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. 2.1, pp. 35-36

Section 2.1.5.3.2. Non-coplanar beam-path systems

A. Kerna*

aBruker AXS, Östliche Rheinbrückenstrasse 49, Karlsruhe 76187, Germany
Correspondence e-mail: arnt.kern@bruker-axs.de

2.1.5.3.2. Non-coplanar beam-path systems

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Non-coplanar (or `in-plane') grazing-incidence diffraction is a technique for investigating the near-surface region of specimens (ten or fewer nanometres beneath the air–specimen interface). It exploits the high intensity of the total external reflection condition while simultaneously involving Bragg diffraction from planes that are nearly perpendicular to the specimen surface.

As illustrated in Fig. 2.1.11[link], the incident beam is set at an angle αI, enabling total external reflection in the coplanar direction (that is coplanar to the diffraction plane); related applications include reflectometry and grazing-incidence small-angle X-ray scattering (GISAXS). `In-plane' grazing-incidence diffraction (IP-GID) may be measured at angles 2θIP-GID in the non-coplanar direction at an exit angle αF.

[Figure 2.1.11]

Figure 2.1.11 | top | pdf |

Illustration of coplanar and in-plane diffraction. S: X-ray source. θI, θD: incident and diffracted beams for coplanar diffraction. αI, αF, 2θIP-GID: incident-beam angle, exit angle and diffracted-beam angle, respectively, for in-plane grazing-incidence diffraction.

There are two principal instrument designs implementing coplanar and in-plane data collection. Firstly, as is obvious from Fig. 2.1.11[link], a dual-goniometer system may be employed. The most sophisticated implementation has two goniometers placed vertically one above the other, allowing simultaneous coplanar and in-plane measurements using two independent scattered-beam optical X-ray benches as shown in Fig. 2.1.12[link]. Alternatively, the second goniometer may be integrated into the scattered-beam optical X-ray bench, allowing sequential coplanar and in-plane measurements. As a further alternative, a single goniometer may be used, with a Eulerian cradle mounted at the detector position, allowing the detector to be moved around the specimen to perform in-plane measurements. Secondly, a single goniometer equipped with a Eulerian cradle may be used, where the specimen is simply turned by 90° in ψ. As line focus is usually employed for IP-GID measurements, the X-ray source is also turned by 90° to increase the flux.

[Figure 2.1.12]

Figure 2.1.12 | top | pdf |

Sophisticated IP-GID implementation by placing two goniometers vertically with respect to each other, allowing simultaneous coplanar and in-plane measurements using two independent scattered-beam optical X-ray benches (compare with Fig. 2.1.2[link]). The sample stage may be mounted at position 3 or 3′.

For all systems, the diffracted-beam optical X-ray benches may be equipped as for multiple beam-path systems, as described in Section 2.1.5.3.1[link], providing extremely high flexibility. The choice of the most appropriate design depends on issues such as specimen size and weight, the weight of any components in the diffracted-beam path, related spheres of confusion, and the potential need to measure the specimen in a horizontal position.








































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