Aim

The basic aim of the experiment is to identify the lattice and to determine its lattice constant.
Apparatus Used:
Set up for X- Ray Simulation, Samples

INTRODUCTION
Regular arrangement of atoms in molecules and extended solids is very common. In
crystalline solids the atoms are arranged in repeating three-dimensional arrays or lattices.
Information regarding atomic bond distances and angles is fundamental to understanding the
chemical and physical properties of materials. Since atomic dimensions are of the order of
angstroms (10-10 m), unraveling the relative atomic positions of a solid requires a physical
technique that operates on a similar spatial scale, Diffraction experiments involving X-ray,
electron and neutron sources have therefore played a very crucial role in unraveling these
structures. The significance of these experiments in science and engineering courses has been
recognized. However, the cost of the equipment and the hazards associated with these
experiments have made them very difficult to be integrated and included in a teaching
laboratory setting.
The present set-up overcomes these limitations. An increase in scale by thousands
from short wavelengths of X-rays to the long wavelengths of visible light, and by hundreds
of thousands from an array of atoms in a crystal or an extended solid to an array of dots,
allows us to replicate the basic features of a structural determination experiment in a teaching
laboratory. The set-up consists of a small battery powered laser and a pattern of arrays of dots
and only needs a darkened room.

THEORY
 Laue recognized at the beginning of the last century that X-rays having wavelengths
on the order of atomic dimensions would be scattered by the atoms in a crystalline
solid. Interference would occur among the many resulting waves (coming from
different atoms in the crystal). For most directions of observation, destructive
interference will occur, but in specific directions constructive interference is observed
(Figure 1).

 The condition for constructive interference, the Bragg condition, is illustrated in
Figure 2 and is often described in terms of reflection from parallel plane of atoms in
the crystal, since the angle of incidence equals the angle of diffraction.

 As the figure shows, if the atomic planes (represented by the rows of dots) are
separated by a distance d, then X-rays arriving at and scattered at an angle  relative
to the plane will arrive at a detector in phase, if the additional distance traveled by the
lower light ray relative to the upper light ray is an integral number of wavelengths, nλ
(n = 1, 2, 3, …..; n = 1 is called first order diffraction, n = 2 is second order
 diffraction, etc.). From the figure, this extra path length is 2(d sin), leading to
Bragg’s law,
2(d sin) = nλ (1)
 The diffraction patterns thus provide evidence for the periodically repeating
arrangement of atoms in crystals. Their overall symmetry corresponds to the

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symmetry of the lattice and permits identification of the lattice type and determination
of interatomic distances.

Figure 1: X-Ray Diffraction

Figure 2: Bragg Diffraction

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 Figure 3: Optical Transform

Figure 4: Fraunhofer Diffraction

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  In place of Bragg diffraction whose results are to be simulated, let us now consider
Fraunhofer diffraction with a change in spatial scale by several orders of magnitude
by using much larger spacing compared to interatomic distances and electromagnetic
radiation with much larger wavelength compared to X-rays, viz., visible light in a
simple, safe and inexpensive set-up. Visible laser light passes through an array of
scattering centers (dots) on a 35 mm slide as shown in Figure3.


 It is viewed at what is effectively infinite distance (a meter or so). This arrangement is

capable of illustrating many of the essential features of the standard X-ray experiment.
For Bragg diffraction the condition for constructive interference is 2dsinφ = nλ, while
in the present case, which is Fraunhafer diffraction it is:
d sinφ = nλ (2)
where the perpendicular spacing d between rows of dots and scattering angle φ are
defined in Figure 4. The scattered rays in the figure are in phase if the lower ray
travels an additional distance (d sinφ) which is an integral multiple of wavelength λ.
Mathematically, the equations for Fraunhofer and Bragg diffraction have a similar
functional dependence on d, λ and scattering angle.
 In the illustration of Fraunhofer diffraction in Figure 4, just one row of two-
dimensional arrays is shown. These arrays are formed by stacking additional rows
above and below the row shown in the figure. The symmetry of the diffraction pattern
is same as the symmetry of the lattice causing the diffraction.

 The central piece of the setup is a slide (transparency) with eight (A-H) different
arrangements of scattering centers (dots) on different portions of the slide (Figure 5).

 The examples presented here serve to illustrate how the spacing, symmetries, spot
intensities and systematic absences in a diffraction pattern are related to the lattice
from which it is derived. Although these are two-dimensional lattices, they mimic
what would be observed for diffraction from particular three-dimensional structures
that are viewed in projection perpendicular to a face. For example, Arrangements B
and D are the arrays of atoms in a simple cubic (sc) structure, a structure having atoms
only at the cube corners. The centered array of Arrangement A mimics the projection
of a body-centered cubic structure (bcc), which has atoms at the cube corners and in
the center of the cube. The array of Arrangement C simulates the projection of the
cubic ZnS structure, having two different kinds of atoms, each surrounded by four
atoms of the other type in a tetrahedral arrangement (fcc). This is also the array that
would be seen for a single layer of the NaCl rock salt structure. The rectangular
structures Arrangements E and G are derived from orthorhombic structures, wherein
all angles are 90o but the sides are of unequal length. The array of Arrangement F
mimics a monoclinic structure where the non-90o lattice angle is in the plane of the
paper. Arrangement H represents a closest packing structure, the basis for a layer of
the hexagonal closest packing or cubic closest packing structures.

 Figure 6 shows the diffraction patterns obtained with different arrangements in the
slide.

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Figure 5: Slide Figure 6: Diffraction Patterns

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COMMENTS ON THE DIFFRACTION PATTERNS
1. Arrangement B is a square array. It leads to a diffraction pattern having the same
square symmetry. The four spots (0, ±X) and (±X, 0) correspond to first order
diffraction with horizontal / vertical spacing distance d (=0.07mm) . The four spots
( ) correspond to first order diffraction with spacing d/ along 45o with
the vertical or horizontal direction. A general feature of reciprocal lattice effect is a
90° rotation of the diffraction pattern with respect to the arrangement of atoms in the
lattice.
2. Arrangement D is a square array like Arrangement B, but with a larger spacing
(d=0.105mm). The square symmetry is again seen in D, the spacing of the diffraction
spots in D is closer than in B. This is the reciprocal lattice effect: a larger separation of
dots in the diffraction pattern and vice versa. This effect comes from the diffraction
equation, since the product of spacing d and diffraction angle sinφ is a constant in the
diffraction equation. Higher order diffraction spots are also visible in this pattern.
3. The symmetry of the diffraction patterns B and D shows that the corresponding array
of dots is planar version of the simple cubic (sc) lattice.
4. Arrangement A is a square array with the same dimensions as B, but with a duplicate
dot in the center of the cell (a ‘centered’ cell). It is found that every other spot
disappears in the diffraction pattern of A relative to that of B, although the square
symmetry of the array A is preserved in its diffraction pattern. This set of ‘systematic
absences’ arises because the additional dots placed at the centers of the squares in
Arrangement A lead to destructive interference: the scattered waves produced by the
dots at the center of the squares are out of phase by half a wavelength with waves
produced by the dots at the squares’ corners, causing every other spot to disappear.
Another way to look at this effect is as an illustration of the reciprocal lattice effect:
the array of A can be described as a simple square (rotated by 45o) with a smaller
repeat distance between the dots leading to a larger spacing between spots in the
diffraction pattern (rotated by 45o).
5. This pattern (A) which is the result of destructive interference between the waves
scattered by the dots at the center of the squares and the waves by the dots at the
corners of the squares yet preserving the overall symmetry of the square array is thus
an indicator of centered square array. This array here mimics body-centered and face-
centered cubic (bcc and fcc) lattices.
6. Arrangement C has the same repeat spacing as Arrangement D, but each square array
of dots contains a larger dot in its center. Dots of different sizes scatter light
differently. Same square diffraction pattern is observed for both Arrangements, C and
D, but the diffraction pattern from C shows a different distribution of spot intensities.
This illustrates another fundamental aspect of the diffraction experiment: the
positions of the spots depend on the repeat spacing (unit cell dimension), while the
intensity of the spots depends on the identity and content (location of specific atoms
in the unit cell). Arrangement C can also be described as having small dots at the
center of squares formed by large dots, i.e., this slide has interpenetrating square
arrays of small and large dots.

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7. This diffraction pattern (C) thus corresponds to a square arrangement where the dots
at the centers and the corners are of different size. This arrangement mimics the
projection of a cubic structure having two different kinds of atoms each surrounded by
four atoms of the other type.
8. Arrangement E has a rectangular symmetry (d1=0.067mm, d2=0.135mm), as does its
diffraction pattern. The reciprocal lattice effect can be seen again as the long direction
in the rectangular slide becomes the shorter direction in the diffraction pattern, and
vice versa.
9. Arrangement F has the symmetry of a non-orthogonal parallelogram and represents
the effects of changing the angle from 90o in the Arrangement E. The inter-dot
distance on the lines is 0.04mm. The reciprocal lattice effect can be seen as a reversal
of the long and short sides of the parallelogram between the Arrangement and the
diffraction pattern.
10. Arrangement G has a glide plane symmetry with d1=0.14mm and d2=0.175mm. The
glide plane is an imaginary mirror placed parallel to and half way between the
columns of L’s in the array. Reflecting across this mirror plane, followed by raising or
lowering the columns by half the repeat distance along a direction parallel to the glide
plane gives an array that is indistinguishable from the original. Glide symmetry causes
systematic absences in the diffraction pattern: every alternate dot in the central
vertical column is missing due to destructive interference resulting from the glide
plane.
11. Arrangement H has the symmetry of a hexagon with hexagonal side d equal to
0.135mm. Its diffraction pattern also has hexagonal symmetry with 90° rotation which
is the reciprocal lattice effect. This pattern is signature of hexagonal closest packing
(hcp) or cubic closest packing (ccp) structure, whose projection is Arrangement H.
12. The symmetry of the diffraction pattern is the same as the symmetry of the lattice
causing the diffraction. Arrangements A to D exhibit square symmetry, so is the case
with the corresponding diffraction patterns. Arrangements E and G have rectangular
symmetry, their diffraction patterns have the same symmetry. The diffraction pattern
of Arrangement H has hexagonal symmetry.
13. In actual crystallographic studies, it should be noted that both the intensity and the
phase of the diffracted beams are require to calculate the atomic positions from
experimental data. But only the intensity can be measured. The intensities of the
diffraction peaks depend on the contents of the unit cell, and the diffraction pattern
can be calculated for any set of atoms with known coordinates in a periodic array.
Solving for a crystal structure involves matching the observed intensities with those
predicted for a trial structure. The phases of the calculated structure are assigned to
the observed amplitudes and a new structure is calculated. The computation-intensive
process is repeated and least-squares procedure is used to minimize the differences.

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 X1
X5 X6

X7

X
2

X3 X4
X
8

Figure 7. Diffraction pattern corresponding to Arrangement A

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SET-UP
The laser (=6500A.U.) mounted on a stand is put at one end of the optical bench. The
slide is mounted on another stand which is kept at about 10-20 cm away from the laser
such that the laser light falls normally on the slide. The slide on this stand can be moved
sideways and vertically so that the laser light falls on different portions of the slide. The
diffraction pattern is observed on a clear perspex screen fixed normal to the laser light at
the other end of the optical bench. The whole set is put in a darkened room where the
experiment is performed.

PROCEDURE, CALCULATIONS AND RESULTS

The basic aim is to identify the lattice and to determine its lattice constant.

The procedure is identical for all the eight different arrangements of dots on the slide. As
an illustration, we present in the following the details of the observations, calculations
and results for all the arrangements on the slide.

1. ARRANGEMENT A
This is two dimensional version of centered simple cubic lattice. The center and
corner spots, corresponding to center and corner atoms in the lattice, are identical. If
any direction φ corresponds to nth order for the line of corner spots in any principal
direction it will correspond to n/2th order for alternate corner and central spots in the
same direction. The result is that alternate orders (those corresponding to odd n) will
be missing. The diffraction pattern will look as shown in Figure 7.
The distance between adjacent circles along principal directions are measured
randomly and their average is taken. Note that these correspond to orders differing by
two.
X1 = 18mm X2 = 18mm
X3 = 18mm X4 = 18mm
X5 = 18mm X6 = 18mm
X7 = 18mm X8 = 18mm

Average X = 18mm
Distance L between the slide and the screen = 1000mm
sinφ  φ  tanφ = 18/1000 = 0.018

Lattice constant d = 2λ/sinφ = (2X65X10-5)/ 0.018 = 0.072mm

Given value of d = 0.07 mm Error = 2.8%
This pattern with square symmetry and with alternate missing orders is indicative of a
square array of identical dots at the centers and corners. Such an array is projection of
centered simple cubic lattice.

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 X
1

X5
X2

X
6 X3

X7

X8
X4

Figure 8. Diffraction pattern corresponding to Arrangement B

X1

X2
X3
X4
X5
X6

Figure 9. Diffraction pattern corresponding to Arrangement C

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2. ARRANGEMENT B
This is two dimensional version of a simple cubic lattice. The slide is adjusted on the
stand such that the laser light falls on the portion B. The diffraction pattern as shown
in Figure 8 will appear on the perspex screen without any further adjustments.
The dark circle corresponds to the central spot (direct light). Other circles correspond
to Fraunhofer diffraction given by Eq.(2). In the present set-up λ/d is very small and
therefore sinφ is equal to φ for all orders visible in the pattern. The result is that the
distance between adjacent circles, corresponding to consecutive orders, is same.
Random measurements are made and average taken.
X1 = 9mm X2 = 9mm
X3 = 9mm X4 = 9mm
X5 = 9mm X6 = 9mm
X7 = 9mm X8 = 9mm

Average X = 9mm
Distance L between the screen and the slide = 1000mm
sinφ  φ  tanφ = X/L = 9/1000 = 0.009

Lattice constant d = λ/sinφ = (65X10-5)/0.009 = 0.072mm

Given value of d= 0.07mm Error = 2.8%
The square symmetry of this diffraction pattern is manifestation of the square of the
square array of dots. This array is the projection of simple cubic (sc) lattice.

3. ARRANGEMENT C
This is two dimensional version of centered simple cubic lattice like
ARRANGEMENT A, but with the difference that the center and corner spots
corresponding to center and corner atoms in the lattice are NOT identical. Here again
if any direction corresponds to nth order for the line of corner spots in any principal
direction, it will correspond to n/2 th order for alternate corner and central spots in the
same direction. The intensity of scattering by the centers and the corners is however
different. The result is that alternate orders (those corresponding to odd n) are of
different intensity. These are shown by blank circles. The diffraction pattern will look
as shown in Figure 9.
The distance between adjacent similar circles along principal directions are measured
randomly and their average is taken. Note that these correspond to orders differing by
two.

X1 = 12.8 mm X2 = 12.8 mm X3 = 12.8 mm

X4 = 12.8 mm X5 = 12.8 mm X6 = 12.8 mm
Average X = 12.8 mm

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 Distance L between the slide and the screen = 1000 mm

sinϕ 12.8/1000 = 0.0128

Lattice constant d = 2 λ/sinφ = (2 X 65X10-5)/0.0128 = 0.102 mm
Given value of d = 0.11 mm Error = 7.3%
This pattern with square symmetry and with alternate orders of different intensity is
indicative of a square array of different sized dots at the canters and the corners. It
corresponds to a cubic structure having two different kinds of atoms each surrounded by four
atoms of the other kind. A typical example is cubic ZnS crystal.

4. ARRANGEMENT D
This arrangement is exactly similar to ARRANGEMENT B. Difference is only in the
mesh size leading to a difference in the inter-spot distances in the diffraction pattern
(Figure 10). Random measurements are taken as before:
X1 = 6 mm X2 = 6 mm X3 = 6 mm
X4 = 6 mm X5 = 6 mm X6 = 6 mm
Average X = 6 mm

Distance L between the slide and the screen = 1000 mm

sinϕ = 0.006
Lattice constant d = λ/sinφ = (65X10-5)/0.006 = 0.108mm
Given value of d = 0.11 mm Error = 1.8%

5. ARRANGEMENT E
The diffraction pattern shows rectangular symmetry as expected (Figure 11). Random
measurements of inter-spot distances in the x- and y- directions are made and average
is taken.
X1 = 9 mm X2 = 9.5 mm X3 = 9.5 mm
X4 = 9.5 mm X5 9 mm X6 = 9 mm
Average X = 9.25 mm
Y1 = 4.5 mm Y2 = 4.5 mm Y3 = 4.5 mm
Y4 = 4.5 mm Y5 = 4.5 mm Y6 = 5.5 mm
Average Y = 4.5 mm
Distance L between the slide and the screen = 1000 mm
sinϕ1  tan = 9.25/ 1000 = 0.00925
sinϕ2  tan = 4.5/ 1000 = 0.0045

Lattice constant d1 = λ/sinφ1 = (65X10-5)/0.00925 = 0.07 mm

Lattice constant d2 = λ/sinφ1 = (65X10-5)/0.0045 = 0.144 mm

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Given value of d1 = 0.067 mm Error = 4.5%
Given value of d2 = 0.135 mm Error = 6.7%
Note the reciprocal lattice effect, Horizontal lines of dots in the slide have led to vertical lines
of spots in the diffraction pattern.

6. ARRANGEMENT F
This arrangement has the symmetry of a non-orthogonal parallelogram. The inter-spot
distance in the diffraction pattern (Figure 12) is measured randomly as shown and the
average is taken.
X1 = 16 mm X2 = 16 mm X3 = 16 mm
X4 = 16 mm X5 = 16 mm X6 = 16 mm
Average X = 16 mm
Distance L between the slide and the screen = 1000 mm

Sinϕ ϕ 16/1000 = 0.016

Inter-dot distance d1 = λ/sinφ1 = (65X10-5)/0.016 = 0.041mm
Given value of d = 0.04 mm Error = 2.5%

7. ARRANGEMENT G
This arrangement has a glide plane symmetry which leads to systematic absences in
the diffraction pattern. For example, every alternate dot in the central vertical column
is missing due to destructive interference resulting from the glide plane (Figure 13).
Inter-dot distance along the central vertical column = 54/6 mm = 9.0 mm
The adjacent dots in the central column correspond to orders differing by two.
Distance L between the slide and the screen = 1000 mm

sinϕ ϕ tanϕ = 9.0/1000 = 0.009

Lattice constant d1 = 2λ/sinφ1 = (2X65X10-5)/0.009 = 0.144 mm
Given lattice constant d1 = 0.14 mm Error = 2.9%
Measurement of inter-dot distances along the horizontal direction:
X1 = 4.0 mm X2 = 4.0 mm X3 = 4.0 mm
X4 = 4.0 mm X5 = 4.0 mm X6 = 4.0 mm
Average X = 4.0 mm

sinϕ ϕ tanϕ = 4/1000 = 0.004

Lattice constant d2 = λ/sinφ2 = (65X10-5)/0.004 = 0.1625 mm
Given value of d2 = 0.175 mm Error 7.1%

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8. ARRANGEMENT H
The diffraction pattern has hexagonal symmetry with 90o rotation with respect to the
dot arrangement in the slide. The hexagons in the pattern have vertical sides
corresponding to the horizontal sides in the slide (Figure 14). This is just a
manifestation of the reciprocal lattice effect.
Measurements of the sides of the hexagons in the pattern are made randomly and their
average is taken:
X1 = 4.9 mm X2 = 4.9 mm
X3 = 4.9 mm X4 = 4.9 mm
X5 = 4.9 mm X6 = 4.8 mm
X7 = 4.9 mm X8 = 5.0 mm
Average X = 4.9 mm
Distance L between the slide and the screen = 1000 mm

sinϕ ϕ tanϕ = 4.9/1000 = 0.0049

Lattice constant d = λ/sinφ = (65X10-5)/0.0049 = 0.133 mm
Given value of d = 0.135 mm Error = 1.5%

SAFETY PRECAUTION
The low power and long wavelength of the lasers employed in this experiment make them
relatively safe to use. However, care should be taken when using any laser not to point it
directly in anyone’s eye. If the central spot of the diffraction pattern is felt as being to
bright, a filter should be placed in front of the beam to diminish the intensity.

REFERENCES
1. Kittel, C. Introduction to Solid State Physics, John Wiley & Sons, New York, 1967

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