本研究以熱注入法製備CuSbSe2晶體，首先於此製程下瞭解以十八烷基胺和三乙二醇等溶劑對於合成CuSbSe2晶體之影響，結果顯示以十八烷基胺為反應溶劑時，其易與陽離子反應，先形成氧化銻。而使用三乙二醇為反應溶劑時，當反應時間足夠時，即可獲得CuSbSe2之單一相。其生成過程為Cu3SbSe4因三乙烯四胺將其中之Cu2+還原至Cu+，轉變成CuSbSe2，釋放出多餘之銅離子與硒離子，銅離子會在Sb2Se3表面進行成核反應，最終變成CuSbSe2。當反應溫度為190 ℃時，未能提供足夠能量使三乙烯四胺發揮其還原之效果；當三乙烯四胺之添加量過少時，只能使Cu3SbSe4中Cu2+部分還原至Cu+，而添加量過多時，則還原性過高，而生成金屬銻。

In this study, a novel and facile hot injection method for the synthesis of single phase CuSbSe2 crystallites was developed by using low toxic triethylene glycol (TEG) as both the solvent and reducing agent and triethylenetetramine (TETA) as co-reducing agent. The effects of the amounts of TETA addition and reaction temperatures on the phase development were investigated. The crystalline structures, morphologies, chemical compositions and optical characterization of the synthesized products were investigated using XRD, TEM, EDS, XPS, and UV–Vis-NIR. A single phase CuSbSe2 crystallites can be obtained by using triethylene glycol as the solvent and reducing agent and triethylenetetramine as co-reducing agent. TETA addition plays a key role in determining the final phase. The presence of the intermediate phase, Cu3SbSe4 phase could be due to the existence of Cu2+, resulting from the insufficient reducibility in the solution. A sufficient amount of TETA can facilitate the reduction of Cu2+ into Cu+, leading to the preformed Cu3SbSe4 phase dissolved and reacted with Sb2Se3 to form CuSbSe2. Rietveld refinement of X-ray diffraction patterns confirmed formation of single CuSbSe2 phase without any second phase. The obtained CuSbSe2 phase had a direct band gap with the band gap value of 1.06 eV.

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