MSE 2021 Stereology Lab Grade Sheet

Student Name:

Section:

Date of Lab:

Date of Report:

Lab Participation Lab Report

Possible Points Possible Points

Points Awarded Points Awarded
Attentiveness
/ Following 5 Procedure 10
Directions

Teamwork 5 Results 20

Task
10 Discussion 30
Completion

Adherence to
10 Conclusions 10
Safety

SUBTOTAL 30 SUBTOTAL 70
 Lab 5: Sample Preparation, Optical Microscopy, and Stereology

Abstract
Grain size and porosity are two important microstructural characteristics that
affect the magnetic properties in inductor cores. In this laboratory, standard
metallographic procedure is employed to prepare an iron inductor core sample for
inspection using optical microscopy. Stereological techniques are then applied to the
digitally captured micrographs in order to determine the porosity and grain size in the
material.

Introduction
Toroidal inductor cores are commonly used in electronic applications to regulate
electromagnetic interference. These cores are economically manufactured by compacting
and sintering iron powder. Compaction occurs along the Radial direction (Fig 1) and may
deform the powder particles and grains, while increasing the overall density of the core.
Porosity and grain size of the core material both impact the electromagnetic properties of
the inductor, and also indicate the processing path used for an inductor core.

AXIAL

HOOP

RADIAL

Figure 1: Toroidal Inductor Core

Quantitative information on the porosity and grain size in the three-dimensional

material can be obtained by applying stereological techniques to optical microscope
images of carefully chosen two-dimensional sections.
Porosity as a volume fraction can be shown to be statistically equivalent to the
area fraction or point fraction of voids in a representative two dimensional slice:

f  AA  [1]
f  PP  [2]

where AA is the area of void, A, per unit area, and PP is likewise the number of points
lying in void divided by the total probe points. The brackets indicate an average over
many samples.
Grain size can be quantified for dense materials with low porosity by measuring
the mean intercept grain size, G, which can be determined by overlaying test lines on the
microstructural image:

1
G [3]
 IL 
where IL is the number of intersections between the test lines and the grain boundaries per
unit test line length. For high porosity materials, G can be found by:

1  P 
G  [4]
 IL 

ASTM grain size number n can be calculated from G using the following equation given
in the ASTM E-112 standard

n = [-6.644 log G] - 3.288 [5]

In equation [5], the mean intercept grain size G is expressed in the units of millimeters.

The Effective Density of the material can be found using:

EffectiveDensity  (1  Porosity ) xDensityFE [6]

Procedure
Metallography & Imaging
A was used to cut the inductor core sample normal to the hoop plane.
In order to isolate undamaged microstructure features for later viewing, the specimen was
then mounted in and polished manually. Table 1 indicates the polishing
schedule used.

Table 1: Polishing Schedule for Sample

Speed
Step Media Grit Time (min) Comments
(rpm)
1 SiC Paper 600 2.00 120 N/A
2 SiC Paper 800 2.00 120 Rotated 90o from last face
3 SiC Paper 1200 2.00 120 Rotated 90o from last face
4 Al2O3 1 µm 2.00 120 Rotated 90o from last face
5 Al2O3 0.3 µm 2.00 120 Rotated 90o from last face
6 Al2O3 0.05 µm 2.00 120 Rotated 90o from last face

Care was taken during abrasion to keep constant pressure and direction of wheel
motion constant. When grit sized was changed the sample was also rotated in order to
distinguish the newly introduced scratches from those that were introduced in the
previous step. The final sample preparation step was chemical etching using a Nital
solution to highlight grain boundaries.
An __Electron_ microscope was used to capture digital images. Magnification
choice was crucial because image quality had to allow inspection of grain boundaries and
their relative position. 12 images were taken for analysis.
Porosity Measurement
A set of test points ( 7 x 5 grid) was overlaid on the microstructural image, and
the number of test points contained in the porosity area was counted. The fraction of test
points falling on the porosity area was calculated for each image and the average value of
this point fraction  PP  is reported as the volume fraction of porosity in the sample.

Grain Size Measurement

Grain size was measured by superimposing a set of test lines on the
microstructural image and counting the number of intersections between the test lines and
the grain boundaries. 0, 30, 60, and 90 degree straight lines were used as the test lines. A
set of __6__ straight lines, each of length _0.254___ mm was superimposed on the
microstructural images in a direction perpendicular to the vertical axis. The number of
intersections between the test lines and the grain boundaries per unit test line length was
noted down. The procedure was repeated with the test lines parallel to the vertical axis.
The mean intercept grain size G was calculated in both cases and the values were
compared.
Results
Fill out the required tables from the images taken during class and the calculations given
in the template. Include images representative of those that you used for data
collection, including the lines you used, to give a sense of the data you are working
from.

Table 2: Porosity measurements

Test points in Total no. of test
Image ID PP Average <PP>
porosity area points
P1 14 35 0.400
P2 12 35 0.343
P3 12 35 0.343
0.349
P4 10 35 0.286
P5 13 35 0.371
P6 N/A N/A N/A
Fig 1: Using a 7x5 grid on a 20x image of the sample to find Porosity. The points in the porosity area are
marked with red circles. This is Sample P5
Fig 2: Other 20x samples used for porosity. Going across from the top right to left the sample numbers are
P1,P2,P3 and P4.

Table 3: Intercept measurements using straight line probes

Probe Horizontal (Radial) Vertical (Axial)

ID
L(mm)
I IL <IL> G I IL <IL> G
SL1 0.254 8 31.5 14 55.1
SL2 0.254 16 63 17.5 68.9
SL3 0.254 11 43.3 45.3 0.0144 16.5 65 57.7 0.0113
SL4 0.254 12 47.2 13 51.2
SL5 0.254 10 39.4 14 55.1
SL6 0.254 12 47.2 13 51.2
Fig 3: Picture of sample SL3 with horizontal lines drawn on it for determining grain size. The circles
represent the starting or the end of a grain.
Fig 4: Examples of Vertical, 30o and 60o grain size measurements. The Images from top right to bottom
left are of samples SL3, SL3 and SL 4.
Table 4: Intercept measurements using 30 and 60 degrees

Probe 30 degrees 60 degrees

ID
L(mm)
I IL <IL> G I IL <IL> G
SL1 0.254 9 35.4 12.5 49.2
SL2 0.254 15 59.1 15.5 61
SL3 0.254 11.5 45.3 54.8 0.0119 20 78.7 61.7 0.0106
SL4 0.254 15.5 61 13 51.2
SL5 0.254 13.5 53.1 16 63
SL6 0.254 19 74.8 17 66.9

Discussion
What other mounting alternatives exist? Discuss why the specimen was mounted in
thermoset plastic instead of leaving it unmounted or mounting it in an alternative.

A: There exist multiple alternatives to mounting samples depending on the requirements

and constrains of the sample and the techniques being used. Resin can be used for hot
mounting a sample, hot mounting is used when the mounting needs to be done in a fast,
inexpensive and uniform manner. Substances like Epoxy, Acrylic and Polyester can be
used in cold mounting, this technique is used with samples are sensitive to heat.

Does the porosity volume fraction vary with each image? How can we get a better
estimate of the overall volume fraction of the porosity in the material?

A: Yes, it is apparent from the tables that the porosity can vary by a lot, in the calculated
values of porosity the standard deviation is ~4%. To get a better overall volume of the
material it would be beneficial to increase the number of samples and also get samples
from different layers of the material. It could also help to measure more sample points on
each image.

What was the average porosity? Use this to estimate the density of the part (for Fe,
=7.87 g/cm3)

A: The average porosity was 0.349. Thus, the average density of the part would be
Fe x (1-<PP>). Which comes out to be 5.12 g/cm3 .

For volume fraction estimation, is it required to know the magnification at which the
images were taken? Why or why not? What magnification should the measurements be
performed at for optimum efficiency and precision?
A: For volume fraction estimation, it is not required to know the magnification of the
image as no matter what the magnification is the random points have an equal chance of
landing on a grain or a void. It would be beneficial to perform the porosity calculations at
the 50x setting as it would lead to a smaller offset created by unusually sized grains.

For grain size measurement, is it required to know the magnification at which the images
were taken? Why or why not?

A: In order to determine the grain size we need to know what the magnification is, this is
because without knowing the magnification there is no way to measure the size of the
grains as we won’t know what units to use.

Does G vary along horizontal and vertical directions when measured using straight line
test probes? What does this imply?

The G value for the horizontal grains is about 27.4% larger than the vertical grains. This
implies that the grains are more inclined to be in a certain orientation. This implies that
either the grains were set in that way because of the forces acting on the metal during
manufacturing or that they adopted the orientation because of thermal or compressive
forces acting on them.

Keeping in mind that porosity and grain size are important factors in the performance of
induction cores, suppose you wanted to analyze a set of new processes (ie pressure used,
size of powder used, duration of sintering, etc) for fabricating these cores: how could you
determine which processes produced significant changes to the cores’ properties?

A: To determine whether some of the processes are significantly better than the others I
would design an experiment that is similar to the one we did above. I would get samples
of different layers of the materials and find out their porosity by counting the void spaces
and calculate the average grain sizes by finding the intersections in with the lines.

The samples used in this lab had high porosity, which is detrimental in the performance
of induction cores. If the samples had been prepared using iron nano-powders, the
porosity of the cores would have been greatly reduced. Why would you not decide to use
the nano-powders to fabricate the induction cores?

A: Even though the nano-powders would reduce the porosity of the solid, they would
lead to a very small grain size. It is recommended that induction cores have a large grain
sizes. Furthermore, the cost of creating cores with nanoparticles would render the
induction core manufacturing uneconomical.
Suppose you determine a process which greatly reduces porosity in the induction cores.
How would this process benefit more than just the induction core fabrication industry?

A: If a way to reduce the porosity of compressed powders was found then it would
benefit a lot of other processes that involve powder metallurgy. Furthermore, it would
increase the quality of metals manufactured using powder compression and thus save a
lot energy that is used in smelting metals.

Conclusion

Write a summary of what was done in lab and the results you obtained. Be sure to include
numbers where appropriate. Also include any additional analysis you may be able to
provide about grain size in induction cores or other metallic parts.

The objective of this lab was to learn how to prepare a sample for electron microscopy.
So, in the first part of the lab we were given a scratched sample of the induction core in
order to polish it so that the surface was smooth enough to etch. First, the samples were
polished with the Silicon Carbide at 600, 900 and 1200 grain. Then they were polished
with Aluminum Oxide with 1µm, 0.3 µm and 0.05 µm grating. Each of the samples was
polished for 2 minutes at 120 rpm. The samples were rotated 90 o after every polish. After
the last polish the surface of the sample was smooth enough to reflect my face.

In the second part of the lab we looked at an etched sample under an electron microscope.
We took 6 pictures of the sample at 50x and 6 pictures of the sample at 20x. These
pictures were used in order to find the Porosity and the average Grain size of the material.
The 20x sample was used to find the porosity, a grid was superimposed on the image and
the intersections of the lines were selected as random points to find how many voids the
materials had. After the calculations, the Porosity came out to be 0.349.

The 50x sample was used to find the grain size of the material. Lines were superimposed
on the images at 0o, 30o, 60o and 90o then the intersections between the lines and the
grains were found. After that the lines were measured and the following formula was
used to find the average grain size-
1  P 
G 
 IL 
In this formula the P is porosity that was found in the previous part of the experiment and
the IL is the intersections per line.

This experiment was really useful in teaching everyone how to prepare a sample foe
observation and how to actually use the data collected in the lab. Thus, as all the
objectives were completed the experiment can be deemed a success.