimen to be used in them.
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IMPACT TEST
The principle employed in all impact testing procedures is that a material absorbs a certain amount of energy before it breaks. The quantity of energy thus absorbed is characteristic of the physical nature of the material. If it is brittle, it breaks rapidly, i.e., absorbs a lesser quantity of energy, and if tough, it needs more energy in order to fracture. The methods of testing are also very similar. A swinging hammer is made to strike the specimen held firmly in a vice. The hammer breaks the specimen on accounts of it potential energy. The height of rise of the hammer on the other side indicates the residual energy of the hammer. The energy actually absorbed by the specimen in order to fracture is given by the difference between initial and final energies of the hammer.

The standard specimen for Impact test is a square rod of 10 mm side. There is a 2mm deep, 45 notch made at a distance of 28 mm from the end of the specimen. The root of the notch is finished with a 0.25mm radius.

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IMPACT TEST
The actual testing procedure as follows: 1. 2. 3. 4. 5. The pendulum weight is brought up and clamped. The specimen is fixed in the vice. The scale is adjusted to read zero. The pendulum weight is released from the clamp. The energy absorbed by the specimen is read on the scale to give the impact strength of the material.

The Impact strength, as explained above is the energy absorbed by the material. It is expressed in ft.lbs., or kilogram force metres.

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DROP WEIGHT TEAR TEST


DROP WEIGHT TEAR TESTER, ZWICK ROELL, GERMANY, 80000 JOULES

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DROP WEIGHT TEAR TEST


The drop weight tear test (DWTT) has been in use for over 40 years now, as a practical laboratory-scale way of ensuring that steel used in the manufacture of line-pipe is not subject to brittle failure when in service. Drop weight and dynamic tear tests are widely used in the steel industry to determine material characteristics such as fracture resistance, transition temperature ranges and suitability of use of a steel for a specific application. During these tests the specimens are cooled or heated over a range of temperatures in order to determine the highest temperatures at which the sample fractures. Below this Nil-Ductility Transition temperature the material will consistently fracture, but above the material does not. The American Petroleum Institute (API) 5L test standard is used to determine the fracture ductility of metal line pipe. Specimens are cut from sections of pipe, soaked at a prescribed temperature and tested within 10 seconds. ASTM E 436, similar to API-5L, is used to establish the temperature range over which ferritic steels undergo a fracture mode transition from ductile to brittle. In both standards a determination regarding ductile to brittle behavior is based upon visual inspection of the specimens in conjunction with, at times, a calculation to determine the percentage of shear seen the materials fracture.
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DROP WEIGHT TEAR TEST

Shear area is calculated by the formula:

T = Thickness of the sample in mm

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BEND TEST Specimen prior to test Specimen after test

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BEND TEST
This is a simple test which indicates the behavior of the metal under bending loads. The metal piece under test is fixed in a vice vertically and bent through an angle of 90. Some designers specify that the bending should be continued further. In such cases, the sheet is taken of the vice and hammered so as to double it. Thus it is bent through an angle of 180. Reversed Bend Test: This is a more drastic test than the bend test. The specimen, after being bent, is straightened and again bent in the opposite direction. Instead of performing the test with a vice and hammer, if it is conducted in a sheet metal press, the magnitude of the bending load can also be measured. The above test serve only as guides, in addition to the conventional tensile test data regarding the percentage elongation. The ease with which the sheet or plate is bent or reverse bent gives us an idea about the work-hardening tendency of the metal, in addition to its formability.

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PRODUCT SPECIFICATIONS USED AT PLATE & COIL MILLS


1. API 5L 2. ASTM A36 3. IS 2062 4. EN 10025

REQUIRED TESTING AS PER STANDARDS


1. API 5L TENSILE ASTM A370 DWTT API RP 5L3 IMPACT ASTM A370 HARDNESS ASTM E92 CHEMICAL ASTM A751 MICRO ASTM E112 BEND (SUPPLEMENTARY) 3. IS 2062 TENSILE IS 1608 IMPACT IS 1757 BEND IS 1599 CHEMICAL IS 228
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2. ASTM A36 TENSILE ASTM A370 CHEMICAL ASTM A751 IMPACT ASTM A673 (SUPPLEMENTARY)

4. EN 10025 TENSILE EN1002 IMPACT EN 10045 CHEMICAL ISO 14284

SAMPLING LOCATION
Sampling Location means from where we can take sample to perform the testing from the plate: 1. API 5L 2. ASTM A36

TT (Transverse tensile test) taken at locations B, C, F, or G CIL (Charpy impact longitudinal) taken at any location, A through H
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SAMPLING LOCATION
Sampling Location means from where we can take sample to perform the testing from the plate: 3. IS 2062 4. EN 10025

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REQUIREMENTS OF SAMPLE POSITION IN DIFFERENT GRADES FOR DIFFERENT TESTS

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SAMPLE SIZE
API 5L
160mm x 700mm (for Transverse Samples) 350mm x 700mm (for Transverse/Longitudinal Samples)

ASTM A36
70mm x 400mm (Normal case) 250mm x 400mm (In case of Impact requirement)

EN 10025
250mm x 550mm

IS 2062
250mm x 550mm

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MICROMICRO-STRUCTURE
1. Metallography
Metallography is the science and art of preparing a metal surface for microstructual analysis of features by grinding, polishing and etching. A systematic method to examine microstructure of materials (mainly metallic materials).

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MICROMICRO-STRUCTURE
1. Metallography
Most engineering alloys are polycrystalline. This means that each piece of a metal is made up of a large number of tiny 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 Microstructure: It is the geometric arrangement of grains and the different phases present in a material Grain Boundaries: It is the interface between two grains in a polycrystalline material where the crystal is disordered due to rapid change in crystallographic directions

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MICROMICRO-STRUCTURE
1. Metallography
Why Metallography ? To Study and characterization of materials To Ensure the correlation between properties and structure To Predict properties of materials To Design alloys with new properties To Check if the material has been correctly processed Requirements of Sample for Success Metallography: Be flat and free from imperfections Stable mounting No chipping Free of all debris Ideally smooth and flawless. Uses of Metallography: Shows grain size, inclusions, impurities Quality control in metal processing Failure analysis Research studies Alloy development

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MICROMICRO-STRUCTURE
1. Metallography
Steps in metallographic sample preparation: 1. Sectioning 2. Mounting 3. Grinding Rough & Fine 4. Polishing Rough & Fine 5. Etching

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1. Sectioning

Why sectioning? 1. Size limitation of specimen to be examined under optical microscope. 2. To select a small area for microscopic examination from a large sample. Abrasive Cutting is the most common sectioning method. The abrasive cut-off disc is usually made by silicon carbide particles, or diamond particles (called Diamond saws).

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2. Mounting

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2. Mounting
Mounting is required when Sample is small or oddly shaped to be handled. When the sample edge area needs is to be examined. Why mounting ? Small samples are at times difficult to hold safely during grinding and polishing operations, and their shape may not be suitable for observation on a flat surface. They are therefore mounted inside a polymer block or mount. Cold mounting can be done using two component resins (epoxies) as liquid to start with but which set solid shortly after mixing. It requires very simple facilities consisting of a cylindrical ring which serves as a mould and a flat piece which serves as the base of the mould. The sample is placed on the flat piece within the mould and the mixture poured in and allowed to set. Cold mounting takes few minutes to hours to complete Hot-mounting: the sample is surrounded by an organic polymeric powder (Bakelite) which melts under the influence of heat (about 200 0C). Pressure is also applied by a piston, ensuring a high quality mould free of porosity and with intimate contact between the sample and the polymer
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3. Grinding
Grinding removes the damages on the surface produced by sectioning At the end of grinding phase, the only grinding marks present must be from the last grinding step Such marks will be removed by polishing Grinding materials: Abrasive papers (coated with silicon carbide grits) Commonly, a series of abrasive papers are used, from coarse to fine one Grit sequence: 120-, 240-, 320-, 400-, & 600-mesh Grinding is done using rotating discs covered with silicon carbide paper and water There are a number of grades of paper, with 120, 180, 240, 400, 600, grains of silicon carbide per square inch 120 grade represents the coarsest particles and this is the grade to begin the grinding operation. Always light pressure is applied at the centre of the sample

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3. Grinding
Grinding is continued until all the blemishes have been removed, the sample surface is flat, and all the scratches are in a single orientation The sample is washed with water and moved 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 After the final grinding operation on 600 paper, the sample is washed in water followed by alcohol wash and dried before moving to the polishers Artifact structure from improper grinding

Surface deformation from improper grinding should be avoid, otherwise the microstructure may be obscured as shown below

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4. Polishing

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4. Polishing
After being ground to a 600-grit finish, the sample is polished to produce a flat and scratch-free surface with high reflectivity. Coarse polishing: abrasives in the range of 30 ~ 3 m using diamond grits of several micrometers Fine polishing: abrasives in the range of 1 m using diamond grits of 1 m, followed by 0.3 ~ 0.05 m alumina slurries. 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 m Begin with the coarse slurry and continue polishing until the grinding scratches have been removed

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4. Polishing
Polishing sequence

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4. Polishing
Artifacts from improper polishing Polishing should produce a scratch-free surface. Excessive pressure may cause artifact of second phase particles as shown below.

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4. Polishing
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.

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5. Etching
What is Etching ? Etching is controlled corrosion process resulting from electrolytic action between surface areas of different potential. Etching reveals the microstructure of a material by selective dissolution of the material from the surface. The purpose of etching is two-fold. 1. Grinding and polishing operations produce a highly deformed, thin layer on the surface which is removed chemically during etching. 2.To attack 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. Using chemical to dissolve selectively the surface of materials in order to reveal the inhomogeneous nature in microscopic scale.

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5. Etching
Different Kind of Etchant used for Steel:

Etchant
Nital (2 ml HNO3 + 98 ml ethanol) Picral (10 g Picric acid + 100 ml ethanol) Nital (2 ml HNO3 + 98 ml ethanol) Picral (10 g Picric acid + 100 ml ethanol) Vilella (1 g Picric acid + 5 ml HCl + 100 ml ethanol) Vilella (1 g Picric acid + 5 ml HCl + 100 ml ethanol)
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Sample
Steels and cast irons Carbon & low alloy steels Steels and cast irons Carbon & low alloy steels High carbon & high alloy steels High carbon & high alloy steels

Microscopic Examination

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Microscopic Examination
Crystallites (grains) and grain boundaries. Vary considerably in size. Can be quite large Crystallites (grains) can be quite small (mm or less) necessary to observe with a microscope.

Microscopic techniques:
Optical microscopy is used to obtain an enlarged image of a small object. In general, a microscope consists of a light source, a condenser, an objective, and an ocular or eyepiece. The scope of optical microscope is limited by the wavelengths of the light used and by the materials available for manufacturing the lenses.

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Microscopic Examination
Optical Microscope

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Microscopic Examination
Determination of the Grain Size according to ASTM E 112

Standard ASTM Grain Size

N = 2n -1 , n = ASTM grain size number


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INCLUSION
Inclusion distribution form different API 5L X65 steels

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MICROSTRUCTURE

200 X
GRAIN SIZE : 7.70 PEARLITE : 22.58 %
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200 X GRAIN SIZE 8.38 PEARLITE 15.37%

SPECTROMETER
OPTICAL EMISSION SPECTROMETER, SHIMADZU, JAPAN

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