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Quantitative Metallography

Lab 2 :: Monday 9/28/2009 9:30am


TAs: Uttarwar & Yang

Lab Report
Chad Huard
Matt Hartley
Sean Lechkun
Mike Menking

uantitative Metallography 9/28/09

Introduction
uantitative metallography is the study of metallic crystal structures from the perspective of numeric quantities.
Examples of quantitative metallographic measurements include number of grains per unit area and fraction of
specic phase per unit volume. ese two quantities are what we will investigate in this lab.
e grain size of a metal can have direct eects on its material properties. In general, the smaller the grain size the
stronger the metal. is is due to the misalignment of crystal structures in adjacent grains resisting the spread of
dislocations through the material. Dislocations tend to pile up at grain boundaries and a ner grained material
has more area of boundary per volume. Conversely, coarse grained metals, which have relatively few grain
boundaries to resist dislocations, will yield at lower stress levels than ne grained metals. [1]
e volume fraction of carbon in cast iron also has direct eects on the material properties, but they are much
harder to dene. e properties of the imbedded carbon in a cast iron can aect strength, hardness and ductility
as well as other properties. Unfortunately the volume fraction is not the only property of the carbon content that
aects the material properties of the cast iron. Other factors include the composition of carbon precipitation
(Fe3C or graphite) and the shape of carbon precipitate in the matrix (ake or spheroidal). All of these factors
change the way the volume fraction of carbon aects the material properties of the sample. In short, volume
fraction plays an important role in determining material properties, but only in conjunction with other traits. [2]
is lab introduces students to quantitative metallography by using an optical metallurgical microscope to nd
the grain size of a sample of steel and the carbon volume fraction in a cast iron sample.

Procedure
is lab required the use of a video capture metallurgical microscope, the output of which was displayed a TV
monitor for convenient measurement. Two dierent samples were measured, one single-phase alloy (steel or high
purity iron) and one two-phase alloy
(cast iron). From these
Fig ure 1 - Fl ow Chart
measurements we will calculate grain
size and intercept length for the
single phase alloy and volume
C al ibr ate M icros cope
fraction of graphite in the two-phase
sample.

Calibrate Microscope
In order to accurately count grain
size we need to have an accurate
understanding of the total
magnication of the system
including the enlargement due to the
TV. A stage micrometer is placed in
the microscope and measured on the
monitor. e divisions of the
micrometer are 0.01mm, and we
measured the distance between every
tenth division. erefore:

Huard, Hartley, Lechkun & Menking

M ea su re On e P ha se
Alloy

Me asu re Two P h as e
A lloy

Ca lc ula te Gr a in
Si ze

C al cul ate Volum e


Fr ac tion

Ca lc ula te Gr a in
I n te rc ept Le ngth

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d=

D
10

and

M=

d
0.01mm

Where:

D = average measurement between 10 divisions on micrometer.


d = distance of one micrometer division.
M = Magnication of system.
(1)

is magnication is used in calculating the grain size and intercept length which are measurements per area and
length respectively. Magnication is not needed for the volume fraction because it is a ratio of two measurements
at the same magnication.

Measure One Phase Alloy


For the single phase alloy a sample of high purity iron or stainless steel, suitably prepared, is loaded in the
microscope. Two measurements are taken of the single phase alloy: grain size and intercept length.
Grain Size:
1. Find area of specimen with clearly visible grain structure.
2. Use a plastic sheet over the monitor to lay out 150mm 150mm square.
3. Using a marker count grains within the square. Grains that are completely within the boundary count as 1,
those that touch one boundary line count as 1/2 and those in the corners (touching 2 boundary lines) count
as 1/4, as shown in gure 2.
4. Repeat measurement 5 times.

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Fig ure 2 - Grain S iz e

Grain Intercept Length:


1. Find area of specimen with clearly visible grain structure.
2. Use a plastic sheet over the monitor to lay out 150mm diameter circle.
3. Using a marker count the number of grain intercepts that intersect the boundary as shown in gure 3.
4. Repeat measurement 5 times.

Fig ure 3 - Inte rce pt Le ng th

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Measure Two Phase Alloy


A specimen of nodular cast iron is loaded in the microscope and the optics are changed from 4 to 40. Only
one measurement is taken of the two phase alloy: volume fraction of carbon.
1. Focus a random sample of the specimen on the screen.
2. Use plastic lm to superimpose a 66 grid on the screen (exact size not important)
3. Count and record number of grid points that lie on black graphite nodules. If point is entirely inside carbon
nodule count it as 1, if exactly on the border count as 1/2 as shown in gure 4.
4. Repeat 14 times.

Fig ure 4 - Inte rce pt Le ng th

Calculate ASTM Grain Size


Once all data is recorded calculation of ASTM grain size (n) is straightforward:
1. Calculate average number of grains ( N ) from the ve measurements.
2. Calculate uncertainty of N .
3. Calculate number of grains per mm2 at magnication M using:

NM =

N
150 150
(2)

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4. Calculate actual number of grains per mm2 using:

N1 = N M M 2
(3)

5. Calculate number of grains in 0.0645mm2 using:

N = N1 0.0645
(4)

6. Calculate ASTM grain size (n) using:

N = 2 n 1
(5)

Calculate ASTM Grain Size Using Intercept Length


is calculation will also give the ASTM grain size as a result, but using a dierent measurement:
1. Calculate average grain boundary intercepts ( N )
2. Calculate uncertainty of N .
3. Calculate number of boundary intercepts per mm at magnication M using:

PLM =

N
D
(6)

4. Calculate actual number of intercepts per mm using:

PL = PLM M
(7)

5. Calculate mean grain intercept length using:

L3 =

1
PL
(8)

6. Calculate ASTM grain size (n) using:

n = 3.36 2.88 ln L3
(9)

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Calculate Volume Fraction of Graphite in Two Phase Alloy (Fe + C)


is calculation results in a ratio of graphite to iron in a sample of nodular cast iron:
1. Calculate average number of grid points that lie within graphite nodules ( N G )
2. Calculate uncertainty of N G .
3. Calculate volume fraction of graphite using:

VV = PP =

NG
NT

Where:

N T = 6 6 = 36 = Total number of points in grid


(10)

Results
Sample 1:
Table 1 - Grain Size by Average Number of
Grains
Average number of grains at magnication M: 13.8
Uncertainty in number of grains at M (UA): 18.4
ASTM grain size (n): 2.17

Table 2 - Grain Size by Average Intercept Length


Average number of grain boundary intercepts: 12.4
Uncertainty in number of intercepts (UA): 7.51
ASTM grain size (n): 1.93

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Sample 2:
Table 3 - Volume Fraction of Carbon
Total number of grid points within graphite nodes: 12.18
Uncertainty in number of grid points (UA): 7.13
Volume fraction of carbon: 33.8%

Discussion
Uncertainty:
Each of the measurements taken in this experiment resulted in a large uncertainty relative to the measurement.
ere are several reasons for this. First, the uncertainty in each measurement is a combination of measurement
precision and the natural variation in the metal. When measurements are taken from dierent areas of the sample,
the sizes of grains and average number of grains per mm can change drastically such that one position may have
21.5 grains, yet another yields only 5. is uctuation is due mainly to a nonuniform grain structure in the metal,
but in this case cannot be dierentiated from uncertainty in the result. Furthermore, the American Society for
Metals explains in Applications of Modern Metallographic Techniques, that due to the range of grain sizes,
many are ignored[3]. Indeed, both visual and automatic methods tend to ignore very small particles actually
revealed by the microscope, and it must in most cases be anticipated that there are in fact some particles so small
that they are not revealed[3]. Also, all visual methods possess some bias when experimenters debate over the
inclusion or exclusion of grains that are extremely close to the boundaries. In an experimental setting, a procedure
that requires a judgment to be made by the experimenter oen will yield higher uncertainty. On the other hand,
we did achieve very good correlation between the two methods of determining grain size, which speaks well for
the accuracy of the measurements.

Grain Size:
e ASTM grain size was found to be 2, which in can be described as a course grained steel. is indicates
several characteristics of the alloy. At room temperature, the mechanical properties of ne-grain alloys are usually
superior to those of coarse-grained alloys [1]. Furthermore, ne grained materials [have] better biaxial stretching
capabilities in both tempers[4]. us, with a grain size of 2, the sample will yield a weaker building material than
a ne grained alloy. is superior strength of ne grained materials is a result of the discontinuity of slip planes.
Since ne-grained materials possess more grain boundaries, motion of grains that would otherwise deform the
alloy are impeded resulting in a stronger material.

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Fig ure 5 - Grain S iz e ve rsus Yield Stress [5]*

*Please notice that grain size is reported in m which is inversely proportional to the ASTM grain size (n).

Volume Fraction:
Our results show a metal with 33.8% carbon by volume. Unfortunately this is not enough information do draw
many conclusions about the material. Carbon content is usually described by weight, with average values for cast
iron being from 2%-4%[2]. Assuming the carbon in the sample is precipitated as graphite, and assuming a density
of 2.1g/cm3 for graphite and 7.9g/cm3 for iron we can approximate the weight percentage as 13.6%. is is
considerably outside the standard range for cast iron. is leads us to believe that there is more going on than a
simple volume to mass conversion. Without more information the only conclusion that we can draw from the
results is simply that the carbon is 33.8% of the total volume of the metal.

Conclusion
Table 4 - Results
ASTM Grain Size by number of grains 2.17
ASTM Grain Size by intercept length 1.93
Volume fraction of carbon: 33.8%
Sample 1 is a steel or high purity iron with coarse grain.
Sample 2 is a cast iron with 33.8% carbon by volume.

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Appendix
Raw Data:
D1

D2

D3

DAVE

MAVE (m)

Hor.

24.000

23.000

24.000

23.667

2.367

236.667

Vert.

24.000

24.000

24.000

24.000

2.400

240.000

MAVE = 238.333

Table 5 - Mag nification

Trial

# of 1

# of 1/2

# of 1/4

Total

13

15

21.500

5.000

14

19.000

13

10.500

10

13.000

Average: 13.800
kc: 2.7800

Ua: 18.404

u: 6.6200

Table 6 - Grain siz e by numbe r of g rains

Trial

# of Intercepts

12

10

12

11

17

AVE: 12.400
kc: 2.780
u: 2.702
Ua: 7.511

Table 7 - Grain siz e by inte rce pt l e ng th

Trial

# of 1

# of 1/2

Total

18

20.5

9.5

10

10

12.5

8.5

7.5

13

13.5

12

16.5

10

12.5

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Trial

# of 1

# of 1/2

Total

11

10.5

12

12.5

13

13

15.5

14

10

10

Average: 12.036
Ua: 7.712
kc: 2.160
u: 3.571

Table 8 - Volume Fraction

6
5
4
3
2
1
0

0-4

4-6

6-8

8-10

10-12

12-14

14-16

16-18

18-20

20-22

Fig ure 6 - D istribution of olume f raction mea sure me nts

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Bibliography
1.

Callister, W.D. and D.G. Rethwisch, Fundamentals of materials science and engineering : an integrated approach. 3rd
ed. 2008, Hoboken, NJ: John Wiley & Sons. xxv, 882 p.

2.

Yescas-Gonzalez, M.A. and H.K.D.H. Bhadeshia. Cast Irons. Available from: http://www.msm.cam.ac.uk/phasetrans/2001/adi/cast.iron.html.

3.

ASM, Applications of Modern Metallographic Techniques. American Society of Metals.

4.

Kennedy, S. and R. Dorward, Forming Characteristics of Coarse and Fine Grained Aluminum Alloy Sheet. SAE
Digital Library, 1993. SAE 3.

5.

Liverpool, U.o. M A T T E R - Materials Science & Engineering educational soware. 2000 [cited 2009 9/3];
Available from: http://www.matter.org.uk/steelmatter/metallurgy/strength/6_1_1.html.