A furnace for the in situ study of the formation of inorganic solids at high temperature using time-resolved energy-dispersive x-ray diffraction

Abstract

The design, construction, and use of a furnace from which time-resolved x-ray diffraction data may be measured from reacting mixtures of solids or of solids and liquids is described. The furnace is a vertical tube design, constructed from commercially available components, and can operate at temperatures of up to 1000 °C. The apparatus is designed to heat sample tubes of up to 3 cm diameter. The use of high-intensity synchrotron-generated white-beam x rays allows the tube and its contents to be penetrated; thus x-ray diffraction data can be measured from reactions taking place in laboratory-sized reaction vessels. The energy-dispersive diffraction geometry allows rapid data collection (of the order of seconds); hence reactions can be followed continuously in real time. The use of the furnace is demonstrated by results from experiments performed on Station 16.4 of the Daresbury Synchrotron Radiation Source, UK. Two distinct reaction types are studied, both used to prepare the layered perovskite RbCa2Nb3O10: first, a solid state route at 800 °C and second a flux route, performed in molten RbCl, also at 800 °C.

Mechanistic Aspects in the Formation, Growth and Surface Functionalization of Metal Oxide Nanoparticles in Organic Solvents

“…In situ X‐ray diffraction (XRD) techniques have mainly been applied in the investigation of solid state transformations . However, with the development of suitable reaction cells, also the study of crystallization processes became easier and more popular . X‐ray diffraction provides information about the crystallization kinetics, evolution and composition of the crystalline phase(s), phase transformations, crystal size and anisotropy.…”

“…[90] However,w ith the development of suitable reaction cells, also the study of crystallization processes becamee asier and more popular. [33,79,91,92] X-ray diffraction provides information about the crystallization kinetics, evolution and composition of the crystalline phase(s), phase transformations, crystal size and anisotropy.S tructures without long-range order can be probed by total X-ray scattering combinedw ith atomic pair distribution function. Especially information on precrystalline species and processes such as molecular transformations,d iscrete clusters or small nanoparticles are accessible, even under supercritical conditions.…”

Applications of in situ synchrotron XRD in hydrometallurgy: Literature review and investigation of chalcopyrite dissolution

“…Important advances in the construction materials of the reaction cells have allowed in situ S-XRD measurements in acidic and alkaline solutions, at low and high temperatures, as can be seen in Table 1. More detailed information on the specifications of the different cell designs can be found in the original publications (Barlow et al, 1989;Clark et al, 1995;De Marco et al, 2006a;Evans et al, 1994;Ferrer et al, 2012;Geselbracht et al, 2000;Loan et al, 2005;Norby, 1996;Wall et al, 2011a;Webster et al, 2009). From Table 1 it can also be seen that in order to optimize resolution and minimize beam attenuation in sample cells, beams of different characteristics (i.e., energy, spot size, and angular position) have been focused on the materials and minerals under analysis.…”

“…The EDD is particularly useful for investigating reactions under nonambient conditions. By using an intense incident beam, so that penetration of thick-walled reaction vessels is possible, and a detector with fixed geometry, which allows the simultaneous measurement of the diffraction patterns, in situ synchrotron EDD-based experiments can be conducted with a reaction cell which is very similar to a laboratory autoclave, as well reviewed by Geselbracht et al (2000) and Norby (2006). On the other hand, the use of a monochromatic X-ray beam requires the development of relatively small reaction cells (Morón, 2000;Norby, 2006;Parise, 2000), typically capillary-based cells.…”

In situsystem for X-ray absorption spectroscopy experiments to investigate nanoparticle crystallization

“…Among this and others studies, several kinds of cells have been developed, e.g. high pressure (Betta et al, 1984), electrochemical (Braun et al, 2003), catalysis cell (Girardon et al, 2005;Pettiti et al, 1999), furnaces for studying the synthesis of materials by X-ray absorption (Huwe & Frö ba, 2004;Dent et al, 1995) and X-ray diffraction (Geselbracht et al, 2000;Puig-Molina et al, 2001;Capitá n et al, 1999).…”