Cation and anion ordering and clustering in the system Lithian muscovite, Trilithionite and Polylithionite

更新项目的目标是首先完成合成系列，然后用固体核磁共振和X射线衍射仪进行标准表征。这意味着沿着白云母-三锂亚硫石的结合完成剩余的合成，并沿着聚锂亚硫石-三锂亚硫石结合和白云母-三锂亚硫石结合进行选定的合成，并根据前两个主要系列的结果增加羟基和/或氟含量。第二个目标是使用新的Bruker Avance NEO 400固态核磁共振仪进行复杂的核磁共振实验，包括一个新的2.5 mm快速MAS核磁共振探头，假设从07/20开始工作，同步加速器衍射实验和获取具有Rietveld晶体结构优化的高分辨率X射线粉末衍射数据。复杂的核磁共振实验主要包括{19F}和/或{1H}X-CPMAS核磁共振和HETCOR谱(X=29Si，27Al，7Li，6Li)，旋转速度高达35 kHz的快速19F和1H MAS核磁共振，以及27Al MQMAS和DQ-SQ核磁共振实验。新的数字核磁共振控制台促进了一系列新的实验(斜坡式CPMAS、带z-Filter的MQMAS、DQ-SQ核磁共振等)。由于采用了数字滤波，因此可以获得比老式光谱仪更高的分辨率。同步辐射衍射实验和高分辨率X射线粉末衍射数据的获取，以及Rietveld晶体结构的改进，将提供有关结构中存在的不同多型(1M、2M1、2M2)和层错的信息。从~(19)F-MAS核磁共振谱和快速MAS核磁共振谱信号中得到的1M和2M1多型的存在，必须通过X射线衍射实验来证实。[6]Al和[4]Al的邻域必须用{19F}和{1H}~(29)Si-CPMAS HETCOR和~(27)Al Dq-Sq核磁共振谱研究。此外，用WIEN2K程序进行密度泛函计算，可以给出不同多型体的理论化学位移和电场梯度。与实验值相比，它将提供关于19F和27Al环境的有价值的信息。此外，不同研究的结果将给出对相和场稳定性的洞察。到目前为止，关于白云母-三锂亚硫石-多锂亚硫酸盐交界处云母稳定性的研究很少。

The goal of the renewal project is firstly the completion of the syntheses series followed by the standard characterisation with Solid State NMR and XRD. This means to finish the remaining syntheses along the muscovite – trilithionite join and doing selected syntheses along the polylithionite – trilithionite join and the muscovite – trilithionite join with increased hydroxyl and / or fluorine content depending on the results of the two former main series.The second goal is to do sophisticated NMR experiments with the new Bruker AVANCE NEO 400 Solid State NMR Spectrometer including a new additional 2.5 mm FAST MAS NMR probe, which is assumed to operate starting at 07/20, synchrotron diffraction experiments and the acquisition of high-resolution X-ray powder diffraction data with Rietveld crystal structure refinements. Sophisticated NMR experiments involve mainly {19F} and / or {1H} X-CPMAS NMR and HETCOR Spectroscopy (X = 29Si, 27Al, 7Li, 6Li), FAST 19F and 1H MAS NMR with spinning speeds up to 35 kHz, as well as 27Al MQMAS and DQ-SQ NMR experiments. The new digital NMR console facilitates a series of new experiments (ramped CPMAS, MQMAS with z-filter, DQ-SQ NMR, etc.) and because of the digital filtering a much higher resolution compared to the old spectrometer can be achieved. Synchrotron diffraction experiments and the acquisition of high-resolution X-ray powder diffraction (XRD) data with Rietveld crystal structure refinements will give information about the different polytypes present (1M, 2M1, 2M2) and stacking faults in the structure. The presence of the polytypes 1M and 2M1 as derived from the signals in the 19F MAS NMR and FAST MAS NMR spectra has to be verified by XRD experiments. The neighbourhood of [6]Al and [4]Al has to be investigated by {19F} and {1H} 29Si-CPMAS HETCOR and 27Al DQ-SQ NMR spectroscopy. In addition, DFT calculations with the WIEN2K code can give theoretical chemical shift values and electric field gradients for the different polytypes. Compared with the experimental values it will give valuable information about the 19F and 27Al environment.As an additional effect, the results derived from the different investigations will give an insight into phase and field stabilities. So far, very few studies exist on the stability of micas located at the join muscovite – trilithionite - polylithionite.