1

MATERIALS CHARACTERIZATION TECHNIQUES

PROJECT

BATCH: 2013-14
By:
SYED MUNIR AZEEM
MM-029
Advisor:
S. M. Mohsin Jaffri

D E PARTM E N T O F M ATE R I A L S E N G I N E E R I N G
NED UNIVERSITY OF ENGINEERING & TECHNOLOGY
Materials
1 Engineering Department
NED University of Engineering And Technology

CERTIFICATE
Submitted in partial fulfilment of the requirements for the degree of Bachelors of
Engineering in Materials.
SYED MUNIR AZEEM

MM-029 Batch-2013-14

It is certified that the work contained in this report entitled: Characterisation of

Materials of different grades, has been accepted in partial fulfilment of the
requirements of Bachelors of Engineering in Materials.

_______________________
Supervisor

Chairman, MMD

D E PARTM E N T O F M ATE R I A L S E N G I N E E R I N G
NED UNIVERSITY OF ENGINEERING & TECHNOLOGY

Materials
2 Engineering Department
NED University of Engineering And Technology

Abstract
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, and polishing, etching
and microscopic examination. Specimens must be kept clean and preparation
procedure carefully followed in order to reveal accurate microstructures. Each student
will prepare and examine, ferrous and non-ferrous sample for metallographic
examination. Additionally, ferrous and non-ferrous sample with different composition
will be examined under the metallographic microscope. Photographs will be taken of
the samples and the ASTM grades will be find out to provide heat treatment to each of
the specimen and observe the changes occurring in each.

Materials
3 Engineering Department
NED University of Engineering And Technology

Acknowledgement
I take this opportunity to express my profound gratitude and deep regards to my guide
Engr. S.M.Mohsin Jaffri and Engr. Humair Ahmed for his exemplary guidance,
monitoring and constant encouragement throughout the course of this thesis. The
blessing, help and guidance given by him time to time shall carry me a long way in
the journey of life on which I am about to embark.
I also take this opportunity to express a deep sense of gratitude to all the staff
members

especially

Mr.

Zahid,

Mr.

Imran

Mr.

Salam

and

Mr.

Kamran for their cordial support, valuable information and guidance, which helped
me in completing this task through various stages. I am grateful for their cooperation
during the period of my project.
Lastly, I thank almighty Allah, my parents, and friends for their constant
encouragement without which this project would not be possible.

Materials
4 Engineering Department
NED University of Engineering And Technology

Table of Contents
CHAPTER 1: INTRODUCTION..................................................................................6
1.1 IMPORTANCE OF MATERIAL CHARACTERIZATION.................................6
1.3 PICTORIAL VIEW OF PARTS........................................................................7
CHAPTER 2: LITERATURE REVIEW..............................................................10
2.1 METALLOGRAPHY AND SAMPLE PREPARATION...............................10
2.1.1 SECTIONING:............................................................................................10
2.1.2 MOUNTING:...............................................................................................11
2.1.3 GRINDING:.................................................................................................12
2.1.4 POLISHING:...............................................................................................13
2.1.5 ETCHING:...................................................................................................15
2.1.6 DRYING:.....................................................................................................16
2.1.7 MICROSCOPIC EXAMINATION:............................................................17
2.1.8 X-RAY FLUORESCENCE:........................................................................17
2.1.9 HARDNESS:...............................................................................................18
2.1.10 HEAT TREATMENT.................................................................................23
CHAPTER 3: EXPERIMENTAL WORK...................................................................25
3.1 Sample 1:............................................................................................................25
3.1.1 PHASE DIAGRAM FOR ALUMINIUM...................................................25
3.1.2 X-Ray Fluorescence (XRF) Result:.............................................................25
3.1.3 STUDY OF AS RECEIVED SAMPLE:......................................................25
3.2 Sample: 2............................................................................................................28
3.2.1 PHASE DIAGRAM OF STEEL..................................................................29
3.2.2 X-RAY FLUOROSCENCE (XRF) Result:.................................................29
3.2.3 STUDY OF AS RECEIVED SAMPLE:......................................................29
CHAPTER 4: RESULTS AND DISCUSSIONS.........................................................33
CHAPTER 5: CONCLUSION.....................................................................................34
5.1 REFERENCES:..................................................................................................35

CHAPTER 1: INTRODUCTION
Materials
5 Engineering Department
NED University of Engineering And Technology

This semester takes the student through the metallographic sample preparation
process step-by-step with demonstrations and explanations of sectioning, mounting,
course & fine grinding, polishing, etching and microscopic examination.

1.1 IMPORTANCE OF MATERIAL CHARACTERIZATION

The goal of material characterization is to identify and quantify the physical and
chemical constituents of a material. This concept is laid out in sections 4.1 and 4.2 of
ISO 10993-1: "In the selection of materials to be used in device manufacture, the first
consideration should be fitness for purpose having regard to the characteristics and
properties of the material, which includes chemical, toxicological, physical, electrical,
morphological and mechanical properties.
The
definition
selected
for
the
ASM-International Materials
Characterization Handbook is as follows: "Characterization describes those features
of composition and structure (including defects) of a material that are significant for a
particular preparation, study of properties, or use, and suffice for reproduction of the
material."
The characterization Techniques provide information about composition, structure,
and defects and excludes those methods that yield information primarily related to
materials properties, such as thermal, electrical, and mechanical properties.

1.2

TECHNIQUES

INVOLVED

IN

MATERIAL

CHARACTERIZATION:
Characterization, when used in materials science, refers to the use
of external techniques to probe into the internal structure and
properties of a material. Analysis techniques are used simply to
magnify the specimen, to visualize its internal structure, and to gain
knowledge as to the distribution of elements within the specimen
and their interactions.
Magnification and internal visualization are normally done in a type
of microscope, such as:
o Optical Microscope
o Scanning Electron Microscope (SEM)
o Transmission Electron Microscope (TEM)
o Field Ion Microscope (FIM)
o Scanning Tunneling Microscope (STM)
o Atomic Force Microscope (AFM)
o X-ray diffraction topography (XRT)
1.3 PICTORIAL VIEW OF PARTS
Materials
6 Engineering Department
NED University of Engineering And Technology

+1.3.1 PART 1:

Figure 1: tank water ball rod

1.3.2 PART 2: pipe steering head:

Figure 2: pipe steering head

1.3.1.1 CALIBERATION VIEW OF BOTH PARTS:

Materials
7 Engineering Department
NED University of Engineering And Technology

Figure 1 & 2: Length and diameter of

the tank water ball rod

Figure 3 & 4: Length and diameter of the pipe steering head

CHAPTER 2: LITERATURE REVIEW

Materials
8 Engineering Department
NED University of Engineering And Technology

2.1 METALLOGRAPHY AND SAMPLE PREPARATION

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
Following are the steps followed in metallography for the sample preparation.

Sectioning
Mounting
Grinding
Polishing
Etching
Drying

2.1.1 SECTIONING:
Operations such as shearing produce severe cold work, which can alter the
microstructure of a sample. Abrasive cutting (sectioning) offers the best solution to
eliminate these undesirable features; the resultant surface is smooth, and the
sectioning task is quickly accomplished. Abrasive Cut-Off Wheels consist of abrasive
grains (such as Aluminum Oxide or Silicon Carbide), bonded together with rubber or
other materials in the form of a thin wheel. During the sectioning process, coolant is
being supplied continuously which flows readily to both cool and clean the cutting
area. An experienced operator can tell whether the wheel is cutting or merely
"dragging" by the feel of the control arm and monitoring of the power consumption of
the cutting equipment.

Materials
9 Engineering Department
NED University of Engineering And Technology

10

Figure 3: Abrasive cut off machine

2.1.2

MOUNTING:

Small samples are generally mounted in plastic for convenience in handling and to
protect the edges of the specimen being prepared. Compression-type molding is
commonly applied to encase specimens in 1 to 1.5inch diameter plugs of a hard
polymer. Compression molding materials are classified as either thermosetting or
thermoplastic:
1) Bakelite is a low cost, relatively hard thermosetting polymer that is commonly
utilized.
2) Expensive Trans optic Thermoplastics are utilized when transparency is required.

Figure 4: Hot mounting machine

By definition, thermosetting materials require heat and pressure during the molding
cycle. During mounting, the pressure and molding temperature are generally held
Materials
10 Engineering Department
NED University of Engineering And Technology

11

constant thus time is the only variable. The metal sample is placed in the mounting
cylinder which is then encased in a pre-measured amount of powdered polymers. The
mounting cylinder is then sealed, pressurized and heated to complete the
polymerization process necessary to solidly encase the metal sample.

Figure 5: Cold Mounted samples

2.1.3 GRINDING:
2.1.3.1 Coarse Grinding
In view of the perfection required in an ideally prepared metallographic sample, it is
essential that each preparation stage be carefully performed. The specimen must:
1. Be free from scratches, stains and others imperfections which tend to mark the
surface.
2. Retain non-metallic inclusions.
3. Reveal no evidence of chipping due to brittle intermetallic compounds and phases.
4. be free from all traces of disturbed metal.
The purpose of the coarse grinding stage is to generate the initial flat surface
necessary for the sub sequent grinding and polishing steps. As a result of sectioning
and grinding, the material may get cold worked to a considerable depth with a
resultant transition zone of deformed material between the surface and the undistorted
metal.
Course grinding can be accomplished either wet or dry using 80 to 180 grit
electrically powered disks or belts, but care must be taken to avoid significant heating
of the sample. The final objective is to obtain a flat surface free from all previous tool
marks and cold working due to specimen cutting. An important factor throughout the
Coarse Grinding and Fine Grinding Stages is that the scratches be uniform in size and
parallel to each other in any one grinding stage. Proper grinding involves rotation of
Materials
11 Engineering Department
NED University of Engineering And Technology

12

the sample by 90 between stages while the grinding angle must be held constant
during the grinding at any one stage. The sample MUST be washed thoroughly before
proceeding from one grinding stage to the next. Failure to follow this rule will result
in transferring abrasive particles between stages and will cause time consuming,
frustrating problems in removing unwanted scratches

Figure 6: Mechanical Grinding machine

2.1.3.2 Medium and Fine Grinding

Medium and Fine Grinding of metallurgical samples are closely allied with the Coarse
Grinding which precedes them. Each stage of metallographic sample preparation must
be carefully performed; the entire process is designed to produce a scratch free
surface by employing a series of successively finer abrasives. Failure to be careful in
any stage will result in an unsatisfactory sample. The idea is to carefully move from
one stage to the next where the abrasives become finer at each successive stage.
Movement from one stage to the next should only proceed when all of the scratches
from the preceding stage are completely removed. In general, successive steps are
240, 320, 400 and 600 grit SiC and the grinding rate should steadily decrease from
one stage to the next. Proper grinding involves the rotation of the sample between
stages while the grinding angle must be held constant during the grinding at any on
stage.
2.1.4 POLISHING:
Polishing involves the use of abrasives, suspended in a water solution, on a clothcovered electrically powered wheel. Diamond abrasives provide the best, and most
expensive, compounds utilized in polishing; standard sized aluminum oxide powders
are applied for general use purposes. Following the final 600 grit fine-grinding stage,
the sample MUST be washed and carefully dried before proceeding to the first
polishing stage. At the polishing stages, even hard dust particles in the air which
settles on the polishing cloth can cause unwanted scratching of the specimen! Careful

Materials
12 Engineering Department
NED University of Engineering And Technology

13

washing of the specimen and the operator's hands must be carried out prior to each
stage of polishing.
Beginning with 25-micron suspended aluminum oxide particles (suspended in water)
on a Nylon-cloth, the final fine-grinding surface layer resulting from the previous
grinding procedure should be completely removed with a rotation rate of 150-200
rpm. The specimen is initially held at one position on the wheel, without rotation,
until most of the previous grinding marks are removed. It can be rotated slowly,
counter to the wheel rotation, until only scratches from the 25-micron aluminum
oxide are visible. During the initial polishing stage, moderate pressure can be applied
to the specimen and the entire stage should generally take 1 or 2 minutes.
After carefully washing the specimen, proceed to the 5-micron stage where a separate
polishing wheel with 5-micron particles; repeat the procedure outlined above using
lighter pressure and a gradual rotating motion across the polishing cloth. The final
polishing stage with 1-micron suspended aluminum oxide particles should be carried
out on a separate polishing wheel following "Careful washing of the specimen and
operator's hands" at a slower speed of 100 - 150 rpm using a napped cloth.

Figure 7: Diamond polishing machine

After 1 or 2 minutes a properly polished specimen should have a mirror-like surface

free of scratches! During final polishing, minimal pressure should be applied and time
should be kept to a minimum since the napped material will conform to the specimen
shape under pressure. The wetness of the cloth used for Final Polishing has a great
influence on the end result. If the cloth is too wet the sample will show pits; if too dry,
buffing and/or smearing will result.
The following general flow sheet is included for the various stages of sample
preparation.
Materials
13 Engineering Department
NED University of Engineering And Technology

14

2.1.5 ETCHING:
Microscopic examination of a properly polished, unetched specimen will reveal only a
few structural features such as inclusions and cracks or other physical imperfections.
Etching is used to highlight, and sometimes identify, microstructural features or
phases present. Even in a carefully prepared sample, a surface layer of disturbed
metal, resulting from the final polishing stage, is always present and must be
removed. Etchants are usually dilute acid or dilute alkalis in a water, alcohol or some
other solvent. Etching occurs when the acid or base is placed on the specimen surface
because of the difference in rate of attack of the various phases present and their
orientation. The etching process is usually accomplished by merely applying the
appropriate solution to the specimen surface for several seconds to several minutes.

Figure 8: Fume hood for etching of samples

2.1.5.1 Etchants:
Materials
14 Engineering Department
NED University of Engineering And Technology

15

2.1.6 DRYING:

Figure 9: Dryer used for drying etched samples

Drying of a surface after cleaning or etching is very important. The specimen must be
dried quickly to prevent staining or corrosion.
2.1.7 MICROSCOPIC EXAMINATION:

Materials
15 Engineering Department
NED University of Engineering And Technology

16

Initial microscopic viewing should be done utilizing a stereomicroscope, which

reveals a three-dimensional 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
(3) Flatness of field.

Figure 10: Optical microscope

2.1.8 X-RAY FLUORESCENCE:

Figure 13: XRF equipment

X-ray Fluorescence (XRF) and X-ray Diffraction (XRD) Analyzers provide

qualitative and quantitative material characterization for detection, identification,
analysis, quality control, process control, regulatory compliance, and screening, for
Materials
16 Engineering Department
NED University of Engineering And Technology

17

metals and alloys, mining and geology, scrap and recycling, environmental and
consumer safety, education and research, and general manufacturing.
2.1.8.1 Applications
X-Ray fluorescence is used in a wide range of applications, including

research in igneous, sedimentary, and metamorphic petrology

soil surveys

mining (e.g., measure

ng the grade of ore)

cement production

ceramic and glass manufacturing

metallurgy (e.g., quality control)

environmental studies (e.g., analyses of particulate matter on air filters)

petroleum industry (e.g., sulfur content of crude oils and petroleum products)

field analysis in geological and environmental studies (using portable, handheld XRF spectrometers)

X-Ray fluorescence is particularly well-suited for investigations that involve

bulk chemical analyses of major elements (Si, Ti, Al, Fe, Mn, Mg, Ca, Na, K,
P) in rock and sediment

bulk chemical analyses of trace elements (in abundances >1 ppm; Ba, Ce, Co,
Cr, Cu, Ga, La, Nb, Ni, Rb, Sc, Sr, Rh, U, V, Y, Zr, Zn) in rock and sediment detection limits for trace elements are typically on the order of a few parts per
million

X-ray fluorescence is limited to analysis of

relatively large samples, typically > 1 gram

materials that can be prepared in powder form and effectively homogenized

Materials
17 Engineering Department
NED University of Engineering And Technology

18

materials for which compositionally similar, well-characterized standards are

available

Materials containing high abundances of elements for which absorption and

fluorescence effects are reasonably well understood.

2.1.9 HARDNESS:
Indentation hardness tests such as Brinell, Rockwell, Vickers, Knoop, and
instrumented indentation are frequently used methods for determining hardness. The
basic concept utilized in all of these tests is that a set force is applied to an indenter in
order to determine the resistance of the material to penetration. If the material is hard,
a relatively small or shallow indentation will result, whereas if the material is soft, a
fairly large or deep indentation will result.
2.1.9.1 MEASURMENT OF HARDNESS:
Hardness is not a fundamental property of a material, yet hardness testing is
considered a useful quality-control tool. Many properties are predicted from hardness
values when combined with additional information such as alloy composition. The
following is a list of such properties: resistance to abrasives or wear, resistance to
plastic deformation, modulus of elasticity, yield strength, ductility, and fracture
toughness. Some of these properties, such as yield strength, have numerical
relationships with hardness values, whereas others such as fracture toughness are
based on observations of cracks surrounding the indentations.
2.1.9.1.1 ROCKWELL TESTING:

Figure 14: Rockwell hardness tester

Materials
18 Engineering Department
NED University of Engineering And Technology

19

The Rockwell hardness test method consists of indenting the test material with a
diamond cone or hardened steel ball indenter. The indenter is forced into the test
material under a preliminary minor load F0 usually 10 kgf. When equilibrium has
been reached, an indicating device, which follows the movements of the indenter and
so responds to changes in depth of penetration of the indenter is set to a datum
position. While the preliminary minor load is still applied an additional major load is
applied with resulting increase in penetration. When equilibrium has again been reach,
the additional major load is removed but the preliminary minor load is still
maintained. Removal of the additional major load allows a partial recovery, so
reducing the depth of penetration. The permanent increase in depth of penetration,
resulting from the application and removal of the additional major load is used to
calculate the Rockwell hardness number.
HR = E - e
F0 = preliminary minor load in kgf
F1 = additional major load in kgf
F = total load in kgf
e = permanent increase in depth of penetration due to major load F1 measured in units
of 0.002 mm
E = a constant depending on form of indenter: 100 units for diamond indenter, 130
units for steel ball indenter
HR = Rockwell hardness number
D = diameter of steel ball

Advantages of the Rockwell hardness method include the direct Rockwell hardness
number readout and rapid testing time. Disadvantages include many arbitrary nonrelated scales and possible effects from the specimen support anvil (try putting a
cigarette paper under a test block and take note of the effect on the hardness reading!
Vickers
and
Brinell
methods
don't
suffer
from
this
effect).
2.1.9.1.2 BRINELL TESTING:

Materials
19 Engineering Department
NED University of Engineering And Technology

20

Figure 15: Brinell hardness tester

The Brinell hardness test method consists of indenting the test material with a 10 mm
diameter hardened steel or carbide ball subjected to a load of 3000 kg. For softer
materials the load can be reduced to 1500 kg or 500 kg to avoid excessive indentation.
The full load is normally applied for 10 to 15 seconds in the case of iron and steel and
for at least 30 seconds in the case of other metals. The diameter of the indentation left
in the test material is measured with a low powered microscope. The Brinell harness
number is calculated by dividing the load applied by the surface area of the
indentation.

The diameter of the impression is the average of two readings at right angles and the
use of a Brinell hardness number table can simplify the determination of the Brinell
hardness. A well structure Brinell hardness number reveals the test conditions, and
looks like this, "75 HB 10/500/30" which means that a Brinell Hardness of 75 was
obtained using a 10mm diameter hardened steel with a 500 kilogram load applied for
a period of 30 seconds. On tests of extremely hard metals a tungsten carbide ball is
substituted for the steel ball. Compared to the other hardness test methods, the Brinell
ball makes the deepest and widest indentation, so the test averages the hardness over a
wider amount of material, which will more accurately account for multiple grain
structures and any irregularities in the uniformity of the material. This method is the
best for achieving the bulk or macro-hardness of a material, particularly those
materials with heterogeneous structures.
2.1.9.1.3 VICKER TESTING:

Materials
20 Engineering Department
NED University of Engineering And Technology

21

Figure 16: Vicker hardness tester

The Vickers hardness test method consists of indenting the test material with a
diamond indenter, in the form of a right pyramid with a square base and an angle of
136 degrees between opposite faces subjected to a load of 1 to 100 kgf. The full load
is normally applied for 10 to 15 seconds. The two diagonals of the indentation left in
the surface of the material after removal of the load are measured using a microscope
and their average calculated. The area of the sloping surface of the indentation is
calculated. The Vickers hardness is the quotient obtained by dividing the kgf load by
the square mm area of indentation.

F= Load in kgf
d = Arithmetic mean of the two diagonals, d1 and d2 in mm
HV = Vickers hardness

Materials
21 Engineering Department
NED University of Engineering And Technology

22

When the mean diagonal of the indentation has been determined the Vickers hardness
may be calculated from the formula, but is more convenient to use conversion tables.
The Vickers hardness should be reported like 800 HV/10, which means a Vickers
hardness of 800, was obtained using a 10 kgf force. Several different loading settings
give practically identical hardness numbers on uniform material, which is much better
than the arbitrary changing of scale with the other hardness testing methods. The
advantages of the Vickers hardness test are that extremely accurate readings can be
taken, and just one type of indenter is used for all types of metals and surface
treatments. Although thoroughly adaptable and very precise for testing the softest and
hardest of materials, under varying loads, the Vickers machine is a floor standing unit
that is more expensive than the Brinell or Rockwell machines.

2.1.10 HEAT TREATMENT:

Heat treatment involves the use of heating or chilling, normally to extreme
temperatures, to achieve a desired result such as hardening or softening of a material.
Heat Treatment is often associated with increasing the strength of material, but it can
also be used to alter certain manufacturability objectives such as improve machining,
improve formability, and restore ductility after a cold working operation. Thus it is a
very enabling manufacturing process that can not only help other manufacturing
process, but can also improve product performance by increasing strength or other
desirable characteristics.
2.1.10.1 STRESS RELIEVING (post weld heat treatment)
This is by far the most frequently used form of heat treatment which will confront the
authorized inspector. As a result of welding processes used to join metals together, the
base materials near the weldment, the deposited weld metal and, in particular, the heat
affected zones transform through various metallurgical phases. Depending upon the
chemistry of the metals in these areas, hardening occurs in various degrees, dependent
mainly upon carbon content. Again, this is particularly true in the heat affected zone
(HAZ) adjacent to the weld metal deposit where the highest stresses due to melting
and solidification result. Stress relieving, as the name implies, is designed to relieve a
proportion of these imposed stresses by reducing the hardness and increasing ductility,
thus reducing danger of cracking in the vessel weldments.
2.1.10.2 QUENCHING AND TEMPERING
Oriented toward carbide steels such as carbon-moly, this process is designed to
enhance toughness as well as controlling yield strength and ultimate tensile strength
of steel. The steel is heated to above its upper critical temperature and quickly
immersed in fresh water or brine to achieve rapid setting of the desired metallurgical
structure. Oil quenching is sometimes used. The usual practice is to quench until
cooling reaches around 800oF, quickly followed by a tempering period in a fired
Materials
22 Engineering Department
NED University of Engineering And Technology

23

furnace in order to soften the martensitic structure and achieve the desired mechanical
properties in the material including a desired measure of ductility. The tempering
process is, in effort, a stress relieving process.
2.1.10.3 NORMALIZING AND TEMPERING
This process is used for virtually the same purposes as quenching and tempering. It
differs in that normalizing is accomplished by cooling in air in place of fast quenching
in a liquid. Air normalizing, much slower than liquid quenching, may be used by itself
or the material may be subjected to a controlled furnace tempering process in order to
better control desired mechanical properties.
Steel manufacturers will furnish material in either of the above conditions when so
specified on the purchase order or as required by the material specification.
As a cautionary note; alloyed steel mechanical properties are ultimately determined
by the tempering process and if the materials are subsequently welded during
fabrication, subsequent stress relieving temperature, if used, should not exceed that of
the tempering process, otherwise mechanical properties of the material may be
adversely affected.
2.1.10.4 SOLUTION HEAT TREATMENT (solution annealing)
While the Code sections state that heat treatment of austenitic stainless steel (P-8) is
neither required nor prohibited, this refers to post weld stress relieving. There are
certain processes to which this material may be subjected. These are performed almost
exclusively by the material manufacturers due to the fact that temperature ranges and
holding time are critical and require careful controls, otherwise damage to the
material can result from either too high or too low a furnace temperature. Material
manufacturers have the metallurgical staffs to determine requirements.
In solution heat treatment the material is subjected to a high heat, around 2000oF, and
rapidly cooled in liquid in order to achieve an evenly distributed solution of carbon
and austenite in the metallurgical structure of the material.
2.1.10.5 STABILIZING HEAT TREATMENT
Everything said in the first paragraph under solution heat treatment also applies to
stabilizing heat treatment. In the latter process the material is cooled slowly in order
to bring as much carbon as possible out of solution and into evenly distributed
concentrations apart from the austenite.
Both solution heat treatment and stabilizing heat treatment are used to reduce
susceptibility to intergranular stress corrosion and embrittlement also to increase high
temperature creep strength.

Materials
23 Engineering Department
NED University of Engineering And Technology

24

CHAPTER 3: EXPERIMENTAL WORK

3.1 Sample 1:
This project deals with the study of brass, its microstructure and hardness of as
received sample as well as heat treated samples including normalizing, annealing,
quenching and tempering of the samples. It is a heat treatable alloy with good
corrosion resistance and high strength.

3.1.2 PHASE DIAGRAM FOR BRASS

Materials
24 Engineering Department
NED University of Engineering And Technology

25

Component: Rod of tank ball

Material: Brass
Grade: C35350
X-Ray Fluorescence (XRF) Result:
Zn

Pb

Ni

Fe

Cu

35.38 0.24

4.21 0.16

0.73 0.04

0.74 0.04

59.96

3.1.3 STUDY OF AS RECEIVED SAMPLE:

3.1.3.1 Metallographic Sample Preparation:
Grinding at 180, 220, 400 & 600 grit SiC paper.
Polishing at 5, 1 & 0.05 micron.

3.1.3.2 HARDNESS:
Hardness Type

Result

Rockwell hardness testing

72,71,72 (HRC)

3.1.3.3 POST HEAT TREATMENT HARDNESS:

TYPE OF TREATMENT

RESULTS

WATER QUENCHED

72,73,73 HRB

TEMPERED

68,72,71 HRB

NORMALIZED

72,72,70 HRB

3.1.3.4 HEAT TREATMENT CYCLES

Materials
25 Engineering Department
NED University of Engineering And Technology

26

500
450
400
350
300

quenching

250

tempering

200

normalizing

150

annealing

100
50
0
10 min

20 min

30 min

40 min

50 min

60 min

70 min

SCALE:
X axis: Time (minutes)
Y axis: Temperature (centigrade)

3.1.3.5 MICROSTRUCTURE OF AS RECEIVED BRASS SAMPLE:

Figure 17: As received structure of brass at 400x

Materials
26 Engineering Department
NED University of Engineering And Technology

27

3.1.3.6 POST HEAT TREATMENT MICROSTRUCTURES:

Figure 18: Normalized structure of brass

Figure 19: Water quenched structure of brass

Materials
27 Engineering Department
NED University of Engineering And Technology

28

Figure 20: tempered structure of brass

3.1 Sample 2:
The second sample is characterized to be 1050 steel 1050 is a medium carbon,
medium tensile steel with good strength, toughness and wear resistance. This grade of
steel is used for the manufacture of forged shafts and gears and for a wide range of
applications that can make use of its good combination of mechanical properties. And
use 2% nital as an etchant for this steel.

3.2.1 PHASE DIAGRAM OF STEEL:

Materials
28 Engineering Department
NED University of Engineering And Technology

29

Component: pipe steering head

Material: Steel
Grade: AISI 1050

3.2.2 X-RAY FLUOROSCENCE (XRF) Result:

Fe

Mn

94.46-98.92

0.60-0.90

0.470-0.55

0.050

0.040

3.2.3 STUDY OF AS RECEIVED SAMPLE:

3.2.3.1Metallographic Sample Preparation:
Grinding at 180, 220, 400 & 600 grit SiC paper.
Polishing at 5, 1 & 0.05 micron.
3.2.3.2 HARDNESS
Hardness Type

Result

Rockwell hardness testing

78,79,78 (HRB)

Materials
29 Engineering Department
NED University of Engineering And Technology

30

3.2.3.3 HARDNESS POST HEAT TREATMENT:

TYPE OF TREATMENT

RESULTS

WATER QUENCHED

82,82,82 HRB

ANNEALED

43,42,42 HRC

NORMALIZED

72,72,73 HRB

3.2.3.4 HEAT TREATMENT CYCLES:

900
800
700
600
500
400
300

annealing

quenching

normalizing

200
100
0

3.2.3.5 MICROSTRUCTURE OF AS RECEIVED SAMPLE:

Materials
30 Engineering Department
NED University of Engineering And Technology

31

Figure 21: As received structure of steel

3.2.3.6 POST HEAT TREATMENT MICROSTRUCTURES:

Figure 22: Water quenched structure of steel

Materials
31 Engineering Department
NED University of Engineering And Technology

32

Figure 23: Annealed structure of steel

Figure 24: Normalized structure of steel

Materials
32 Engineering Department
NED University of Engineering And Technology

33

CHAPTER 4: RESULTS AND DISCUSSIONS

The data which was collected during the experimental work elaborates clearly the
steps for reverse engineering and the effect of heat treatment on microstructure and
hardness. First consider the 1050 steel sample, it was seen that the as received
structure of steel was normalized after heat treatment it was transformed to different
microstructure comparing to the initial one. Quench treatment made martensitic
structure because C in brass didnt get appropriate time to escape from the structure
and got trapped in microstructure due to fast cooling rate but with a little grain
growth. Normalize treatment made the grains to grow more compared to quench
sample because of moderate cooling. Annealing treatment releases all the stresses
from the sample and the grain growth is maximum in this treatment because of very
slow cooling rate. Also the hardness gives the same response as the grains react on
heat treatment. The hardness of water quenched sample is maximum, than as received
simple, than normalized, and minimum hardness was obtained from the annealed
sample all effect is due to the holding time and cooling rate. As the quenched sample
has the fastest cooling rate, so it should give the structure more distorted which yields
maximum hardness among all heat treated samples and the minimum hardness of
annealed sample due to furnace cooling cools very slowly so C in it gets a lot of time
to relax them. The same reason is for all the heat treated samples.
Now, consider steel, the results of steel samples were in contrast with respect to
quenched and normalized samples of brass. As received structure of brass has coarse
grains because it didnt cold treated. Quenching does not affect highly on the sample
and the results have very less difference both in microstructure and in hardness.
Normalizing treatment has strong effect; it gives maximum hardness, and more
complex structure comparing to all although the cooling rate is moderate. Annealing
treatment gives long grains with low hardness valves. Annealing with long soaking
time gives the minimum hardness and the grain growth is maximum due to extreme
holding time, which gives maximum time to grow grains. Since, the grain growth is
maximum so the hardness reduces very suitably as according to the phenomena.
So, this result can be taken from the whole project that by given inadequate holding
time (greater than its thickness requirement) hardness of the sample decreases very
effectively. Therefore, hardness has inverse relation with grain size.

Materials
33 Engineering Department
NED University of Engineering And Technology

34

CHAPTER 5: CONCLUSION
MCTP material characterization technique project base on reverse engineering. In
which we compare the microstructure of different heat treated simples like annealed,
quenched, tempered, normalized etc. with the as received simple of heat treated
simples and then decided why the manufacturer want this structure of the material in
working environment. And Materials characterization techniques project helps a lot in
understanding the methodology of reverse engineering and fracture analysis. The
phenomena of heat treatment are well elaborated during the whole literature survey
and experimental works concerning the heat treatment processes. Moreover, the heat
treatment can be noticeably put its effects on the hardness property of the materials.
By some little variations in the manufacturing or post manufacturing process, anyone
may get the desired output from the materials. Also the effect of alloying elements is
well understood in this project. The effect of holding time was seen clearly. Hence,
this project at this level is unsurpassed practice for engineering students to learn
effectively.

5.1 REFERENCES:
1. (2011, 11). Metallography. StudyMode.com. Retrieved 11, 2011, from
http://www.studymode.com/essays/Metallography-824588.html
2. Material Science and Engineering- An introduction by W. D. Callister
3. ASM Handbook, Metallography and Techniques
4.

Materials
34 Engineering Department
NED University of Engineering And Technology