1 Procedure

The procedures are standard. They work for any crystal structure regardless
of whether the material is metal, a ceramic, a semiconductor, a zeolite, etc.....
there are two methods of analysis. The first one is mathematical method and
the second one is analytical method.

1.1 Mathematical Method

Interplanar spacing in cubic crystals can be written in terms of lattice parame-
ters using the plane spacing equation:

1 h2 + k 2 + l 2
= (1)
d2 a2
You should recall Bragg’s law (λ = 2dsinθ), which can be rewritten either as:

λ2 = 4d2 sin2 θ
λ2
sin2 θ =
4d2
Combining this relationship with the plane spacing equation gives us a new
relationship:

1 h2 + k 2 = l2 4sin2 θ
= =
d2 a2 λ2
which can be rearranged to:

λ2
sin2 θ = ( )(h2 + k 2 + l2 )
4a2
λ2
The term in parentheses ( ) is constant for any one pattern (because the
4a2
X-ray wavelength λ and the lattice parameter a do not change). Thus sin2 θ is
proportional to h2 + k 2 + l2 . This proportionality shows that planes with higher
Miller indices will diffract at higher values of θ.
λ2
Since( 2 ) is constant for any pattern, we can write the following relationship
4a
for any two different planes:

λ2
2
sin θ1 ( )(h21 + k12 + l12 )
= 4a2
sin2 θ2 λ2
( 2 )(h22 + k22 + l22 )
4a
or
sin2 θ1 (h2 + k12 + l12 )
= 21
2
sin θ2 (h2 + k22 + l22 )

1
The ratio of sin2 θ values sacles with the ratio of h2 + k 2 + l2 values.
In cubic systems, the first XRD paek in XRD pattern will be due to diffraction
from planes with the lowest Miller Indices, which intrestingly enough are the
close packed planes(ie.): simple cubic,(100), h2 + k 2 + l2 = 1; body- centered
cubic, (110) h2 + k 2 + l2 ; and face- centered cubic, (111) h2 + k 2 + l2 = 3