POWTEX visits POWGEN

Andreas Houben; Yannick Meinerzhagen; Noah Nachtigall; Philipp Jacobs; Richard Dronskowski

doi:10.1107/S1600576723002819

POWTEX visits POWGEN

J Appl Crystallogr. 2023 Apr 25;56(Pt 3):633-642. doi: 10.1107/S1600576723002819. eCollection 2023 Jun 1.

Authors

Andreas Houben¹, Yannick Meinerzhagen¹, Noah Nachtigall¹, Philipp Jacobs², Richard Dronskowski¹

Affiliations

¹ Chair of Solid-State and Quantum Chemistry, Institute of Inorganic Chemistry, RWTH Aachen University, D-52056 Aachen, Nordrhein-Westfalen, Germany.
² Chair of Glass and Glass-Ceramic, Institute of Mineral Engineering, RWTH Aachen University, D-52074 Aachen, Nordrhein-Westfalen, Germany.

Abstract

The high-intensity time-of-flight (TOF) neutron diffractometer POWTEX for powder and texture analysis is currently being built prior to operation in the eastern guide hall of the research reactor FRM II at Garching close to Munich, Germany. Because of the world-wide ³He crisis in 2009, the authors promptly initiated the development of ³He-free detector alternatives that are tailor-made for the requirements of large-area diffractometers. Herein is reported the 2017 enterprise to operate one mounting unit of the final POWTEX detector on the neutron powder diffractometer POWGEN at the Spallation Neutron Source located at Oak Ridge National Laboratory, USA. As a result, presented here are the first angular- and wavelength-dependent data from the POWTEX detector, unfortunately damaged by a 50g shock but still operating, as well as the efforts made both to characterize the transport damage and to successfully recalibrate the voxel positions in order to yield nonetheless reliable measurements. Also described is the current data reduction process using the PowderReduceP2D algorithm implemented in Mantid [Arnold et al. (2014). Nucl. Instrum. Methods Phys. Res. A, 764, 156-166]. The final part of the data treatment chain, namely a novel multi-dimensional refinement using a modified version of the GSAS-II software suite [Toby & Von Dreele (2013). J. Appl. Cryst.46, 544-549], is compared with a standard data treatment of the same event data conventionally reduced as TOF diffraction patterns and refined with the unmodified version of GSAS-II. This involves both determining the instrumental resolution parameters using POWGEN's powdered diamond standard sample and the refinement of a friendly-user sample, BaZn(NCN)₂. Although each structural parameter on its own looks similar upon comparing the conventional (1D) and multi-dimensional (2D) treatments, also in terms of precision, a closer view shows small but possibly significant differences. For example, the somewhat suspicious proximity of the a and b lattice parameters of BaZn(NCN)₂ crystallizing in Pbca as resulting from the 1D refinement (0.008 Å) is five times less pronounced in the 2D refinement (0.038 Å). Similar features are found when comparing bond lengths and bond angles, e.g. the two N-C-N units are less differently bent in the 1D results (173 and 175°) than in the 2D results (167 and 173°). The results are of importance not only for POWTEX but also for other neutron TOF diffractometers with large-area detectors, like POWGEN at the SNS or the future DREAM beamline at the European Spallation Source.

Keywords: DREAM beamline; POWGEN beamline; POWTEX detector; Rietveld refinement; angular-dispersive refinement; multi-dimensional refinement; neutron detectors; powder diffraction; time-of-flight diffraction; wavelength-dispersive refinement.

Grants and funding

Parts of this work are based upon data measured with the POWTEX detector operated on the POWGEN instrument at the Spallation Neutron Source (Oak Ridge National Laboratory) and were thus sponsored by the Scientific User Facilities Division, Office of Basic Energy Sciences, US Department of Energy. Financial support by the German Federal Ministry of Research and Education (BMBF) for the POWTEX project (05K16PA2 and 05K19PA1) is gratefully acknowledged.