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首页> 外文期刊>Chemistry: A European journal >Organo-Gallium/Indium Chalcogenide Complexes of Copper(I): Molecular Structures and Thermal Decomposition to Ternary Semiconductors
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Organo-Gallium/Indium Chalcogenide Complexes of Copper(I): Molecular Structures and Thermal Decomposition to Ternary Semiconductors

机译：铜（I）的有机镓/铟硫属化物配合物：三元半导体的分子结构和热分解

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摘要

Several organo-gallium/indium chalcogenide complexes of copper(I), stabilized by trialkylphosphines, were isolated, structurally characterized by using single-crystal Xray diffraction, and investigated in thermolysis experiments. The syntheses with [E(Me_3Si)_2] (E=S, Se) as a starting material and a chalcogen source involve the elimination of volatile silyl acetate, silyl ethers, and methane from copper(I) acetate, and Group 13 metal trimethyl compounds, respectively. Chalcogenide complexes, according to the general formulas [(R_3PCu)_4(MeM)_4E_6] (1–6) and [(R_3PCu)_6(MeM)_4M_4S_(13)] (7–9; with R=alkyl and M=Ga, In), and mixed chalcogenide–phenylchalcogenolate complexes [(iPr_3PCuEPh)_3(MeGaE)_4] (10, 11) were isolated. The heavy atom cores of 1–6 consist of an octahedron of chalcogen atoms, interpenetrated by a cube of metal atoms. Depending on the steric demand of the phosphine ligands, two constitutions are observed; the metal atoms of the same element either forming tetrahedra, or parallelograms, respectively. This constitutional isomerism is further investigated by quantum chemical calculations. Complexes 7–9 contain a central sulfur atom, surrounded by two interpenetrating tetrahedra of Group 13 metal atoms, an octahedron of copper atoms, and an icosahedron of twelve outer sulfur atoms; the heavy atom framework of 10 and 11 is a "cut-out" of this structure. Thermolysis experiments include thermogravimetry measurements and subsequent Rietveld phase analysis of the residues by using powder X-ray diffraction. The homologous compounds 1, 3, 4, and 6 yield the respective crystalline ternary semiconductor material CuME_2 at temperatures below 3008C. Partial release of Me_3M during the thermolysis process results in excess copper in the residue and therefore in small amounts of additional binary copper chalcogenide phases or metallic CuM alloys. Compound 8 produces nanocrystalline CuGaS2 at about 300 8C.
机译：分离了由三烷基膦稳定化的铜（I）的几种有机镓/铟硫属化物配合物，使用单晶X射线衍射对其结构进行了表征，并在热解实验中进行了研究。以[E（Me_3Si）_2]（E = S，Se）为起始原料和硫族元素来源的合成方法涉及从乙酸铜（I）和13族金属三甲基锡中除去挥发性的乙酸甲硅烷基酯，甲硅烷基醚和甲烷化合物。根据通式[（R_3PCu）_4（MeM）_4E_6]（1-6）和[（R_3PCu）_6（MeM）_4M_4S_（13）]（7-9;其中R =烷基且M = Ga ，In）中，并分离出硫族化物-苯基硫属元素酸酯的复合物[（iPr_3PCuEPh）_3（MeGaE）_4]（10，11）。 1-6的重原子核由硫族元素原子的八面体组成，并由金属原子的立方相互渗透。取决于膦配体的空间需求，观察到两种结构。同一元素的金属原子分别形成四面体或平行四边形。通过量子化学计算进一步研究了这种结构异构性。配合物7–9包含一个中心硫原子，被两个互穿的第13组金属原子的四面体，一个铜原子的八面体和一个十二个外部硫原子的二十面体包围; 10和11的重原子框架是该结构的“切除”。热解实验包括热重测量和随后的残留粉末的Rietveld相分析（通过使用粉末X射线衍射进行分析）。同源化合物1、3、4和6在低于3008℃的温度下产生相应的晶体三元半导体材料CuME_2。在热解过程中Me_3M的部分释放会导致残留物中过量的铜，因此会导致少量额外的二元硫属铜化物相或金属CuM合金。化合物8在约300 8 C下产生纳米晶体CuGaS 2。

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