Lab 4 Crystal Structure and

Diffraction Geometry
Objectives
Investigate the relationship between the geometry of
diffraction and the orientation of crystallographic planes in
single crystals
Plot crystallographic planes and diffraction experiments in
reciprocal space

Experiment
Diffraction of Si powder
Diffraction of single crystal Si (001)
Locate diffraction peaks from single crystal wafer
Copper X - ray source (Cu k1)
40 KV, 30 mA for powder scan
40 KV, 30 mA for Si (001)

Powder Diffraction

The orientation of the powder is random

on the glass surface. Just by this random
distribution, any planes can end up such
that they are parallel to the surface. Thus
all possible reflections will show up in a
2- scan.

(110)

(200)

(211)

Equations we already know

Braggs Law
n = 2 dhkl sin
D-Spacing Calculations

Si PDF

Single Crystal Diffraction

The orientation of the single crystal is

fixed on the surface. Thus only the
surface symmetric planes that are
possible reflections will show up in a
normal 2- scan.

(004)

10

Powdered vs Single Crystal

Diffraction
(004)

10

Single Crystal Si
Powdered Si

10

Intensity (cps)

10

10

10

(220)

10

10

-1

10

-2

10

10

20

30

40

50

60

70

2 (degrees)

80

90

100

110

Question: How can we

access other diffraction
peaks in a single
crystal?

(hkl)

d ()

G.E./G.I.

2Theta

111
111
220
202
202
113
113

004
331
331
224
224
115
115
333
333
404
404

???

Omega

Phi

Intensity

(hkl)

d ()

G.E./G.I.

2Theta

Omega

Phi

111
111
220
202
202
113
113

004
331
331
224
224
115
115
333
333
404
404

What is the surface to plane angle for (110)?

Intensity

Interplanar Angles
Cubic
cos = (h1h2 + k1k2 + l1l2) / sqrt ((h12 + k12 + l12)(h22 + k22 + l22))
(004) and (110)
cos = ((0)(1)+(0)(1)+(4)(0))/ sqrt ((16)(2))
cos = 0
= 90

(hkl)

d ()

G.E./G.I.

2Theta

Omega

111
111
220
202
202
113
113

004
331
331
224
224
115
115
333
333
404
404

Is there a relationship between these three columns?

What is GI and GE?

Phi

Intensity

Glancing Incidence
Incident

Diffracted

= b -

Glancing Exit
Incident

Diffracted

= b +

What difference can we expect

from G.E. and G.I.?
Sampling area
Outgoing intensity
Resolution

Reciprocal Space
An easier way to represent diffraction
geometries, easier to visualize than real
space

Real space

Reciprocal space

Reciprocal Space
Interplanar spacing reciprocal value
Angles preserved
Crystal structure preserved
[001]
(003)
(001)
1 / d002

1 / d001

(002)
(001)
[110]

(110)
What is larger d001 or d002 ?

(000)

Reciprocal Space
[001]

d111

(220)

(111)

[110]

What is larger d001 or d110 ?

Remember reciprocal space
is a 3d space, not all
reflections will be shown
here.

d110

Lab preparation
Si lattice parameter: 5.4309
X-ray wavelength: 1.54056
Single crystal Si wafer surface: (001)
Fill in blanks of the table on the handout.
Available diffraction spot:
h, k, l are all odd.
h, k, l are all even and h+k+l can be divided by 4.

d ()

G.E./G.I.

2Theta

Omega

220

1.92011

90

G.E.

47.302

113.651

202

1.92011

45

G.E.

47.302

68.651

202

1.92011

45

G.I.

47.302

-21.349

1.35773

Symmetric

69.129

34.564

(hkl)

Phi

111
111

113
113
004

331
331
224
224

115
115
333
333
404
404

Arbitrary

Intensity

(hkl)

d ()

G.E./G.I.

2Theta

Omega

Phi

111

3.13553

54.736

G.E.

28.442

68.957

N/A

111

3.13553

54.736

G.I.

28.442

-40.515

N/A

220

1.92011

90.000

G.E.

47.302

113.651

N/A

202

1.92011

45.000

G.E.

47.302

68.651

N/A

202

1.92011

45.000

G.I.

47.302

-21.349

N/A

113

1.63748

25.239

G.E.

56.121

53.300

113

1.63748

25.239

G.I.

56.121

2.821

004

1.35773

Symmetric

69.129

34.564

Arbitrary

331

1.24593

76.737

G.E.

76.375

114.925

N/A

331

1.24593

76.737

G.I.

76.375

-38.550

N/A

224

1.10858

35.264

G.E.

88.028

79.279

224

1.10858

35.264

G.I.

88.028

8.750

115

1.04518

15.793

G.E

94.950

63.268

115

1.04518

15.793

G.I

94.950

31.682

333

1.04518

54.736

G.E.

94.950

102.211

N/A

333

1.04518

54.736

G.I

94.950

-7.260

N/A

404

0.95988

45.000

G.E.

106.706

98.353

45

404

0.95988

45.000

G.I.

106.706

8.353

45

Intensity