电化学合成5-二乙基胺钽及钽阳极电溶解机理  

Electrochemical Synthesis of Pentakis(Diethylamido) Tantalum and Electro-Dissolving Mechanism of Tantalum Anode

作　　者：杨建广[1,2] 吴玉山[1] 杨济豪[1] 陈胜龙[1] 高亮[1] 刘小文[1] 

机构地区：[1]中南大学,湖南长沙410083 [2]广西堂汉锌铟股份有限公司博士后科研工作站,广西南丹547200

出　　处：《稀有金属材料与工程》2012年第10期1799-1803,共5页Rare Metal Materials and Engineering

基　　金：国家自然科学基金(50804056)

摘　　要：以金属钽板为阳极,不锈钢板为阴极,以四丁基溴化铵为导电剂,在二乙胺体系中直接电化学合成5-二乙基胺钽(Ta[N(C2H5)2]5)。采用红外光谱(FT-IR)、核磁共振(NMR)、差热分析(TG-DTG.)及等离子质谱(ICP-Mass)对5kPa压力下减压蒸馏分离得到Ta[N(C2H5)2]5产品进行了分析检测。分析结果表明得到的产品确实是纯度99.997%的有机胺钽化合物Ta[N(C2H5)2]5。钽阳极溶解机理研究表明,钽阳极在电流的作用下发生点腐蚀,钽阳极在电流及四丁溴化铵的作用下首先生成Ta(NH10C4)n(Br)m,之后Ta(NH10C4)n(Br)m不断被传输到阴极后继续与二乙胺反应,逐步脱去溴离子Br-,并最终生成有机胺钽盐Ta[N(C2H5)2]5。Pentakis（diethylamido） tantalum（Ta[N（C2H5）2]5） was synthesized by electrochemical reaction involving diethylamide with a sacrificial tantalum anode and stainless steel cathode in the presence of tetraethylammonium bromine as the conductive additive.The condensates were isolated by the reduced pressure distillation of as-synthesized crude Ta[N（C2H5）2]5 below 5 kPa.The final product was characterized by FT-IR and NMR spectroscopy.The thermal properties of the resulting Ta[N（C2H5）2]5 were analyzed by TG-DTG.Results indicate that the resulting compound is indeed Ta[N（C2H5）2]5.The concentration of the impurities in the sample was detected via ICP-Mass spectroscopy,and it is found that the purity of the compound synthesized could reach 99.997%.Electro-dissolving mechanism investigation shows that tantalum anode is spot corroded participation in the direct current and tetraethylammonium bromine.Tantalum is firstly electro-dissolved into Ta（NH10C4） n（Br） m and subsequently transmitted to cathode.Ta（NH10C4） n（Br） m gradually reacts with ethylamine at cathode and releases Br continuously,and Ta[N（C2H5）2]5 is synthesized therein.

关 键 词：电化学合成 5-二乙基胺钽 表征 电溶机理 

分 类 号：TN405[电子电信—微电子学与固体电子学]