Powder-X-Ray-Diffraction

直到最近，多特蒙德大学化学与化学生物学学院除了两台单晶X射线衍射仪外，还只能使用一台粉末X射线衍射仪，经过31年的运行，由于无法经济地进行维修，现在不得不永久停止使用。这意味着多特蒙德工厂不再提供分析微晶样品的标准方法。然而，在过去3年中，在无机化学教学领域的新任命旨在加强特别是多特蒙德工业大学的材料科学重点，因此迫切需要这种方法，现在被认为是一种高通量的标准分析方法。因此，这一大型设备应用是用于替换X射线粉末衍射仪，该X射线粉末衍射仪用于已知化合物的基本晶体学分析（相鉴定，相纯度和定量相分析）以及学院无机化学教学领域未知化合物的结构解决方案。测量数据将能够或支持建立光活性金属络合物、刺激响应框架化合物和（金属）有机材料的结构-性质关系。非常多样化的复合类和相关的科学问题，这在很大程度上反映在目前的研究和计划的进一步专题发展的教师在官方发展计划的框架内，提出了具体的要求，补充大型设备采购。所介绍的研究项目包括在相当大的程度上对空气和水分敏感以及吸湿化合物，因此除了反射几何测量（Bragg-Brentano）外，还需要对密封在箔之间的粉末样品进行透射测量。对于高灵敏度的样品和粉末衍射测量，为了解决未知化合物的结构问题，随后进行Rietveld精修，也可以在熔融玻璃毛细管中进行测量。一个重要的方面是在80-500 K范围内的温度依赖性结构分析的可能性，以研究熵驱动的和熵驱动的相变，这可以影响例如结晶MOF材料的密度和孔隙率，以及确定响应性分子和聚集发光体的线性/非线性光学现象。该设备代表了现有结构分析的重要补充扩展，开辟了新的研究视角，并代表了实施CCB教师发展计划的重要一步。

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.