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0% found this document useful (0 votes)
25 views13 pagesLab 7
Uploaded by
Tilak SharmaCopyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
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/ 13
la
|
—EE lL
Experiment No. 7
7.1. Objectives: To study optical microscope, practising microstructure examination procedure
of standard specimens, and performing its microstructural examination or metallography.
7.2. Material and Equipment: (1) Cutting tools like hacksaw, diamond and abrasive
sectioning saws, cut-off wheels, abrasive cutter, cutting coolant, coarse and fine files, (2)
Abrasive paper or emery paper of different grids like 100, 220, 320, 400, 600, $00, ..., 2000
mesh sizes, (3) Disc polisher, (4) Optical Microscope, (5) Material specimen of standard sizes
(say 50 mm x 50 mm x 5 mm), (6) Acetone, (7) Cotton cloth, (8) thermoplastic or thermosetting
polymer disc like epoxy polymer mould, (9) Marker
73. Theory:
‘Metallography is the study of metals and their behaviour with particular reference to their
microstructure (Microstructure is the characteristic appearance and physical arrangement of
metal molecules as observed with a microscope) and macrostructure (Macrostructure is the
appearance and physical arrangement as observed with the naked eye). The credit for these
studies goes to Alloys Beck Von Widmanstatten (1808 - 1840). The microscope was employed
for this purpose in 1841 when Paul Annosow used it to examine the etched surfaces of oriental
steel blades. It was around 1890 when the metallographic technique received general
recognition, largely as a result of the work of Professor Henry C. Sorby in England. We must
know about the Optical microscope and Specimen preparation procedure to understand the
exercise.
‘A microscope is an essential scientific instrument that has revolutionized our
‘understanding of the microscopic world, It allows us to magnify objects and organisms that are
too small to be seen with the naked eye, revealing intricate details and structures that are
“otherwise hidden from view. Microscopes have played a crucial role in various fields of seience,
including biology, chemistry, physics, material science, and medicine, by enabling researchers to
explore and analyze the microcosmos in great detail.
Historical Background: The development of the microscope has a rich history dating back to the
ate 16" century. The Dutch inventor Zacharias Janssen is often credited with creating one of the
earliest compound microscopes around 1595, This early microscope consisted of a simple
arrangement of lenses that could magnify objects several times their actual size, However, a
an Leeuwenhoek, made significant advancements in microscopy
Dutch scientist, Antonie vi
during the 17th century, Leeuwenhoek’s meticulously erafted single-lens microscopes allowed
him to observe and document @ myriad of microorganisms, laying the foundation for
microbiology.
Page 7.1 of 13 ec Tosa te
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‘ign the requited objects
Produces ist
hong el een tage sin
‘one dbe bral mnt
Condenser: Condes tei
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through th tage apo
Kr For vertical movement
‘eondonet
aioe (ght Ere Recep
‘through the substage condense 2
sage opera cia beeen”
ope ogi 330
tinea back
Figure 7.1 Optical microscope
1s of an Optical Microscope: Optical microscopes consist of the following essential
‘Components of an Optical Microscope:
components:
1. Objective Lens: This is the primary lens closest fo the specimen. It gathers light and
‘magnifies the sample, producing the initial image.
2. Eyepiece (Ocular): The eyepiece lens further magnifies the image created by the objective
lens and allows the observer to view it.
3. Illumination Source: A light source (often an adjustable lamp) is used to illuminate the
specimen, making it visible,
4 Stage: The stage is where the specimen is placed for observation. It may have mechanical
controls forthe precise movement ofthe specimen,
$.
Focus Mechanism: i i
be Oiliel aleracsp esate ost eeatiatn, which can be coon
snd ine edjstnents to bg th ecient shar foes
© Condenser: The condenser lens focuses a
I sant cnn nd direets light onto the specimen, enhanciné
Tepes Of Microscopes: Over the
specialized instruments, each ge
of microscopes include:
centuries,
microscope ‘ :
signed for gp Pes have evolved into various types 24
cif
'© Purposes, Some of the most common typ
A i bs
Optical Microscope: This isthe ‘Most fami
and a series of lenses 19 magnif iliar type of mi
ope, Which uses visible lig!
biology,
sed it
materials :
ence, and scopes are widely U 2. Electron Microscope: &
tron microscopes use a beam of electrons instead of visible
Hight to achieve much higher magnification and resolution. Transmission Electron
Microscopes (TEM) and Scanning Electron Microscopes (SEM) are two common types
of electron microscopes used for detailed imaging at the nanoscale
3. Confocal Microscope: Confocal microscopes use @ focused laser beam and a pinhole to
eliminate out-of-focus light, resulting in high-resolution three-dimensional images. They
are commonly used in cell biology and neuroscience.
4. Fluorescence Microscope: These microscopes are equipped with specialized filters and
light sources to visualize fluorescently labelled samples. They are invaluable in cell
biology and molecular biology for studying biomolecules and cellular structures
s
Phase-Contrast Microscope: Phase-contrast microscopy enhances the contrast of
transparent and colourless specimens, making it useful for observing living cells and
delicate structures.
6. Scanning Tunneling Microscope (STM) and Atomic Force Microscope (AFM): These
scanning probe microscopes can image surfaces at the atomic and molecular scale. They
are widely used in nanotechnology and materials science.
Applications of Microscopes: Microscopes have a wide range of applications, including
1. Biology: Microscopes are fundamental tools for studying cells, tissues, and
microorganisms, contributing to our understanding of genetics, microbiology, and
pathology.
2. Materials Science: Microscopy is used to investigate the structure and properties of
materials, aiding in the development of new materials and quality control.
3. Medicin
‘blood, tissues, and pathogens.
4, Nanotechnology: Microscopes play a vital role in nanoscale research and manipulating
individual atoms and molecules.
: Microscopes are indispensable in clinical diagnostics, allowing for examining
5, Environmental Science: Microscopes help analyze environmental samples, such as soil
‘and water, for the presence of microorganisms and pollutants.
Optical microscopes are of signi \¢ several reasons
1. Visualization of Microstructure: Optical microscopes allow researchers to observe and
study the microstructure of materials, This includes the arrangement of grains, crystalline
structures, defects, and phase boundaries in materials, Understanding the microstructure is
crucial for determining material properties and performance, :
2, Quality Control: In industries that prod > materials or components, optical microscopes
are used for quality control, Manu can inspect materials for defects, surface auots meet specific standar the
g that pror ,
«, ensuring a
consist’ :
rections, and ine goncie .
imperfections: ..
satal in particle size analy, es
specications + meroaeopes ate instrume’ p lysis, By
sins Opt! MT arial, researchers can deten i of
3. Particle Size Analyst Opt ' ae wail materi i ae 4 :
cand stare is like pharmaceuticals, cos, ;
reaming tees AMPS NT jal i Tadic ota Hie
os, which 18 ¢
jicle Sizes.
distribution of part
and powder metallurgy’ sas tito experience unexpected behaviour, opie,
rials :
«gingers and scientists can examine
4, Failure Anal
microscopes es of failure, whether it is die iy
fractured surfaces 3
manufacturing defects,
5, Identification of Phase
such as poly
the root call
factors,
sopy oan ep identify different phases witin g
nerial, mers, alloys, This is important for
material, :
understanding the composition and behaviour of
6. Grain Size Measurement: Grain siZ° plays a cruci
al microscopes are used t
is, especially in metals. Optic
jal strength, ductility, and other mechanical
‘al role in determining material
1 measure and analyze
properts 2
rain sizes, aiding in the assessment of mater
properties.
7. Surface Roughness Analysis: O
in fields like engineering and mam
rica microscopes are used to quantify surface roughness
facturing. Accurate measurements of surface
roughness are essential for optimizing the performance and durability of componens
8. Corrosion Analysis: Understanding the effects of corrosion on materials is vital im
industries such as construction, automotive, and aerospace. Optical microscopes can P®
employed to examine the extent and type of corrosion damage on material surfae
9. Research and Development: Researchers use optical microscopes to explore ne s
materials and test hypotheses related to their properties and behaviour. Opttl
microscopy serves as a fundamental tool for advancing material science and innovation
10. Educational Purposes: Educational institutions widely use optical microscopes ©
students about material science, microscopy techni et
iques, and the microscopic world
provide hands-on experience and promote scientific curiosi
riosity.
While advanced technique: e
echniques like eleetton microscopy (eg, SEM and TEM) offer néY
resolution and specialized cay
‘abilities, optics microscopes remain essential due 10 thie"
ial du
use, cost-effectiveness, and the abi 3
ee ility to provide valuable insights into the microstruc” and
ide range of applications, They vol
material scientists and engineers, enabling them, . They serve as a foundation? 5
inthe field, ‘© make informed decisions and advance gample preparation: Proper preparat;
: ‘Per Preparation of metallogra
the accurate microstructure of a material booms esl caer
terial becau
principle of reflection of light from the
he spe
structure, Following are the necessary
Se the metallurgical microscope makes use of the
cimen surface to get the final image of the metal
steps involved
specimen: PS involved in the preparation of metallographic
Selecti eh: WI
lection of specimen: When investigating the properties of a metal or afl
‘operties of a metal or a
loy, the specimen
must be selected from that el
area (of the pl asin an be tal
rea (of the alloy plate or casting), which ¢ =
representative of the whole mass,
— ‘or Cutting of the specimen: After selecting a particular area in the whole mass,
the pee be cut with the help of appropriate cutting tools. It involves many types
and sizes of diamond and abrasive sectioning saws that ensure no alteration in
microstructure or damage fracture features while cutting the specimen. Low-speed cut-off
wheels are utilized in cases where the heat created by standard abrasive culters must be
avoided or to avoid cold working a material, We must ensure ample coolant (when
allowable) and proper speed controls during sectioning operations
Mounting the specimen: If the specimen is too small to be held in hand for further
processing, it should be mounted on a thermoplastic or thermosetting resin dise or some
other low melting point alloy. Mounting samples in plastic provides convenience in
handling and protecting the edges of the specimen being prepared during polishing
operations. Specimens are generally mounted in epoxy polymers (1 to 1-5 inch diameter
moulds, sce Figure 7.2). Mounting materials are typically cither thermosetting or
thermoplastic.
Edges of mounted samaie
Specimen ‘are rounded using oorse
Mount ae
f=
————>
3mm
ed in epoxy resin and hardener matrix
Figure 7.2 Sample mount
surface: It is necessary 19 obtain « reasonably flat surface on the
yy using @ fairly coarse file or machining or grinding. Coarse
Obtaining flat specimen
en. This is achieved b.
Bene 1 flat surfuce necessary for the subsequent grinding and
20
generates the init
Course grinding gan be aepomptished thar wot o* dry using 80 to
Mises Care must be taken 0 avoid sigiiant Heating oF the
‘on rotating: “
oan oat surtice {ree from tool marks due to cutting
ective is {0 obta
grinding
polishing step’
grit sandpaper
sample. The final obj
Page 7.5 of 13 5
6
8
9.
grinding is carrieg
and fine
ediate
er, Aner ea
fine grindine porters ge. Fine Brindle utilizes UP £0 1,209 poe
Intermediate and fine finer Bree series of Successive
i ae ty employing # 8° ! Vely fine
using emery papers © ve surface ;
atch free
proaace #87
particle size aboy
emery papet (0
mond powder (
abrasives. iy
quantity jon cloth-covered sur
tube is placed O” the ny!
very small
the cloth of the rot
Rough polishing: A
paste that is 0" Gi
1, The spec
and is moved a
sure a more uniform 80
4 alumina (AlZOs) powder placed on 5
is used as a lubricant. Fine polishing
essed
imen is presse
round the
ion (see Figure 7.3).
microns) carried 19 #
ofa totating polishing WHEE
nsiderable pre
hneel in the direction opposi
ne
whee! with co!
ion of the wheel to en
1g compound use
ate
to the rotati
Fine polishing: The polishin
loth covered rotating wheel: Distilled
ave ayers remaining from the rough polishing
removes fine scratches a hin distorted |
stage (see Figure 7.4).
the granular structure in a specimen
sity: Even aftr fine polishing
cause
best, and the resolving power of a
Etching and its neces
be seen under the microscope bec grain boundaries in metal have a
usually cannot
thickness of the order of a few atom diameters 2
scope is much too low to reveal their pres
the metal specimens are usually et
ence. In order to make the grain
micro
boundaries visible, tched after polishing. Etching
imparts unlike appearances to the metal constituents and thus makes metal structure
apparent under the microscope. Etching occurs when the acid or base placed on the
specimen preferentially attacks specific phases present. Nital (i.e. 3% Nital having 3 ce
See fa.
itric acid and 97 ce ethanol, with 30 sec. etching time) is an etchant commonly utilized
with irons and steels. An etchant having either ammonium hydroxide, nitric acid or ferric
chloride for brass and bronze alloys.
Method of etching: The
mes Be Polished specimen is thoroughly washed in running water before
After that (i) Immersing the polished 4
pe oy surface of the specimen in the etchine
7 lished surface ge ‘i
face gently with a cotton swab wetted with the
etching reagent. After et he washed th
gent. After etching, the g
the specimen can be studied Peclmen is again washed thoroughly and dried. Now
udied under the microscope. ws
ICopper specimen ground win
180 grit paper Figure 7.4 Double dise polishing m
chine
7.4. Procedure:
Cut the sample into suitable specimens for analysis, ensuring they represent the material
Mount the specimens in metallographic mounts using an appropriate adhesive
Grind the specimens using finer grit abrasive papers gradually to remove any surface
imperfections.
4. Polish the specimens using polishing compounds and a polishing machine until a mirror-
like finish is achieved.
Place the polished specimen on the microscope stage
Select the appropriate magnification and illumination for your analysis.
Focus on the microscope and observe the microstructure of the material
Document and photograph any features of interest, such as grain boundaries, phases, or
defects
9, Identify and describe any phases, grain sizes, inclusions, or defects present in the
material.
10. Analyze the data and conclude the materials characteristics and poten applications
75. Observations: The following microstructure is observed! during metallogeaphy
Page 7.7 of 13, _ Cementite
—— Ferrite
Pearlite Formation
‘Austenite
por austenite grain boundary
Lamellar structure AS: Alloy Steet
PCS: Phain-carton Steet
Austenite
Rectoat Tempered
Martensite
ce showing penetration afong the grain boundaries:
(a) Core
1 SEM images of 750°C
page 7.901 13, Graphite
G- ferrite
Ferritic gray iron
crostructure of grey cast iron
Microstructure of mild steel
Figure 7.5 Microstructure images
7.6. How to find out the average grain size or diameter (D)
To determine the average size of grain in a microstructure, We must have a clear image of the
microstructure, and the following steps need to be noted:
‘Seep 1: Draw a line of length Li mm that may pass 2s many grains as possible over the
iorostructure or optical microscope image:
‘Step 2: Count the number of intersection points this line made with grain boundaries (say Ni).
Step 3: Note the magnification of the microstructure.
Magnification (M) = ‘measured scale length (converted to-microns) é eo
err cmewacmateeas °° cxemele, 2 100 um scale tr
‘measures 16 mm in length (or 16,000 um). then M = “SESS = 160.
km
‘Step 4: The ine is of
eal length ofthe line sof “+ , and we can compute intercept length or mean gr=it
seas Dj mm = 7
‘Step 5: Repeat
es steps 1 t0 4 for various such test lines drawn in random directions (say 20 test
6: Find the m 4
= neun D mn = debt Dao)
raph and W0 determine Fp Tt can now be used in the Hall-Piteh equation oF
me ie dimes z
(© shouldbe ism), atv a ASTM grain sige number @
satlo N= ae where, N ae x
magnifleation, Ty obtain ihe nuinby a hoa wun: “gUAINS per square inch at 100X
where 4 16 the average onilimetre at 1X, multiply by 15:50. P ©
84
5
ral Wee =e
eoreaning, THe VabiW OF G Nainy wr lameten AS the G inereases, the D wil be
imicrontructure, "TNE relative
‘grain sizes among ‘ gestion Fk Lr = 350. mm, Ni = 58 grain bound:
an
yoy find the mea. intercept Length Dy
eet. _ 380
solution: since Dies Teoxgs = 0.0377 mm
=~ [6.6857 ¥ log D } =3.298 = — [6.6457
question 2: Find the mean grain size of
* log 0.0377]
y intersectio
Imlersection, and the magnification M
3.298 = 6.163
the following microstructures;
160 an 0.013
| o_o
5 160 [oot
| | oe 160 | 0011 |
| Pal 160 | 0014
=| 9a)
Exercise: Find the mean grain size of the following microstructures:
page 7.11 0f 13, alysis
a7. Analy 4nd conclusions: The
standard specimen are (write Salient observations
from the metallography
in yo)
Your own words, summarize t
- narize the findings of the
he experiment}
2
78. Precautions:
1, Always wear appro}
priate safety equi
'Y equipment, including lab coats, safety glasses, and
gloves.
2, Follow the safe
fety guidelines and protocols established by your institution.
3. Be cautious when handling chemicals and f
Is and follow the recommended safety procedures.
4, CLEANLINESS! K fata
I Keep the room and the work areas clean, especially the polishing
area, Each step i oe eee
ae p in the polishing process uses a finer grade of abrasive, so good results
require that both your sample and your hands are free from abrasive at each stage before
proceeding to the next stage of the process, Turn the power off and cover the wheels when
you are through. Clean up any spilled water and wipe up the countertop.
5. Throw away the leftover etchants into the sink with a liberal amount of water. Swabs
should be rinsed and thrown into the trash bin IMMEDIATELY AFTER USE. Wash your
containers with water, rinse in methanol, and place them on the shelf above the sink.
6. Use goggles and gloves while handling chemicals. Contact the T.A. or the Instructor in
etchants are needed. Be extra careful when using
in the lab. Wash your
the case of an acid spill, or if new
hydrofluoric acids, 4) Do not eat or drink anything while workin
hands thoroughly with soap before leaving the lab.
Some viva questions
1. Explain the importance of proper sample preperation in microstructural analysis
Barreto ee potentaliectier azecucs
