Powder
X-ray Diffraction (XRD) is one of the primary techniques
used by mineralogists and solid state chemists to examine the physico-chemical
make-up of unknown solids. This data is represented in a collection of
single-phase X-ray powder diffraction patterns for the three most intense D
values in the form of tables of interplanar spacing (D), relative intensities
(I/Io), and mineral name.
X-ray powder
diffraction (XRD) is a rapid analytical technique primarily used for phase
identification of a crystalline material and can provide information on unit
cell dimensions. The analyzed material is finely ground, homogenized, and
average bulk composition is determined.
Max von Laue, in 1912, discovered
that crystalline substances act as three-dimensional diffraction gratings for
X-ray wavelengths similar to the spacing of planes in a crystal lattice. X-ray
diffraction is now a common technique for the study of crystal structures and
atomic spacing.
X-ray
diffraction is based on constructive interference of monochromatic X-rays and a
crystalline sample. These X-rays are generated by a cathode ray tube, filtered
to produce monochromatic radiation, collimated to concentrate, and directed
toward the sample. The interaction of the incident rays with the sample
produces constructive interference (and a diffracted ray) when conditions
satisfy Bragg's Law (nλ=2d sin θ). This law relates the
wavelength of electromagnetic radiation to the diffraction angle and the
lattice spacing in a crystalline sample. These diffracted X-rays are then
detected, processed and counted. By scanning the sample through a range of
2θangles, all possible diffraction directions of the lattice should be attained
due to the random orientation of the powdered material. Conversion of the
diffraction peaks to d-spacings allows identification of the mineral because
each mineral has a set of unique d-spacings. Typically, this is achieved by
comparison of d-spacings with standard reference patterns.
All
diffraction methods are based on generation of X-rays
in an X-ray tube. These X-rays are directed at the sample, and the diffracted
rays are collected. A key component of all diffraction is the angle between the
incident and diffracted rays. Powder and single crystal diffraction vary in
instrumentation beyond this.