Cu_2ZnSnS（Se）_4、CdIn_2S_4纳米结构的制备及其光电性质的研究
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摘要
太阳能被认为是取之不尽用之不竭的可再生能源。在太阳能电池的研究中，不断探索寻找具有潜在应用前景的新型光电材料，以及开发高效低成本的制备方法是非常重要的研究方向。目前，研究最多的太阳能电池是薄膜化合物太阳能电池，薄膜太阳能电池具有光吸收系数大、制备方法简单、抗腐蚀性强等优点。在薄膜太阳能电池中CuIn(Ga)Se_2太阳能电池有着优异的表现，其能量转换效率已接近20%。然而材料中的In和Ga是稀有贵金属元素，限制了CuIn(Ga)Se_2太阳能电池的大面积生产。
近年来, Cu_2ZnSnS(Se)_4由于具有与CuIn(Ga)Se_2材料相似的结构和光学性质并且材料中不包含贵金属元素而受到越来越多的重视。Cu_2ZnSnS(Se)_4材料是直接带隙半导体，禁带宽度在1.3-1.6eV之间，光吸收系数大于104cm-1，被认为是理想的薄膜太阳能电池吸收层材料。但是,目前制备Cu_2ZnSnS(Se)_4的方法主要局限在热蒸发技术、磁控溅射、激光脉冲沉积、原子束溅射等。这些方法都有着各自的缺点如反应物昂贵、设备复杂、制备中产生有毒物质等。溶剂热法是一种制备半导体材料常用的化学方法，具有设备简单、易于操作等特点。但是目前关于溶剂热法制备Cu_2ZnSnS(Se)_4的报道依然很少。针对这种情况，我们在本文中研究了利用简单方便的溶剂热方法制备不同形貌结构的纳米结构和薄膜，并首次制备了Cu_2ZnSnSe_4的纳米管阵列，讨论了纳米管阵列的生长机制。此外，我们研究发现具有片状结构的CdIn_2S_4薄膜同样可以通过水热法制备，并且展现出良好的光电性质。
(1)利用溶剂热技术，以二甲基甲酰胺为溶剂，制备了具有空心球状的Cu_2ZnSnS_4纳米结构。实验表明，溶剂中的PEG对空心球状Cu_2ZnSnS_4的形成起关键作用。
(2)根据不同反应条件的对比试验结果详细地讨论了空心球状的Cu_2ZnSnS_4的生长机制。空心球状Cu_2ZnSnS_4的生长可以分为三个过程，首先是溶液中的金属离子与PEG分子作用，吸附在PEG分子表面。之后是在反应温度下溶液中产生S~(2-),金属离子与S~(2-)反应生成球状的Cu_2ZnSnS_4结构。最后经过Ostwaldripening过程形成空心球状的Cu_2ZnSnS_4纳米结构。
(3)利用乙二胺为反应溶剂，成功制备了具有花状结构的Cu_2ZnSnSe_4。对样品测试分析的结果表明得到的Cu_2ZnSnSe_4具有黝锡矿结构和理想的化学成分比例，并讨论了花状Cu_2ZnSnSe_4颗粒的形成过程。
(4)采用溶剂热法在FTO导电基片上直接生长了均匀的Cu_2ZnSnS_4薄膜样品。详细研究了不同退火温度(250-550℃)对样品结构、形貌和成分的影响。当退火温度为550℃时，薄膜样品具有锌黄锡矿结构并且展现出良好的光响应特性。为制备其他硫化物薄膜提供了一种方便低耗的制备方法。
(5)首次在FTO基片上制备出均匀一致的纳米管阵列。Cu_2ZnSnSe_4纳米管阵列是以ZnO纳米棒阵列作为模板，结合了离子交换反应与溶解热技术制备得到的。首先在FTO基片上制备了均匀的ZnO纳米棒阵列。之后，利用材料容积度常数的不同(ZnO＞ZnSe＞CuSe)，通过离子交换反应制备了ZnO/CuSe的电缆结构阵列。最后在溶剂热反应过程中外层的CuSe与Zn~(2+)和Sn~(4+)反应生成Cu_2ZnSnSe_4，同时内部的ZnO与反应中生成的H~+反应而溶解，最终形成了Cu_2ZnSnSe_4的纳米管阵列。
(6)通过改变ZnO纳米棒阵列长度和直径制备了具有不同长度和直径的Cu_2ZnSnSe_4纳米管阵列，并研究了不同长度纳米管阵列的光电化学性质,讨论了光电流的变化规律。结果表明，长度为2μm的Cu_2ZnSnSe_4纳米管阵列的光电化学性质最好。
(7)采用水热法以半胱氨酸为硫源在FTO基片上直接生长了具有片状结构的CdIn_2S_4薄膜。讨论了片状CdIn_2S_4薄膜的生长机制，其生长主要经历三个过程：1）利用H_2SO_4和H_2O_2溶液处理FTO基片；2）CdIn_2S_4在FTO基片表面的异质成核过程；3）CdIn_2S_4在基片成核处的晶体生长过程。
(8)对片状CdIn_2S_4薄膜样品的光电化学性质进行了研究，结果表明，CdIn_2S_4具有良好的光电性质，退火处理后转换效率可以达到0.162%明显好于类似的半导体薄膜材料如In_2S_3，CdS等。
Solar energy is considered to be the most economic and effective among allavailable renewable energy resources. In the solar energy research field, synthesis ofnovel PV materials with simple method is an important research direction. Recently,chalcopyrite-type semiconductors like Cu(In,Ga)Se2or Cu(In,Ga)S2have verybeneficial properties for photo-voltaic applications. Obtained efficiencies areremarkably high, up to nearly20%; however, gallium and indium used for thepreparation of the active layer are very rare and expensive elements. This could leadto a shortage in the supply of these elements and would inhibit a cost-effectivelarge-scaleproduction.
A quaternary semiconductor of Cu_2ZnSnS(Se)_4, which is a direct band gapsemiconductor having a high absorption coefficient of the order of104cm-1, has beenregarded as one of most promising materials for light-absorbing materials in solarcells because of its content of only low-toxicity elements that are abundant in theearth crust. Recently, Cu2ZnSn(Se)S4thin films can be prepared using variousmethods, such as atom beam sputtering, RF magnetron sputtering, thermalevaporation, pulsed laser deposition, etc. However, these methods have somedrawbacks such as expensive precursors, complicated apparatus and even some toxicbyproducts evolved during their synthesis. In this thesis, we synthesizedCu2ZnSn(Se)S4and CdIn_2S_4nanostructures via a simple solvothermal route and investigated their photoelectric properties. The main content and innovation of thisthesis are listed as following:
(1) Pure Cu_2ZnSnS_4in a hollow sphere morphology has been successfullysynthesized in a PEG-assisted solvothermal reaction with N, N-dimethylformamide asthe solvent. The extensive investigations demonstrated that the PEG plays animportant role in the formation of the hollow spheres.
(2) The growth mechanism for the hollow sphere-like particles has beendiscussed.
(3)Cu_2ZnSnSe_4particles with flowerlike morphology have been successfullysynthesized in a solvothermal reaction with ethylenediamine as the reaction solvent.Stannite Cu_2ZnSnSe_4with a near stoichiometry composition synthesized bysolvothermal process. A possible growth process of the films was also proposed.
(4) The Cu_2ZnSnS_4thin films have been deposited onto FTO glass substrate by asolvothermal method for the first time. These as-deposited films were annealed atdifferent temperatures from250°C to550°C. The influence of the annealingtemperature on the structure, morphology, and composition of the films has beenstudied. The photelectrochemical measurement with CZTS thin films shows that filmsare photoactive which proves itself to be a promising candidate for cost-effective,high efficiency solar cells in future.
(5) For the first time, arrays of Cu_2ZnSnSe_4nanotubes were directly grown onfluorine-doped tin oxide glass substrate by using ZnO nanorods as sacrificialtemplates. The solubility product constant (Ksp) of ZnO is larger than those of ZnSeand CuSe. This implies that the arrays of ZnO nanorods can be used as sacrificialtemplates to synthesize more stable ZnSe by anion exchange and further convert intoCuSe by cation exchange to obtain ZnO/CuSe nanocables. Arrays of CZTSe naotubescan be prepared by using the ZnO/CuSe nanocables as self-sacrificial templates toreact with Zn~(2+)and Sn2+via a polyol reduction process. The ZnO cores are slowlydissolved by the H~+ions produced in the reaction.
(6) The length and diameter of the CZTSe nanotubes can be adjusted by turningthe length of the ZnO nanorods. The effect of the length on the performance of the photoelectrochemical cells was also investigated. We found the CZTSe nanotubeswith the length of2μm showed the best performance of photoelectrochemical cells.
(7) CdIn_2S_4films composed of nanosheets have been directly deposited onfluorine-doped tin oxide substrates using a simple hydrothermal method. TheL-cysteine acting as sulfur source was found to play an important role in theformation of the final films. A possible growth mechanism for the formation CdIn_2S_4films on FTO substrates has been proposed. It was found that the formation ofuniform CdIn_2S_4films attached the FTO substrates underwent the following steps:1)piranha treatment of FTO substrate;2) formation of hetero-nucleation sites on thesubstrate surface;3) growth of CdIn_2S_4film from the nucleation sites.
(8) From the results of the photoelectronchemical properties studies, thephotoelectric conversion efficiency of0.162%was obtained under100mW cm-2illumination.
近年来, Cu_2ZnSnS(Se)_4由于具有与CuIn(Ga)Se_2材料相似的结构和光学性质并且材料中不包含贵金属元素而受到越来越多的重视。Cu_2ZnSnS(Se)_4材料是直接带隙半导体，禁带宽度在1.3-1.6eV之间，光吸收系数大于104cm-1，被认为是理想的薄膜太阳能电池吸收层材料。但是,目前制备Cu_2ZnSnS(Se)_4的方法主要局限在热蒸发技术、磁控溅射、激光脉冲沉积、原子束溅射等。这些方法都有着各自的缺点如反应物昂贵、设备复杂、制备中产生有毒物质等。溶剂热法是一种制备半导体材料常用的化学方法，具有设备简单、易于操作等特点。但是目前关于溶剂热法制备Cu_2ZnSnS(Se)_4的报道依然很少。针对这种情况，我们在本文中研究了利用简单方便的溶剂热方法制备不同形貌结构的纳米结构和薄膜，并首次制备了Cu_2ZnSnSe_4的纳米管阵列，讨论了纳米管阵列的生长机制。此外，我们研究发现具有片状结构的CdIn_2S_4薄膜同样可以通过水热法制备，并且展现出良好的光电性质。
(1)利用溶剂热技术，以二甲基甲酰胺为溶剂，制备了具有空心球状的Cu_2ZnSnS_4纳米结构。实验表明，溶剂中的PEG对空心球状Cu_2ZnSnS_4的形成起关键作用。
(2)根据不同反应条件的对比试验结果详细地讨论了空心球状的Cu_2ZnSnS_4的生长机制。空心球状Cu_2ZnSnS_4的生长可以分为三个过程，首先是溶液中的金属离子与PEG分子作用，吸附在PEG分子表面。之后是在反应温度下溶液中产生S~(2-),金属离子与S~(2-)反应生成球状的Cu_2ZnSnS_4结构。最后经过Ostwaldripening过程形成空心球状的Cu_2ZnSnS_4纳米结构。
(3)利用乙二胺为反应溶剂，成功制备了具有花状结构的Cu_2ZnSnSe_4。对样品测试分析的结果表明得到的Cu_2ZnSnSe_4具有黝锡矿结构和理想的化学成分比例，并讨论了花状Cu_2ZnSnSe_4颗粒的形成过程。
(4)采用溶剂热法在FTO导电基片上直接生长了均匀的Cu_2ZnSnS_4薄膜样品。详细研究了不同退火温度(250-550℃)对样品结构、形貌和成分的影响。当退火温度为550℃时，薄膜样品具有锌黄锡矿结构并且展现出良好的光响应特性。为制备其他硫化物薄膜提供了一种方便低耗的制备方法。
(5)首次在FTO基片上制备出均匀一致的纳米管阵列。Cu_2ZnSnSe_4纳米管阵列是以ZnO纳米棒阵列作为模板，结合了离子交换反应与溶解热技术制备得到的。首先在FTO基片上制备了均匀的ZnO纳米棒阵列。之后，利用材料容积度常数的不同(ZnO＞ZnSe＞CuSe)，通过离子交换反应制备了ZnO/CuSe的电缆结构阵列。最后在溶剂热反应过程中外层的CuSe与Zn~(2+)和Sn~(4+)反应生成Cu_2ZnSnSe_4，同时内部的ZnO与反应中生成的H~+反应而溶解，最终形成了Cu_2ZnSnSe_4的纳米管阵列。
(6)通过改变ZnO纳米棒阵列长度和直径制备了具有不同长度和直径的Cu_2ZnSnSe_4纳米管阵列，并研究了不同长度纳米管阵列的光电化学性质,讨论了光电流的变化规律。结果表明，长度为2μm的Cu_2ZnSnSe_4纳米管阵列的光电化学性质最好。
(7)采用水热法以半胱氨酸为硫源在FTO基片上直接生长了具有片状结构的CdIn_2S_4薄膜。讨论了片状CdIn_2S_4薄膜的生长机制，其生长主要经历三个过程：1）利用H_2SO_4和H_2O_2溶液处理FTO基片；2）CdIn_2S_4在FTO基片表面的异质成核过程；3）CdIn_2S_4在基片成核处的晶体生长过程。
(8)对片状CdIn_2S_4薄膜样品的光电化学性质进行了研究，结果表明，CdIn_2S_4具有良好的光电性质，退火处理后转换效率可以达到0.162%明显好于类似的半导体薄膜材料如In_2S_3，CdS等。
Solar energy is considered to be the most economic and effective among allavailable renewable energy resources. In the solar energy research field, synthesis ofnovel PV materials with simple method is an important research direction. Recently,chalcopyrite-type semiconductors like Cu(In,Ga)Se2or Cu(In,Ga)S2have verybeneficial properties for photo-voltaic applications. Obtained efficiencies areremarkably high, up to nearly20%; however, gallium and indium used for thepreparation of the active layer are very rare and expensive elements. This could leadto a shortage in the supply of these elements and would inhibit a cost-effectivelarge-scaleproduction.
A quaternary semiconductor of Cu_2ZnSnS(Se)_4, which is a direct band gapsemiconductor having a high absorption coefficient of the order of104cm-1, has beenregarded as one of most promising materials for light-absorbing materials in solarcells because of its content of only low-toxicity elements that are abundant in theearth crust. Recently, Cu2ZnSn(Se)S4thin films can be prepared using variousmethods, such as atom beam sputtering, RF magnetron sputtering, thermalevaporation, pulsed laser deposition, etc. However, these methods have somedrawbacks such as expensive precursors, complicated apparatus and even some toxicbyproducts evolved during their synthesis. In this thesis, we synthesizedCu2ZnSn(Se)S4and CdIn_2S_4nanostructures via a simple solvothermal route and investigated their photoelectric properties. The main content and innovation of thisthesis are listed as following:
(1) Pure Cu_2ZnSnS_4in a hollow sphere morphology has been successfullysynthesized in a PEG-assisted solvothermal reaction with N, N-dimethylformamide asthe solvent. The extensive investigations demonstrated that the PEG plays animportant role in the formation of the hollow spheres.
(2) The growth mechanism for the hollow sphere-like particles has beendiscussed.
(3)Cu_2ZnSnSe_4particles with flowerlike morphology have been successfullysynthesized in a solvothermal reaction with ethylenediamine as the reaction solvent.Stannite Cu_2ZnSnSe_4with a near stoichiometry composition synthesized bysolvothermal process. A possible growth process of the films was also proposed.
(4) The Cu_2ZnSnS_4thin films have been deposited onto FTO glass substrate by asolvothermal method for the first time. These as-deposited films were annealed atdifferent temperatures from250°C to550°C. The influence of the annealingtemperature on the structure, morphology, and composition of the films has beenstudied. The photelectrochemical measurement with CZTS thin films shows that filmsare photoactive which proves itself to be a promising candidate for cost-effective,high efficiency solar cells in future.
(5) For the first time, arrays of Cu_2ZnSnSe_4nanotubes were directly grown onfluorine-doped tin oxide glass substrate by using ZnO nanorods as sacrificialtemplates. The solubility product constant (Ksp) of ZnO is larger than those of ZnSeand CuSe. This implies that the arrays of ZnO nanorods can be used as sacrificialtemplates to synthesize more stable ZnSe by anion exchange and further convert intoCuSe by cation exchange to obtain ZnO/CuSe nanocables. Arrays of CZTSe naotubescan be prepared by using the ZnO/CuSe nanocables as self-sacrificial templates toreact with Zn~(2+)and Sn2+via a polyol reduction process. The ZnO cores are slowlydissolved by the H~+ions produced in the reaction.
(6) The length and diameter of the CZTSe nanotubes can be adjusted by turningthe length of the ZnO nanorods. The effect of the length on the performance of the photoelectrochemical cells was also investigated. We found the CZTSe nanotubeswith the length of2μm showed the best performance of photoelectrochemical cells.
(7) CdIn_2S_4films composed of nanosheets have been directly deposited onfluorine-doped tin oxide substrates using a simple hydrothermal method. TheL-cysteine acting as sulfur source was found to play an important role in theformation of the final films. A possible growth mechanism for the formation CdIn_2S_4films on FTO substrates has been proposed. It was found that the formation ofuniform CdIn_2S_4films attached the FTO substrates underwent the following steps:1)piranha treatment of FTO substrate;2) formation of hetero-nucleation sites on thesubstrate surface;3) growth of CdIn_2S_4film from the nucleation sites.
(8) From the results of the photoelectronchemical properties studies, thephotoelectric conversion efficiency of0.162%was obtained under100mW cm-2illumination.
引文
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