International
Tables for
Crystallography
Volume H
Powder diffraction
Edited by C. J. Gilmore, J. A. Kaduk and H. Schenk

International Tables for Crystallography (2018). Vol. H, ch. 2.5, p. 138

## Section 2.5.4.2.3. Data-collection strategy

B. B. Hea*

aBruker AXS Inc., 5465 E. Cheryl Parkway, Madison, WI 53711, USA
Correspondence e-mail: bob.he@bruker.com

#### 2.5.4.2.3. Data-collection strategy

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Since a one-dimensional pole-density mapping is created from each 2D frame, it is important to lay out a data-collection strategy so as to have the optimum pole-figure coverage and minimum redundancy in data collection. The pole-figure coverage can be simulated from the diffraction 2θ angle, detector swing angle, detector distance, goniometer angles and scanning steps. When a large 2D detector is placed close to the sample, it is possible to collect a pole figure with a single ϕ scan. Fig. 2.5.20(a) shows an example of a scheme generated by a single ϕ scan of 5° steps with a detector 10.5 cm in diameter and D = 7 cm. The data collected with a single exposure at ϕ = 0° would generate a one-dimensional pole figure as shown in the curve marked by A and B. The pole figure can be generated by a full-circle rotation of 360°. The pole density at the centre represents the diffraction vector perpendicular to the sample surface. It is important to have the pole-density information in the centre region of the pole figure, especially for fibre texture. The pole-figure angle at the centre is α = 90°, and the best strategy is to put point A at the centre of pole figure. That is

 Figure 2.5.20 | top | pdf |Data-collection strategy: (a) 2D detector with D = 7 cm; (b) 2D detector with D = 10 cm; (c) point detector.

In some cases, a single ϕ scan is not enough to cover sufficient pole-figure angles because of a large detector distance or limited detector area, so it is necessary to collect a set of data with ϕ scans at several different sample tilt angles. Fig. 2.5.20(b) illustrates the data-collection scheme with a detector that is 10.5 cm in diameter and D = 10 cm for the (111) plane of a Cu thin film. In this case, each pole figure requires two ϕ scans at different sample orientations. The data-collection strategy should also be optimized for several crystallographic planes if all can be covered in a frame. The step size of the data-collection scan depends highly on the strength of the texture and the purpose of the texture measurements. For a weak texture, or quality control for metal parts, ϕ (or ω, or ψ) scan steps of 5° may be sufficient. For strong textures, such as thin films with epitaxial structure, scan steps of 1° or smaller may be necessary.

The effectiveness of two-dimensional data collection for a texture can be compared with that using a point detector with the data-collection strategy of the Cu thin film as an example. Fig. 2.5.20(c) shows the pole-figure data-collection strategy with a point detector. For the same pole-figure resolution, significantly more exposures are required with a point detector. Considering that several diffraction rings are measured simultaneously with a 2D detector, the pole-figure measurement is typically 10 to 100 times faster than with a point detector. Therefore, quantitative high-resolution pole-figure measurements are only practical with a 2D-XRD system (Bunge & Klein, 1996).

### References

Bunge, H. J. & Klein, H. (1996). Determination of quantitative, high-resolution pole-figures with the area detector. Z. Metallkd. 87(6), 465–475.Google Scholar