METALLOGRAPHY

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DETERMINATION OF GRAIN SIZE & CARBON CONTENT FROM A MICROSECTION

EXPERIMENT 1: METALLOGRAPHY
DETERMINATION OF GRAIN SIZE & CARBON CONTENT FROM A MICROSECTION
OBJECTIVES
 To enable the student to acquire familiarity with the techniques of preparing microsections for
metallographic examinations and to become acquainted with the different pieces of equipment found in a

typical metallurgical laboratory;
 To enable the student to become acquainted with photomicrography and make use of it in determination
of the grain size for a microsection as well as its carbon content if it is a steel sample.
BACKGROUND
Study MICROSCOPIC EXAMINATION (Sec 4.9 to 4.11) of Ch 4: Imperfection in Solids about basic concepts of
microscopy, microscopic techniques and grain size determination.
Study THE IRON-CARBON SYSTEM (Sec 9.18 to 9.20) of Ch 9: Phase Diagrams about the iron-iron carbide
(Fe-Fe3C) phase diagram, development of microstructure in iron-carbon (Fe-C) alloys, i.e., steels, and the
influence of other alloying elements.
Refer to the two ASTM International (formally American Society for Testing and Materials) publications:


 ASTM E 112: Standard Test Methods for Determining Average Grain Size, 2013.


 Introduction to Steels & Cast Irons, Metallographer’s Guide: Ch 1, ASTM International, 2002.
EQUIPMENT
 A set of metallographic preparation units (cutting, mounting, grinding, polishing and ultrasonic cleaning

units, etc.)
 An optical microscope equipped with camera and PAX-it image management/analysis software
MATERIALS AND SPECIMENS
A group of bakelite-mounted, microsectioned metallic samples, including carbon steels (such as 1020, 1040)
and non-ferrous metals (e.g., brass, zinc, etc.)
PROCEDURES
1. Prepare bakelite-mounted, microsectioned metallic samples (Demo by technician).
2. Examine each specimen under the microscope using different magnifications (40, 100, 400, etc.).
Make sure the grain boundaries are clearly visible.
3. Take an image of one of the microsectioned metallic samples in your bakelite specimen. Seek the
assistance of the instructor when selecting the camera setting. It usually takes more than one attempt to
obtain the optimal camera setting that yields the most clear photomicrographic image, in which the grain
boundaries are evident and well defined. The magnification factor used should be at least 100. Repeat
the same for all other samples contained in the bakelite specimen.
4. Grain Size Determination: Use PAX-it image to determine the grain size of each metallic
microsectioned sample in your specimen and save the results.
5. Print out the a photomicrograph and draw a circle or a rectangle of known area on the photomicrograph.
Determine the nominal number of grains in that area, counting each whole grain as 1 and each boundary
grain (i.e., a grain intercepted by the perimeter of the outlined area) as ½.
6. Following Example Problem 4.5: Grain-Size Computations Using ASTM and Intercept Methods
(textbook pp. 117-118) for grain size determination. Specifically,

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DETERMINATION OF GRAIN SIZE & CARBON CONTENT FROM A MICROSECTION

a. Calculate the number of grains per square inch at the magnification you used to obtain the
photomicrograph. Modify the calculation to obtain the number of grains per square inch at 100
magnification, using the following equation:
2
 M 
n100  nM  
(1.1)
 100 
where n100 is the number of grains per square inch at 100 magnification and nM is the number of
grains per square inch at the magnification M of the photomicrograph.
b. As exemplified in the publication: ASTM E 112, the ASTM grain size number G is calculated from the
following equation:
ln  n100 
G 1 (1.2)
ln  2 

i.e., n100  2G 1 ~ See also Eq (4.17) on textbook, p. 115. (1.3)

7. Carbon Content Determination: Capture the image of each microsectioned metallic sample mounted
in the bakelite specimen. Identify which microsections are plain-carbon steel alloys whereas which are
not.
Note: Seek the assistance of the instructor when capturing the images to ensure all information/data are
inputted properly. The scale bar for the captured image must be entered in relation to the
magnification.
8. Generally speaking, in a typical photomicrograph of a plain-carbon steel alloy, microstructural grains of
two distinct shades coexist, as shown in Fig 9.30 (textbook p. 293). In order to use the Region of Interest
(ROI) method in PAX-it to find the total areal percentage of all grains of the darker shade, which is
called pearlites, one can move the color slider upwards and/or downwards slowly. The aim here is to
ensure these pearlite grains are completely shaded without shading the other (i.e., lighter) grains, which
are proeutectoid ferrites (also called pro-). Both pearlite and pro- are solid phases of steels and will
be explained later.
9. To find the areal percentage of pearlite Apearlite , click on the “Measurement Total”, then “Finish” button.
10. Assume the same microstructure exists through the entire thickness of the microsectioned sample, then
Apearlite is the volume percentage of pearlite, Vpearlite . Of course, the volume percentage of pro- is the
reminder; that is, Vpro-  1  Vpearlite .
11. Some useful background in understanding steel microstructures is presented here. First, in plain-carbon
steel, ferrite (also called the  phase, see Fig 9.25a, textbook p. 288) has a BCC (body-centered cubic)
structure and up to a carbon content by weight of C  0.022 wt%C (Fig 9.24, textbook p. 287). With
no other alloying additions, the ferrite phase has a density very close to that of pure iron, i.e., about
  7,870 kg m3 . Secondly, cementite (also called iron carbide) on the other hand is a ceramic with a
chemical compound: Fe3C and a carbon content by weight of CFe3C  6.70 wt%C (Fig 9.24, textbook
p. 287). It has a theoretical density approximately Fe3C  7,640 kg m3 . This value is obtained as
follows:

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DETERMINATION OF GRAIN SIZE & CARBON CONTENT FROM A MICROSECTION

From Fig 2.8 (textbook, p. 28), the atomic weights of carbon (C) and iron (Fe) are 12.01 and 55.845
g mol , respectively. The molecular weight of cementite ( Fe3C ) is thus, 179.545 g mol (= 55.8453 +
12.011).
The molar volumes of carbon and iron are 5.29 and 7.09 cm3 mol , respectively. The theoretical molar
volume of cementite is thus, 26.56 cm3 mol (= 7.093 + 5.291). However, we will choose a published
value of 23.5 cm3 mol since the crystal structure of Fe3C is no longer BCC.
The density of cementite can then be calculated as:
mass of Fe3C per mole 179.545 g mol
Fe C    7, 640 kg m3 (1.4)
3
volume of Fe3C per mole 23.5 cm3 mol
Thirdly, pearlite, as shown in Fig 9.27, textbook p. 291, is a composite phase of alternating layers of
ferrites (88 %vol) and cementites (12 %vol). It has a carbon content by weight of Cpearlite  0.76 wt%C ,
which is the value of the eutectoid composition of plain-carbon steel (see Fig 9.24, textbook p. 287). The
density of pearlite can then be calculated as:
pearlite   V   Fe C VFe C  7,842 kg m3
3 3
(1.5)
Finally, Consider a plain-carbon steel with a carbon content by weight lower than the eutectoid
composition (0.76 wt%C per Fig 9.24, textbook p. 287). When the metal is cooled down from the
austenite phase (also called -phase, which has an FCC microstructure), which exists above the eutectoid
temperature (727°C per Fig 9.24, textbook p. 287), the pro-eutectoid ferrite (i.e., pro-) phase will
form before the occurrence of eutectoid reaction. Note that at the instant of eutectoid reaction, the
pearlite phase, which is a composite of interlacing cementite + eutectoid ferrite, will be produced. A steel
with a carbon content by weight lower than the eutectoid composition is called a hypoeutectoid alloy.
Details of the above-mentioned various solid phases of steel alloys are discussed in Chapter 9.
12. The following Lever Rules can then be applied to calculate the percentage of carbon content ( C0 ) in a
plain-carbon steel alloy:
 C0  C
mass of pearlite: Wpearlite 
 Cpearlite  C
 (1.6)
mass of pro- : Cpearlite  C0
Wpro- 
 Cpearlite  C

 Wpearlite  pearlite
 volume of pearlite: Vpearlite 
D Wpearlite Wpro-
 where D   (1.7)
 volume of pro- : Wpro-  pro- pearlite pro-
Vpro- 
 D
The percentage of carbon C0 of the steel sample can thus be found by substituting Eqs (1.6) into either of
Eqs (1.7).
REVIEW QUESTIONS
1. How and why is the metallurgical microscope different from the biological type?
2. Why is grinding (or polishing) conducted in more than one step?
3. Why is fine grinding performed wet?
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DETERMINATION OF GRAIN SIZE & CARBON CONTENT FROM A MICROSECTION

4. What is the purpose of etching?

5. If your bakelite specimen contains any non-steel microsection, identify the metal and explain how.
6. Comment on the validity of the assumption made in Step 10 of PROCEDURE; that is the areal fraction of
pearlite  Apearlite  in a photomicrograph is also the volume fraction of pearlite Vpearlite  .
7. Study Example Problem 9.4: Determination of Relative Amounts of Ferrite, Cementite and Pearlite
Microconstituents (textbook pp. 296-297) to find
a. the fractions of total ferrite and cementite phases
b. the fractions of proeutectoid ferrite and pearlite phases
c. the fraction of eutectoid ferrite
8. Based on the binary phases of total ferrite and cementite, re-derive another set of Lever Rules similar to
Eqs (1.6 & 7), which are based on proeutectoid ferrite and pearlite phases.
9. In this experiment, we assume any of the steel microsections has a weight percentage of carbon C0 less
than that of eutectoid composition (i.e., Ceutectoid  Cpearlite  0.76 wt%C ), thus forming the pro-eutectoid
ferrite (pro-) phase from the FCC austenite -phase before the eutectoid reaction occurs. What if,
instead, C0  Ceutectoid  Cpearlite  0.76 wt%C , which pro-eutectoid phase will present as the steel alloy is
cooled from the austenite -phase before the occurrence of eutectoid reaction (that is, at 727°C per
Fig 9.24, textbook p. 287)? Identify which figure and the associated page number in the textbook
represents the microstructure of this type of steel alloys.
Hint: The steel with C0  Ceutectoid is called a hypereutectoid alloy.
10. With respect to a hypereutectoic steel, re-derive another two sets of Lever Rules similar to Eqs (1.6 & 7)
and those derived in Question 8 above.

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