Full reciprocal-space mapping up to 2000 K under controlled atmosphere: the multipurpose QMAX furnace

J Appl Crystallogr. 2020 Apr 23;53(Pt 3):650-661. doi: 10.1107/S160057672000432X. eCollection 2020 Jun 1.

Abstract

A furnace that covers the temperature range from room temperature up to 2000 K has been designed, built and implemented on the D2AM beamline at the ESRF. The QMAX furnace is devoted to the full exploration of the reciprocal hemispace located above the sample surface. It is well suited for symmetric and asymmetric 3D reciprocal space mapping. Owing to the hemispherical design of the furnace, 3D grazing-incidence small- and wide-angle scattering and diffraction measurements are possible. Inert and reactive experiments can be performed at atmospheric pressure under controlled gas flux. It is demonstrated that the QMAX furnace allows monitoring of structural phase transitions as well as microstructural evolution at the nanoscale, such as self-organization processes, crystal growth and strain relaxation. A time-resolved in situ oxidation experiment illustrates the capability to probe the high-temperature reactivity of materials.

Keywords: controlled atmosphere; high temperature; in situ; reciprocal-space mapping; structural and microstructural evolution under extreme conditions.

Grants and funding

This work was funded by Agence Nationale pour la Recherche grants ANR-09-NANO-031 and ANR-12-RMNP-0007. Commissariat à l’Énergie Atomique et aux Énergies Alternatives grant .