POWTEX visits POWGEN.

IF 6.1 3区 材料科学 Q1 Biochemistry, Genetics and Molecular Biology Journal of Applied Crystallography Pub Date : 2023-06-01 DOI:10.1107/S1600576723002819
Andreas Houben, Yannick Meinerzhagen, Noah Nachtigall, Philipp Jacobs, Richard Dronskowski
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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.

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POWTEX访问POWGEN。
用于粉末和质地分析的高强度飞行时间(TOF)中子衍射仪POWTEX目前正在德国慕尼黑附近Garching的研究堆FRM II的东部引导大厅建造。由于2009年世界范围内的3He危机,作者迅速开始开发无3He探测器替代品,以满足大面积衍射仪的要求。兹报告2017年在美国橡树岭国家实验室散裂中子源POWGEN中子粉末衍射仪POWGEN上运行最后一个POWTEX探测器安装单元的企业。因此,本文提供了来自POWTEX探测器的第一个依赖于角度和波长的数据,不幸的是,该探测器被50g冲击损坏,但仍在运行,以及为表征传输损伤和成功重新校准体素位置而做出的努力,以便产生可靠的测量结果。还描述了使用Mantid中实现的PowderReduceP2D算法的当前数据缩减过程[Arnold et al.(2014)]。诊断。Instrum。物理方法。[j].科学通报,2004,(6):349 - 349。数据处理链的最后一部分,即使用GSAS-II软件套件的修改版本进行新的多维细化[Toby & Von Dreele(2013)]。j:。crystal .46, 544-549]与对相同事件数据的标准数据处理进行了比较,这些数据通常被简化为TOF衍射图,并用未修改版本的GSAS-II进行了细化。这包括使用POWGEN的粉末金刚石标准样品确定仪器分辨率参数,以及对友好用户样品BaZn(NCN)2进行细化。虽然在比较常规(1D)和多维(2D)处理时,每个结构参数本身看起来都很相似,但在精度方面,仔细观察会发现微小但可能显著的差异。例如,由于一维细化(0.008 Å),在Pbca中结晶的BaZn(NCN)2的a和b晶格参数有些可疑的接近性在二维细化(0.038 Å)中不那么明显。在比较键长和键角时也发现了类似的特征,例如,两个N-C-N单元在一维结果(173°和175°)中的弯曲程度低于二维结果(167°和173°)。这一结果不仅对POWTEX具有重要意义,而且对其他具有大面积探测器的中子TOF衍射仪也具有重要意义,比如在SNS的POWGEN或未来在欧洲散裂源的DREAM光束线。
本文章由计算机程序翻译,如有差异,请以英文原文为准。
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来源期刊
CiteScore
10.00
自引率
3.30%
发文量
178
审稿时长
4.7 months
期刊介绍: Many research topics in condensed matter research, materials science and the life sciences make use of crystallographic methods to study crystalline and non-crystalline matter with neutrons, X-rays and electrons. Articles published in the Journal of Applied Crystallography focus on these methods and their use in identifying structural and diffusion-controlled phase transformations, structure-property relationships, structural changes of defects, interfaces and surfaces, etc. Developments of instrumentation and crystallographic apparatus, theory and interpretation, numerical analysis and other related subjects are also covered. The journal is the primary place where crystallographic computer program information is published.
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