Preparation, Structural Characterization, and Thermal Ammonolysis of Two Novel Dimeric Transition Silylamide Complexes

作者: Fei Cheng , Christopher N. Hope , Stephen J. Archibald , John S. Bradley , Stephen Clark

DOI: 10.1111/J.1744-7402.2009.02452.X

关键词: Transition metalLithiumMaterials scienceHafniumSilicon nitrideMesoporous materialImideZirconiumSiliconInorganic chemistryCrystallography

摘要: The preparation and molecular structures of two novel dimeric transition metal silylamide complexes {Li0.5Zr[NHSi(NMe2)3]1.5[NSi(NMe2)3]0.5[μ-NSi(NMe2)3]}2 {Li0.5Hf[NHSi(NMe2)3]1.5[NSi(NMe2)3]0.5[μ-NSi(NMe2)3]}2 with a tetrahedral coordination environment are reported. Thermal ammonolysis in an autoclave yields mesoporous partially lithiated silicon zirconium imide powder Si3Zr(N)(NH)x(NH2)y(NMe2)z surface area 440 m2/g. A microporous hafnium Si3Hf(N)(NH)x(NH2)y(NMe2)z 232 m2/g was obtained via similar process {Li0.5Hf[NHSi(NMe2)3]1.5[NSi(NMe2)3]0.5[μ-NSi(NMe2)3]}2. Both these powders have disordered octahedral environment. Pyrolysis leads to the formation mixtures porous or lithium nitride ceramics regular They contain some residual exhibit much reduced due almost total collapse pores during pyrolysis process.

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