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IGCAR : Annual Report - Indira Gandhi Centre for Atomic Research

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IGC<br />

<strong>Annual</strong> <strong>Report</strong> 2007<br />

VI.12. X-ray Diffraction Studies using Imaging Plate as<br />

an Area Detector<br />

Imaging plate based X-ray<br />

area detectors were initially<br />

used <strong>for</strong> protein crystallography<br />

in the 1980s and more recently,<br />

their use has extended to smallmolecule<br />

structural analyses<br />

and powder diffractometry. The<br />

usage of imaging plate is<br />

particularly advantageous <strong>for</strong><br />

the characterization of<br />

polycrystalline materials since it<br />

permits simultaneous collection<br />

of many orders of Bragg<br />

reflections. There is also a<br />

significant size advantage<br />

compared to CCD based area<br />

detector. In addition to the<br />

enormous reduction of data<br />

acquisition time <strong>for</strong> analyses,<br />

two-dimensional diffraction<br />

patterns contain much more<br />

in<strong>for</strong>mation than conventional<br />

linear scans (i.e. - 2 scans)<br />

collected using standard<br />

powder diffractometers. Two<br />

dimensional diffraction patterns<br />

of polycrystalline samples<br />

typically consist of concentric<br />

(Debye-Scherrer) rings<br />

produced by the superposition<br />

of reflections from many<br />

crystals illuminated by the X-ray<br />

beam, which are oriented with<br />

a set of (hkl) crystallographic<br />

planes oriented to fulfill the<br />

Bragg condition. Depending on<br />

sample characteristics, these<br />

rings might be continuous or<br />

spotty and display specific<br />

variation in the intensities along<br />

them. These features contain<br />

important in<strong>for</strong>mation about<br />

the microstructure of the<br />

sample: grain size, preferential<br />

orientation, mosaicity, stress<br />

etc. Additionally, twodimensional<br />

patterns can be<br />

converted into conventional<br />

linear scans by radial or<br />

azimuthal integration of pixel<br />

intensities. The generated linear<br />

scans can be processed as<br />

usual <strong>for</strong> mineral phase<br />

identification, crystallinity or<br />

Rietveld refinement studies.<br />

Nevertheless, during this data<br />

reduction procedure, most of<br />

the in<strong>for</strong>mation regarding the<br />

microstructure of the material is<br />

lost. Hence to get the full<br />

advantage of two-dimensional<br />

diffraction <strong>for</strong> polycrystalline<br />

materials we have to extract the<br />

in<strong>for</strong>mation contained in the<br />

two dimensional diffraction<br />

patterns. Here we are reporting<br />

the diffraction experiment<br />

results obtained using the<br />

imaging plate as an area<br />

detector <strong>for</strong> both single crystal<br />

and powder experiments. The<br />

imaging plate reader has 5<br />

mega pixel resolution <strong>for</strong> 250<br />

mm X 200 mm size plate with<br />

each pixel size of 100 the<br />

data file size is 10 Mbytes.<br />

Fig.1 Laue diffraction pattern of a Si single crystal obtained using the<br />

Imaging plate as an area detector (the plate read using reader developed<br />

at MSD <strong>IGCAR</strong>). The inset shows the maximum zoom of a diffraction point<br />

and its intensity profile in surface and line plot.<br />

Laue X-ray diffraction is<br />

historically the first diffraction<br />

method <strong>for</strong> structural<br />

166 BASIC RESEARCH

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