Transactions of Nonferrous Metals Society of China The Chinese Journal of Nonferrous Metals

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中国有色金属学报

ZHONGGUO YOUSEJINSHU XUEBAO

第14卷    第11期    总第68期    2004年11月

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文章编号: 1004-0609(2004)11-1969-08
乙酰丙酮铑(Ⅲ)的化学性质
梁  广1,刘伟平1, 高文桂1
普绍平1,闫革新1, 侯  英2

( 1. 昆明贵金属研究所 国家贵金属材料工程技术研究中心,
 昆明 650221;
2. 云南瑞升科技有限公司, 昆明 650106
)

摘 要: 合成了乙酰丙酮铑, 并采用紫外、 红外、 核磁和质谱等手段研究了乙酰丙酮铑(Ⅲ)的化学结构特征。 结果表明: 乙酰丙酮铑属于低自旋的惰性配合物; 由于配合物中离域π键的形成, 配体羰基已不具备典型的羰基特征; 在快原子的轰击下, 乙酰丙酮铑的配位键逐一断裂, 释放出游离的乙酰丙酮, 最后形成103Rh+, 同时伴随共价键的断裂与重排; 在磁场中, 由于Rh3+的强吸电子效应以及螯合环的环电子流效应, H核化学位移向低场移动。 通过TG-DTA和GC-MS分析并探讨了乙酰丙酮铑的热分解行为, 为其应用提供了热学依据和理论参考, 并建议以300 ℃作为以乙酰丙酮铑为前驱体的CVD铑沉积工艺的沉积温度。

 

关键字: 乙酰丙酮铑; 结构特征; 热分解; 化学气相沉积

Chemical properties of rhodium(Ⅲ) acetylacetonate
LIANG Guang1, LIU Wei-ping1, GAO Wen-gui1
 PU Shao-ping1, YAN Ge-xin1, HOU Ying2

1. National Engineering Research Center of Precious Metal,
Kunming Institute of Precious Metals, Kunming 650221, China;
2. Yunnan Reascend Science and Technology Co. LTD, Kunming 650221, China

Abstract: Rhodium(Ⅲ) acetylacetonate [Rh(acac)3], a precursor for preparing Rh layers by CVD technique, was prepared. Its spectroscopic properties were investigated via UV-vis, IR, 1HNMR and MS and its thermal decomposition behavior via TG-DTA and GC-MS. The results show that, 
Rh(acac)3 is a low spinning and inert coordination compound, the characteristics of carbonyls in the ligand disappear due to the formation of conjugate π bonds in 
Rh3+—acac- chelating ring, after bombarded by fast atoms, the coordination bonds break and the organic covalent bonds are splited with the formation of 103Rh+, chemical shifts of H nuclei go downward to low field because of electron-attraction of Rh3+ and electron-cyclic effect in the chelating rings, and it sublimates and decomposes at 247 ℃ and 245 ℃ in air and argon, respectively. Series of new complexes, different with the temperatures, appear in the course of the decomposition, according to which it is suggested that a better deposit temperature should be 300 ℃ when plating Rh layers via CVD technique with Rh(acac)3 as the precursor.

 

Key words: rhodium(Ⅲ) acetylacetonate; chemical structure; thermal properties; CVD

ISSN 1004-0609
CN 43-1238/TG
CODEN: ZYJXFK

ISSN 1003-6326
CN 43-1239/TG
CODEN: TNMCEW

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