X-Ray Diffraction and Crystal Structure

Objective
The goals of this experiment are to use x-ray spectrums to identify unknown materials.
This is done by matching reflection peaks with a plane in the crystal structure of the unknowns.
The crystal structure and lattice constant of the material can then be identified, and the
unknown’s identity can be determined from this information.
Background
A crystal is simply a lattice and a basis, put together. A basis is a “unit” of a crystal, and
it is repeated according to the lattice, a 3-dimensional set of points. The basis can contain any
amount of atoms, these atoms are just repeated on every point of the lattice.
Not all lattices are the same though. In particular, cubic crystal systems will have simple
cubic (sc), body-centered cubic (bcc), or face-centered cubic (fcc) lattices. For the purposes of
this experiment, the diamond lattice is also considered. For each lattice type, there are certain
planes that are reflected in x-ray diffraction and ones that are not. These are called the extinction
rules for each lattice, and they are shown in the appendix. This will appear as a peak in the x-ray
spectrum of the material. Once the wavelength of said peak is determined, we can use the Bragg
condition to determine the lattice constant of the material

λ √h2 + k 2+ l2
sin θ=
2a
Where a is the lattice constant, and h, k, and l are numbers used to represent the plane in the
crystal. These numbers are also how we define the extinction rules:
 Sc: all h,k,l allowed
 Bcc: h+k+l must be even
 Fcc: h,k,l must be all even or all odd
 Diamond: must be all even or all odd, and if all even then h+k+l=4n where n is an
integer
Experimental Procedures
Using a TEL-X-OMETER like in the previous experiment, we find the k alpha and k beta
peaks of a single NaCl crystal, and unknown alkali halide crystal, and two silicon wafers, cut
differently.
Data & Analysis
The silicon powder has a diamond structure, thus, according to the extinction rules for
diamond structure, the 111, 220, 311, 400, 331 reflection peaks are seen.
 Identify peak of Si wafer by hkl value
o The first, cut horizontally and parallel to the 100 plane, must be 400, the lowest
allowable peak parallel to 100.
 o The second, cut diagonally, must be 111
 Identify hkl of NaCl peak and explain why d spacing is half lattice constant
o 200, d spacing is a/2 according to eq. 1
 Explain why d spacing of LiF is half of lattice constant
o The LiF peak must have also been 200
 Identify hkl of unknown crystal, lattice constant, and the compound
o Hkl is 200,
 Identify compound of unknown powder
 Identify hkl of second order LiF peak
o Must be 220 (fcc)
Conclusions
Using the extinction laws and the Bragg condition, we can determine the lattice constant
of unknown materials.
Appendix

Extinction Rules

plane h2+k2+l2 Sc? Bcc? Fcc? Diamond?

100 1y n n n
110 2y y n n
111 3y n y y
200 4y y y n
210 5y n n n
211 6y y n n
220 8y y y y
221 9y n n n
300 9y n n n
310 10 y y n n
311 11 y n y y
222 12 y y y n
320 13 y n n n
321 14 y y n n
400 16 y y y y
322 17 y n n n
410 17 y n n n
330 18 y y n n
411 18 y y n n
331 19 y n y y