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摘要 I
Abstract II
1.引言 1
1.1多元金屬硫化物概述 1
1.2三元金屬硫化物概況 1
1.3 CuSbS2簡述 2
1.4 XRD衍射技術(shù) 2
1.5 溶劑熱法 3
2.實(shí)驗(yàn)部分 4
2.1水-油混合溶劑熱合成CuSbS2反應(yīng)原理 4
2.2試劑及儀器 5
2.3實(shí)驗(yàn)過程 6
2.3.1不同前驅(qū)合成CuSbS2 6
2.3.1.1乙基黃原酸鉀制備前驅(qū)合成CuSbS2 6
2.3.1.2二乙基二硫代氨基甲酸鈉制備前驅(qū)合成CuSbS2 6
2.3.1.3乙酰丙酮制備前驅(qū)合成CuSbS2 7
2.3.1.4各前驅(qū)不同反應(yīng)條件下合成CuSbS2 7
2.3.2 二乙基二硫代氨基甲酸鈉制備前驅(qū)，不同溶劑、溫度、水油比合成CuSbS2 8
2.3.2.1以二乙基二硫代氨基甲酸鈉為試劑制備前驅(qū) 8
2.3.2.2不同溶劑下制備CuSbS2 8
2.3.2.3不同水、油配比下制備CuSbS2 9
2.3.2.4不同溫度下制備CuSbS2 9
3.結(jié)果與討論 10
3.1產(chǎn)物的X射線衍射分析（XRD）物相分析 10
3.2產(chǎn)物的掃描電鏡（SEM）檢測及圖像分析 12
3.2.1前驅(qū)對產(chǎn)物形貌的影響 12
3.2.2溶劑對產(chǎn)物形貌的影響 14
3.2.3水與溶劑配比對產(chǎn)物形貌的影響 15
3.2.4反應(yīng)溫度對產(chǎn)物形貌的影響 16
4.結(jié)論 17
參考文獻(xiàn) 18
致謝 21

水-油混合溶劑熱合成CuSbS2

摘要
金屬三元硫族化合物具有特殊的物理化學(xué)性質(zhì)，在半導(dǎo)體材料，催化劑載體，固體化學(xué)，電磁及光學(xué)特性等高科技領(lǐng)域具有不可替代的重要性。它們的合成研究已成為目前無機(jī)合成化學(xué)的一個(gè)十分活躍的研究領(lǐng)域。本實(shí)驗(yàn)采用水-油混合溶劑熱法，制備CuSbS2半導(dǎo)體材料，探討了不同前驅(qū)對制備CuSbS2半導(dǎo)體材料的影響；探討了以二乙基二硫代氨基甲酸鈉制備前驅(qū)下，不同溶劑、不同水油比、不同溫度因素對CuSbS2半導(dǎo)體材料的影響，采用X射線衍射（XRD）和掃描電鏡（SEM）對CuSbS2半導(dǎo)體材料進(jìn)行了表征。試圖得出采用水-油混合溶劑熱法制備CuSbS2半導(dǎo)體材料的最佳反應(yīng)條件。

關(guān)鍵詞：銅銻硫；半導(dǎo)體材料；水-油混合溶劑熱；溶劑熱。



Synthesis of CuSbS2 by the oil – water mixing solvothermal reaction
Abstract
Three element metal chalcogenide has special physical and chemical properties on semiconductor materials, catalyst carrier, solid chemistry, electromagnetic and optical properties and it has irreplaceable importance in these high-tech fields. Their synthesis has become a very active research field of inorganic synthetic chemistry now . This experiment adopts the oil – water mixing solvothermal reaction as the preparation of cusbs2 , discusses the influence of different precursor on cusbs2 preparation; Discussed within sodium diethyl dithiocarbamate preparation of precursor, the influence of different solvents, different water oil ratio and different temperature factors on cusbs2, using X-ray diffraction (XRD) and scanning electron microscopy (SEM) to cusbs2 for being characterized. Results showed that the optimum of oil - water mixed solvent thermal process for synthesis of cusbs2: apply reagent DDTC as the preparation of the precursor , liquid paraffin as organic solvent, water and paraffin ratio is 1:3, the reaction under 200 ℃ for 12 hours. Try reach a conclusion about the optimum condition of Synthesis of CuSbS2 by theoil-watermixing solvothermal reaction.

Key words: copper antimony sulfur; semiconductor materials; the oil – water mixing solvothermal; Solvent heat.