International
Tables for
Crystallography
Volume C
Mathematical, physical and chemical tables
Edited by E. Prince

International Tables for Crystallography (2006). Vol. C. ch. 7.4, pp. 663-664

Section 7.4.4.3. Detecting system

P. Suorttic

7.4.4.3. Detecting system

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The detecting system is an integral part of the X-ray optics of a diffraction experiment, and it can be included in the phase-space diagrams. In single-crystal diffraction, the detecting system is usually a rectangular slit followed by a photon counter, and the slit is large enough to accept all the reflected beam. The slit can be stationary during the scan (ω scan) or follow the rotation of the sample (ω/2θ scan). The included TDS depends on these choices, but otherwise the amount of background is proportional to the area of the receiving slit. It is obvious from a comparison between Fig. 7.4.4.1[link] and Fig. 7.4.4.3[link] that a much smaller receiving slit is sufficient in the parallel-beam geometry than in the conventional divergent-beam geometry. Mathieson (1985[link]) has given a thorough analysis of various monochromator–sample–detector combinations and has suggested the use of a two-dimensional ω/2θ scan with a narrow receiving slit. This provides a deconvolution of the reflection profile measured with a divergent beam, but the same result with better intensity and resolution is obtained by the parallel-beam techniques.

The above discussion has concentrated on improving the signal-to-background ratio by optimization of the diffraction geometry. This ratio can be improved substantially by an energy-dispersive detector, but, on the other hand, all detectors have some noise, which increases the background. There have been marked developments in recent years, and traditional technology has been replaced by new constructions. Much of this work has been carried out in synchrotron-radiation laboratories (for references, see Thomlinson & Williams, 1984[link]; Brown & Lindau, 1986[link]).

A position-sensitive detector can replace the receiving slit when a reciprocal space is scanned. TV area detectors with an X-ray-to-visible light converter and two-dimensional CCD arrays have moderate resolution and efficiency, but they work in the current mode and do not provide pulse discrimination on the basis of the photon energy. One- and two-dimensional proportional chambers have a spatial resolution of the order of 0.1 mm, and the relative energy resolution, [\Delta E/E\simeq 0.2], is sufficient for rejection of some of the parasitic scattering.

The NaI(Tl) scintillation counter is used most frequently as the X-ray detector in crystallography. It has 100% efficiency for the commonly used wavelengths, and the energy resolution is comparable to that of a proportional counter. The detector has a long life, and the level of the low-energy noise can be reduced to about 0.1 counts s−1.

The Ge and Si(Li) solid-state detectors (SSD) have an energy resolution ΔE/E = 0.01 to 0.03 for the wavelengths used in crystallography. The relative Compton shift, Δλ/λ, is [(0.024\,{\rm \AA}/\lambda)\times(1-\cos2\theta)], where 2θ is the scattering angle, so that even this component can be eliminated to some extent by a SSD. These detectors have been bulky and expensive, but new constructions that are suitable for X-ray diffraction have become available recently. The effects of the detector resolution are shown schematically in Fig. 7.4.4.5[link] for a scintillation counter and a SSD.

[Figure 7.4.4.5]

Figure 7.4.4.5| top | pdf |

Components of scattering at small scattering angles when the incident energy is just below the K absorption edge of the sample [upper part, (a)], and at large scattering angles when the incident energy is about twice the K-edge energy [upper part, (b)]. The abbreviations indicate resonant Raman scattering (RRS), plasmon (P) and Compton (C) scattering, coherent scattering (Coh) and sample fluorescence (Kα and Kβ). The lower part shows these components as convoluted by the resolution function of the detector: (a) a SSD and (b) a scintillation counter (Suortti, 1980b[link]).

Crystal monochromators placed in front of the detector eliminate all inelastic scattering but the TDS. The monochromator must be matched with the preceding X-ray optical system, the sample included, and therefore diffracted-beam monochromators are used in powder diffraction only (see Subsection 7.4.4.4[link]).

References

First citation Brown, G. S. & Lindau, I. (1986). Editors. Synchrotron radiation instrumentation. Proceedings of the International Conference on X-ray and VUV Synchrotron Radiation Instrumentation. Nucl. Instrum. Methods, A246, 511–595.Google Scholar
First citation Mathieson, A. McL. (1985). Small-crystal X-ray diffractometry with a crystal ante-monochromator. Acta Cryst. A41, 309–316.Google Scholar
First citation Suortti, P. (1980b). Components of the total X-ray scattering. Accuracy in powder diffraction, edited by S. Block & C. R. Hubbard, pp. 1–20. Natl Bur. Stand. (US) Spec. Publ. No. 567.Google Scholar
First citation Thomlinson, W. & Williams, G. P. (1984). Editors. Synchrotron radiation instrumentation 3. Proceedings of the Third National Conference on Synchrotron Radiation Instrumentation. Nucl. Instrum. Methods, 222, 215–278.Google Scholar








































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