X-RAY POWDER DIFFRACTIONS

The atomic planes of a crystal cause an incident beam of X-rays to interfere with one another as they leave the crystal. The phenomenon is called X-ray diffraction

Why XRD? Measure the average spacings between layers or rows of atoms

Determine the orientation of a single crystal or grain Find the crystal structure of an unknown material Measure the size, shape and internal stress of small crystalline regions

Identification of single-phase materials minerals, chemical compounds, ceramics.

Identification of multiple phases in microcrystalline mixtures (i.e., rocks)

English physicists Sir W.H. Bragg and his son Sir W.L. Bragg developed a relationship in 1913 to explain why the cleavage faces of crystals appear to reflect X-ray beams at certain angles of incidence (theta, q). The variable d is the distance between atomic layers in a crystal, and the variable lambda l is the wavelength of the incident X-ray beam; n is an integer. This observation is an example of X-ray wave interference (commonly known as X-ray diffraction (XRD), and was direct evidence for the periodic atomic structure of crystals postulated for several centuries.

Instrumentation

X-ray tube Sample holder Detector slits

Production of x-rays

Principles of generation

Sample preparation The Ideal Specimen is a statistically infinite amount of randomly oriented powder with crystallite size less than 10 m, mounted in a manner in which there is no preferred crystallite orientation.

The radiation produced in the tube includes K1, K2, and K We generally use the K for analytical work. The K radiation is usually removed by use of a filter, a monochromator or an energy-selective detector. The K2 radiation is removed from the X-ray data electronically during data processing Filters for removing K may be located in the beam path on the generator or detector side of the path; a series of parallel plates (soller slits) arranged parallel to the plane of the diffractometer circle and several scatter and receiving slits (arranged perpendicular to the diffractometer circle) are used to create an incident beam of X-rays that are (approximately) parallel.

scintillation counter.
large-window position sensitive detector or PSD

Legacy Methods:, X-ray diffraction data derived by film methods or by diffractometers using paper strip-chart recorders. The resultant data were derived by physically measuring peak positions and intensities, and the diffraction data recorded as a list of peaks (in degrees 2) and relative intensities (scaled from 0 to 100).