METALLOGRAPHY

COURSE CODE: WEC 122

PREPARED BY: ENGR. BUNMI ONASOLA

OBJECTIVES

(1) To learn and gain experience in the preparations of Metallographic specimen

(2) To examine and analyse the micro structures of metals and metallic alloys.

DEFINITIONS

Metallography can be defined as the study of the microstructure of metals and their alloys by any of a variety

of techniques. Metallography consists of the study of the constitutions and structure of metals and alloys.

Much can be learnt through specimen examination with the naked eye; but more refined techniques require

magnification and preparations of the material’s surface. Metallography is similar to a process for utilising

metal plates in a manner similar to Lithographic process.

PURPOSE AND ADVANTAGE OF METALLOGRAPHY

Examinations of metals specimen for microstructures analysis are used for information gathering, analysis,

diagnosis, inference or decision making for further knowledge and understanding . i.e research and

development (R&D). It aids in determining if the material has been processed correctly and it’s therefore a

critical step for determining products reliability and for determining why materials fail in service (Quality

Control and Forensic Investigation)

HISTORY

Macroscopic metallography, which does not generally involve the use of any optical instrument

other than a hand held magnifier (Magnifying Glass) originated at the beginning of the Nineteenth

century with Aloys Beck Von -Widmanstatten’s classical observations of the surface structure of

Meteorites.

Microscopic Metallography was introduced, in 1840 but did not begin to flourish until 1860, with

Professor Henry Sorby’s detailed investigations into the structure of Steels.

Modern microscopical metallography involves not only the use of high quality optical microscopes

of special design, but also the use of instrument in which beams of electrons replace rays of light in

order to obtain much higher magnifications of the order of Millions rather than in hundreds.

Since metallography is a very important field of metallurgical investigation, a good knowledge of

the preparations of metallographic specimens (samples) will be necessary. Optical microscopy is

sufficient for general purpose examination. However, advanced examination and research laboratories often

contain Electron Microscopes (SEM, TEM) X-Ray and Electron Beam Diffractometers and possibly other

scanning devices.

FEATURES OF METALLOGRAPHY

The entire Metallographic work centres on the following:

(1) SPECIMEN

(2) MATERIALS NEEDED

(3) INSTRUMENT NEEDED

(4) METHODS OF OPERATIONS

(5) RECORDING AND DOCUMENTATION

THE BASICS OF METALLOGRAPHIC SAMPLES PREPARATION

The basic steps or procedures to follow for metallographic sample preparation include:

(1) Documentation

(2) Sectioning and Cutting

(3) Mounting

(4) Planar Grinding

(5) Rough Polishing

(6) Final Polishing

(7) Etching

(8) Microscopic Analysis / Examination

(9) Hardness Testing

(10)Report Writing and Documentation

SELECTING THE SPECIMEN FOR METALLOGRAPHY

To be of any value for investigative or any studies or information; the specimen must meet the

following conditions:

(1) “Be a representative of the material being studied.” The structure and /or composition of a large

body of alloy may vary considerably from one section or region of the part to another. In such

situation, it is expedient to select samples or specimens from the various parts of the body in

order to adequately represent each section of the body.

(2) Both Transverse and Longitudinal section of the material must be chosen. Some materials

exhibit directionality in structure; e.g, a rolled Mild Steel will show “Stringer “ of Manganese

Sulphide elongated in the direction of rolling if a longitudinal section is examined,

Fig. 1 Longitudinal Sectioning/ Cutting

whilst these Manganese Sulphide inclusions will appear misleadingly as “Round

Structures(Globules) if a transverse section is examined.

Fig. 2 Transverse Sectioning/ Cutting

Incorrect techniques in preparing a sample for metallographic examination may result in altering the true

microstructure and will most likely lead to erroneous conclusions. It is therefore necessary not to alter the

microstructure. Hot or Cold working can occur during the specimen preparation process, if the metallurgist

or Technician is not careful. Expertise at the methods employed to produce high quality metallographic

samples require training and practise. The basic techniques can be learnt through patient, persistence and

perseverance.

DOCUMENTATION
Metallographic analysis is a valuable tool. By properly documenting the initial sample conditions

and the proceeding microstructural analysis, metallography provides a powerful quality control as

well as an invaluable investigative tool. This should include; Specimen Name, Specimen Type,

Dates, Materials needed / used etc.

SECTIONING AND CUTTING

Following proper documentation, most metallographic samples need to be sectioned to the area of

interest and for easier handling. Depending on the material, the sectioning operations can be done

or obtained by abrasive cutting (Metal and Metal Matrix Composites), Diamond Water Cutting

(Ceramics, Electronics, Bio-Materials, Minerals) or thin sectioning with a microtomes (Plastics).

Proper sectioning is required to minimise damage, which may alter the microstructure and produce

false metallographic characterisation. Proper cutting requires the correct section of the abrasive

types, bonding and size, as well as proper cutting speed, load and coolant.

MOUNTING THE SPECIMEN

A specimen of approximately Ø20mm (200mmSquare) is a convenient size for a beginner to

handle. If the specimen is smaller than this, then it is advisable to mount it in some inert plastic

materials which will neither have a Galvanic effect leading to uneven etching nor dissolve in any of

the de-greasing agents or reagents used.

The specimen, whatever its size will need to be mounted also, if its sectional surface is to be

examined, otherwise the surface edge will be lost due to bevelling during the polishing process.

Similarly, surface cracks are best examined by cutting a specimen so that it contains the crack,

mounting it in Bakelite (or other plastic compound) and then grinding it down until the crack

becomes exposed.
Most of the plastic substance used as mounting moulding materials flow at about 150 ⁰C which is

too low a temperature to cause any structural change in most metallic alloys. Alternatively, the

specimen may be mounted in some cold-setting compounds (which generally consists of white

powder which is sprinkled over the specimen, followed by a colourless liquid (Araldite, Super glue

etc.) the whole item is retained in a metal ring or by two L-Shaped angle pieces of metal until

Polymerisation of the powder and the liquid are completed to provide a hard rigid mount.

GRINDING AND POLISHING

One of the most paramount thing to achieve in specimen grinding operation apart from smooth

polished surface is to have an “absolutely flat” surface since when using high magnifications with

microscope, the depth of field which is in focus at any time is extremely small. For this reason, the
surface must first be filed absolutely flat and this is best achieved by rubbing the specimen “To and

Fro” on the file instead of attempting to file the specimen flat with fil as in the normal regular way.

When the saw marks has been filed out, the specimen and the operator’s hands should be washed to

remove coarse fillings and other abrasive particles. Intermediate and fine grinding is then carried

out using emery cloths/ papers of progressively finer grades. These should be of the finest quality

with regards to uniformity of particles size (150, 220, 320, 400, 600 ) grit sizes with modern

papers/cloths.

Wet grinding is now generally used with the emery papers being manufactured to be water-proof.

Whichever methods is being used, rotary grinding machine or stationary grinding desk with strips

of emery papers clamped side by side on a slopping sheet of glass plate over which a current of

water runs unto it. The specimen is first ground on the 150-Grade paper with the specimen held at

90⁰ to the furrow of the cutting / grinding furrows created, this is progressively done on the

specimen on the other grades of emery papers till the final one. (320=>400=>600). The specimen is

then washed to remove the free grits at every end of the each grades of paper.

After the series of grinding operations, the surface of the specimen if examined under a 100 X

magnification Microscope, it will be seen to be covered by a series of parallel grooves cut by the

600 grit size emery paper. The final operation of polishing is somewhat different in character since

it removes the “ridged surface by means of a “Burnishing Operation”. This drags the ions of the

metal across the surface to provide an amorphous or Flowed” layer which effectively hides the

crystal structure beneath. This amorphous layers must be dissolved therefore by suitable etching

reagents.
 (i) Groove produced in the metal by the final grinding operations caused by the particles of

grit size 600

(ii) Polishing produced a flowed layer which will hide the scratch (S) surface.

(iii) Etching dissolves the flowed layer, revealing the crystal structure and the deep scratch

beneath.

Ferrous metals (Iron and Steels) are polished on a rotating cloth pad impregnated with some

suitable polishing medium. Polishing compounds containing Diamond dusts carried in a cream

based (KEMET) are now being used for polishing. Two polishing wheels are being used, the first

wheel is charged with 6micron (6µ) grade Diamond paste and the second with 1 micron (1µ) grade.

Non-Ferrous metals specimen are often polished by hand on a small square of “Selvyt” cloth held

on a glass plate, a few spots of “Silvo” is being employed as polishing medium. A circular sweep of

the hand should be employed rather than the “To and Fro (Back and Forth) motion used in grinding.
In any polishing process, very light pressure should be applied as this will give a lower incidence of

scratching or scratches. Polishing should be accomplished in only two or three minutes. If a longer

period is necessary, it indicates that deep seated scratches are present and it is wise to go back to

400-grit size grinding paper. A specimen polished for too long a time will suffer a rippled surface.

ETCHING

In order to reveal the crystal structure, the flowed layer produced by polishing must be dissolved by

a suitable etchant. Firstly, it is essential however, to remove every trace of dirt and grease from the

specimen, otherwise, uneven etching and staining will be the result. Unmounted specimen can be

de-greased very easily by first washing off any loosely adhering polishing compound under a

running tap of water and then simply immersing the specimen in boiling alcohol (Industrial

Methylated Spirit) for about one minute. By using hot alcohol in this way, the specimen dries

immediately on withdrawal from the bath and does not stain.

Rapid drying to avoid staining is accomplished for a thermoplastic material mounted specimen after

degreasing using cold alcohol through the use of hot / warm dry air, using hand held hair dryer.

Specimen may be examined in this unetched condition for the presence of slag inclusions and other

non-metallic inclusions which will be more easily visible at this stage.

After having degreased the specimen, it should NOT be touched by the finger but handled with a

tong until after it has been etched. Otherwise, traces of grease may cause staining. The specimen is

first cooled in cold running water and then immersed immediately in the etching reagents, agitating

it rigorously/ vigorously until etching is complete. This will be indicated by surface of the specimen

becoming dull or sometimes with colour change.

Etching time varies from a few seconds with plain carbon Steels and Brasses to several minutes for

Stainless Steel. Practising a near clinical standard of cleanliness in the later stages of de-greasing

and etching will be found to be a recipe for a good result. As soon as the specimen has been

adequately etched, it must be washed in running water without delay otherwise, the surface will

begin to stain due to the combined effects of the etchants and atmospheric oxygen. Having washed

the specimen, it is rapidly dried in alcohol as previously described. Many different etchants are used

in Metallographic laboratories such as( sodium bromide ). After etching, the specimen is then

mounted for microscopical examination.

ETCHANTS AND THEIR APPLICATIONS

GROUP ETCHANT COMPOSITION USES/ CHARACTERISTIC

NAME

STEEL Nital 2Cm3 Nitric acid+ 98 Best general etching reagent

Cm3 Alcohol for Iron and Steel
(Industrial Methylated
Spirit)
Alkaline Sodium 2g Picric Acid + 25g
Picrate Sodium Hydroxide +
100 Cm3 Water
Mixed Acid and 10 Cm3 Nitric Acid + Suitable for Nickel-Chromium
Glycerol 20 Cm3 Hydrochloric alloys and most Stainless
Acid + 20 Cm3 Steels and most high Carbon
Glycerol + 10 Cm3 Steels (HSS)
Hydrogen Peroxide
COPPER & Ammonia- 50Cm3 Ammonium The best general etchant for

ITS ALLOYS Hydrogen Peroxide Hydroxide + 50Cm3 copper and most Copper based

Water + 20Cm3 alloys

Hydrogen Peroxide

(just before use)

Acid Ferric 10g Ferric Chloride +

Chloride 30 Cm3 Hydrochloric
 Acid
+ 120 Cm3 Water
ALUMINIUM Dilute Hydroflouric 0.5Cm3 Hydroflouric
Acid Acid + 100 Cm3 Water
and Its Alloys

GROUP ETCHANT COMPOSITION USES/ CHARACTERISTIC

NAME

STEEL Nital 2Cm3 Nitric acid+ 98 Best general etching reagent

Cm3 Alcohol for Iron and Steel
(Industrial Methylated
Spirit)
Alkaline Sodium 2g Picric Acid + 25g
Picrate Sodium Hydroxide +
100 Cm3 Water
Mixed Acid and 10 Cm3 Nitric Acid + Suitable for Nickel-Chromium
Glycerol 20 Cm3 Hydrochloric alloys and most Stainless
Acid + 20 Cm3 Steels and most high Carbon
Glycerol + 10 Cm3 Steels (HSS)
Hydrogen Peroxide
COPPER & Ammonia- 50Cm3 Ammonium The best general etchant for

ITS ALLOYS Hydrogen Peroxide Hydroxide + 50Cm3 copper and most Copper based

Water + 20Cm3 alloys

Hydrogen Peroxide

(just before use)

Acid Ferric 10g Ferric Chloride +

Chloride 30 Cm3 Hydrochloric
Acid
+ 120 Cm3 Water
ALUMINIUM Dilute Hydroflouric 0.5Cm3 Hydroflouric
Acid Acid + 100 Cm3 Water
and Its Alloys
FACTORS THAT AFFECT THE RATE OF BREAKDOWN OF THE ABBRASIVE BOND

(1) The hardness of the bond

(2) Hardness and workability of the metal samples

(3) The size and speed of the wheel

(4) The power of the driving motor

(5) The type and amount of the coolant used and the method of application of the coolant

(6) The amount of pressure by which the wheel is applied to the sample

(7) The amount or degree of vibration in the machine

NB:

Cut-off wheels are indexed from “Hard to Soft” and are referred to by Grades. As a rule of thumb, a

hard bonded wheel should be selected for sectioning “soft stock” and a soft wheel for sectioning

harder materials. A reasonable amount of wheel pressure is applied so the abrasive grain will “Bite”

and remove the metal in fine chips.

CAUTION:

Proper cutting procedures must be followed, abrasive cut-off wheels will crack and become flying

projectiles when NOT used or handled properly.

METALLURGICAL MICROSCOPES AND THEIR USES

The optical system of any microscope consist basically of two lenses,

1. The Objective lens “ O”

2. The Eye Piece lens “E”

The Objective lens is the most optically critical of the lenses, with respect to its influence on the

quality of the image produced and it must be able to resolve fine details. Objective lenses have

to be “corrected” to minimize the effect of spherical and chromatic aberrations; for which

reason microscope objective as well as camera and telescope or binoculars lenses are of

compound construction.

The magnification given by an objective depends on its “focal length” the shorter the focal

length, the higher the magnifications. In addition to this magnification, Resolving Power is very

important. This is the ability of the objective to produce sharply defined separate images of two

lines which are very close together. Resolving Power depends on the quality of the lens and also

upon the numerical aperture.

Numerical Aperture (NA) = Sin x =a/b

Fitness Detail = h/NA

Where h = wavelength of the light illumination. Working on the above exposition, the

maximum useful magnification obtainable from most optical microscopes is about 1000 X.

The purpose of the eyepiece lens is to magnify the image produced by the objective lens; and to

focus the mage so that it can be observed by the metallographer. Eye piece lens is supplied in a

number of “power” X6, X8; X10; X15. These are of simple and inexpensive construction as

compared with objective lenses. The overall approximate magnification given by a microscopic

system can be derived from;

Magnification = Tube length (mm) X Power of Eyepiece

Focal length of Objective

NB: Most bench microscopes have a tube length of 200mm = 20Cm

Metallurgical microscope is similar to any other optical microscope; it is in the method of

illuminating the specimen / sample that differentiate them. In most microscopes used for

Biological examinations, a relatively simple illumination system is employed because the

specimen are often transparent enough to allow light transmission through them. Hence, a

simple concave mirror is fixed beneath a hole in the microscope stage to collect the light

required to illuminate the specimen. Metallurgical specimens or samples for metallography are

“opaque’ in nature and must be examined therefore by “reflected light”.

An illumination system with the light source within the microscope (inside the microscope ) is

employed for metallographic / metallurgical microscope.

ELECTRON MICROSCOPE
Higher magnifications are sometimes needed or desirable and optical microscopes are incapable of

providing useful magnification much above 1000X or 2000X maximum. In order to obtain

magnification far above 1000x and up to several hundreds of thousand magnification, some form of

microscope using Electron beams / streams rather than light rays are used. Although, the bulk of

metallographic examinations are carried out at magnifications between 50X to 500X.

The high resolution power or resolving power of the Electron beams microscope arises from the

fact that just as light can be considered as both having wave-like and particle-like properties; so is

moving Electron beams seem to behave both as particles and waves. Thus, like light, electrons can

produce interference and diffraction effects. However, the wavelength associated with a moving

Electron can be controlled since it depends upon the “speed” and the “pd”( Potential Differences

Voltage), causing it to accelerate since the resolution or resolving power of the microscope

increases as the wavelength of the radiation reaching the system decreases. it follows that much

finer details will be resolved using Electron beams(h = 3.5 x 10 -12m) than using light (h = 6 x 10 -
5
m) on the average.

Since Electron beams tend NOT to be reflected in the regular manner of light rays, specimens must

therefore be viewed by “transmitted” rather than by “reflected” electrons.

The Electron path in an electron microscope is very similar to the light path in an optical

microscope. In the case of electron microscope, the lenses are electromagnetic type in which

electromagnetic fields are used to focus the electron beams in order to form an image on a

flourescent screen or a photographic plate or film.

The focal lengths of these electromagnetic lenses are of course variable and depend upon the

current passing through the coils. The body of the electron microscope must be vacuumed, so that

molecules of Nitrogen and Oxygen would seriously not obstruct the passage of the relatively small

electrons.
Technological advancements has produced electron microscope like the High Voltage Electron

Microscope that permits the use of thicker replica of specimen for observation at the same time can

produce greater magnifications.

Scanning Electron Microscope

This is very different in working principle from the orthodox electron beams microscope in that

electron reflected and generated from the actual surface of the specimens are used to form the

image. The image produced is of very high resolutions which is at least three hundred times better

than that of optical microscope. This enables even unprocessed or un-prepared surfaces to be

systematically explored at very high magnifications up to 50,000X.