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本文以醋酸钯为钯源,二甲基亚砜为硫源,在乙二醇和醋酸存在的条件下通过一步法制备了一种六核钯–甲硫醇团簇化合物[Pd(SCH_3)_2]_6.其具有特征的类花冠形结构.对其反应机制进行了探讨,首先二甲基亚砜分解生成甲硫醇和甲醛,钯与甲硫醇反应原位生成钯–甲硫醇团簇.这些生成的团簇分子进一步组装成微米尺寸大小的棱柱.通过向反应体系中引入一种表面活性剂,产物的形貌从微米棱柱转变为纳米球.350°C下,[Pd(SCH_3)_2]_6的微米棱柱在空气中分解得到金属钯单质.对其热解产物进行电镜表征,发现其在保持原有棱柱形貌的基础上形成了孔道结构.在不同的热解条件下可以得到钯或硫化钯热解产物.
In this paper, a palladium (Pd (CH_3) _2] 6-palladium complex was prepared by one-step method using palladium acetate as palladium source and dimethylsulfoxide as sulfur source in the presence of ethylene glycol and acetic acid. Its characteristic corolla-like structure, its reaction mechanism was explored, first, dimethylsulfoxide decomposed to form methanethiol and formaldehyde, and palladium reacted with methanethiol to generate palladium-methylthiol clusters in situ. These The resulting cluster molecules were further assembled into micrometer-sized prisms by introducing a surfactant into the reaction system, the morphology of the product was changed from a prism to a nanosphere.350 ° C [Pd (SCH_3) _2] _6 micron prism in the air to decompose metal palladium element. The pyrolysis products were characterized by electron microscopy and found that the original prismatic morphology of the formation of the pore structure on the basis of different pyrolysis conditions can be obtained palladium or Palladium sulfide pyrolysis products.