MOCVD前驱物Fe(DPM)3的制备与性能表征 |
Synthesis and Characterization of MOCVD Precursor Fe(DPM)3 |
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摘要: 以FeCl3和四甲基庚二酮(HDPM)为原料,在醇/水混合溶剂中合成β-二酮金属有机化合物Fe(DPM)3。利用红外吸收光谱、元素分析、原子吸收光谱、差热-热重和质谱分析等技术,分析了Fe(DPM)3的结构、纯度、热稳定性、挥发性以及热分解机理。结果显示,合成的Fe(DPM)3在空气气氛和氮气气氛下均具有良好的挥发性,气化失重率达到98%以上,空气气氛中氧的存在对Fe(DPM)3的气化和分解具有一定的促进作用;质谱分析结果表明:在Fe(DPM)3的分解过程中,首先有一个DPM配体解离,然后在剩余两个DPM配体中先解离出-C(CH3)3基团,随后分裂出剩下的-OCCH2COC(CH3)3基团,最后得到+Fe(DPM)碎片。本文同时以新合成的Fe(DPM)3作为前驱物,采用气溶胶辅助的金属有机化学气相沉积(Aerosol Assisted MOCVD,AA-MOCVD)技术在α-Al2O3衬底上成功沉积制备了α-Fe2O3薄膜。 |
关键词: MOCVD β-二酮螯合物 挥发性 热分解 |
基金项目: |
Abstract: High purity Fe(DPM)3 (DPM=2,2,6,6-tetramethyl-3,5-heptanedionato) powder was synthesized from FeCl3 and HDPM in ethanol/aqueous solution followed by reduced pressure distillation and recrystallization from toluene. This metal β-diketonate complex used as precursor for metal-organic chemical vapor deposition (MOCVD) of Fe2O3 film has been characterized by elemental analyses, metal atomic absorption spectrophotometric analysis, thermogravimetry-differential thermal analysis (TG-DTA analysis), infrared spectroscopy and mass spectroscopic analysis. The weight loss of Fe(DPM)3 amounts to over 98% of initial weight when heated either in air or in N2, indicating the high volatility of the sample. The decomposition mechanism of Fe(DPM)3 at elevated temperature was proposed: at the beginning, one DPM ligand is detached from the center ion Fe3+, and then the -C(CH3)3 and -OCCH2COC(CH3)3 group dissociate from Fe(DPM)2 fragment successively, leading to the formation of the Fe(DPM) fragment finally. Meanwhile, using as-obtained Fe(DPM)3 as precursor, α-Fe2O3 thin film was deposited on α-Al2O3 substrate by AA-MOCVD technique, and then characterized by X-ray diffraction and Scanning electron microscope. |
Keywords: metalorganic chemical vapor deposition β-diketonate complex volatility thermal decomposition |
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王艳艳,姜银珠,高建峰,刘铭飞,孟广耀.MOCVD前驱物Fe(DPM)3的制备与性能表征[J].无机化学学报,2006,22(7):1269-1274. |
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