Copper(II) and triphenylphosphine copper(I) ethylene glycol carboxylates: synthesis, characterisation and copper nanoparticle generation.
Copper(II) and triphenylphosphine copper(I) ethylene glycol carboxylates: synthesis, characterisation and copper nanoparticle generation.
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DOI：
10.1039/c3dt51913a
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发表时间：
2013-10
影响因子：
4
通讯作者：
David Adner;Stefan A. Möckel;M. Korb;R. Buschbeck;T. Rüffer;S. Schulze;L. Mertens;M. Hietschold;M. Mehring;H. Lang
中科院分区：
文献类型：
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作者：
David Adner;Stefan A. Möckel;M. Korb;R. Buschbeck;T. Rüffer;S. Schulze;L. Mertens;M. Hietschold;M. Mehring;H. Lang
通过[Cu_2（Ac）_4·2 H_2 O]与CH_3 O（C_2 H_4 O）_nCR_2CO_2 H（1a ~ e）反应，合成了乙二醇官能化的羧酸铜配合物Cu[O_2CCR_2（OC_2 H_4）_nOCH_3]_2（n = 0-3; R = H，Me）（2a ~ e）。在用三苯基膦还原2a-e时，获得相应的三（三苯基膦）铜（I）配合物3a-e，其可以通过去除一个膦配体而转化为双（三苯基膦）铜（I）配合物4a-e。通过红外光谱和单晶X-射线结构分析，讨论了铜离子上羧基的结合模式。通过DSC、TG和TG-MS分析了2-4的热分解机理。配合物4c被用作通过在十六胺中热分解而不需要任何另外的反应物来生成铜纳米颗粒的前体。根据前体浓度的不同，得到了平均直径为10 ~ 85 nm的球形铜纳米颗粒以及长度为1.3 μm的纳米棒（长径比为2 ~ 32）。电子衍射分析表明，棒，它们由五个域是围绕一个五倍的旋转轴排列。
Ethylene glycol-functionalised copper(II) carboxylates Cu[O2CCR2(OC2H4)nOCH3]2 (n = 0-3; R = H, Me) (2a-e) have been prepared by the reaction of [Cu2(OAc)4·2H2O] with CH3O(C2H4O)nCR2CO2H (1a-e). Upon reduction of 2a-e with triphenylphosphine, the corresponding tris(triphenylphosphine)copper(I) complexes 3a-e were obtained, which could be converted to the bis(triphenylphosphine)copper(I) complexes 4a-e by removal of one phosphine ligand. Based on IR spectroscopy and single crystal X-ray structure analysis the binding motif of the carboxylato group on the copper ion is discussed. DSC, TG and TG-MS experiments were performed to analyse the thermal decomposition mechanism of 2-4. Complex 4c was used as a precursor for the generation of copper nanoparticles by thermal decomposition in hexadecylamine without the need of any further reactants. Depending on the precursor concentration, spherical copper nanoparticles with a mean diameter ranging from 10 to 85 nm as well as nanorods with a length of up to 1.3 μm (aspect ratios ranging between 2 and 32) were obtained. Electron diffraction analysis of the rods suggested that they consist of five domains which are arranged around a fivefold rotational axis.