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Synthesis, plasmonic properties, and CWA simulant decontamination activity of first row early transition metal nitride powders and nanomaterials

机译:第一排早期过渡金属氮化物粉末和纳米材料的合成,等离子体性能和CWA模拟去污活性

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摘要

The complexes MCl_3(THF)_3 (M = Ti, V, Cr) were used as precursors to form early transition metal nitrides, and solid solutionsof these isomorphous complexes MxM’ 1−xCl_3(THF)_3 were prepared by co-crystallization. Heating the precursor underNH_3 flow from 800 to 950 ℃ produced powders of the nitride MN, and solid solutions of these precursors producedalloys of the nitrides. Nanomaterials were synthesized by two methods: (1) reaction of a MCl_3(THF)_3 solution with 3 eqof KNH_2 in THF in the presence (or absence) of oleylamine, followed by nitridation under NH_3flow at 650–950 ℃ and (2) loading a porous catalyst support such as pelletized Al_2O_3with the MCl_3(THF)_3 complex, followed by similar heat treatment.The materials were characterized by powder X-ray diffraction, elemental analysis, SEM, and optical spectroscopy.Diffuse reflectance and UV–Vis-NIR spectroscopy showed the local surface plasmonic resonances (LSPRs). Although diffusereflectance and UV–Vis-NIR spectroscopy showed LSPRs whose position was sensitive to surface functionalizationand conditions of preparation, preliminary results show TiN nanoparticles have some activity in the degradation of theChemical Warfare Agent (CWA) simulant DEMETON-S, but light plays no role in the mechanism.
机译:配合物MCl_3(THF)_3(M = Ti,V,Cr)被用作前体以形成早期过渡金属氮化物和固溶体通过共结晶制备了这些同构配合物MxM’1-xCl_3(THF)_3。在下加热前体NH_3在800至950℃的温度下产生了氮化锰的粉末,并产生了这些前体的固溶体氮化物的合金。通过两种方法合成纳米材料:(1)MCl_3(THF)_3溶液与3 eq反应油胺存在(或不存在)下在THF中溶解KNH_2,然后在NH_3下氮化在650–950℃下流动,(2)加载多孔催化剂载体,例如颗粒状的Al_2O_3与MCl_3(THF)_3配合物,然后进行类似的热处理。通过粉末X射线衍射,元素分析,SEM和光学光谱对材料进行表征。漫反射和UV-Vis-NIR光谱显示了局部表面等离子体共振(LSPRs)。虽然弥漫反射率和UV-Vis-NIR光谱显示LSPR的位置对表面功能化敏感在制备条件和条件下,初步结果表明TiN纳米颗粒具有一定的降解活性。化学战剂(CWA)模拟物DEMETON-S,但光在该机理中不起作用。

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