本文選題：銅基硫硒化物 + 溶劑熱法�。� 參考：《電子科技大學(xué)》2015年碩士論文

【摘要】：銅基硫硒化物納米材料繼承了銅基硫族化合物的眾多材料特性,具有廣泛的應(yīng)用前景;同時(shí),通過(guò)調(diào)節(jié)材料硫硒比例,可實(shí)現(xiàn)對(duì)材料形貌、結(jié)構(gòu)、導(dǎo)電系數(shù)、禁帶寬度等性能的可控調(diào)節(jié)。因此眾多研究人員致力于制備性能優(yōu)良的銅基硫硒化物納米材料,并希望實(shí)現(xiàn)其商業(yè)化應(yīng)用。銅基硫硒化物納米材料制備工藝種類眾多,其中,部分基于真空或高溫條件下的制備工藝設(shè)備造價(jià)昂貴,難以實(shí)現(xiàn)商業(yè)化制備,因此本文選取非真空制備工藝進(jìn)行深入研究。其中溶劑熱法制備工藝具有成本低廉,操作簡(jiǎn)便,環(huán)境友好,材料轉(zhuǎn)換率高,易于實(shí)現(xiàn)規(guī)�；a(chǎn)等諸多優(yōu)點(diǎn)。但其瓶頸在于溶劑熱法合成銅基硫硒化物納米材料反應(yīng)時(shí)間過(guò)長(zhǎng)。為解決這一問(wèn)題,本文從反應(yīng)動(dòng)力學(xué)角度出發(fā),對(duì)溶劑熱制備工藝反應(yīng)動(dòng)力學(xué)相關(guān)影響因素進(jìn)行總結(jié)分析,得推論:Se源反應(yīng)活性及溶解度過(guò)低是導(dǎo)致溶劑熱制備工藝反應(yīng)時(shí)間過(guò)長(zhǎng)的主要原因。根據(jù)這一推論,本文提出了一種溶劑熱制備工藝優(yōu)化方案用以合成銅基硫硒化物納米材料。并通過(guò)設(shè)計(jì)一系列對(duì)照實(shí)驗(yàn),對(duì)以上推論及本文提出的溶劑熱法優(yōu)化方案進(jìn)行驗(yàn)證。所得實(shí)驗(yàn)結(jié)果與推論相一致。在后續(xù)工作中,應(yīng)用溶劑熱法優(yōu)化方案制備了一系列銅基硫硒化物,以驗(yàn)證優(yōu)化方案的有效性與可重復(fù)性。主要研究成果如下:(1)在乙二胺反應(yīng)環(huán)境下用NaBH4活化硫/硒單質(zhì)制備高反應(yīng)活性硫/硒前驅(qū)體,并用于溶劑熱法合成銅基硫硒化物納米材料,實(shí)驗(yàn)結(jié)果表明溶劑熱制備工藝反應(yīng)時(shí)間縮短至2 h。(2)使用溶劑熱法優(yōu)化方案制備了三元Cu2-x(SySe1-y)納米材料、四元Cu In(SxSe1-x)2納米材料、五元Cu2ZnSn(SxSe1-x)4納米材料。通過(guò)對(duì)材料形貌、物相、結(jié)構(gòu)、成分及禁帶寬度特性的表征,驗(yàn)證了該優(yōu)化溶劑熱法優(yōu)化方案的有效性與普適性。實(shí)驗(yàn)結(jié)果表明,本文提出的銅基硫硒化物溶劑熱制備工藝優(yōu)化方案有效可行,能夠大幅縮短反應(yīng)時(shí)間至2 h,所制備銅基硫硒化物半導(dǎo)體材料性能良好,適于制備薄膜太陽(yáng)能電池吸收層材料,為今后的薄膜太陽(yáng)能電池商業(yè)化生產(chǎn)積累了經(jīng)驗(yàn)。
[Abstract]:Copper based sulfur selenides nanomaterials inherit many properties of copper based sulfur compounds and have a wide application prospect. At the same time, by adjusting the ratio of sulfur to selenium, the morphology, structure and conductivity of the materials can be realized. Controllable adjustment of bandgap and other properties. Therefore, many researchers are committed to the preparation of copper-based sulphoselenides nanomaterials and hope to realize their commercial applications. There are many kinds of preparation processes for copper based sulfur selenides nanomaterials, among which, part of the preparation process equipment based on vacuum or high temperature is expensive, so it is difficult to realize commercial preparation. Therefore, the non-vacuum preparation process is selected for further study in this paper. The solvothermal preparation process has many advantages, such as low cost, simple operation, friendly environment, high material conversion rate, easy to realize large-scale production and so on. However, the bottleneck is that the reaction time is too long for the solvothermal synthesis of copper-based sulphoselenides nanomaterials. In order to solve this problem, from the point of view of reaction kinetics, this paper summarized and analyzed the factors related to the reaction kinetics of solvothermal preparation process. It is inferred that the low activity and solubility of the reaction of 1: se source are the main reasons for the excessive reaction time of solvothermal preparation process. Based on this inference, an optimized solvothermal preparation method is proposed for the synthesis of copper based sulphoselenides nanomaterials. A series of controlled experiments were designed to verify the above inference and the solvothermal optimization scheme proposed in this paper. The experimental results are consistent with the corollary. In the following work, a series of copper-based sulphoselenides were prepared by solvothermal optimization to verify the effectiveness and repeatability of the optimized scheme. The main research results are as follows: (1) in the presence of ethylenediamine, the highly reactive sulfur / selenium precursor was prepared by using NaBH4 activated sulfur / selenium single substance and used in the solvothermal synthesis of copper based sulphoselenides nanomaterials. The experimental results show that the reaction time of solvothermal preparation process is shortened to 2 h. 2) Ternary Cu In(SxSe1-x)2 nanomaterials, quaternary Cu In(SxSe1-x)2 nanomaterials and quintuple Cu2ZnSn(SxSe1-x)4 nanomaterials have been prepared by solvothermal optimization method. The properties of morphology, phase, structure, composition and band gap width of the optimized solvothermal method were characterized, and the effectiveness and universality of the optimized solvothermal optimization scheme were verified. The experimental results show that the proposed solvothermal preparation method is effective and feasible, and can greatly shorten the reaction time to 2 h. The prepared copper-based sulfide-selenide semiconductor material has good properties. It is suitable for the preparation of thin film solar cell absorbent layer material, which accumulates experience for the commercial production of thin film solar cell in the future.
【學(xué)位授予單位】：電子科技大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2015
【分類號(hào)】：TB383.1;TM914.4

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本文編號(hào)：1780228