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研究生：	徐國欽 Hsu, Kuo-Chin
論文名稱：	II-VI族衍生物材料(SnS, CuInSe2, Cu2ZnSnS4)之新型合成及其特性分析 Novel synthesis and characterization of II-VI group derivative materials, including SnS, CuInSe2, and Cu2ZnSnS4
指導教授：	廖峻德 Liao, Jiunn-Der
學位類別：	博士 Doctor
系所名稱：	工學院 - 材料科學及工程學系 Department of Materials Science and Engineering
論文出版年：	2016
畢業學年度：	104
語文別：	英文
論文頁數：	105
中文關鍵詞：	二六族、水熱法、固態合成法、放電紡絲法、吸光材料
外文關鍵詞：	II-VI group, hydrothermal process, solid state reaction, electrospinning process, absorption materials
相關次數：	點閱：110 下載：0
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本論文之目的在於II-VI族衍生物太陽電池吸收材料之開發，包含了硫化亞錫 (SnS)，二硒化銅銦 (CuInSe2, CIS) 與硫化銅錫鋅 (Cu2ZnSnS4, CZTS)。本研究採用非真空製程，包含水熱法、低溫固態合成法與放電紡絲法來製備II-VI族材料。在水熱法的自組裝環境下，我們可以控制適當的反應環境如: 反應時間、反應溫度以及前驅物的濃度來獲得純度高且單一相的P型Cu2ZnSnS4粉體。薄膜CuInSe2則使用CuSe與InSe二元前驅物在低溫固態法的合成下獲得。所製備出來的P型CuInSe2 薄膜有良好的熱穩定性與結晶性以及擁有適合用於太陽電池吸收層的能隙值。
在本研究中，我們使用金屬氯化物與硫脲並搭配高分子聚乙烯醇縮丁醛 (polyvinylbutyral) 與醋酸纖維素 (cellulose acetate) 製備出均相的前驅物溶液，再透過放電紡絲法收集得到polyvinylbutyral/SnS與cellulose acetate/CZTS 複合纖維，並經過鍛燒可獲得SnS與CZTS的中孔纖維。SnS與CZTS的中孔纖維經由儀器檢測為P型半導體、單一相、高結晶性且良好的化學組成比。SnS與CZTS的中孔纖維能隙值亦適合使用於薄膜太陽電池的吸光層。
綜上所述，我們製備出多種類的高品質薄膜吸光材料並提供一些簡易、低成本且低環境汙染的非真空製程應用於薄膜太陽能電池。

The objective of this thesis is the synthesis and characterization of the II-VI group solar absorption materials, including SnS, CuInSe2 (CIS), and Cu2ZnSnS4 (CZTS). We used a hydrothermal, solid state reaction, and electrospinning processes to prepare these absorption materials. In the hydrothermal process, we optimized the experimental condition, such as reaction time, reaction temperature and concentration of the reactant, to obtain optimum high purity single phase CZTS powders with P-type conductivity. In the low temperature solid state reaction, CuInSe2 could be prepared by using CuSe and InSe binary precursors via solid state reaction. The as-prepared CuInSe2 films have good thermal stability, suitable bandgap value, and a good crystallinity chalcopyrite structure with P-type conductivity. The results can provide a shortcut to producing CIS thin films for absorption layers.
In addition, polyvinylbutyral/SnS (PVB/SnS) and cellulose acetate/CZTS (CA/CZTS) composite fibers were synthesized through a relatively simple electrospinning process. In a typical synthesis, SnCl2·2H2O, CH4N2S, and PVB were dissolved in ethanol under magnetic stirring at room temperature for 2h to obtain a homogenous precursor of PVB/SnS composites. CuCl, ZnCl, SnCl4·5H2O, CH4N2S, and CA were also dissolved in acetone and DI water under magnetic stirring at room temperature for 2h to obtain a homogenous precursor of CA/CZTS composites. Homogeneous precursor solutions of PVB/SnS and CA/CZTS composites were prepared and used immediately for the electrospinning process. Finally, PVB/SnS and CA/CZTS composites fibers were obtained, then transferred to a combustion boat, and calcined in the N2 atmosphere to obtain SnS and CZTS mesoporous fibers. The SnS and CZTS mesoporous fibers were then characterized using X-ray powder diffraction, scanning electron microscopy, thermogravimetric analysis, and transmission electron microscopy. The optical and electrical properties of SnS and CZTS mesoporous fibers were also recorded by UV-Vis absorption spectroscopy and Hall effect measurements, respectively. The results showed that the synthesized SnS and CZTS mesoporous fibers had a p-type conductivity, single phase, high crystallinity and a stoichiometric composition with suitable band gap value. The as-prepared SnS and CZTS mesoporous fibers are thus a suitable material to achieve visible light absorption in a thin film solar cell.
As described above, we plan to fabricate high quality absorption materials and provide a simple, low-cost, and low environmental pollution procedure for thin film solar cells by using non-vacuum process.

Abstract (Chinese)	I
Abstract (English)	II
Acknowledgments	IV
Contents	VI
List of Tables	IX
List of Figures	IX
Chapter 1 Introduction	1
1 Background	1
2 Solar energy and solar cell principle	2
3 Introduction of thin film solar cells	4
4 Theoretical analysis of a solar cell	8
5 The band-gap estimation value of absorption material	10
Chapter 2 Literature review	12
1 Preparation method of thin film absorber materials	12
1.1 Vacuum process	12
1.2 Non-vacuum process	13
2 SnS absorber materials	15
2.1 Electrical and optical properties	15
2.2 Phase diagram and chemical composition	16
2.3 Preparation of SnS materials	18
3 CuInSe2 (CIS) absorber materials	22
3.1 Electrical and optical properties	22
3.2 Phase diagram and chemical composition	23
3.3 Preparation of CIS materials	26
4 Cu2ZnSnS4 (CZTS) absorber materials	32
4.1 Electrical and optical properties	32
4.2 Phase diagram and chemical composition	34
4.3 Preparation of CZTS material	37
5 The study motivation and objectives	45
Chapter 3 Experimental	48
1 Materials	48
2 Experimental procedure	48
2.1 Preparation of SnS mesoporous fibers via electrospinning process	48
2.2 Preparation of CuInSe2 film via a low temperature solid state reaction	49
2.2.1 Synthesis of InSe powder	49
2.2.2 Synthesis of In2Se3 powder	50
2.2.3 Synthesis of CuSe powder	50
2.2.4 Synthesis of Cu2Se powder	50
2.2.5 Synthesis of CuInSe2 films	51
2.3 Preparation of Cu2ZnSnS4 powders by hydrothermal process	51
2.4 Preparation of Cu2ZnSnS4 mesoporous fibers via electrospinning process	51
3 Measurement and analysis	52
Chapter 4 Polyvinylbutyral-assisted synthesis and characterization of SnS mesoporous fibers via electrospinning process	54
1 Morphologies of the electrospun PVB/SnS composite fibers	55
2 Thermal behavior and structure of PVB/SnS fibers produced by electrospinning	58
3 Optical and electrical properties of SnS mesoporous fibers	61
4 Summary	63
Chapter 5 Fabrication and Characterization of CuInSe2 Thin Film Applicable for a Solar Energy Light Absorption Material via a Low Temperature Solid State Reaction	64
1 Structures and morphologies of tetragonal chalcopyrite CuInSe2	65
2 TGA analysis of the CIS precursor materials and CIS film	69
3 Optical and electrical properties of chalcopyrite CuInSe2 film	71
4 Summary	72
Chapter 6 Fabrication and Characterization of Cu2ZnSnS4 Powders by a Hydrothermal Method	74
1 Effects of thiourea concentrations on the growth and microstructure of CZTS	74
2 Effects of reaction time on the growth and microstructure of CZTS	77
3 Effects of reaction temperature on the growth and microstructure of CZTS	77
4 Optical and electrical properties of CZTS powders	79
5 Summary	82
Chapter 7 Cellulose acetate assisted synthesis and characterization of kesterite quaternary semiconductor Cu2ZnSnS4 mesoporous fibers by an electrospinning process	83
1 Morphologies of electrospinning CA/CZTS fiber formation	84
2 The electrospinning parameters of CA/CZTS fibers formation	86
3 Thermal behavior of CA/CZTS composite fibers produced by electrospinning process	88
4 Structure of the formation of tetragonal kesterite CA/CZTS fibers	89
5 Optical and electrical analysis of the formation of tetragonal kesterite CZTS mesoporous fibers	92
6 Summary	93
Conclusion	94
References	96


                                    

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