A new micro‐furnace for in situ high‐temperature single‐crystal X‐ray diffraction measurements. (1st August 2015)

• Record Type: Journal Article
• Authors: Alvaro, M.; Angel, R. J.; Marciano, C.; Milani, S.; Scandolo, L.; Mazzucchelli, M. L.; Zaffiro, G.; Rustioni, G.; Briccola, M.; Domeneghetti, M. C.; Nestola, F.
• Is Part Of: Journal of applied crystallography. Volume 48:Part 4(2015:Aug.)
• Page Start: 1192
• Page End: 1200
• Publication Date: 2015-08-01
• Subjects: Crystallography -- Periodicals; 548.05
• DOI: 10.1107/S1600576715011371
• Languages: English
• ISSNs: 0021-8898

Abstract

<abstract abstract-type="main" xml:lang="en"> <title> <x xml:space="preserve">Abstract</x> </title> <p>A new micro‐furnace equipped with an H‐shaped resistance heater has been developed to conduct <italic>in situ</italic> single‐crystal X‐ray diffraction experiments at high temperature. The compact design of the furnace does not restrict access to reciprocal space out to 2θ = 60°. Therefore, unit‐cell parameters and intensity data can be determined to a resolution of 0.71 Å with Mo radiation. The combined use of mineral phases with well characterized lattice expansion (<italic>e.g.</italic> pure Si and SiO₂ quartz) and a small‐diameter (0.025 mm) K‐type thermocouple allowed accurate temperature calibration from room temperature to about 1273 K and consequent evaluation of thermal gradients and stability. The new furnace design allows temperatures up to about 1273 K to be reached with a thermal stability better than ±5 K even at the highest temperatures. Measurements of the lattice thermal expansion of pure silicon (Si), pure synthetic grossular garnet (Ca₃Al₂Si₃O₁₂) and quartz (SiO₂) are presented to demonstrate the performance of the device. Its main advantages and limitations and important considerations for using it to perform high‐temperature diffraction measurements are discussed.</p> </abstract>