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Todays objective

To know the limitations of the texture measurement procedure and ways to overcome them

Limitation of Schultz method


Defocussing error: X-ray beam becomes defocused at large tilt angles (>~60). The combination of the -2 setting and the tilt of the specimen face out of the focusing plane spreads out the beam on the specimen surface. Above a certain spread, not all the diffracted beam enters the detector. Therefore, at large tilt angles, the intensity decreases for purely geometrical reasons. This loss of intensity must be compensated for, using the defocussing correction.

How to correct the Defocussing error? Narrow divergence slit

affects total count rate and statistical significance of the measurement reduces peak to background ratio

Wide receiving slit-

Larger Bragg angle by changing to a lower wavelengthsevere reduction in count rate

Background count must be subtracted. Icorr = Imeas (,) BG () Defocusing correction required to increase the intensity towards the edge of the PF. Icorr = Imeas (,) BG () U() Random texture (=uniform dispersion of orientations) means same intensity in all directions. measured intensity from random sample decreases towards edge of PF.
Some other corrections are also desired:
Absorption I(t)/I = 1- exp(-2t / Sin Cos ) Couting Statistics

Pole figure normalization


In X-ray diffraction experiments, as done during the determination of pole figures, the intensities are obtained in the form of counts (or counts per second; cps). The pole density is measured in terms of multiples of random intensity Normalization is the operation that ensures that random is equivalent to an intensity of one.

Inorm(, ) = (1/N). Icorr (, )


This is achieved by integrating the un-normalized intensity, f(,), over the full area of the pole figure, and dividing each value by the result, taking account of the solid area. Thus, the normalized intensity, f( ,), must satisfy the following equation, where the 2 accounts for the area of a hemisphere:

Questions
(1) What can be directly measured by experiment: (a) inverse pole figure (b) orientation distribution function (c) pole figure (d) all the above (2) In the Schulz reflection method, which of the following is correct: (a) the tilt angle enables most of the grains to come under diffraction condition (b) the rotation angle enables most of the grains to come under diffraction condition (c) the tilt angle brings the diffraction vector coincident with the specimen axes alternately (d) the rotation angle brings the diffraction vector coincident with the specimen axes alternately (3) Which of these are the limitations of pole figures: (a) specific (hkl) planes can not be plotted (b) poles in the final plot for a polycrystalline material are not identified with particular crystals (c) information about the crystallite location in a sample is absent (d) the orientation of a crystal must be described relative to another

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