X-ray powder diffraction (XRD) is used to analyze crystalline compounds on an atomic level. By shooting an X-ray beam at a sample, XRD can measure how the beam is diffracted by different sections of the compound, providing information about its composition, structure, and crystalline size. The basic components of an XRD instrument include an X-ray source like an X-ray tube or radioactive isotope, a wavelength selector using filters or monochromators, a sample holder that rotates the sample, and an X-ray detector like a gas detector, scintillation counter, or semiconductor detector.

1. Instrumentation- XRD
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2. Basics
X-ray powder diffraction---or XRD---is used to measure crystalline compounds and
provides a quantitative and qualitative analysis of compounds that cannot be measured
by other means. By shooting an X-Ray at a compound, XRD can measure the diffraction
of the beam from different sections of the compound. This measurement can then be
used to understand the composition of the compound on an atomic level, since all
compounds diffract the beam differently. XRD measurements show structural make-up,
content and size of crystalline structures.

5. COMPONENTS
Source
Wavelength selector
Sample holder
Detector
Recorder

6. Source
X-ray tube
Radioisotope

7. X-ray tube or Coolidge tube
• Most common source
• Cathode
• Anode
• Berrylium window
• Disadvantage:
• Poor output efficiency (5%)

8. Production of X-rays using
radioisotopes:
• Certain radioactive substances
produce X-rays as a result of their
radioactive decay process.

9. Wavelength selector
Filters-
◦ thin metallic strips of definite thickness eg. Zirconium filter
Monochromators-
◦ these are crystals which can diffract X-rays according to their wavelength.

10. A crystal monochromator
• A useful wavelength range from a
crystal is determined by its lattice
spacing d
• Crystal is placed on a rotating table
or a goniometer
• Works on the principle of Bragg’s
equation
• Rays of different wavelengths can
be collected by varying angle θ.

11. Sample holder
It is a rotating table called as crystal mount
Sample is placed at the centre of a crystal mount, which is kept rotating
at a particular speed.

12. Detector
Gas filled detector
Scintillation counter
Semiconductor detector

13. Gas filled detector

15. Semiconductor detector

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