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

International Tables for Crystallography (2018). Vol. H, ch. 2.9, p. 189

Section 2.9.2. Historical perspective

W. van Beeka* and P. Pattisona,b

aSwiss–Norwegian Beamlines at ESRF, CS 40220, 38043 Grenoble CEDEX 9, France, and bLaboratory for Quantum Magnetism, Institute of Physics, Ecole Polytechnique Federale de Lausanne, CH-1015 Lausanne, Switzerland
Correspondence e-mail:

2.9.2. Historical perspective

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Within a decade of the discovery of the Bragg law, Westgren & Lindh (1921[link]) had already observed several different polymorphs of iron as a function of temperature using powder diffraction. We have recently celebrated the centenary of the founding of X-ray crystallography, and during this time the use of in situ powder diffraction has become immensely popular. Although most of the pioneering powder-diffraction experiments were performed with X-ray tubes and scanning point detectors or with neutrons and an array of detectors, the real breakthrough came with the advent of synchrotron sources, providing high-energy penetrating X-rays, in combination with area detectors. This combination of source and detector type allowed diffraction experiments to be performed with both good angular and time resolution, thus opening up many new applications in chemical, physical, material and biological sciences. The topic of in situ cells for chemical reactions is therefore an enormous field and we cannot claim to provide an exhaustive list of instruments. We rather intend to point out the major cell designs, and to provide the reader with an overview to allow them to select the appropriate device for their application and available diffraction apparatus. We have tried to select where possible in situ case studies that use the full power of crystallography by solving structures and/or performing Rietveld refinements. A large number of review articles and book chapters written by some of the pioneers in this field have appeared during the last two decades with some overlap but slightly different emphasis. Walton & O'Hare (2000[link]) describe many aspects of the crystallization of inorganic solids. Norby (2006[link]) looks at zeolite synthesis, including an excellent commented reference list. Evans & Radosavljelić Evans (2004[link]) focus on what can be performed with conventional equipment available in many university departments. Majuste et al. (2013[link]) illustrate reactions relevant to hydrometallurgy studied with in situ synchrotron X-ray diffraction (XRD). Parise et al. (2000[link]) also concentrate on synchrotron-based examples, and already foresee the abundance of data coming from modern third-generation powder-diffraction beam­lines. Automated analysis tools are still underdeveloped, and we will comment on possible future developments in this area. Norby & Schwarz (2008[link]) discuss powder diffraction under non-ambient conditions using X-ray sources, cells and diamond-anvil cell work. In situ gas–solid reactions are discussed by Møller et al. (2014[link]), and Sharma et al. (2015[link]) review the rapidly growing field of crystallographic–electrochemical investigations for both X-rays and neutrons. References to review articles for neutrons are given below (see Section[link]).


Evans, J. S. O. & Radosavljević Evans, I. (2004). Beyond classical applications of powder diffraction. Chem. Soc. Rev. 33, 539–547.Google Scholar
Majuste, D., Ciminelli, V. S. T., Eng, P. J. & Osseo-Asare, K. (2013). Applications of in situ synchrotron XRD in hydrometallurgy: literature review and investigation of chalcopyrite dissolution. Hydrometallurgy, 131–132, 54–66.Google Scholar
Møller, K. T., Hansen, B. R. S., Dippel, A.-C., Jørgensen, J.-E. & Jensen, T. R. (2014). Characterization of gas-solid reactions using in situ powder X-ray diffraction. Z. Anorg. Allg. Chem. 640, 3029–3043.Google Scholar
Norby, P. (2006). In-situ XRD as a tool to understanding zeolite crystallization. Curr. Opin. Colloid Interf. Sci. 11, 118–125.Google Scholar
Norby, P. & Schwarz, U. (2008). Powder Diffraction, Theory and Practice, edited by R. E. Dinnebier & S. J. L. Billinge, pp. 439–463. Cambridge: The Royal Society of Chemistry.Google Scholar
Parise, J. B., Cahill, C. L. & Lee, Y. (2000). Dynamic powder crystallography with synchrotron X-ray sources. Can. Mineral. 38, 777–800.Google Scholar
Sharma, N., Pang, W. K., Guo, Z. & Peterson, V. K. (2015). In situ powder diffraction studies of electrode materials in rechargeable batteries. ChemSusChem, 8, 2826–2853.Google Scholar
Walton, R. I. & O'Hare, D. (2000). Watching solids crystallise using in situ powder diffraction. Chem. Commun. pp. 2283–2291.Google Scholar
Westgren, A. & Lindh, A. E. (1921). Zur Kristallbau des Eisens und Stahl. I. Z. Phys. Chem. 98, 181.Google Scholar

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