EXPERIMENT 4

THE EFFECTS OF HEAT TREATMENT ON THE MICROSTRUCTURE OF STEEL

OBJECTIVES
I.
II.
III.

To study on preparing of metallographic sample for microstructures observation.

To study the effects of heat treatment on the microstructure of steel.
To discover the microstructure of ferrite, pearlite, cementite, austenite and martensite under
microscopic view.

APPARATUS
I.

Five different sample of heat treated steel

Sample number
1
2
3
4
5

Abrasive cutter machine ( MEGA T-300 SAW )

Type of heat treatment

Without heat treatment
Water quenched
Oil quenched
Normalizing
Annealed

Etching machine

Compression Mounting Press

Grinding-polisher machine ( NANO 2000T )

Hand polishing machine

Fume hood

Optical microscope

SUMMARY
The properties of steels can be changed or altered by several techniques such as alloying and heat
treatment. Heat treatment process is a process is a process of ability to change the properties by applying
heat. Such treatment modifies microstructures, producing a variety of mechanical properties that are
important in manufacturing, such as improve formability and machinability.
Heat Treatment Process
I.
Annealing
Annealing is the process to makes metal as soft as possible. The material is exposed to an
elevated temperature for an extended time period and then slowly cooled to allow phase
changes.
There are three stages of annealing
Heating to the desired temperature: The material is austenitized by heating to 1 55C to
40 5C above the A or A lines under equilibrium is achieved which is the alloy
changes to austenite.
Soaking or holding time : the material is held for an hour at the annealing
temperature for the every inch of thickness
Cool slowly, usually to room temperature. Cooling method is slowly cooled in air or
turn off the furnace.
The purposes of annealing are
I.

Relieve internal stresses. Internal stresses can build up in metal such as a result of
processing. Such as welding, cold working, casting, forging or machining. If internal
stresses are allowed to remain in a metal, the part may eventually distort or crack. Thus,
Annealing helps relieve internal stresses and reduce the chances of distortion and
cracking.

II.

Increasing softness, machinability and formability. A softer and more ductile material is
easier to machine in the machine shop. An annealed part will respond better to forming
operations.
Refinement of grain structures. After some types of metalworking, the crystal structures
are elongated. Annealing can change the shape of the grains back to the desired form.

III.

II.

Normalizing

The name of normalizing comes from the original intended purpose of the process- to return steel
to normal condition it was in before it was altered by cold working or order processing.
Heating the alloy to 55 C
5 to 85 C
5 above the A and holding for sufficient time so that the alloy
completely transforms to austenite , followed by air cooling.
The process of normalizing

Heat up to critical temperature, at which point the structure is all austenite.

Cool slowly in air

The purpose of normalizing

I.

III.
IV.

To refine the grains and produce a more uniform and desirable size distributions for steels
that has been plastically deformed.
A normalized part will usually be a little stronger, harder and more brittle than a fullannealed part.
To improve machinability
Make the steels higher in strengthens and harder.

III.

Quenching

II.

Quenching is the act of rapid cooling of alloy from an elevated temperature to harden the steel in
any quenching media. Various quenching mediums can be used during the process. For example
water, oil, air and brine which will give different result on the structures and materials properties.

The process of quenching

Heated to 30 C
5 to 50 C
5 above the upper critical temperature and then quenched.

The effect of cooling rate on the material can be summarized as in table below:
Cooling rate
Properties
Microstructure
Grain size

Quenching
Hard
Strong
Brittle
Martensite
Small

Slow
Soft
Weak
Ductile
Ferrite-Pearlite-Cementite
Large

SAMPLE PREPARATION
The objectives of sample preparation for metallographic observations with a mirror like surface. Proper
preparation of metallographic specimens to determine microstructure and content requires that a rigid
step-by-step process be followed. In sequence, the steps include sectioning, mounting, course grinding,
fine grinding, polishing, etching and microscopic examination. Specimens must be kept clean and
preparation procedure carefully followed in order to reveal accurate microstructures.
Metallography consists of the study of the constitution and structure of metals and alloys. Much can be
learned through specimen examination with the naked eye, but more refined techniques require
magnification and preparation of the material's surface. Optical microscopy is sufficient for general
purpose examination; advanced examination and research laboratories often contain electron microscopes
(SEM and TEM), x-ray and electron diffract meters and possibly other scanning devices. Incorrect
techniques in preparing a sample may result in altering the true microstructure and will most likely lead to
erroneous conclusions. It necessarily follows that the microstructure should not be altered. Hot or cold
working can occur during the specimen preparation process if the metallurgist is not careful. Expertise at
the methods employed to produce high quality metallographic samples requires training and practice. The
basic techniques can be learned through patient persistence in a matter of hours.
In order to obtain the smooth and flat surface, several techniques are required. These include cutting,
molding, grinding, polishing and etching.
I.

Cutting

When cutting a specimen from a larger piece of material, care must be taken to ensure that it is
representative of the features found in the larger sample, or that it contains all the information required to
investigate a feature of interest.

One problem is that preparation of the specimen may change the microstructure of the material, for
example through heating, chemical attack, or mechanical damage. The amount of damage depends on the
method by which the specimen is cut and the material itself.
Cutting with abrasives may cause a high amount of damage, while the use of a low-speed diamond saw
can lessen the problems. There are many different cutting methods, although some are used only for
specific specimen types. MTI provides the SYJ-150 low speed diamond saw for cutting OM (optical
microscope), SEM (scanning electron microscope), and even TEM (transmission electron microscope)
specimen.
Proper sectioning is required to minimize damage, which may alter the microstructure and produce false
metallographic characterization. Proper cutting requires the correct selection of abrasive type, bonding,
and size; as well as proper cutting speed, load and coolant. Table I list the most common type of abrasive
blades used for metallographic sectioning and Table II lists cutting parameters for diamond wafer cutting

Table 1
Materials ( alloy)
Aluminum, brass, zinc, etc.
Heat treated alloys
<Rc 45 steel
>Rc 45 steel
Super alloys

Classification
Soft non-ferrous
Hard non-ferrous
Soft ferrous
Hard ferrous
High Ni-Cr alloys

Abrasive/bond
SiC/ Rolled rubber
Alumina/ Rubber resin
Alumina/ Rubber resin
Alumina/ Rubber resin
SiC/ Rolled rubber

Table 2
Material
Silicon substrate
Gallium arsenide
Boron composites
Ceramic fibre
composites
Glasses
Minerals
Alumina ceramic
Zirconia
Silicon nitride
Metal matrix
composites
General purpose
II.

Mounting

Characteristics
Soft/brittle
Soft/brittle
Very brittle
Very brittle

Speed(rpm)
<300
<200
500
1000

Load(grams)
<100
<100
250
500

Blade(grit/conc.)
Fine/low
Fine/low
Fine/low
Fine/low

Brittle
Friable/brittle
Hard/tough
Hard/tough
Hard/tough
-

1000
>1500
>1500
>3500
>3500
>3500

500
>500
>500
>800
>800
>500

Fine/low
Fine/low
Medium/low
Medium/low
Medium/low
Medium/high

Variable

Variable

Medium/high

Mounting of specimens is usually necessary to allow them to be handled easily. It also minimizes the
amount of damage likely to be caused to the specimen itself.
The mounting material used should not influence the specimen as a result of chemical reaction or
mechanical stresses. It should adhere well to the specimen, and if the specimen is to be electropolished
later in the preparation then the mounting material should also be electrically conducting.
Specimens can be hot mounted (about 150 C) using a mounting press either in a thermosetting plastic,
e.g. phenolic resin, or a thermo softening plastic e.g. acrylic resin. If hot mounting will alter the structure
of the specimen a cold-setting resin can be used, e.g. epoxy, acrylic or polyester resin. Porous materials
must be impregnated by resin before mounting or polishing, to prevent grit, polishing media or etchant
being trapped in the pores, and to preserve the open structure of the material.
Castable mounting resins are commonly used for electronic and ceramic materials. Castable mounting
resins are recommended for brittle and porous materials. These mounting compounds are typically two
component systems (1- resin and 1-hardener). Typical curing times range from minutes to hours with the
faster curing resins producing higher exothermic temperature which causes the mounting material to
shrink away from the edge during curing. For example, the Acrylic Cold Mounting Resins cure in less
than 10 minutes and Epoxy Castable Resins cure in approximately 4-6 hours. Note that adding an external
energy source such as heat or microwave energy can enhance the Epoxy Castable Resin curing cycle. It is
recommended that the room temperature be less than 85 F to avoid overheating and uncontrollable
curing of the mounting compound. Table IV lists the basic properties of castable
A mounted specimen usually has a thickness of about half its diameter, to prevent rocking during grinding
and polishing. The edges of the mounted specimen should also be rounded to minimize the damage to
grinding and polishing discs.

III.

Grinding
Surface layers damaged by cutting must be removed by grinding. Mounted specimens are ground
with rotating discs of abrasive paper, for example wet silicon carbide paper. The coarseness of the
paper is indicated by a number: the number of grains of silicon carbide per square inch. So, for
example, 180 grit paper is coarser than 1200 grit.

The grinding procedure involves several stages, using a finer paper (higher number) each time. Each
grinding stage removes the scratches from the previous coarser paper. This can be easily achieved by
orienting the specimen perpendicular to the previous scratches. Between each grade the specimen is
washed thoroughly with soapy water to prevent contamination from coarser grit present on the
specimen surface. Typically, the finest grade of paper used is the 1200, and once the only scratches
left on the specimen are from this grade.
The series of photos below shows the progression of the specimen when ground with progressively
finer paper.

Copper specimen ground with 180 grit paper

Copper specimen ground with 800 grit paper

paper

Copper specimen ground with 400 grit paper

Copper specimen ground with 1200 grit

Grinding Direction - The orientation of the specimen can have a significant impact on the preparation
results, especially for specimens with coatings. In general, when grinding and polishing materials
with coatings the brittle component should be kept in compression. In other words, for brittle coatings
the direction of the abrasive should be through the coating and into the substrate. Conversely, for
brittle substrates with ductile coatings, the direction of the abrasive should be through the brittle
substrate into the ductile coating.
Manual Preparation - In order to insure that the previous rough grinding damage is removed when
grinding by hand, the specimen should be rotated 90 degrees and continually ground until all the
scratches from the previous grinding direction are removed. If necessary the abrasive paper can be
replace with a newer paper to increase cutting rates.

Automated Preparation - The key to successful automated preparation is to thoroughly clean the
specimens between each abrasive grit size that is used. The tracking of the specimens should also
uniformly break down the SiC paper, otherwise non-uniform grinding will occur (especially for hard
specimens in soft mounts). In other words, the specimen should track across the entire diameter of the
SiC paper.
Abrasive Selection - The most common abrasive used for planar grinding metal and polymer
metallographic specimens is silicon carbide (SiC). Silicon carbide is an excellent abrasive for planar
grinding because it is very hard and maintains a sharp cutting edge as it breaks down during cutting.
SiC abrasives are typically listed by the grit size. Table VI shows the two most common grit sizenumbering systems, along with their respective median diameter particle size and Table below
provides a list of recommendation for planar grinding specific materials.

Metallic
Specimens

Electronic
Specimens

Plasma Spray
Components

Ceramics and
Ceramics

Planar Grinding Recommendations

For metallic specimen grinding, sequential grinding with silicon carbide (SiC)
abrasive paper is the most efficient and economical rough grinding process.
Although extremely coarse grit abrasive papers can be found, it is recommended
that a properly cut specimen not be rough ground with an abrasive greater than
120 grit SiC paper. A typical abrasive grinding procedure would consist of 120
or 240 grit SiC paper followed by decreasing the size of the SiC paper (320,
400, and 600 grit). Finer papers are also available for continued abrasive paper
grinding (800 and 1200 grit). In addition to the correct sequence and abrasive
size selection, the grinding parameters such as grinding direction, load and
speed can affect the specimen flatness and the depth of damage. The basic idea
is to remove all of the previous specimen damage before continuing to the next
step while maintaining planar specimens
Grinding electronic components is very dependent upon both the substrate
(silicon, alumina, barium titanate, plastic PCB's, etc) and the metallic materials
used. In general, when grinding plated or coated materials, it is recommended
that the coating be prepared in compression to prevent the coating from
separating from the substrate. Silicon specimens should be have been sectioned
with a fine grit diamond blade and cut as near as possible to the area of interest.
For rough grinding, fine abrasives such as 400 or 600 grit SiC or a 15-micron
diamond lapping film is recommended to avoid producing more damage than
created during sectioning. Hard ceramic substrates (especially porous materials)
should be rough polished with diamond lapping films to minimize edge
rounding and relief between the widely varying materials hardness'
Similar to the preparation of electronic components, plasma spray coatings
should be kept in compression to minimize the possibility of delamination at the
coating/ substrate interface. For ceramic plasma spray coatings, diamondlapping films are recommended to minimize edge rounding or relief and to
maintain the integrity of any inclusions within the coating.
Rough grinding ceramics and ceramic matrix composites should be performed
with 15 or 30 micron diamond on a metal mesh cloth in order to obtain adequate

Composites
Plastics and
Plastics
Composites

IV.

stock removal and to minimize surface and subsurface damage.

Plastics are generally very soft and therefore can be planar ground with
sequentially decreasing SiC abrasive paper grit sizes. When plastics are used in
conjunction with hard ceramics, planar grinding can be very tricky. For these
composite materials cutting must minimize damage as much as possible because
almost all grinding and polishing will cause relief between the soft plastic and
the hard ceramic. Following proper cutting, grinding with as small as possible a
diamond (6-micron diamond) on a metal steel mesh cloth or the use of lapping
films is suggested.

Polishing

Polishing discs are covered with soft cloth impregnated with abrasive diamond particles and an oily
lubricant or water lubricant. Particles of two different grades are used : a coarser polish - typically
with diamond particles 6 microns in diameter which should remove the scratches produced from the
finest grinding stage, and a finer polish typically with diamond particles 1 micron in diameter, to
produce a smooth surface. Before using a finer polishing wheel the specimen should be washed
thoroughly with warm soapy water followed by alcohol to prevent contamination of the disc. The
drying can be made quicker using a hot air drier.
Rough Polishing - The purpose of the rough polishing step is to remove the damage produced during
cutting and planar grinding. Proper rough polishing will maintain specimen flatness and retain all
inclusions or secondary phases. By eliminating the previous damage and maintaining the
microstructural integrity of the specimen at this step, a minimal amount of time should be required to
remove the cosmetic damage at the final polishing step. Rough polishing is accomplished primarily
with diamond abrasives ranging from 9 micron down to 1-micron diamond. Polycrystalline diamond
because of its multiple and small cutting edges, produces high cut rates with minimal surface damage,
therefore it is the recommended diamond abrasive for metallographic rough polishing on low napped
polishing cloths. Table below show the basic rough polishing guidelines for a number of materials.
Metals (ferrous, nonferrous, tool
steels, ys, etc.)
Ceramics and ceramic matrix
composites (CMC)

Polymer matrix composites (PMC)

Rough polishing typically requires two polishing steps, such

as a 6-micron diamond followed by a 1-micron diamond on
low napped polishing cloths.
Low nap-polishing pads using polycrystalline diamond
alternating with colloidal silica. This provides a chemical
mechanical polishing (CMP) effect, which results in a
damage free surface finish.
Diamond lapping films

Biomaterials

Microelectronic specimen
Plastics and polymers
Plasma spray materials

Low napped polishing pads with polycrystalline diamond

alternating with colloidal silica. Alternatively, diamond
lapping films may work well
Diamond lapping films
800 and 1200 grit SiC abrasive paper
Diamond lapping films or low napped polishing pads with
alternating diamond and colloidal silica abrasives

Fine Polishing The purpose of fine polishing is to remove only surface damage such as scratches. It
should not be used to remove any damage remaining from cutting and planar grinding. If the damage
from these steps is not complete, the rough polishing step should be repeated or continued. Table
below describes the most common polishing pads for metallographic specimen preparation.
Metals (ferrous, nonferrous,
tool steels, ys, etc.)
Ceramics and ceramic matrix
composites (CMC)
Polymer matrix composites
(PMC)
Biomaterials

Microelectronic specimens
Plastics and polymers
Plasma spray materials

High napped polishing pads with a colloidal alumina polishing

abrasive. The polishing times should nominally be less than 30
seconds
Low napped polishing pads using 1 um polycrystalline diamond
alternating with colloidal silica or colloidal silica alone.
Fine abrasive diamond lapping films followed by a very light polish
on a high napped polishing pad.
Low napped polishing pads with polycrystalline diamond, alternating
with colloidal silica. Alternatively, diamond lapping films may work
well
Diamond lapping films followed by a very light polish on a high
napped polishing pad
Light polish with alumina on a high napped polishing pad
Diamond lapping films followed by a very light and short alumina or
colloidal silica polish on a high napped polishing pad

Copper specimen polished to 6 micron level

V.

Copper specimen polished to 1 micron level

Etching

The purpose of etching is to optically enhance microstructural features such as grain size and phase
features. Etching selectively alters these microstructural features based on composition, stress, or
crystal structure. The most common technique for etching is selective chemical etching and numerous
formulations have been used over the years. Other techniques such as molten salt, electrolytic,
thermal and plasma etching have also found specialized applications. Chemical etching selectively
attacks specific microstructural features. It generally consists of a mixture of acids or bases with
oxidizing or reducing agents. For more technical information on selective chemical etching consult
corrosion books which discuss the relationship between pH and Eh (oxidation/reduction potentials),
often known as Eh-pH diagrams or Pourbaix diagrams. Over the years numerous chemical etchants
have been formulated. Some of the more common chemical etchants are listed in the following table.
Table below lists some of the more common etchants.
Etchant
Kellers Etch

Krolls Reagent

Composition
190 ml Distilled water 5
ml Nitric acid
3 ml Hydrochloric acid 2
ml Hydrofluoric acid
92 ml Distilled water

Applications
Aluminum alloy

Conditions
10-30 second
immersion. Use only
fresh etchant

Titanium

15 seconds

Nital
Kallings Reagent

Lepitos Reagent
Marbles Reagent

Murakami Reagent

Picral
Vilellas Reagent

6 ml Nitric acid
2 ml Hydrofluoric acid
100 ml Ethanol
1-10 ml Nitric acid
40 ml Distilled water
2 grams Copper chloride
(CuCl2)
40 ml Hydrochloric acid
40-80 ml Ethanol (85%) or
Methanol (95%)
50 ml Acetic acid
50 ml Nitric acid
50 ml Distilled Water 50
ml Hydrochloric acid
10 grams Copper sulfate
100 ml Distilled Water 10
grams K3Fe(CN)8 10
grams NaOH or KOH
100 ml Ethanol
2-4 grams Picric acid
45 ml Glycerol
15 ml Nitric acid
30 ml Hydrochloric acid

Carbon steels, tin and

nickel alloys
Wrought stainless steel,
Fe-Ni-Cr alloys

Seconds to minutes

High temperature
steels
Stainless steel, Nickel
alloys

Swab

Wrought stainless steel,

tungsten alloys, silver
alloys, SiC, B4C
Iron and steel,
Tin alloys
Stainless steel, carbon
steel, cast iron

Immerse or swab for

few seconds to a few
minutes

Immersion or swab
etching for a few
seconds
Immerse or swab for
seconds to minutes
Seconds to minutes
Seconds to minutes

Electrolytic etching is another fairly common etching technique. It is similar to chemical etching in
that acids and bases are used for modifying the pH, however the electrochemical potential is
controlled electrically by varying the voltage and current externally as opposed to chemically.
Electrolytic etching is often used for harder to etch specimens that do not respond well to basic
chemical etching techniques. Electrolytic techniques require that the specimen be conductive and are
therefore limited primarily to metals. The most common electrolytic etching equipment uses a twoelectrode design (anode and cathode) with acids or bases for the electrolyte. Procedures for this type
of electrolytic etching are fairly common and can be found in the literature. Another type of
electrolytic etching requires more sophisticated electrochemical equipment (potentiostats). This
equipment uses a three-electrode configuration (anode, cathode, and reference) which allows the
current and voltage to be adjusted independent of each other. In comparison to the two-electrode
system, voltage is altered with the electrolyte dictating the current conditions. On the other hand, the
electrolyte for the three-electrode configuration only requires a conductive solution such as KCl,
instead of highly corrosive acids or bases.
Molten Salt etching is a combination of thermal and chemical etching techniques. Molten salt etching
is useful for grain size analysis for hard to etch materials such as ceramics. The technique takes

advantage of the higher internal energy associated at a materials grain boundaries. At the elevated
temperature of molten salts, the higher energy at the grain boundaries is relieved, producing a
rounded grain boundary edge, which can be observed by optical, or electron microscope techniques.
Thermal etching is a useful etching technique for ceramic materials. Thermal etching is technique that
relieves the higher energy associated at the grain boundaries of a material. By heating the ceramic
material to temperatures below the sintering temperature of the material and holding for a period of
minutes to hours the grain boundaries will seek a level of lower energy. The result is that the grain
boundary edge will become rounded so that it can be evaluated by optical or electron microscope
techniques. Depending upon the ceramic material, the atmospheric condition of the furnace may need
to be controlled. For example, etching silicon nitride will require either a vacuum or an inert
atmosphere of nitrogen or argon to prevent oxidation of the surface to silicon dioxide.
Plasma etching is a lesser-known technique that has been used to enhance the phase structure of high
strength ceramics such as silicon nitride. For silicon nitride, the plasma is a high temperature fluoride
gas, which reacts with the silicon nitride surface producing a silicon fluoride gas. This etching
technique reveals the intragrain microstructure of silicon nitride.

Etched copper specimen

VI.

Over etched copper specimen

Microscopic Examination

Initial microscopic viewing should be done utilizing a stereomicroscope, which reveals a threedimensional scanning of the specimen surface. The specimen is placed on the stage of the microscope
so that its surface is perpendicular to the optical axis. Detailed viewing is done with a Metallurgical
Microscope. A metallurgical microscope has a system of lenses (objectives and eyepiece) so that
different magnifications (25X to 1000X) can be achieved. The important characteristics of the
microscope are: (1) magnification, (2) resolution and (3) flatness of field. The resultant magnification
is the product of the magnifying power of the objective and that of the ocular. Scanning Electron
Microscopes (SEMs) are capable of magnifications up to 20,000X and Transmission Electron
Microscopes (TEMs) are utilized to view at magnifications up to 100,000X for highly detailed
microstructural study.

EXPERIMENT PROCEDURES
1. We were provided with five different samples of heat- treated steel.
2. The microstructure of each sample were observed and sketched.
3. We identified and labeled the microstructures.
RESULTS

Austenite

Ferrite

Pearlite

Martensite

Upper bainite

Lower bainite