Chemistry, University of Southampton, Southampton SO17 1BJ, United Kingdom.
Inorg Chem. 2013 Sep 3;52(17):9994-9. doi: 10.1021/ic4012718. Epub 2013 Aug 15.
Reactions of Ta(NMe2)5 and n-propylamine are shown to be an effective system for sol-gel processing of Ta3N5. Ordered macroporous films of Ta3N5 on silica substrates have been prepared by infiltration of such a sol into close-packed sacrificial templates of cross-linked 500 nm polystyrene spheres followed by pyrolysis under ammonia to remove the template and crystallize the Ta3N5. Templates with long-range order were produced by controlled humidity evaporation. Pyrolysis of a sol-infiltrated template at 600 °C removes the polystyrene but does not crystallize Ta3N5, and X-ray diffraction shows nanocrystalline TaN plus amorphous material. Heating at 700 °C crystallizes Ta3N5 while retaining a high degree of pore ordering, whereas at 800 °C porous films with a complete loss of order are obtained.
Ta(NMe2)5 和正丙胺的反应被证明是 Ta3N5 溶胶-凝胶处理的有效体系。通过将这样的溶胶渗透到交联的 500nm 聚苯乙烯球的密堆积牺牲模板中，然后在氨中进行热解以除去模板并结晶 Ta3N5，在二氧化硅衬底上制备了有序的 Ta3N5 大孔薄膜。通过控制湿度蒸发制备具有长程有序的模板。在 600°C 下对溶胶浸渍的模板进行热解会除去聚苯乙烯，但不会结晶 Ta3N5，X 射线衍射显示出纳米晶 TaN 和非晶材料。在 700°C 下加热会结晶 Ta3N5，同时保持高度的孔有序性，而在 800°C 下会得到完全失去有序性的多孔薄膜。
