Lecture Notes - Powder Diffraction
• X-ray diffraction by mineral powders is one of the mineral identification and
characteriziation techniques most used by geologists. Powder diffraction experi-
ments require only a small quantity of a mineral. As little as 10 mg can yield good
data, although 500 mg is the quantity required for common sample mounts. Sample
preparation is extremely simple — no crystal faces or cleavages are needed for
crystallographic orientation, because no sample orientation is required. Reliable,
accurate results are obtained in a relatively short time (10 minutes to 2hours).
• The principle behind the design of powder diffraction experiments is the random
orientation of crystals in a mineral powder. If the powdered crystals are randomly
oriented, then for all sets of planes (hkl) some of the crystals in the powder will be
in the correct orientation (usually horzontal) with respect to the x-ray source to
satisfy Bragg’s law for the proper angle θ. In other words, at least a few of the
mineral grains in the powder will diffract for each of the planes (hkl) during a scan
through the angles θ. The more finely ground the powder, the more likely that all
orientations are present in abundance. The ideal powder size is 5-10 µm.
• Two main types of powder diffraction experiments are possible at Smith: automated
powder diffractometer experiments yielding (digital) computer output and Debye-
Sherer experiments providing (analog) film output. In the Debye-Sherer camera, a
strip of film is wrapped around the powder sample so that diffracted beams from a
fixed x-ray source may be recorded for all values of θ simultaneously. The powder
diffractometer moves both the x-ray source and an electronic detector through arcs
X-ray
s tor
detec
θ θ
θ
2θ
of θ values and sends to a computer periodic signals proportional to the averaged
diffracted x-ray intensity. Both experiments provide the intensities for diffracted
beams as a function of the diffraction angle θ (or 2θ).
Powder Diffraction 2
• Mineral unknowns may be identified from powder diffraction data using the ICDD
Powder Diffraction File. Both intensity and 2θ (or dhkl) values are used in the
search. Computer searchs of the file (on CDROM) may lead to a unique match
with a known powder diffraction pattern. However, because the chemical composi-
tion of most minerals is variable, because some aspects of a minerals structure may
depend on its history, and because any measurement contains some error, the ob-
served diffraction data may not exactly match the standard data for a given mineral.
This makes identification more challenging and chemical data or other physical
property data may be needed to confirm a result for some samples.
• Once a mineral has been identified, the Powder Diffraction File data card may be
used to index the observed diffraction peaks. Miller indices along with measured
2θ values (from which dhkl can be calculated using Bragg’s law) may be used to
determine the unit cell parameters of the specimen. In principle, six measured dhkl
values are sufficient to determine the six unknown unit cell parameters. However, a
more accurate result will be obtained if more dhkl values are used to "over deter-
mine" the solution. Various computer programs are available to perform a least
squares data reduction on the over-determined data set to give a “best fit” unit cell.
If the unit cell of a standard is known, values for each dhkl can be calculated and
compared with observed d’s to see how closely the data match the standard unit
cell.
33-1161 Qualit y: Qualit y Dat a
Si O2
Silicon Oxide
Quart z, Syn
Rad:CuKa1 Lambda:1.540598 Filt er:Monochromat or cryst al used d sp:Diffract omet er
Cut off: Int :Diffract omet er I/Icor:3.6
Ref:Swanson, Fuyat ., 18 61, (1981)
Sys:Hexagonal S.G.:P 3221
a:4.9133±0.0002 b: c:5.4053±0.0004
α: β: γ: Z:3 mp
Ref2
Dx:2.649 Dm:2.649 SS/FOM: F30=76.6(0.0126,31) Volume[CD]:113
εα: ηωβ :1.544 εγ:1.553 Sign:+ 2V:
Ref3
Color:Colorless
Sample from t he Glass Sect ion at NBS, Gait hersburg, Maryland, USA, ground single-cryst als of opt ical qualit y. T o replace 5-490.
P lus 6 reflect ions t o 0.9089. P att ern at 25 C. P at t ern reviewed by J. Holzer and G. McCart hy, Nort h Dakota St at e Universit y,
Fargo, Nort h Dakot a, USA, \IT JCP DS Grant -in-Aid Report \RG (1990). Agrees well wit h experimental and calculat ed pat t erns.
39 reflect ions in pat t ern.
2θ Int . h k l 2θ Int . h k l 2θ Int . h k l 2θ Int . h k l
20.8501 22 1 0 0 55.3283 2 1 0 3 77.6619 1 2 2 0 94.6651 1 1 0 5
26.6519 100 1 0 1 57.2380 1 2 1 0 79.8778 2 2 1 3 95.1187 1 4 0 1
36.5421 8 1 1 0 59.9485 9 2 1 1 80.0461 1 2 2 1 96.2267 1 2 1 4
39.4559 8 1 0 2 64.0009 1 1 1 3 81.1475 3 1 1 4 98.7375 1 2 2 3
40.2836 4 1 1 1 65.7605 1 3 0 0 81.4721 3 3 1 0 102.1991 1 4 0 2
42.4650 6 2 0 0 67.7497 6 2 1 2 83.8208 1 3 1 1 102.5594 1 3 1 3
45.8092 4 2 0 1 68.1305 7 2 0 3 84.9713 1 2 0 4 103.8839 1 3 0 4
50.1407 14 1 1 2 68.3227 8 3 0 1 87.4640 1 3 0 3 104.1993 1 3 2 0
50.6111 1 0 0 3 73.4620 2 1 0 4 90.8583 2 3 1 2 106.1453 1 2 0 5
54.8689 4 2 0 2 75.6706 2 3 0 2 92.8224 1 4 0 0
