本文是以非真空法製備二硒化銅銦與硫硒化銅銦吸收層，且依其研究內容與發展順序共分為三個主題。首先為二硒化銅銦粉末合成之研究。此部分是採用溶熱法(Solvothermal)合成二硒化銅銦粉末，並針對合成條件影響其結晶相、型貌與顆粒大小進行探討。溶熱法所使用之溶劑為乙二胺(ethylenediamine)、二乙胺(diethylamine)；所使用之反應物為氯化銅、氯化銦與硒粉。先將反應物與溶劑充分混合後置入鐵氟龍壓力容器中密閉，升溫150至200℃並持溫15至48小時。透過此法，所得之二硒化銅銦粉末的結晶相、型貌與顆粒大小均可獲得控制。第二部分為二硒化銅銦粉末之燒結研究。在此項目中，先製備二硒化銅銦粉末之糊劑(paste) ，再以刮刀法(Doctor blading)將粉末糊劑塗佈於基板上，然後置於硒蒸氣的氣氛中進行燒結。其中升溫速率、基板、燒結溫度、燒結氣氛與助燒劑(sintering aid)對於燒結結果之影響，將有詳盡之探討。在特定的燒結條件下，此法可成功製備連續緻密且單一相之二硒化銅銦薄膜。第三部分是對燒結後二硒化銅銦吸收層進行硫化(sulfurization)，形成硫硒化銅銦(CuIn(S,Se)2)之四元化合物。研究結果發現其硫化效果與燒結後之二硒化銅銦吸收層條件有關，並影響其結晶相、拉曼光譜與成分。以有機化合物黏著劑(binder)調配的二硒化銅銦粉末糊劑，經過燒結後會有碳殘留於吸收層中，這樣含有殘碳的二硒化銅銦吸收層會使得硫化溫度大幅降低。反之，無碳殘留之二硒化銅銦吸收層，需較高之硫化溫度。此外，研究結果亦發現，硫化後的吸收層產生二硒化銅銦與二硫化銅銦兩相分離的現象。然而透過硫化條件之控制，最終可得單一相之硫硒化銅銦或二硒化銅銦與二硫化銅銦兩相的吸收層，且S/(S+Se)之成分亦比例可獲得控制。

There are three topics would be discussed in this dissertation. The first investigation was synthesis of crystalline chalcopyrite semiconductor CuInSe2 nanostructures which were preparing by solvothermal route. Effects of reaction time, reaction temperature, solvent type, and reactant concentration were studied. The results show that through selective processing conditions, the phase, morphology, and dimensions of the obtained CuInSe2 nanostructures can be controlled. Second, the powder of single crystal CuInSe2, synthesized by previous process, was sintered to form CuInSe2 films on glass and Mo-coated glass substrates in a horizontal furnace in the presence of Se vapors. Sintering time, temperature, and heating rate were varied to study the effects on the resulting film characteristics. It was found that the sintering is closely related to supply of the Se vapor to the samples while the Se supply depends on the sintering conditions and substrate type. Finally, the CuIn(S,Se)2 film was prepared by the sulfurization of CuInSe2 film obtained by sintering single crystal CuInSe2 powders. The sintering of CuInSe2 powders was performed with and without an organic binder. The sulfurization was performed in a sulfur vapor environment which was generated by heating sulfur powders. The effects of sulfurization time and temperature, and the amount of sulfur powders on the S/(Se+S) ratio and phase transformation were investigated. We show that the ratio of S/(Se+S) and phase transformation can be controlled such that film exhibiting either single CuIn(S,Se)2 phase or two separate CuInSe2 and CuInS2 phases can be obtained.

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