Powder-X-Ray-Diffraction

粉末X射线衍射

• 批准号: 524781995
• 金额: --
• 依托单位: Technische Universität Dortmund
• 依托单位国家: 德国
• 项目类别: Major Research Instrumentation
• 财政年份: 2023
• 资助国家: 德国
• 起止时间: 2022-12-31 至 无数据
• 项目状态: 未结题
• 来源: https://gepris.dfg.de/gepris/projekt/524781995?language=en
• 关键词: Powder; Ray; Diffraction

Until recently, the Faculty of Chemistry and Chemical Biology at TU Dortmund University only had access to one powder X-ray diffractometer in addition to two single-crystal X-ray diffractometers, which after 31 years of operation has now had to be taken out of service for good due to repairs that cannot be carried out economically. This means that a standard method for analysing microcrystalline samples is no longer available at the Dortmund site. However, the new appointments made in the past 3 years in the teaching area of inorganic chemistry are intended to strengthen the materials science focus of the TU Dortmund in particular, so there is an urgent need for this method, which is now considered a high-throughput standard analysis method. This large-scale equipment application is therefore for the replacement of an X-ray powder diffractometer, which is to be used both for basic crystallographic analysis of known compounds (phase identification, phase purity and quantitative phase analysis) and for structure solution of unknown compounds of the faculty's Inorganic Chemistry teaching area. The measurement data will enable or support the establishment of structure-property relationships of photoactive metal complexes, stimulus-responsive framework compounds and (metal)organic materials. The very diverse compound classes and the associated scientific questions, which are reflected to a considerable extent in the current research and planned further thematic development of the faculty within the framework of the official development plan, place concrete demands on a complementary large-scale equipment procurement. The research projects presented include to a not inconsiderable extent air- and moisture-sensitive as well as hygroscopic compounds, so that in addition to measurements in reflection geometry (Bragg-Brentano), transmission measurements of powder samples sealed between foils are also necessary. For highly sensitive samples and for powder diffraction measurements with the aim of structure solution of unknown compounds with subsequent Rietveld refinement, it should also be possible to carry out measurements in melted glass capillaries. An important aspect is the possibility of temperature-dependent structure analysis in the range of 80-500 K to investigate entropy- and enthalpy-driven phase transformations, which can influence the density and porosity of e.g. crystalline MOF materials, as well as determine linear/non-linear optical phenomena of responsive molecular and aggregated luminophores. This equipment represents a significant complementary extension of existing structural analytics, opens up new research perspectives and represents an important step in the implementation of the CCB faculty development plan.

直到最近，多特蒙德大学的化学和化学生物学学院除了使用两个单晶X射线衍射仪外，还可以使用一个粉末X射线衍射仪，该测量仪在31年后必须从中取出。由于无法在经济上进行的维修，因此可以进行良好的服务。这意味着在多特蒙德站点不再使用用于分析微晶样品的标准方法。但是，在过去三年中，在无机化学教学领域进行的新任命旨在加强多特蒙德tu的材料科学重点，因此迫切需要这种方法，现在被认为是一种高级 - 吞吐量标准分析方法。因此，这种大规模设备的应用是用于替换X射线粉末衍射仪，该剂量既可用于已知化合物的基本晶体学分析（相位识别，相纯度和定量相分析），又用于未知化合物的结构解决方案教师的无机化学教学领域。测量数据将实现或支持建立光活性金属复合物，刺激反应性框架化合物和（金属）有机材料的结构性质关系。非常多样化的复合类别和相关的科学问题，在当前的研究中反映在很大程度上，并计划在正式发展计划的框架内进一步发展教师的主题发展，对补充大规模设备采购的框架提出了具体需求。提出的研究项目包括不足的空气和水分敏感以及吸湿化合物，因此除了反射几何形状的测量（Bragg-brentano）外，还需要密封箔之间粉末样品的传输测量。对于高度敏感的样品和粉末衍射测量，以未知化合物的结构溶液和随后的Rietveld细化的目的，也应该在融化的玻璃毛细管中进行测量。一个重要方面是在80-500 K范围内进行温度依赖性结构分析的可能性，以研究熵和焓驱动的相变，这可能会影响例如晶体MOF材料，并确定反应性分子和聚集的发光体的线性/非线性光学现象。该设备代表了现有结构分析的显着互补扩展，开发了新的研究观点，并代表了CCB教师发展计划实施的重要一步。