本研究以熱分解法製備CIGS奈米粉體，首先於此製程下瞭解熱注入法(Hot-injection method)與直接升溫法(Heating-up process)對CIGS粉體生成之合成機制。結果顯示利用直接升溫法可獲得單一黃銅礦結構與均勻化學組成之奈米粉體，且其粒徑尺寸分佈約為15.0 nm±3nm，其相生成過程為CuSe→CuInSe2 →CIGS。而熱注入法由於銦錯合離子之反應性較鎵錯合離子來得高，使得合成過程中產生相分離之現象，因而產生富銦與富鎵之銅銦鎵硒奈米粉末。然而，以此製程條件下雖可獲得近單分散粉體，但其產率極低，故藉由直接升溫法合成粉體過程中改變溶劑種類與Se/陽離子前驅比例，當隨非配位型溶劑(ODE)添加量增加，其CIGS外型會由片狀晶逐漸轉變為球狀粉體，若Se/陽離子前驅比例增加，生成CIGS粉體之粒徑尺寸均一且細小，其粒徑分佈約9-20nm，適當改變溶劑種類與溶質比例，可有效調節金屬單體之活性，並控制其粒徑尺寸分佈。
以此奈米CIGS奈米粉末為原料，分別以膠體成型及熱壓成型技術製備具有較高生胚密度及較佳顯微結構之胚體。由於經高溫長時間之熱壓燒結時易造成CIGS組成中In、Ga及硒之揮發，使得組成偏離原始計量比。因此本研究將CIGS奈米晶粒以低溫短時間(≦550oC, 10分鐘)熱壓，先行打破奈米粉末之凝聚體，促進胚體之緻密化，使胚體達到中期燒結之階段，再經硒保護氣氛下於低溫燒結(≦550oC)，以避免組成及Se之揮發，可獲得高緻密性且為單一黃銅礦相CIGS燒結體。透過離心力成型法能使生胚產生均質堆積，凝聚體間的孔洞就會因此減少，可使坯體之燒結活性大幅增加，於450℃燒結2小時下可使晶粒成長，550℃燒結3小時即可獲得高緻密性燒結體。

Nearly mono-dispersed CuIn0.7Ga0.3Se2(CIGS) nanocrystals were successfully synthesized using the thermal decomposition of copper, indium, gallium, and selenium-oleylamine complexes via a heating-up process in this study. The CIGS nanocrystals exhibited single chalcopyrite phase and its chemical composition was closely to stoichiometric. It was observed that the morphology of CIGS nanocrystallites changed from flake shape into spherical shape as the ODE addition increased. As the selenium/ cation ratio increased, the CIGS nanocrystals of size 9-20nm were obtained. The reactivity of the monomers in the solution can be adjusted by changing the solvent kind and selenium/cation ratio, and hence affect the crystallite size and size distribution. Sintered CuIn0.7Ga0.3Se2 ceramics with a relative density above 92% and grain size of about 3-4 μm can be obtained by centrifugal forming nearly mono-dispersed CuIn0.7Ga0.3Se2 nano-crystals. The packing density and microstructure of the CIGS green body were improved significantly using the centrifugal forming method because it prevented inter-agglomerate pore formation. Besides, hot-pressed sintering effectively breaks up the agglomerates and promotes the nano-particle rearrangement. CIGS relative density is promoted to 91% by sequentially sintering at 550oC for 1-3 h under Se2 atmosphere. The prepared CIGS ceramics exhibited p-type semiconductor characteristics and the carrier concentration decreased, but the Hall mobility increased with increasing soaking time at 550oC.

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