We have learnt

How do the crystallites arrange in a polycrystalline material How to represent polycrystal information in stereographic projection Macro- and micro- texture The principles of macro or bulk texture measurements by X-ray diffraction

Todays objective
To know the texture measurement procedure by X-ray diffraction

Measurement strategy:
First step: Record the X-ray diffraction pattern (normal Bragg scan) to identify the peak position -Deviation of relative intensities in a /2 scan from powder file indicate the presence of texture but it is not possible to identify the texture component by normal Bragg scan

Second step:Fix the Bragg angle for the peak for which the pole figure is to be measured. -Pole figure is measured with 5-axis goniometer Schulz Reflection Method -X-ray beam must not be transmitted through the specimen thickness>~0.2 mm

What are the 5 axes of the goniometer? 2 axes used to set Bragg angle. One has to choose a specific crystallographic plane with /2 axes, the plane for which the pole figure has be determined. Third axis tilts specimen plane w.r.t. the focusing plane. This is actually the rotation about an axis perpendicular to the sheet surface (angle )

Fourth axis spins the specimen about its normal. This rotation is about an orthogonal axis through angle .
Fifth axis oscillates the Specimen under the beam. This is a simple translation to and fro it improves the statistical averaging of the texture measurement by increasing the number of grains that are sampled

 Diffractometer is set in Bragg-Brentano geometry

In Bragg-Brentano Geometry, Eulerian cradle is set in such a way that the circle coincides with the bisector of the angle between incident and diffracted beam, and any direction on the pole figure can be brought parallel to this direction by the two rotations 90- and corresponding to the pole figure coordinates and .
This geometry also implies that the incident beam is divergent and diffracted beam is convergent

The combination of angles by which the sample rotates, leads to irradiation of almost all the crystallites.

One of the oldest models of X-ray texture goniometer is shown here. The figure clearly depicts all the components of the diffractometer based on Schulz reflection geometry.

Figure adapted from: Introduction to texture by M. Hatherly and W.B. Hutchinson

1. Source; 2. Divergence slit; 3. Narrow horizontal slit; 4. Specimen; 5. Major circle of the goniometer; 6. Receiving slit; 7. Counter.

A modern texture goniometer at Indian Institute of Science, Bangalore Mark the difference!!

 The already set Bragg peak (for example, 111 or 200 for face centred cubic materials) is recorded for all the combinations of angles

Next, the specimen is arranged with RD pointing vertically. This leads to sheet normal bisect angle between incident and diffracted beams, ND coincides with diffracting vector K. In this case, measured intensity comes from the (hkl) planes || sheet plane The specimen is rotated by = 90o (along Euler Cradle). Tphis leads to RD || K . In this situation, the measured intensity corresponds to RD. This type of rotation gives radial scan of the pole figure. Next, the specimen is rotated by = 90o (about axis perpendicular to specimen surface). This situation corresponds to TD || K. The diffracted intesity is sampled around the periphery of the pole figure.

 A fast rotation through + a slow rotation through is equal to the diffracted intensity along the spiral trace Total intensity to the counter
This way for each combination of and , the same Bragg peak (hkl) is recorded. The intensity variation for different angles gives an account of texture present in the material, as shown below.
The intensity is normalised by recording a diffraction pattern from a powder (random) sample. The intensity ratio is plotted on a polar graph to result in a pole figure.

Practical Aspects Typical to measure three PFs for the 3 lowest values of Miller indices.

Why?
A single PF does not uniquely determine orientation(s),

texture components because only the plane normal is

measured, but not directions in the plane (2 out of 3

parameters).
Multiple PFs required for calculation of Orientation Distribution.

1.

Questions If you are given two identical looking samples of a metallic material, how will you decide whether this is a single crystal or a polycrystal? If you are given a single crystal and unable to get a particular diffraction pattern, what will you do to locate the same.

In the measurement complete (111) pole figure, if the data is recorded at 5 intervals in both and angles, how many times the (111) peaks are recorded? 3. Describe the role of all the axes in a five axis goniometer as used in Schulz reflection geometry. 4. Can you measure the (111) pole figure for a steel samples? If yes, which peak will be fixed for measurement of texture? 5. 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 2.