Unit II Basic Materials and Metallography

Unit – II
Basic Materials and Metallography

Syllabus:
Classification of metal observations: their definition, difference & importance.
Microscopy: Various sampling techniques, specimen preparation, specimen mounting (hot & cold
mounting) electrolytic polishing, etching procedure and reagents, electrolytic etching.
Microscopic techniques: optical microscopy, electron microscopy, transmission electron microscopy (TEM),
scanning electron microscopy (SEM), scanning probe microscopy (SPM), AFM etc. (principal & application
only)
Study of Metallurgical microscope .Measurement of grain size by different methods & effect of grain size on
various mechanical properties.
Macroscopy: Sulphur printing, flow line observations.

2.1 Introduction • Ferrous materials are the most important metals in the
• A material is that, out of which anything is made. It relates metallurgical and mechanical industries because of their
itself to matter. extensive use.
• The knowledge of materials and their properties is of great • The commonly used ferrous metals are as follows:
significance for a design engineer. 1. Cast iron
• The machine elements should be made from such a 2. Alloy cast iron
materials which has properties suitable for the operating 3. Steel (Plain carbon steel)
conditions. 4. Alloy steel
• Property of a material is a factor that influences
qualitatively or quantitatively the response of a given Cast Iron
material under the action of forces, temperature, pressure • Cast iron are the alloy of iron and carbon.
etc. • Generally, commercial cast iron are complex in
• Property indicates that, whether a material is suitable or composition and their carbon content is in the range of 2.3
unsuitable for a particular use in industry. to 3.7 % with other elements like sulphur, manganese,
• The material property is independent of the dimension or phosphorus and silicon.
shape of the material. Cast iron are formed by melting a metal and casting with
or without machining to the desired final shape and size,
hence called cast iron.
2.2 Classification of Engineering Materials
The engineering materials are mainly classified as follows.
Characteristics of Cast Iron
• While manufacturing of cast iron, raw materials like pig
iron, scrap limestone, coke etc. are used. All these
elements are relatively cheap, hence the cast iron is the
cheapest amongst all alloys.
• The melting point of cast iron is low i.e. 1140 to 1240°C.
• Due to high fluidity of melt, cast iron has excellent
castability.
• By altering the chemical composition, cast iron can
provide a wide range of metallic properties.

Advantages of Cast Iron

Fig. No. 2.1 Classification of Engineering Materials It is low cost material.
2.2.1 Ferrous Metals • It can provide good damping capacity and high
• The ferrous metals are those which have the iron as their compressive strength.
main element or constituent. • Cast iron has high resistance to wear and abrasion.
• It has high hardness.
 Unit II Micro and Macroscopic Study of Metals

• Corrosion resistance of cast iron is fairly good.

• It has excellent machinability. Properties of Plain Carbon Steel
They are ductile in nature.
Limitations of Cast Iron • They have high fatigue and impact strength.
It is brittle in nature. • Their mechanical properties like toughness, stiffness,
• Its mechanical properties like toughness, stiffness, resilience, etc. are high.
resilience etc. are poor.
• Due to brittleness, it is poor against fatigue and impact Advantages of Plain Carbon Steel
loading. They have high tensile
strength.
Applications of Cast Iron • They have high resilience and toughness.
• Machine beds, columns, hammers, road-rollers. • They can sustain fatigue and impact load.
• Pipe fittings, valves, farm equipment's, automotive parts.
• Camshafts, crank shafts, gears, ordnance parts. Limitations of Plain Carbon Steel
• Motor covers, pump bodies, furnace parts. The vibration damping property of steel is poor.
• Engine frames, piston and cylinder, cylinder blocks and • They cannot be cast into complicated shapes.
bearing blocks etc. • They have low wear resistance.
• Its cost is more than cast iron.
Types of Cast Iron
Cast Iron are classified as follows: Applications of Plain Carbon Steel
1. White cast iron • Stampings, fan blades, rivets, nuts, bolts, wires, structural
2. Gray cast iron steel, grill, shafts.
3. Malleable cast iron • Gears, valves, crank shaft, camshaft, axles, screws,
4. Nodular cast iron springs.
• Cutting tools, milling cutters, blades, drill bits, musical
Alloy Cast Iron instruments, agricultural applications, etc.
• Generally, cast iron has low impact resistance, corrosion
resistance and temperature resistance. Hence, to increase Alloy Steel
these properties certain alloying elements are added in • To obtain the specific properties various alloying elements
suitable amount. are added in steel.
• Usually, nickel, chromium, copper, silicon, vanadium, • The specific properties define the applications of steel.
molybdenum etc. are used for this purpose. • The various alloying elements are as follows:
Carbon, Sulphur, Phosphorus, Silicon, Manganese, Nickel,
Properties of alloy cast iron Chromium, Titanium, Tungsten, Molybdenum, Vanadium,
It has high strength. Cobalt etc.
• It has high oxidation resistance. Properties of Alloy Steel
• It has high wear resistance and corrosion resistance. • They are ductile in nature.
• They have high corrosion resistance.
Applications of alloy cast iron • They have high strength. They are soft and having
• Gear, automobile parts like pistons, piston rings, camshaft, high toughness.
crank shaft, cylinders.
• Brake drum, pulleys, grinding machinery parts, etc. Advantages of Alloy Steel
• They have high tensile and fatigue strength.
Plain Carbon Steel • They have high wear resistance, corrosion resistance and
• Steel is an alloy of iron and carbon with carbon content up creep resistance.
to 1.6 % approximately. • They have high toughness and resilience.
• Carbon content increases the strength and hardness of
steel. Limitations of Alloy Steel
• Plain carbon steel or carbon steel is defined as a steel • Alloy steel cannot be cast into complicated shapes.
which has its properties mainly due to its carbon content • Their vibration damping properties is poor.
and does not contain more than 0.5% of silicon and 1.5% • They are costlier than steel and cast iron.
of manganese.
 Unit II Micro and Macroscopic Study of Metals

Applications of Alloy Steel Advantages of Brasses

• Aircraft engine parts, heat exchangers, wrist watches, It has high corrosion resistance.
sanitary fittings. • It has high ductility and malleability.
• Combustion chamber, furnace parts, gas burners, screws. • Due to addition of zinc, it has high strength.
• Valves, pumps, surgical instruments, razor blades, turbine • It has high machinability.
blades, missiles, structural components, etc.
Limitations of Brasses
2.2.2 Non-Ferrous Metals • It has low thermal and electrical conductivity.
• Non-ferrous metals are those which contain a metal other • Its cost is also high.
than iron as their main element or constituent.
• Non-ferrous metals find wide applications in various Applications of Brasses
industrial sectors because of following advantages: • Coins, needles, jewellery, condenser tubes.
1. Low density, hence light in weight. • Cartridge cases, headlight reflectors, springs.
2. High electrical conductivity. • Shafts, nuts, bolts, welding rods, machine parts etc.
3. Easy to fabricate.
4. High corrosion resistance. Bronzes
• The commonly used non-ferrous alloys are as follows: 1. • Bronzes are alloys of copper and major alloying elements
Copper and its alloys other than zinc or nickel.
a) Brasses b) Bronzes 2. • But, generally bronzes are alloy of copper and tin.
Aluminium and its alloys • Sometimes, it also alloyed with aluminium, beryllium,
silicon etc.
Copper and its Alloys
• Copper is one of the most widely used non-ferrous metal. Advantages of Bronzes
• Various alloying elements are added to copper to improve • It has high corrosion resistance.
and add some properties. • It is comparatively hard than brass.
• Major alloying elements are zinc, silicon, aluminium, lead, • It can be rolled into sheets, rods or wires.
manganese, nickel, phosphorous, tin, magnesium, etc. • It has high tensile strength.
• It has high ductility and malleability.
Properties of Copper
• It has high ductility and malleability. Limitations of Bronzes
• It has high electrical and thermal conductivity. • The cost of bronzes is higher than the brasses.
• It is non-magnetic in nature. • The strength of bronzes is lower than the ferrous metals.
• It can be easily alloyed with other metals.
• Its corrosion resistance is also high. Applications of Bronzes
• Springs, gears, bearings, electrical appliances.
Applications of Copper • Bolts, rivets, pressure vessels, bells, marine containers.
• Electrical parts Valve bodies, ordnance parts, gun barrels, pipe fittings etc.
• Heat exchangers
• Household utensils etc. Aluminium and Its Alloys
• Aluminium is another widely used non-ferrous metal.
Types of Copper Alloys • Aluminium can be easily alloyed with elements like
Copper alloys are basically divided into two major groups: silicon, copper, nickel, zinc, manganese, titanium,
1. Brasses (Alloy of copper and zinc). magnesium etc.
2. Bronzes (Alloy of copper and tin).
Advantages of Aluminium Alloys
Brasses • It has high thermal and electrical conductivity.
• Brasses are alloys of copper and zinc with small amount of • It has high corrosion resistance.
other alloying elements. • It has high toughness.
• According to the percentage of copper and zinc, there are
• They are malleable and ductile.
various types of brasses. For example α-brasses.
• It can be easily cast and rolled.
• The properties of brasses can be changed by adding small
amount of other alloying elements.
 Unit II Micro and Macroscopic Study of Metals

Applications of Aluminium Alloys • It has short life.

• Aluminium alloys are widely used in the aircraft industry. • It has poor dimensional stability.
Motor housings, pump castings, pistons, cylinder
heads. Types of polymers/plastics
• In food industry, food preparation equipment's, Plastic or polymers are classified into two major categories:
refrigeration, storage containers, bakery equipment's etc. 1. Thermoplastic or Thermoplasts (Soften when heated
and harden when cooled).
2.2.3 Non-Metals 2. Thermosetting or Thermosets (Soften when heated
• Now-a-days use of non-metals is increasing in the and permanently harden when cooled).
industries because of following properties:
1. They are having low density. Thermoplastics (Thermoplasts)
2. They are light in weight. • Thermoplastic polymers soften when heated and harden
3. Use of non-metals provides flexibility in the design. when cooled.
4. They have high resistance to heat and electricity. • These types of polymers are soft and ductile.
5. They have low cost. • They have low melting temperatures and can be repeatedly
• The commonly used non-metals are as follows: moulded and remoulded to the desired shapes.
1. Plastics • These polymers are usually fabricated by the simultaneous
2. Ceramics applications of heat and pressure.
3. Composites
Applications
Plastics • These types of plastics are used in electrical insulations,
• A large group of engineering materials which have toys, machine guards, musical instruments, fuel container
increasing importance in industrial applications are coatings, hoses, photographic films, bottles, gaskets,
composed of natural synthetic organic polymers (Plastics). packing’s, refrigerator parts, floor tiles, plastic lenses etc.
• Now-a-days in some of the applications, metal and wood • Some of the commonly used thermoplastics are:
parts are replaced by plastics, which have satisfactory Polyamide, Poly-Tetra-Fluaro-Ethylene (PTFE),
properties and may be produced at lower cost. PolyVinyl-Chloride (PVC), Poly-Propylene (PP),
• Plastics are moulded into any required shape by the PolyEthylene (PE) etc.
applications of pressure and heat, for example toys, chairs,
refrigerator equipment's and radiator fans etc. Thermosetting (Thermosets) polymers
• The plastics can be cast, rolled, laminated and machined • Thermosetting polymers become soft during first heating
easily. and become permanently hard when cooled. Hence, these
• The word ‘mer’ means a unit, monomer stands for a single type of polymers cannot be remoulded or reshaped by
unit and polymer means many units joined together by a subsequent heating’s.
chemical reactions. • These type of plastics are generally more stronger, harder,
brittle and resistant to heat and solvents than the
Characteristics of polymers/plastics thermoplast.
Low density and weight. • It they are heated to high temperature, decompositions and
degradation of the polymer takes place.
• High corrosion resistance.
• Low thermal, mechanical and electrical properties.
Applications
• Low coefficient of friction.
These type of plastics are used in telephone receivers,
• Excellent surface finish can be obtained.
electric plugs, radio and T.V. cabinets, camera parts,
• It can be produced in different colours. automobile parts, switch panels etc.
• It can be produced with close dimensional tolerances.
• Some of the commonly used thermosets are: Phenolic,
• It has good mouldability. Epoxies, Aminos (Urea formaldehyde and melamine
• It is more economical than the metals. formaldehyde), unsaturated polyesters etc.

Limitations of polymers/plastics
• It has low strength and rigidity.
• It has poor tensile strength.
• It has poor temperature resistance.
 Unit II Micro and Macroscopic Study of Metals

Fiber Reinforced Composites

Ceramics • The hard phase consists of fibres of high strength material.
• Ceramics is a compound formed by combination of These fibres are dispersed in the soft and ductile matrix.
inorganic and non-metallic materials. • The combined material has better stiffness, strength and
• Ceramics are hard and brittle materials used for high toughness.
temperature applications. • The function of fibres is to withstand the load, while matrix
• They are mainly oxides, carbides, sulphides and nitrides of ensures uniform distribution of applied load.
metals.
Applications
Properties of Ceramics • These type of composites are used in piston, connecting
• Ceramics have high hardness and stiffness. rods, aerospace applications, aircraft wing applications,
• It consists of high strength at high temperatures. propeller for ships, cutting tool inserts for machining hard
• They have high resistance to abrasion and wear. metals, springs containers, pressure vessels, gaskets etc.
• Chemical stability of ceramics is good.
Particle Reinforced Composites
Advantages of Ceramics • In this type of composites, the strengthening is produced
• Ceramics can have excellent compressive strength. by particles of hard material.
• They have low thermal conductivity. • The function of particles is to impart strength and stiffness
• They have low coefficient of thermal expansion. to the composite mix.
• Also, they possess good electrical insulation properties. • Matrix ensures uniform distribution of applied load on the
composite. It also provides protective covering to the
Limitations of Ceramics particles.
• Due to their hardness machinability of ceramics is very
low. Applications
• They are brittle in nature. • These type of composites are used in cutting tool materials,
crucibles, jet nozzles, aircraft blades, coatings, bearing
Applications of Ceramics bushing, dies, cylinder liners, brake discs etc.
• Spark-plug insulators, vacuum tubes, metal cutting tool
tips, grinding wheels, nuclear equipment’s. Structural Composites
• Rotor blades in turbines, die materials, engine components, • Structural composites are made up of two or more
artificial hip joints, refractory tubes and containers. homogeneous materials.
• Nozzles, bearings, pump parts, electronic parts, • The properties of these composites depend on the
components of paper industry etc. constituent materials and their geometrical design.
• Structural composites can be of laminate type or sandwich
Composites panel type.
• Composite material is defined as a material formed by the • In case of laminated composites, two or more layers or
combination of two or more chemically dissimilar sheets arranged in a stacking order. These sheets are
materials with different boundaries between them. cemented by using a bonding agent.
• Composite material exhibit properties that are vastly • The load on the composites is shared by all the layers. It is
different from those of the individual constituents and used as a skin material for aircraft.
better suited for a particular applications. • In case of sandwich panel composites, two strong outer
• Many composite materials are composed of just two sheets are separated by a layer of less-dense material.
phases; one is called as matrix (soft phase) which is • It is used in roofs, floors and walls of buildings, aircraft
continuous and surrounds the other phase i.e. called as wings etc.
dispersed phase (hard phase).
2.3 Metallography
Types of Composite Materials Metallography consists of microscopic study of the
The composite materials are classified as follows: structural characteristics of a metal or an alloy.
1. Fiber reinforced composites It is the general study of metals and their behaviour with
2. Particle reinforced composites particular reference to their microstructure and
3. Structural composites macrostructure.
 Unit II Micro and Macroscopic Study of Metals

• Microstructure or microscopic examination involves the 3. Mechanical heterogeneity i.e. due to cold working or
study of prepared metal surfaces by using a microscope. heterogeneity occurs in metals or alloy due cold rolling
• When a higher magnification is used, it gives large number or forging etc.
of structural details of the metals or alloys under
examination. 2.5 Specimen Preparation
• Macrostructure or macroscopic examination involves the • Specimen preparation is necessary to study it’s
study of metals either by the unaided eyes or by using a low microstructure as metallurgical microscope makes use of
power magnifying glass. the principle of reflection of light to obtain image of the
• When all features are found by metallographic metal structure.
examination, it is then possible to predict the behaviour of • A satisfactory image of the microstructure can be obtained
the metal for a particular service condition with reasonable only when the specimen has been carefully prepared.
accuracy. • Even the most expensive microscope will not reveal the
• Microstructure and macrostructure of a metal or an alloy metal structure, if the specimen has been poorly prepared.
are closely interrelated with each other and a knowledge of • The procedure to be followed in the preparation of a
both is necessary for full understanding of any metal. specimen is simple but the technique gets develop only
after practice.
2.4 Classification of Metal Observations • The final objective is to produce a flat, scratch free and a
• Metallography is a study of the structural characteristics or mirror like finish surface.
constitution of a metal or alloy, in relation to its physical • The procedure for preparing the specimen for both
and mechanical properties: microscopy and macroscopy examination is the same
• There are two examination methods in metallography: except that in the case of microscopy the final surface finish
1. Microscopy is more important.
2. Macroscopy • The steps required to prepare a metallographic specimen
are as under:
2.4.1 Microscopy 1. Selection of specimen
• In microscopy, the examination is done with the prepared 2. Cutting of specimen
metal specimens, employing magnifications with the 3. Rough grinding
optical metallurgical microscope, from 100X to high as 4. Mounting of specimen
2000X of magnification.
5. Fine grinding
• Microstructural examination can provide quantitative
information about the following parameters: 6. Polishing
1. The grain size of specimen 7. Etching
2. The amount of interfacial area per unit volume.
3. The dimensions of constituent phases. 2.5.1 Selection of Specimen
4. The amount and distribution of phases. • Specimen should be selected from, that area of a metal,
which can be taken as representative of the metal that is
2.4.2 Macroscopy being studied.
• In case of macroscopic examination the nature of in • In case of study of failures, specimen should be taken as
homogeneities and flow lines in a metal by unaided dye or close as possible to the fracture or to the initiation of the
with the help of low power magnifying glass. failure.
• The general distribution and variation in size of • Generally in many cases, specimens are required to be
nonmetallic inclusions, the uniformity of structure, the taken from a sound area for a comparison of structure and
location and extent of segregation, flow lines etc. can be properties.
examine by macroscopy and these cannot be examined by • After deciding the location of the specimen, the type of
microscopy. section to be examined must be decided. The location of
1. Crystalline heterogeneity i.e. manner of solidification surface examined should always be given in reporting
and the crystalline growth of the metal or alloy. results.
2. Chemical heterogeneity i.e. impurities in a metal or • Size of specimen be proper for handling during all sample
alloy. preparation techniques.
 Unit II Micro and Macroscopic Study of Metals

• If the specimen sample is too small, then it should be • Due to rough grinding surface damages, created by cutting
mounted on the mounting press along with thermosetting discs, are reduced by grinding. The belt grinding paper is
resign or cold mounting process. made up of silicon carbide abrasive.

2.5.2 Cutting of Specimen 2.5.4 Specimen Mounting

After selecting a particular area, the specimen may be • It is carried out for convenience in handling it during the
removed from the metallic piece by sawing or cutting using subsequent steps of metallographic preparation and
abrasive wheel which is carried out on abrasive wheel examination. For this the specimen is mounted.
cutting machine as shown in fig. no. 2.2. • Compression mounting involves mouldings around the
specimen by a material like Bakelite, acrylic resins, by
application of heat and pressure. This is known as hot
mounting process.
• Epoxy or polyester resins are used for cold moulding, and
this is known as cold mounting process.

Fig. No. 2.2 Abrasive cut-off wheel

• The specimen shall be kept cool during the cutting
operation. While cutting, care must be taken to minimize,
altering the microstructure of the metal.

2.5.3 Rough Grinding

• After cutting, a soft specimen may be made flat by slowly
moving it up and back across the surface of a smooth file,
and hard specimens may be rough ground on a belt grinder.

Fig. No. 2.4 Mounting Press

• Also due to mounting of metallurgical specimen, serves for
protection of the specimen edges and improvement of its
irregular shape, which become more convenient during
grinding and polishing.

Hot and Cold Mounting

• Specimen mounting is necessary because very thin,
irregular shape specimens are difficult to handle during
sample preparation techniques, due to which those
specimen are mounted by two methods.
1. Hot mounting
2. Cold mounting
Fig. No. 2.3 Belt Grinder
• Rough grinding is continued until all scratches due to the
hacksaw or cut-off wheel are no longer visible and the
surface is flat.
 Unit II Micro and Macroscopic Study of Metals

• The fine scratches caused by final grinding operation are

Hot Mounting removed by polishing. Polishing is carried out on single
• In this process a small hydraulically operated press is used disc or double disc polisher.
and which is consists of a small furnace/ heater to heat the
resin material.
• A temperature up to 200°C and a pressure upto 50 kN are
applied during the embedding of the specimen.
• A thermoplastic resin material is used. A small metallic
mould is used to embedding the specimen, in the resin
material.

Cold Mounting
• As this process is carried out room temperature it is known
as cold mounting. A resign material in the powder form is Fig. No. 2.6 Double disc polishing machine
mixed with a hardener to provide the mounting compound. • The time consumed and the success of polishing depends
This slurry or a mixture is then poured around the largely upon the care that was taken during fine grinding.
specimen, surrounding to metallic mould. Cold mounting • The final approximately flat scratch free surface is obtained
is preferred for specimens that are sensitive to head or by use of a wet rotating wheel covered with special cloth,
pressure, as in case of hot mounting used. charged with abrasive particles.
During polishing, the specimen is rotated in a direction,
2.5.5 Fine Grinding counter to the rotation of the polishing wheel.
• After rough grinding the specimen is finely ground using • In addition the specimen is continuously moved back and
fine abrasive paper (grit sizes from 180 mesh to 600 mesh). forth between the centre and edge of the wheel, thereby
• This abrasive grit size is as per ANSI standards (American ensuring even distribution of the abrasive and uniform wear
National Standards Institute) system units. of the polishing cloth.
• Fine grinding is generally carried out on many papers, of • A wide range of abrasives is available. Generally alpha
grades from 01 to 04 i.e. 01 is coarse grained and its grade of aluminium oxide is used for rough polishing on
fineness goes on increasing towards 04. one polishing wheel while gamma grade of aluminium
oxide is used for fine polishing on other polishing wheel.
• After polishing i.e. after obtaining a mirror finish image on
the specimen surface, the specimen is washed in warm
running water, rinsed with methanol or any other alcohol
that does not leave a residue, and dried in a stream of warm
air.

Electrolytic Polishing
• During metallographic sample preparation techniques,
even most care is taken during mechanical polishing, some
Fig. No. 2.5 Emerry Papers disturbed metal however will remain after preparation of a
• This fine grinding is carried out on a series of stages with metallographic specimen.
increasing the fineness of the paper i.e. from 01 to 04.
• Each grinding operation on a paper, will remove the marks,
produced in the previous operation.
• After each grinding stage the specimen should be
thoroughly washed in order to prevent carry over the
coarser grit to the next grinding paper.
• The grinding direction during each stage should be change
by 90° relative to the direction of the previous stage.
• This makes easier indication of completion of the grinding
stage (removal of the scratches from the previous stage).

2.5.6 Polishing
 Unit II Micro and Macroscopic Study of Metals

• After etching the specimen is again washed thoroughly and

dried. Now the specimen can be studied under a
microscope.
• The selection of the appropriate etching reagent is
determined by the metal or alloy and the specific structure
desired for viewing.
• The common etching reagents used for various metals and
alloys are as under.
Table No. 2.1 Various etching reagents with their
applications

Etching Composition Use

Reagent
White 4 nitric acid “1
Carbon steels
Nitric Acid to 5 ml ethyl or methyl
and cast iron
Fig. No. 2.7 Electrolytic Polishing alcohol”
• If the specimen is to be examined in the as polished Picric acid “4 g ethyl or
Picric Acid Carbon steels
condition, however, or if no surface disturbance can be methyl alcohol”
accepted or tolerated, either electrolytic polishing or Ferric chloride 5 g Structure of
chemical polishing is preferred. Ferric
Hydrochloric acid 50 austenitic nickel
• As shown in fig. no. 2.7, an electrolytic reaction cell chloride
ml water 100 ml stainless steels
containing a liquid electrolyte with two electrodes, an
anode and cathode. Ammonium Ammonium hydroxide
hydroxide & 5 parts water 5 parts Copper and its
• The sample to be polished/etched forms an anode. The
hydrogen hydrogen peroxide 2 to alloys
electrodes are connected to an external power supply and
voltage applied to cause reaction within the cell. peroxide 5 parts
• In electrolytic polishing the specimen is the anode in an Copper, brass,
Ammonium per
electrolytic cell. Direct current from an external cell is Ammonium bronze,
sulphate 10 g water 90
applied to the electrolytic cell under specific conditions, per sulphate aluminium
and anodic dissolution results in a levelling and brightening ml
silver, nickel
of the specimen surface. Chromic oxide 200 g
Electrolytic polishing does not disturb any metal on the Palmerton Zinc and its
sodium sulphate 15 g
specimen surface and therefore ideally suitable for the reagent alloys
water 1000 ml
metallographic preparation of soft metals, most single
phase alloys, alloys that work harden readily. Ammonium Molybdic acid 100 g Lead and its
• The disadvantages of electrolytic polishing includes, molybdate ammonium hydroxide alloys
chemical attack in multiphase alloys due difference in Hydrofluoric Hydrofluoric acid 0.5 Aluminium and
electrical potential between phases. Acid ml its alloy

2.5.7 Etching
• Etching is defined as, a intentionally made chemical attack
on the prepared metallic specimen surface, to reveal
microstructure or micro constituents.
• The purpose of etching is to make visible structural
characteristics of the metal or alloy. This is achieved by a
use of an appropriate etching reagent which carry out
chemical action on a polished surface.
• Etching is done by immersing the polished surface in the
reagent or by rubbing the polished surface gently with
cotton swab, wetted with the etching reagent.
 Unit II Micro and Macroscopic Study of Metals

• As shown in fig. no. 2.9 (a) represent metallic specimen

2.6 Determination of Microstructure surface duly polished and in unattached condition.
All the light rays following on the specimen surface, are all
As shown in the ray diagram of metallurgical microscope
reflected back and passing through objective lenses,
(Refer Fig. No. 2.8).
therefore the complete surface will look brighter under
microscope.
• With fig. no. 2.9 (b) shows and microstructure after etching
which reveals grain boundaries, because the light rays
following on grain boundary are get scattered and due to
which they cannot pass through objective lenses.
• Because of which grain boundary will look dark under
microscope while the grain will look bright.
• With reference to fig. no. 2.9 (c) which shows the
microstructure of a multi-phase metal or alloy. It reveals
grain shading and grain boundaries as a result of etching.
• In this example the amount of reflected light captured by
the objective lens of the microscope will vary from one
grain to another.
• This will lead to some grain appearing to be light in colour
and others appearing dark, even though all the grains may
Fig. No. 2.8 Determination of Microstructure
be identical in composition and type.
• The prepared specimen is placed perpendicular to the
optical axis of the microscope and is illuminated through
the objective lens by light from the source. 2.7 Microscopic Techniques
• The light rays is then reflected from the surface of the The microscopic techniques are base classified as follows:
specimen, which are then magnified in passing through the
objective lens and will continue upward through the plane
glass reflector and gets magnified again by the eye piece.
• The direction of light reflected from specimen depends on
specimen surface condition as shown in fig. no. 2.8.
• The light is reflected from the surface of the specimen in to
objective lens from features approximately normal to the
optical axis and away from objective lens from features
inclined to the optical axis as shown in fig. no. 2.9.

Fig. No. 2.10 Classification of Microscopic Techniques

Fig. No. 2.9 Observation of metallography specimen
• The final image of specimen which is formed by the
eyepiece, is therefore bright for all features normal to the
optical axis (grain) and dark for inclined features (grain
boundary).
• In this way the various grain size determination, and the
various microstructural features, inclusions, precipitated
particles etc. can be revealed.
 Unit II Micro and Macroscopic Study of Metals

2.8 Optical Metallurgical Microscope • Objective - The body tube carries revolving nose piece
carrying the three objectives. This enables quick change of
the objective which helps for a quick resolving the structure
of metal, the magnification of lenses is enlarged on focal
length of the lens used. The important properties of an
objective are- 1 Magnifying Power 2 Resolving Power.
• It is the property by which an objective shows distinctly
represented two small adjacent bonds in the structure of the
object. This is usually expressed as number of lines per mm
that can be separated which depends on the numerical
operator, the wavelength of the light used. Resolution is
particularly important during the microscopy of the micro
constituents of metals consisting of fine lamination with
core resolution which appears as one uniform area, where
as an objective with higher numerical appearance reveals
deeper nature of the structure.
• Eyepiece - It is named, as it is near to the eye. It is made up
of various Powers such as X5, XI0, X 15 etc.
• Uses - The metallurgical microscope is useful in quality
control department in Industries to observe & study 1)
Fig. No. 2.11 Optical Metallurgical Microscope Differential phases 2) Porosity or defects.
Microscope is a device used for obtaining more resolution All these have a great effect on mechanical properties of
and magnification. Finer details can be easily and clearly material List of Modern Microscopes.
examined by using this microscope. 1 Watson Royal Microscope.
2 Van Lanes Hock
Microscope. 3 Glass led
Microscope.
4 Baker series Microscope
5 Leitr Microscope
• Opaque metals cannot be viewed by the transmitted light,
hence they are viewed by the reflected light.
Working
• A horizontal beam of light from a suitable light source (like
electric bulb) falls on a silvered portion of a semi-silvered
glass plate which is kept at an angle of 45° with vertical
axis in the movable tube.
• The light get reflected vertically downwards travel through
the objective and fall on the surface of specimen.
Fig. No. 2.12 Reflected Light Microscope Anatomy • The light rays that are reflected by flat and polished
• It consists of a stand which is attached to a movable tube specimen surface travel through the objective and come to
which contains the optical parts and device for illuminating the eyepiece.
the specimen. Refer fig. no. 2.12. • The image can be observed through the eyepiece, or these
• Constructional Details:- The table type microscopes are rays can be focused on the screen or a photographic plate
consist of can be kept to record the image and view it.
• Stage: - A flat movable table supporting specimen. This • In some of the microscope, instead of semi-silvered glass
can be moved up or down by knobs. plate prism reflectors are used.
• Tubes: - The vertically movable tube containing eyepiece,
objective and plane reflector. The tube length varies from 2.9 Electron Microscopy
160 mm to 250 mm. • Electron microscopes are quite different from optical
• Rough & fine focus Adjustments - The limbs of microscopes.
microscope carry the coarse & fine adjustments to facilitate • In these microscopes, a high velocity electron beam is used
the instead of ordinary light.
 Unit II Micro and Macroscopic Study of Metals

• The resolving power of electron microscope is very high as 2.10Transmission Electron Microscopy (TEM)
the wavelength of electron beam is small i.e. 0.05 to 0.07
A°.
• The magnification obtained is very high in the range of 1
to 5 lakhs.

Fig. No. 2.13 Electron Microscope

The vertical resolution of electron microscope is about 2

microns which is much higher than that of optical Fig. No. 2.14 Transmission Electron Microscopy
microscopes. • In the transmission electron microscopes (TEM), which
All the electron microscopes are built on the principle of were developed in the early stages, the samples used are
transmission and hence it is required to have a very thin made very thin, so that the beam penetrates through the
sample to study the details clearly with TEM. sample and the transmitted beam is used for forming the
• The electron beam reflects at an angle of incidence of about image.
1° and hence examination of bulky specimens is possible • The samples may be replicas of the material surface or
by using this reflected electron beam. original material in the form of thin films made by
• The basic arrangement of electron microscope is shown in electrochemical or electrolytic polishing methods.
fig. no. 2.13. • The electron source (electron gun) can be electrically
heated tungsten filament (or a higher quality source for
probe or high resolution work).
• The electron beam is accelerated by the applied voltage and
collimated by condenser lens, so that a parallel beam of
about 25 µm or smaller is incident on the thin specimen.
• The objective lens collects the electrons from the specimen
to form first image with a magnification of say X 40.
• Further, additional magnification lenses including final
projection lens create the final image on the viewing screen.
• This method is useful in identifying defects, their
crystallographic planes and other parameters.
 Unit II Micro and Macroscopic Study of Metals

• This microscope provides a probe-forming system, with

Advantages each lens condensing and demagnifying the electron source
• It has a good magnification of about 5000000 X. to a focused spot on the sample surface.
• It is possible to investigate the fault into a greater depth of • Commonly the probe is 10-40 nm in size. Smaller probes,
field. around 3 nm or smaller are achieved using higher intensity
• TEM has better resolution of 0.2 nm than SEM which has probes of coherent, field emission gun (FEG) electron
a resolution of only 2 nm. sources.

Disadvantages Advantages
• The images obtained are in black and white form. • SEM is easy to use.
• The specimen required in TEM should be very thin. • The sample/specimen required can be any thickness.
• It is expensive and time consuming process. • The sample can be viewed as a 3D image on viewing
screen.
Applications
• Direct observation of dislocations. Disadvantages
• Observation of stacking faults. • The resolution is not good as that of TEM.
• Formation of sub grains without recrystallization in • The specimen used must be conductive.
warm/hot deformation. • The specimen can be viewed as a 3D image on viewing
• Precipitate behaviour in high temperature alloys. screen.
• The fine phases causing temper brittleness in alloy steels,
etc. Applications
• SEM’s have a variety of applications in a number of
2.11Scanning Electron Microscopy (SEM) scientific and industry related fields, especially where
characterizations of solid materials is beneficial.
• A scanning electron microscope is used to detect and
analyse surface fractures, provide information in
microstructures, examine surface contaminations and
identify the crystalline structure.
• SEM have industrial and technological applications such as
semiconductor inspection, production line of extremely
small products and assembly of microchips for computers.

2.12Scanning Probe Microscope (SPM)

• Scanning probe microscopy (SPM) is a branch of
microscopy that forms images of surfaces using a physical
probe that scans the specimen.
• An image of the surface is obtained by mechanically
moving the probe in a raster scan of the specimen, line by
line, and recording the probe-surface interaction as a
function of position.
• SPM techniques have been applied over a wide range of
materials.
Fig. No. 2.15 Scanning Electron Microscopy
• Types of scanning probe microscopy are:
1. AFM (Atomic Force Microscopy)
• For scanning electron microscopy, bulk specimens can be
2. EFM (Electrostatic Force Microscopy)
suitable as used in optical microscopy, but they have poor
3. MFM (Magnetic Force Microscopy)
resolution and high image distortion.
4. STM (Scanning Tunnelling Microscopy), etc.
In a scanning electron microscope electron microscope, an
electron beam is focused to a spot of about 20-100 nm
diameter and made to scan the sample surface in a raster.
The sample will be a thick sample of conducting material.
• The electron gun may operate at 30-60 kV.
 Unit II Micro and Macroscopic Study of Metals

2.12.1 Atomic Force Microscopy (AFM) If we use AFM tip as an end-effector, an atomic force
microscope can be modified into a nano robot that can
manipulate objects in nanoscale.
Atomic force microscope is now actively used in material
sciences and biological fields.

Comparison between TEM and SEM Table No. 2.2

Comparison of TEM and SEM
S. N TEM SEM
TEM has higher SEM has lower
1 resolution of about 1 nm resolution of about 2
or less. nm only.
Specimen preparation is Specimen preparation
2
time consuming. is simple and fast.
Fig. No. 2.16 Atomic Force Microscope
The specimen required The specimen required
• In atomic force microscope (AFM), the interaction force 3
between the probe and surface structural features is should be thin. can be of any thickness.
measured to reveal the surface topography in a direct
Transmission electron Scanning
fashion.
• The probe is at the tip of a cantilever placed parallel to the microscopes are electron
4
surface. expensive. microscope is cheaper
• In common instruments, the movements of the cantilever comparatively.
are seen in the form of deflection of a laser beam from a The images obtained are The sample can be
mirror at the back of the cantilever. The measured signal is 5
in black and white form. viewed as a 3D image.
then used to control the system. TEM shows multiple SEM shows only the
• The microscope can operate in a constant force or constant
characteristics of object morphology of
height mode. 6
such as crystallization, specimens.
• In general, scanning force microscopes measure forces in
the range of 10-9 to 10-6 N and the mechanical properties of morphology, stress, etc.
the cantilever such as the spring constant, the resonant They are harmful to SEM are safe to use.
7
frequency and stiffness of the beam are important. human health.
• The cantilever must have a very small mass, so
microfabrication techniques are used. Comparison between Electron Microscope and Optical
Microscope
Advantages Table No. 2.3 Comparison of Electron Microscope and
• AFM provides three dimensional surface profile. Optical Microscope
• Samples viewed by AFM do not require and special S. N. Electron Microscope Optical Microscope
treatments that would irreversibly change or damage the In electron microscope, In optical microscopy,
sample.
1 high velocity electron ordinary light is used.
• AFM technique can be used both in air and liquid.
beam I used.
Disadvantages The resolving power is The resolving power is
2
• The AFM can only image a maximum height of the order very high. low comparatively.
10-20 micrometres and maximum scanning area of about The depth of focus is of The depth of focus is of
150 x 150 micrometres. 3
the order 2 µm. the order 0.06 µm.
• The scanning speed of AFM is slow. It cannot scan images Magnetic or Optical lens are used in
as fast as a SEM. electrostatic lens are optical microscope.
4 used in
Applications
• Atomic force microscopy is a powerful and widely used electron
imaging technique that can visualize single molecules both microscope.
in air and liquid (solution).

ENGINEERING METALLURGY (202049) 40

 Unit II Micro and Macroscopic Study of Metals

The visual image is The image is observed 2.14.1 Comparison Method

obtained on a viewing through a eyepiece. • Comparison method is mainly used for equiaxed grains and
5 this method is device by ‘ASTM’.
screen / fluorescent
screen. • ASTM has prepared number of standard comparison
charts, all having different average grain sizes.
The wavelength of The wavelength of
• Each average grain size is characterized by ASTM grain
6 electron microscope is optical microscope is size number.
about 1 nm. about 400-700 nm. N = 2n-1
Where, N= Number of grains per square inch at 100X
magnification n= ASTM grain
2.13 Grain Size size number.
• It is important to study the grain size of polycrystalline
metals. Following Table No. 2.5 shows the ASTM grain size
• The grain size is specified in terms of average grain number along with corresponding average number of
volume, diameter or area. grains.
• The grain size has an influence on the mechanical Table No. 2.5 ASTM Grain Size Numbers
properties of the metal viz. ductility, strength, toughness Average number Actual average
ASTM
etc. of grains per diameter of
S. grain
• Usually, fine grained structures have better mechanical square inch of equivalent spherical
size
properties as compared to coarse grained structures. N. 100X
number grain in microns (1
• Hence, many time, special treatments such as heat magnification
(n) micron= 10-3 mm)
treatment are carried out to refine the grain structure. (N)
• The effect of grain size on some of the mechanical 1 1 1 287
properties is mentioned below: 2 2 2 203
Table No. 2.4 Effect of grain size on mechanical properties
Coarse Fine 3 3 4 144
S.
Property Grained Grained 4 4 8 101
N. Structure Structure
5 5 16 71.8
1 Yield Strength Less More
6 6 32 50.7
2 Tensile Strength Less More
3 Toughness Less More 7 7 64 35.9
4 Resilience Less More 8 8 128 25.4
5 Hardness Less More 9 9 256 18
6 Fatigue Resistance Less More 10 10 512 12.7
7 Creep Resistance More Less
• Larger grain size number represents the smaller grains in
8 Corrosion Resistance More Less size.
9 Ductility Less More • The specimen in this method must be properly prepared to
10 Hardenability More Less disclose the grain structure.
• This specimen is then
2.14 Grain Size Determination photographed at 100 x magnification.
• Determination of grain size essentially depends on the This is known as micrograph.
properties of polycrystalline materials. • The grain structure micrograph is then compared with the
• There are many techniques in which grain size is specified sizes given in the above charts at 100 x magnification.
in terms of average grain volume, diameter or area. • The matching number after matching the structure with
• Following are the techniques commonly used for the grain standard charts is found out.
size determination.
1. Comparison Method
2. Heyn’s Intercept Method
3. Jefferies Planimetric Method
 Unit II Micro and Macroscopic Study of Metals

500 50
2.14.2 Heyn’s Intercept Method 750 112.5
• Intercept method is mainly used for non-equiaxed grains or
elongated grains. 1000 200
• In this method, straight lines of same length are drawn on 1500 450
the photomicrograph of the specimen that shows the grain 2000 800
structure.
• The magnification employed should be such that area
covered is atleast 0.5 mm2 on the actual sample. 2.15 Macroscopy
• Hence, grains intersected by each line are counted. • In case of macroscopic examination the nature of in
• The average grain size at 100 x magnification can be found homogeneities and flow lines in a metal by unaided dye or
out by, with the help of low power magnifying glass.
• The general distribution and variation in size of
nonmetallic inclusions, the uniformity of structure, the
location and extent of segregation, flow lines etc. can be
• The result of the above equation is divided by the linear examine by macroscopy and these cannot be examined by
magnification photo micrograph i.e. by 100 to get the actual microscopy.
grain diameter. • Crystalline heterogeneity i.e. manner of solidification and
the crystalline growth of the metal or alloy.
• Chemical heterogeneity i.e. impurities in a metal or alloy.
2.14.3 Jefferies Plainmetric Method Mechanical heterogeneity i.e. due to cold working or
• It is similar to the Heyn's intercept method, with the heterogeneity occurs in metals or alloy due cold rolling or
difference that it is based on area intercept rather the line forging etc.
intercept. • The results obtained by metallurgical microscopy are not
• A photomicrograph of the grain structure of the sample is representative of entire component because of the
obtained with a suitable magnification. heterogeneous nature of these materials.
• The magnification should be such that at least 50 grains • Macroscopic examination is the process of examining the
should be seen in the above photomicrograph. metals with or without proper etchant and by unaided eyes
• A circle or a rectangle of known area is drawn on the or by a magnifying glass.
photomicrograph. • Macroscopy is mainly used for investigation of defects and
• The actual area covered by the circle or rectangle should be structures.
at least 5000 mm2. • As compared to microscopy, a large surface observation is
• The total number of grains covered by the circle or possible in macroscopy. Also preparation of specimen is
rectangle is counted. easy in macroscopy. 1. Uniformity of structure
2. Distribution of non-metallic inclusions
3. Extent of segregation
• Jefferies Multiplier (f) is a function of the magnification 4. Presence of defects
used as given in the following table no. 2.6. 5. Examination of fractures
Table No. 2.6 Jefferies Multipliers 6. Flow lines in extruded, forged and drawn parts.
Magnification used f • For correct evaluation of the surface details, high level of
skill and experience is required.
1 0.002
• For some of the macroscopic examinations like
10 0.02 examination of fractured surfaces, etching of the surfaces
25 0.125 is not required.
50 0.5
75 1.125
100 2 2.16 Sulphur Printing
• Sulphur printing is used to detect sulphur in ferrous metals
150 4.5
and alloys.
200 8 • It is also produces a permanent record of sulphur
250 12.5 distribution in steel.
• To reduce the harmful effect of sulphur, manganese is
300 18 added.
• Sulphur printing is used to determine distribution of • It is achieved by macro-etching the polished surface of
sulphur impurity in the steel sample. Sulphur impurity has component in a 50% aqueous solution of hydrochloric acid
the effect of including brittleness in the steel or the (HCl) at 60 to 70°C for 5 to 10 minutes.
distribution of such impurities in the steel is very important. • Sometimes, 10 to 12% solution of ammonium per sulphate
• The surface of the specimen is initially polished on 0 or 00 (NH4)2S2O8 can also be used for etching at room
number emery paper and then washed under running water. temperature.
• A matt finish photographic bromide paper is soaked in 2% • If the macro-etched surface shows a directional flow
aqueous solution of sulphuric acid for 3 to 4 minutes. pattern consisting of streaks and striations, it means the
• The paper is taken out from the solution and excess drops component is forged.
of solution are removed. • The flow lines are observed because the elongated
• The emulsion side of the paper is then kept in contact with inclusions and other elongated heterogeneous areas are
polished surface of the specimen for 2 to 3 minutes with attacked by the etching reagent.
moderate pressure. • Highly stressed areas are also etched effectively.
• The photographic paper is then removed from the surface • It is important to note that, observation of flow lines on the
of specimen, washed in running water and then it is macro-etched surface is an indication of mechanical
immersed in photographic fixer solution for about 15 working and not an indication of defect.
minutes.
• Finally, the paper is taken out from the solution, washed in
running water for about 60 minutes and dried.
• Now, the dark brown spots on the print indicates presence
of sulphur segregation whereas a random dispersion of the
spots denote a more uniform and less harmful distribution
of sulphur.
• The chemical reactions that occurs during the sulphur
printing are as follows:
FeS (or MnS) + H2SO4 FeSO4 (or Fig. No. 2.17 Flow Lines Observation

MnSO4) + H2S Fig. no. 2.17 shows the flow lines in a forged component.
Cast component do not show flow lines. Broken and
discontinuous flow lines are observed for a rolled and
2 AgBr + H2S Ag2S + 2HBr machined component.

• The entire sulphur printing process can be conducted in day

light. The good results are obtained only on first and second
print from the prepared surface of a metal.
• Sulphur printing is used to find the sulphur distribution in
an ingot, a forging or a hot rolled product.
2.18. Difference between Microscopic and Macroscopic
Examination
Table No. 2.7 Difference between Microscopic and
Macroscopic Examination
S. Microscopic Macroscopic
N. Examination Examination
2.17 Flow Lines Observations
This is carried out at This is carried at lower
• Flow lines indicate the direction in which the steel was
mechanically worked. 1 higher magnification magnification or with
• We know that, forged components have better properties (more than 50X). naked eyes (less than 50X).
than the cast, rolled and machined components.
This requires higher This does not require
• Also the properties of forged components are governed by
the metal flow pattern. 2 degree of mirror finish mirror finish specimen
• Hence, it is necessary to know whether the component is specimen surface. surface.
manufactured by forging, casting, rolling or machining. Very high skill is required Not very high skill is
3
for investigation. needed for investigation.
 Unit II Micro and Macroscopic Study of Metals

Different types of phases No such phases

4
can be observed. are observed.
Very much time Comparatively fast
5 consuming (slow
process) process.
6 Highly expensive Not so expensive
7 Very high initial cost Very low initial cost
Best e.g. observation of
different phases Best e.g. sulphur printing
8 inclusions, microstructure flow line observation.
of a metal.