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R. E. Napolitano Materials Science & Engineering Iowa State University

The microstructural quantity known as the ASTM Micro Grain Size Number, n, is defined by the following relationship

where N is the number of grains per square inch, measured at a magnification of 100x. The most common methods for estimating the value of n are:

Comparison methods: The overall appearance of the microstructure is simply compared with a standard set of micrographs or "plates" for which the ASTM Grain Size Number has been determined.

Grain counting methods: The number of grains per unit area is counted directly. The ASTM grain size number is then determined according to the definition.

Intercept methods: The number of grain boundary intercepts per unit test line is measured. This is a measure of grain boundary area per unit volume and is, therefore, related to the grain size.

The methods for grain size measurement are described in great detail in the ASTM Standard, BI12, "Standard Test Methods for Determining Average Grain size." The information below is intended to provide a cursory explanation of the three categories listed above.

1. Comparison Method

This is the simplest, yet least quantitative, method, and is described in Section 8 of ASTM BIl2. Because the comparison of grain structures may be influenced by the overall type of microstructure, four standard categories of grain size plates are used for comparison.

Plate 1: Untwinned grains, flat-etch at 100x.

Includes grain size numbers 00, 0, 0.5,1,1.5,2,2.5,3,3.5,4,4.5,5,5.5,6,6.5,7, 7.5, 8, 8.5, 9, 9.5, and 10.

Plate 2: Twinned grains, flat-etch at lOOx.

Includes grain size numbers 1,2,3,4,5,6, 7, and 8.

Plate 3: Twinned grains, contrast-etch at 75x.

Includes nominal grain diameters of 0.2,0.15,0.12,0.09,0.07,0.06,0.05,0.045, 0.035,0.025,0.020,0.015,0.010, and 0.005mm.

Plate 4: Austenite grains in steel at lOOx.

Includes grain size numbers 1,2,3,4,5,6, 7, and 8.

These four plates are shown in the attached Figs. 1-4, taken from ASTM BI12. For any of these categories, a collection of plates, showing microstructures of the listed grain size numbers would be used for comparison.

2. Grain Counting Methods

An example of a grain counting method is the Planimetric Procedure, also known as Jeffries' Method. This method is described in Section 9 of ASTM Ell2. The basic steps of the procedure are as follows:

a) Inscribe a circle (or other shape) of known area, A, on an image of magnification, M.

b) Count the number of grains that are completely within the area.

c) Count the number of grains that are partially within the area.

d) Divide the result from (c) by 2.

e) Add the result from (d) to the result from (b).

f) Divide the result from (e) by A.

g) Convert the result from (f) to grains/in/ @ 100x.

h) Use the definition of ASTM grain size number to determine n.

The method above can be used in every case. The only step that may be confusing is (g), where the magnification must be accounted for. The result from (f) will be given in grains per unit area, measured on the image of magnification, M. To convert this to the 100x equivalent, multiply the result by (MIlOOf

ASTM El12 provides some tools for convenience. The standard contains a table that relates grains/in' @lOOx and grains/rrmr' @Ix to ASTM grain size number (see attached Table 2). To further assist the user, the standard suggests that an area of 5000 mnr' be used for the grain count, so long as this area encompasses at least 50 grains. The standard also includes a table that provides a "Jeffries' Multiplier" corresponding to several magnifications (see attached Table 5). If A=5000 mrrr', the multiplier indicated by this table can be multiplied by the result from step (f) to yield the grain count in terms of grains/rum" @ 1 x. Table 2 can then be used to determine the ASTM grain size.

Example:

Suppose a 2.5 x 3.5 inch area is marked on a 300x micrograph. The grain count indicates that 67 grains are completely contained in this area and 24 grains are partially contained. The result from step (e) would be 79. The area is 8.75 in2 so the result from (f) would be 9.03 grains/in' @300x. To convert to the 100x equivalent, this result is multiplied by (300/100)2, which is 9. The result from (g) is, therefore, 81.27 grains/in" @ lOOx. From Table 2, we see that this indicates a grain size number between 7 and 7.5. From the definition, we can express the grain size number as:

n = 1 + log, N = 1 + 3.321og N

From this expression, we compute the value of 11 to be 7.34.

Alternatively, the analysis area is computed to be (2.5in)(3.5in)(25.4 mmlin)2=5645 mm". The number of grains per 5000 mrrr' is then

N = 79 * (5000) = 69.97

5000 5645

measured at 300x. Using Table 5, we find the Jeffries' grain size multiplier for 300x to be 18.0. Multiplying Nsooo by this value gives 1259 grains/rum' @lx. Referring to Table 2, we see that this value indicates a grain size number between 7.2 and 7.5, in agreement with our previous estimation.

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3. Intercept Methods

An example of an intercept method is the Lineal Intercept Procedure, also known as the Heyn Method. This is described in detail in Section 11 of the ASTM BI12 Standard. The basic steps to this procedure are given here:

a) On a single field of view, randomly place one or more straight test lines of known combined total length, L.

b) Count the total number of intercepts, P, between the test lines(s) and the grain

boundaries. Triple-junctions count as 1.5. If P<50, use additional lines.

c) Divide the number of intercepts, P, obtained from (b) by the total length, L.

d) Repeat (a-c) for 2-4 additional fields of view.

e) Obtain PL as the average of the result from (c) for all fields of view.

f) The ASTM Grain Size Number is given as (ASTM E112 eq.2a)

n = -3.3 + 6.651oglO(pJ

where PL is given in rnm'.

For equiaxed grain structures, it is reasonable to assume that Figure 6 from the standard applies (see attached). This figure can be used to determine the ASTM grain size number from the number of intercepts per 500 mm of test line at various magnifications.

Example:

Suppose that 5 fields of view, at 200x, were used for the measurements resulting in the following data.

**Field Test Line Number of PL
**

of view Length (mm) Intercepts (mm')

1 337 71 42.2

2 216 45 41.6

3 402 89 44.2

4 529 113 42.8

5 395 81 41.0 From the table, the average value of PLis found to be 42.36 mm'. Using the equation given in (f), the grain size number is 7.5.

Alternatively, the attached Figure 6 can be used. The total number of intercepts is 399, and the total test line length is 1879 mm. Dividing, the value of PL at 200x is found to be 0.212 mm". (Of course, this is also equal to 42.36 divided by 200.) The figure requires that we know the number of intercepts per 500 mm test length. This is simply equal to (0.212)(500) = 106. This number is located on the x-axis of the figure. Following this location upward to the point where the 200x diagonal line is intersected and then following across to the y-axis, the grain size number can be read directly as 7.5.

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Fig. 1. Plate 1 - Untwinned grains - flat etch.

Fig. 3. Plate 3 - Twinned grains - contrast etch.

Fig. 2. Plate 2 - Twinned grains - flat etch.

Fig. 4. Plate 4 - Austenite grains in steel.

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~t E 112

**TABLE 2 Micro-Grain Size Relationships Computed for Uniform Randomly Oriented Equiaxed Grains
**

rE-For diameters in inches. see Table 4 (divide by 100).

~----------------,---- ----~.--.- ... ---.- .. - .----~~-

"Diameter" of Average Average

ASTM MI- Grain Section A Average In- Area of Av- Calculated

oro-Grain tercept Intercept erage Grain Number of

Size Nurn- Distance" Count. nil Section. a. Grains per Grains per Grains per

Nominal Feret's J,.

ber G (mm per mm mm2 rnm", njvC rnm? at in2 at WOx.

o.; mm mm

lx.Dn/a n/a

OOE 0.51 0.570 0.453 2.210 0.258 6.11 3.88 0250

0 0.36 0.403 0.320 3.125 0.129 17.3 7.75 0.500

0.5 0.30 0.339 0.269 3.716 0.0912 29.0 11.0 0.707

1.0 0.25 0.285 0.226 4.42 0.0645 48.8 15.50 1.000

1.5 Il.21 0.240 0.190 5.26 0.0456 82 21.9 1.414

(1.W 0.200 0.226 0.177 5.64 0.0400 100 25.0 1.613

2.0~ 0.18 0.202 0.160 6.25 0.0323 138 31.0 2.000

2.5 0.15 0.170 0.135 7.43 0.0228 232 43.8 2.828

>tm um >tm mm2 x 10-3

3.0 125 143 113 8.84 16.1 391 62.0 4.000

(3.2t 120 135 106 9.41 14.4 463 69.4 4.480

3.5 105 120 95 10.51 11.4 657 87.7 5.657

(3.7)" .100 113 89 11.29 10.0 800 100 6.452

4.0 90 101 80.0 12.5 8.07 1105 124 8.000

4.5 75 85 67.3 14.9 5.70 1859 175 11.31

(4.7)F 70 79 62.0 16.1 4.90 2331 204 13.17

5.0 65 71 56 ti 17.7 4.03 3126 248 16.00

(5.2)F 60 68 53.2 18.8 3.60 3708 278 17.92

5.5 55 60 47.6 21.0 2.85 5258 351 22.63

(5.7t 50 56 44.3 22.6 2.50 6400 400 25.81

6.0 45 50 40.0 25.0 2.02 8842 496 32.00

(6.4)F 40 45 35.4 28.2 1.60 12 500 625 40.32

6.5 38 42 33.6 29.7 1.43 14 871 701 45.25

(6.7)" 35' 39 31.0 32.2 1.23 18 659 816 52.67

7.0 32 36 28.3 35.4 1.008 25 010 992 64.00

(7.2( 30 34 26.6 37.6 0.900 29 630 1111 71.68

7.5 27 30 23.8 42.0 0.713 41 061 1403 90.51

(7.7)F 25 28 222 45.1 0.625 51 200 1600 103.23

urn >tm >tm mm2 x 10' 6 xl06 Xl03

8.0 22 25 20.0 50.0 504 0.0707 1.98 128.0

(8.4)F 20 23 17.7 56.4 400 0.1000 2.50 1613

8.5 19 21 16.8 59.5 356 0.1190 2.81 181.0

9.0 16 1'8 14.1 70.7 252 0.200 3.97 256.0

(9.2)" 15 17 13.3 75.2 225 0.237 4.44 286.7

9.5 13 15 11.9 84.1 178 0.336 5.61 362.0

10.0 11 13 10.0 100 126 0.566 7.94 512.0

(10.3)" 10 11.3 8.86 113 100 0.800 1000 645.2

10.5 9.4 10.6 8.41 119 89.1 0.952 11.22 724.1

(10.7)" 9.0 10.2 7.98 125 81.0 1.097 12.35 796.5

11.0 8 8.9 7.07 141 63.0 1.600 15.87 1024

(11.4)" 7.0 7.9 6.20 161 49.0 2.332 20.41 1317

11.5 6.7 7.5 5.95 168 44.6 2.692 22.45 1448

(11.S( 6.0 6.8 5.32 188 36.0 3.704 27.78 1792

12.0 5.6 6.3 5.00 200 31.5 4.527 31.7 2048

(12.3)F 5.0 5.6 4.43 226 25.0 6.40 40.0 2581

12.5 4.7 5.3 420 238 22.3 7.61 44.9 2896

13.0 4.0 4.5 3.54 283 158 12.80 63.5 4096

13.5 3.3 3.7 2.97 336 11.1 21.54 89.8 5793

(13.8)F 3.0 3.4 2.66 376 9.0 29.6 111.1 7168

14.0 2.8 3.2 2.50 400 7.88 36.2 127 8192

(14.3)F 2.5 2.8 2.22 451 6.25 51.2 160 10323

A Ferets diameter = height between tangents; df = all. Values of a., and d, rounded to digits shown.

B Value of Heyn intercept or mean free path.

C Computation of n/v based on grains averaging to spherical shape for which njv = 0.5659 {njl)3

o To obtain grains ;Jer mr;12 at 100x. :nuitiply by 10.4.

E The use of "00" is r8(;ornn1Cnded insfead of "minus 1" to avoid cO:lfuslon

F The G values $llC\fin in parentheses ;"rre ca!culated to one decimal place aflrJ correspond to some of the nominal "diameter" sizes. (01,,) customarily used in reponing

190 grain siz e by the copper orie! tH;:):::;S indust.ry 5

TABLE 5 Relationship Between Magnification Used and Jeffries' Multiplier, t, for an Area of 5000 mrrr' (a Circle of 79.8-mm Diameter) (f = 0.0002 M2)

Magnification Used. M

Jeffries' Multiplier. I, to Obtain Grains/rnm"

1 10 25 50 75A

100 150 200 250 300 500 750

1000

0,0002 0,02 0.125 0.5 1.125 2.0

4.5

8.0

12,5 18,0 50.0

112.5 200.0

A At 75 diameters magnification, Jeffries' multiplier, I, becomes unity if the area used is 5625 mm2 (a circle of 84.5-mm diameter),

~.mJ; E 112

~

QJ .D

E

::J Z

14

13 _.- __ J _

12 .. ---

11--

Q) N

(f)

:2 I(j)

<t

o 10

IS

20

30

SO 60 70 80 100

40

ISO

200

)00

400 500 600

800 1000

N:: Average Intercept Counts on 500mm Length Test Patterns

FIG, 6 Chart for Direct Determination of ASTM Micro-Grain Size Number from Intercept Count on 500-mm Test Pattern

6

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