equilibria of the related [X2GaP(SiMe3)2]2 in solution. The crystal structure determinations showed that 1 and 2 were solvated, 1·C6H5Cl and 2·C7H8, respectively, and that 3 was solvent-free. The thermal decomposition of 1−3 was studied by TGA along with a determination of the volatiles from pyrolysis and analysis of the final solid product. The pyrolyses of 1−3 at 450 °C under vacuum resulted mainly in nanocrystalline
X 3 Ga·P(SiMe 3)3 [X = Cl(1),Br(2),I(3)]加合物是由各自的三卤化
镓与P(SiMe 3)3的组合高产率制备的。在室温下在烃类溶剂中溶解。通过NMR,MS,元素分析和单晶X射线结构测定来表征加合物。特别地,1的1 H NMR研究1 - 3帮助纠正我们关于相关的[X单体-二聚体平衡先前发表的结果2间隙(森达3)2 ]2在解决方案中。晶体结构的测定表明,1和2是溶剂化的,1 ·C 6 H 5 Cl和2 ·C 7 H 8,并且3是无溶剂的。的热分解1 - 3用来自热解和最终固体产物的分析挥发物的确定沿研究通过TGA。的pyrolyses 1 - 3在450℃下在真空下主要导致纳米晶体的GaP 4-5纳米粒子的平均尺寸通过X射线粉末衍射(XRD)和确定,热解2,通过透射电子显微镜(
TEM);此外,还形成了少量的非晶态含Si / C / H相。