Microstructure Laboratory

#2
Group # 4
Jos A. Rojas Cordero

Course ??
Date the experiment was performed
Date the experiment was due
Professor Julio Noriegas, Phd

Introduction
The objective of this investigation is to train
the student on the techniques for
metallographic sample preparation.
The use of optical microscopes to examine the
structure of metals.
Brass and steel specimens will be mounted,
ground, polished, etched, and microscopically
examined.
The history and properties of the metal.
The ASTM specifications.
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Comparision Laboratories
Modern physical metallurgy 8th ed., R.E. SMALLMAN,
A.H.W. NGAN. Fundamentals of physical metallurgy,
and basic techniques of microstructure. (How can
we applicant metals properties).
Ancient Metals: Microstructure and Metallurgy
Vol.1; David A. Scott. 2011. Introduction of
metallographic and ancient metals.
Steel metallurgy: Properties, specifications, and
applications. S.K. Mandal. 2015. (Microstructure
origin, grains sizes, and properties, metals
types,heat tratements, weldings).
Your take
away goes here
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Theory
Using the Jeffries Planimetric Method, for counting the grains. The
number of grains per mm2 is computed using the equation:

M2
n2
N

A
Equation
1 1 2
5000
Where the variables are:
M is the magnification of the photographic image.
n1 is the number of grains completely in the inscribed area.
n2 is the number of grains intersecting the perimeter of the test area.

Equation 1.

Your take
away goes here
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EQUATIONS :

The Heyn-Intercept Method, estimating the average grain

size by counting (On a photomicrograph of a representative
field of the specimen) the number of grains intercepted by
one or more straight lines.
L = L / (M P)

Equation 2.

And the number of intercepts per unit length of test line

is computed using the equation:
NL = 1 / L
Where:
Equation 3.
L is the the mean intercept distance.
LC is the circumference length.
M is the magnification of the photographic
image.
P is the number of grains intersecting the
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perimeter of the testMEarea.
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EQUATIONS :
Euler Triple Point Method as with the Jeffries method, a
circle is drawn on the figure with a diameter of 79.79
mm. This defines an inscribed area of 5000 mm 2.
The value of NA is computed using the equation:

P / 2 1
NA
,
AT

(substitution of P for PY)

Where:
PY is the count of the number of grain boundary triple
points.
AT is the area of the inscribed area at 1X magnification.
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Equipment
For the Microstructure Experiment, the following will be
used.
Three different specimens will be analyzed, which included Brass
SAE 660, Steel 1018 and Steel 4140.
The specimens were grinded using sand paper of 240, 320, 400
and 600.
Polishing was performed using a bench polisher with three
microns Alumina (Al2O3) grid size, and using a polishing velvet
cloth.
The samples were analyzed using a light reflective microscope.
Samples were pictured using a metallographic computer interface.
Etched reagents Nital.

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EXPERIMENTAL PROCEDURES
Specimen Preparation

A specimen for metallographic examination is prepared to reveal its

metal structure. So its surface must be flat and free from scratches
resembling a mirror before etched.

Sampling

Specimen should be carefully selected for examination. Rolled shapes

should be examined on the longitudinal and transversal direction.
Sectioning is performed to remove a suitably sized sample for
subsequent mounting and polishing. Abrasive cutting should be used
whenever possible. Enough cooling should be provided during the
cutting process to avoid changing the structure of the specimen.
When samples must be removed from large parts by destructive
methods such as torches or hacksaws, the cuts should be made at a
reasonable distance from the area of interest. Subsequent cutting to
remove the damage areas should be performed with an abrasive cutter.
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EXPERIMENTAL PROCEDURES
5. After sectioning, samples must be mounted using
compression molding. Compression molding resins are
dry powders which cure at 3,000 to 4,200 psi pressure
and 150C temperature.
6. To mount a specimen using the Specimen Mount
Press, place sample face down upon polished surface of
Mold Base. Carefully lower Mold Cylinder upon Mold
Base (do not force). Pour approximately six to eight
grams of Molding Powder into Mold Cylinder.
7. Carefully lower Mold Ram, polished side down, into
Mold Cylinder. Transfer entire assembly to Insulating
Plate and apply the initial hydraulic pressure (100psi
approximately).
8. Active Heater at Cord Switch for about 20 minutes.
After that increase pressure to 4200psi. Switch off
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Youronto
take
away
goes here
current and lift Heater
Heater
Hook. Allow Mold 9
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EXPERIMENTAL PROCEDURES
Grinding
Any burrs on the edges of the specimen should be removed before
mounting by means of a coarse grinding paper or a file. After
mounting, rough grinding is carried out mechanically using 240 and
320 grit grinding papers.
The sample should be maintained cool, so open the grinder water
valve such that the specimen surface is dipped in water during
grinding.
The grinding operation should be done by a forward motion until only
scratches due to the particular paper can be seen to cover the surface.
When the coarser scratches appear uniform, the next grinding paper
should be used (specimens and hands should be washed with soap and
water before using the next paper).
When using the next paper, the specimen is rotated 90 degrees to
grind at right angles to the scratches formed by previous paper. After
rough grinding operation is finished, fine grinding is carried out
similarly using 400 and 600 grit grinding papers.
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Polishing
After grinding operation is finished, the
specimen is polished by holding it against a
horizontal wheel covered with a velvet cloth
containing Alumina (Al2O3) 3 microns grid
size as polishing media. During polishing the
velvet cloth is supplied with these particles
as an aqueous suspension at regular
intervals.
During this process the surface must attain,
such good polish, as to resemble a mirror.
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Etching

Among the methods of metallographic etching, we have the optical, chemical, and physical
etching. The purpose of this type of etching is to chemically attack the metal surface to bring
out its structure. This results from the different rate of attack of the chemical reagent on
grains that have different orientation, and on constituents present in multiphase materials.
Ferrous samples can be etched with Nital which is a solution of 2-5% nitric acid in alcohol.
Austenitic and stainless steel samples can be etched with ferric chloride solution containing
5g of FeCl in ml of hydrochloric acid and 100ml of water. Cooper and many of its alloys can
be etched with an ammonium solution containing 5 parts of ammonium hydroxide, 5 parts of
water, and 2-5 parts of hydrogen peroxide.
Before etching, the specimen should be thoroughly washed with water and dries with
alcohol.
The specimen, with its polished surface upwards, should be immersed in the etching
solution, contained in a small porcelain dish.
The specimen surface should be examined from time to time, and the specimen is removed
from the etchant when the grain structure is just visible to the unaided eye. The etching time
could range from a few seconds to one minute.
After etching, the specimen is thoroughly washed with water and then dried with alcohol.

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Microscopic Examination
Fix the specimen on a plane sheet
using mounting clay.
Level the etched surface with the aid
of a leveling device.
Place the specimen on the
microscope, and select the most
appropriate magnification to examine
the sample.
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Results
Draw the structure of the samples as watched in the
microscope, use Table 1.1 for this purpose. You could also
take photomicrographs using the Metallograph and 669
Polaroid film.
Describe the shape and distribution of the grains and
constituent phases, i.e. indicate the presence of ferrite,
fine pearlite, coarse pearlite, spheroidite, martensite, etc.
Measure the grain size and the area fraction of
constituent phases in each specimen as standardized by
the American Society for Testing and Materials (ASTM).
Based on the microstructure of the specimens, predict
their properties and relate to their history.

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RESULTS

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B. Specimen No: 2
Designation: Steel 1018
Condition: Polished and etched
sample
Etchant: Nital
Magnification: 40x
( red = shared grains, green =internal
grains)
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Figure 3. Steel 4041

Microstruture at 40X of
magnification.

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Using the Jeffries Planimetric Method:

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Discussion
Three samples of different materials were analyzed to
find their microstructure. The specimens consist in
Brass SAE660 alloy, Steel 1018 and Steel 4140. These
samples passed through the preparation process that
included sample preparation, polishing, and etching.
The Brass SAE 660 alloy sample was etched using
Ammonium Hydroxide. The sample was then analyzed
under the microscope and the grains revealed. The
magnification used was of 40x. The sample was
analyzed to obtain the micro grain size using
Planimetric (or Jeffries) Method. The ATSM micro grain
size obtained by this method was 1.07. With the
number of grains per square millimeter are of .
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The second specimen analyzed was the Steel 1018. After the specimen
was carefully polished and etched with Nital, it was analyzed under the
microscope using a 40x magnification. For this sample the Jeffries
Planimetric Method was used to obtain the micro grain size. The
number of grains per square millimeter was of , with an ASTM micro
grain size of 9.77.
The last specimen analyzed was the Steel 4041. The micro grain sized
was obtained after the sample was carefully polished and etched with
Nital at a magnification of 40x. For this sample the Jeffries Planimetric
Method was used to obtain the micro grain size. The ASTM micro grain
sized obtained was 6.66, with a number of grains per square millimeter
area of .
The dark spots on the steels samples reflect the presence of impurities.
The most common type of impurity found was the ferrite which is also
known as iron; or a solid solution with iron as the main component, with
a body centered cubic crystal structure. It is the component which gives
steel and cast iron their magnetic properties.
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Conclusion

The experiment performed analyzed three different samples of alloys

that included Brass 360, Steel 1018, and Steel 4041. The samples were
analyzed under the microscope using a magnification of 80x and after
the proper etching material was used. The objectives established were
accomplished as the techniques for metallographic sample preparation
were performed and the microstructure for each specimen analyzed
was obtained and grain sized found and compare againg the ASTM E112 Standards.

By using the Jeffries Planimetric Method the ATSM micro grain size
obtain 1.4, 1.2 and 1.5 for Brass360, Steel 1018, Steel 4041
respectively. For the Brass specimen the error between the Jeffries
Planimetric Method vs. Heyn-Intercept Method was of 4.8368 %, the
error between Jeffries Planimetric Method vs. Euler Triple Point Method
was 12.1021 %, and the error between Heyn-Intercept Method vs. Euler
Triple Point Method was 10.818 %.
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Recommendation
Our recommendation would be to have
an electric grinder with a steady slow
speed so the grinding process would be
better. The polishing procedure needs to
be a clean one, would recommend using
clean velvet cloth and pure materials.
The etching part has to be one without
touching the specimen, I would
recommend using gloves.
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Figure 7: Prof. Noriegas

Analizing Specimen

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Figure 8. 40X Zoom

Microscope
Microstructure

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Figure 6: Specimen
setup in the Microscope

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Figure 5: Drying the

specimen after applying the
etching and cleaning with
alcohol.

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Figure 3: Polishing of the

specimen after grinding
with lower viscosity liquid.

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Figure 4: Polished Finish

of the specimen

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Abstract

Figure 1: Grinding of the specimen.

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Figure 2: First Polish after

grinding with higher viscosity
liquid.

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References
Callister, W. D. & Rethwisch, D.W.
(2007). Materials Sciences and
engineering: An introduction, 7 Ed.
New York, USA; John Wiley & Sons, Inc.
ASTM E112-06 ,E407-06
Polytechnic University of Puerto Rico,
Department of Mechanical Physical
Metallurgy Laboratory Manual, pp. 113, 2009.
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