Professional Documents
Culture Documents
Dharmapadmi Pradnya Kasilani - Resume 1 Nanomedicine 3 Ta 2022
Dharmapadmi Pradnya Kasilani - Resume 1 Nanomedicine 3 Ta 2022
195160100111028
X-ray Diffraction
History of X-ray
• In 1895 Anna Bertha Röntgen and Wilhelm Conrad Röntgen discovers x-
rays. In 1901 they received the first Nobel Prize in physics.
• In 1914 Max Von Laue received the Nobel prize for physics, discovery of
the diffraction of x-ray by crystals "Diffraction pattern"
• In 1915 W.H. Bragg and his son W.L. Braggand the diffraction of x-ray by
crystals received the Nobel prize for physics, analysis of crystal structure
using x-rays
Phase identification
Phase identification of the sample includes obtaining XRD patterns,
measuring d-spacings and integrated intensities (dI list), and comparing data
with known standards in JCPDS/ICCDD files (> 200,000 files). JCPDS (Joint
Committee on Power Diffraction Standards, 1969) was replaced by ICDD
(International Center for Diffraction Data) in 1978.
ICCD database contains dI list for thousands of crystalline phases. The
PDF contains more than 200,000 diffraction patterns, a modern computer
program can help you determine what phases are present in your sample by
quickly comparing your diffraction data to all of the patterns in the database,
and the PDF card for an entry contains a lot of useful information (including
literature references).
Sample preparation
Powder in size 0.1µm less than particle size (<40 µm). Peak broadening
less diffraction occurs. Smooth the surface after polishing, specimens should be
thermally annealed to eliminate any surface deformation induce during
polishing. An x-ray diffractometer has an x-ray tube, Gobel mirror, goniometer,
Soller slit, and detector.
Advantages
• Powerful and rapid (<20 min) technique for identification of unknown
inorganic materials
• In most cases, it provides an unambiguous mineral determination
• Minimal sample preparation is required
• XRD units are widely available
• Data interpretation is relatively straightforward
Disadvantages
• Homogeneous and single-phase material is the best for identification of an
unknown
• Must have access to a standard reference file of inorganic compounds (d-
spacings, hkls)
• Requires tenths of a gram of material which must be ground into a power
• For mixed materials, the detection limit is (3% of the sample)
• For unit cell determinations, indexing of patterns for non-isometric crystal
systems is complicated
• Peak overlay may occur and worsens for high angel reflections