Grain Size Measurement

TO:DR-MAGDY KASEM

Introduction;

By:Saed Estftah Elkelany | Section:2 | [Date]

The grain size is often determined when the properties of polycrystalline and singlephase materials
are under consideration. In this regard, it is important to realize that for each material, the
constituent grains have a variety of shapes and a distribution of sizes. Grain size may be specified in
terms of average or mean grain diameter, and a number of techniques have been developed to
measure this parameter. Before the advent of the digital age, grain-size determinations were
performed manually using photomicrographs. However, today, most techniques are automated and
use digital images and image analyzers with the capacity to record, detect, and measure accurately
features of the grain structure (i.e., grain intercept counts, grain boundary lengths, and grain
areas).

1.VISUAL DETERMINATION METHOD:

We now briefly describe two common grain-size determination techniques: (1) linear intercept—
counting numbers of grain boundary intersections by straight test lines; and (2) comparison—
comparing grain structures with standardized charts, which are based upon grain areas (i.e.,
number of grains per unit area). Discussions of these techniques is from the manual perspective
(using photomicrographs).

For the linear intercept method, lines are drawn randomly through several photomicrographs that
show the grain structure (all taken at the same magnification). Grain boundaries intersected by all
the line segments are counted. Let us represent the sum of the total number of intersections as P
and the total length of all the lines by LT. The mean intercept length / [in real space (at 1x—i.e., not
magnified)], a measure of grain diameter, may be determined by the following expression:

The comparison method of grain-size determination was devised by the American Society for
Testing and Materials (ASTM).11 The ASTM has prepared several standard comparison charts, all
having different average grain sizes and referenced to photomicrographs taken at a magnification
of 100x. To each chart is assigned a number ranging from 1 to 10, which is termed the grain-size
number. A specimen must be prepared properly to reveal the grain structure, which is then
photographed. Grain size is expressed as the grain-size number of the chart that most nearly
matches the grains in the micrograph. Thus, a relatively simple and convenient visual
determination of grain-size number is possible. Grain-size number is used extensively in the
specification of steels. The rationale behind the assignment of the grain-size number to these
various charts is as follows: Let G represent the grain-size number, and let n be the average number
of grains per square inch at a magnification of 100x. These two parameters are related to each other

through the expression

For photomicrographs taken at magnifications other than 100x, use of the following modified form

of the previos equation is necessary

PAGE 1
In this expression, nM is the number of grains per square inch at magnification M. In addition, the
inclusion of the (M/ 100)2 term makes use of the fact that, whereas magnification is a length
parameter, area is expressed in terms of units of length squared. As a consequence, the number of
grains per unit area increases with the square of the increase in magnification.

Relationships have been developed that relate mean intercept length to ASTM grain-size number;
these are as follows:

To compute magnification from a scale bar, the following procedure may be used: 1. Measure the
length of the scale bar in millimeters using a ruler. 2. Convert this length into microns [i.e.,
multiply the value in step (1) by 1000 because there are 1000 microns in a millimeter]. 3.
Magnification M is equal to

M=

measured scale length (converted to microns) /the number appearing by the scale bar (in microns)

2.USING XRD:
Using the Scherrer Equation, the variation of the crystal grain size has a great influence on the
FWHM when the grain size is less than 10 nm, however when the crystal grain size increases, the
variation of the FWHM become unapparent with the increasing grain size.Therefore the results
calculated by the Scherrer equation become more imprecise due to the weaker broadening effect
when the crystal grain size increases. because the inverse proportional function coefficient
increases as the X-ray diffraction angle increases ,the FWHM corresponding to the same crystal
grain size is also increased. For that reason, the application scope of the Scherrer equation for
crystal plane with larger diffraction angle is wider than that of crystal plane with smaller diffraction
angle. This is consistent with the conclusion based on the dynamical
theory,whenthediffractionangleislargerthan60°,therangeof the application can be up to 1
µm.However , the above discussion is based on the ideal conditions of X-ray diffraction .In the
actual XRD measurements , the diffraction peak broadening is related to both the physical
broadening and instrumental broadening .Therefore ,the application scope of he Scherrer equation
in practice is far less than that in the ideal condition. The relationship of actual FWHM, FWHM
caused by instrument and FWHM caused by crystal grain size is connected with the shape of
diffraction peak.When the diffraction peak conforms to Lorentz distribution ,the actual FWHM of
X-ray diffraction peak can be expressed as follows:

PAGE 2
The grain size D can be seen as infinite when a mono crystal sample is measured by XRD, so the
FWHM caused by crystal grain size tends to 0:

m2 =

180Kλ /π D cosθ ≈0

Therefore, the FWHM is only caused by instrument in this situation. We make use of the Si(100)
standard sample to measure the FWHM caused by XRD equipment. The equipment was
manufactured by BRUKER company (targetmaterial:Cu,the power of X ray generator: 2.2kw, the
accuracy of measurement). In software of MDI Jade5.0, it can be found that the FWHM of (400)
diffraction plane (2θ =69.13◦) is 0.07°. Thus it can be determined that the FWHM caused by
instrument is 0.07°. Then, the actual FWHM of diffraction peak in Lorentz distribution or Gaussian

PAGE 3
distribution can be expressed respectively as:

The crystal grain size obtained by the Scherrer equation will be unreliable if the FWHM caused by
the crystal grain size is smaller than it caused by the instrument .Therefore, the crystal grain size,
which causes the same value of FWHM as instrument does, is considered to be the maximum value
of the available range of Scherrer equation. In order to determine the maximum applicable range of
the Scherrer equation for Si (100), We take K as 0.89, λ as 0.154056 which is the X-ray diffraction
wavelength and θ as (400) diffraction peak angle of 35°, and that is: (0.07)2 =( 180Kλ /πDcosθ)2

D ≈137 nm . We can see, no matter what shape of diffraction peak it is, the calculating result is
same .Therefore ,the applicable range of maximum crystal grain size for Si(100) is 137 nm. For the
mono crystal film of different material, which has different crystal direction and diffraction angle,
We also calculate the relationship between the diffraction angle and thickness of film ,because the
Scherrer equation can be expressed as follows

PAGE 4
PAGE 5