Cu_2ZnSnS_4薄膜及其太阳电池的溅射法制备和性能研究
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摘要
太阳能来源丰富,可以满足全世界的能源需求，被认为是最具有前景的可再生能源。目前，a-Si, CdTe和CuIn_xGa_(1-x)Se_2(CIGS)薄膜太阳电池已经商品化。其中CIGS电池效率最高，CIGS电池效率已经接近多晶硅电池效率并对其市场构成了一定的竞争。然而，不得不承认的是CIGS薄膜太阳电池将面临很多困难，其中之一就是其组成元素In是一种稀有元素且将在未来10～20年内逐渐减少，同时In的价格则早已显著提升。
Cu_2ZnSnS_4(CZTS)和高度成熟的CIGS和CuInS3材料类似，是薄膜光伏器件领域极富前景的竞争者。CZTS电池因为其组成元素储量丰富价格低廉，具有降低未来电池商业成本的潜在能力。
在制备和研究CZTS薄膜及其电池之前，本文首先研究了SnS薄膜的硫化法制备工艺。硫化法制备SnS薄膜的过程通过二步过程完成，这个过程包括：首先用溅射法制备金属Sn预制层，然后将金属预制层在硫气氛中进行加热硫化。实验中得到的高质量的制备态的SnS薄膜表明本论文实验中选择的硫化法工艺非常适合制备硫化物光伏薄膜。SnS薄膜的硫化法制备工艺和研究方法为后续硫化法制备CZTS薄膜提供了极为实用的研究基础和借鉴。
在二步法制备SnS薄膜及其研究基础之上，本文运用了二步法同样成功制备了CZTS薄膜。二步法制备CZTS薄膜的过程为：首先溅射法制备了Cu, Zn和Sn金属预制层，然后在充有硫气氛的加热炉中通过加热方式进行硫化。
CZTS薄膜的硫化反应、形貌、元素比例、光学、电学以及光响应电流性能与CZTS薄膜的硫化温度、硫化时间和金属预制层中各单层的排列顺序之间的关系通过XRD、Raman光谱、SEM、EDS、UV-VIS-IR分光光度计和Keithely2400数字源表等手段和仪器进行了一系列的研究。研究发现最佳硫化温度为500℃,最佳硫化时间为2h,而最佳金属预制层中各单层的排列顺序为glass/Zn/Sn/Cu。制备的CZTS薄膜表面致密均匀，元素比例非常接近标准化学计量比。
CZTS薄膜具有明显的光响应电流和持续光电导现象。本文首次研究了外加电压对CZTS薄膜光电流衰减时间以及光电流的瞬态跃迁和陡然下降过程持续时间的影响。结果发现CZTS薄膜光生电流的衰减时间随着外加电压从1V下降到1×10~(-4)V的过程中由378s下降到0.341s。在较低的外加电压下即较低的电场强度下，光照时光生电流的瞬态跃迁和在关闭光照时电流的陡然下降过程明显。同时，外加电压和CZTS薄膜光电流的衰减时间之间的关系可以通过e指数函数来表示。
本文运用化学浴的方法成功制备了用于CZTS太阳电池发射极的CdS和ZnS薄膜。CdS和ZnS薄膜的性能通过XRD、SEM、紫外-可见-近红外分光光度计等手段进行了一系列的研究。.测试发现制备态的CdS和ZnS薄膜表面致密，且薄膜中元素比例都接近标准化学计量比。CdS和ZnS的光学带隙值为2.5和3.9eV。制备态的CZTS/CdS和CZTS/ZnS异质结薄膜太阳电池都具有明显的光伏性能。
本文首次制备了无Cd的完全无毒的新型环保型SnS/a-Si和CZTS/a-Si异质结薄膜太阳电池。SnS/a-Si和CZTS/a-Si异质结薄膜太阳电池都具有明显的光伏性能。SnS/a-Si异质结薄膜太阳电池的开路电压，短路电流密度，填充因子和光电转换效率分别为289mV,1.55mA/cm2,38%和0.17%。同时研究了本征非晶硅薄膜即i-a-Si对CZTS/a-Si薄膜太阳电池的影响。结果发现本征非晶硅薄膜即i-a-Si能够明显提升CZTS/a-Si薄膜太阳电池的光伏性能。引入本征非晶硅薄膜即i-a-Si后CZTS/a-Si电池的开路电压，短路电流密度，填充因子和光电转换效率都明显提升，其中光电转换效率更是提升了将近139%。引入本征非晶硅薄膜即i-a-Si后制备的CZTS/i-a-Si/n-a-Si薄膜太阳电池的开路电压，短路电流密度，填充因子和光电转换效率分别为562mV,12.3mA/cm2,43.8%和3.03%。
The most promising renewable energy is solar energy, as it can potentially cover the world’s energyconsumption So far, three thin film materials have been used for industrial production of solar cells:a-Si, CdTe and Cu(In,Ga)(S,Se)2(CIGS), in which CIGS solar cell reached the highest efficienciy andcan compete with polycrystalline silicon. Admittedly CIGS will also have to face some difficulties.One problem is that indium is a rare element and could run low within the next10～20years, whilethe price of indium is already now increasing rapidly.
Cu_2ZnSnS_4(CZTS), similar to the highly successful Cu(In,Ga)(S,Se)2and CuInS2materials, is apromising candidate for thin film photovoltaic devices. It has advantages such as containing no rare orexpensive elements, and cost-reduction potential for commercial systems.
Before the preparation and research of CZTS thin film, SnS film’s preparation by sulfurization wasfirstly carried out in this thesis. A two-stage process for fabrication of SnS films is presented, whichincludes sputtering of Sn layers and a succeeded heat treatment in the presence of S vapour(‘sulfurisation’). The high property of prepared SnS film shows that the sulfurization method issuitable for the preparation of chalcogenide photovoltaic thin films. The research method and thesulfurization process of SnS are useful for the preparation and research of the CZTS thin film.
Based on the successful two-stage process preparation and research on the SnS film, CZTS filmswere successful prepared by a two-stage process which consists of sequential sputtering of Cu, Sn andZn layers followed by a heat treatment in the presence of S vapour (‘sulfurisation’) too.
The sulfurisation reaction and morphology, element ratio, optical, electrical and photoresponsecurrent of CZTS were studied by XRD, Raman spectroscopy, SEM, EDS, UV-VIS-IRspectrophotometer and Keithely2400source meter as a function of temperature, sulfurization timeand the sort order of precursors. It is shown that the best sulfurisation temperature, the bestsulfurization time and the best precursor are500℃,2h, and glass/Zn/Sn/Cu respectively. The surfaceof the prepared CZTS film is compact and the element ratio is close to the stoichiometric.
The CZTS film shows obvious photo response current and persistent photoconductivityphenomenon. The effect of applied voltage on the current decay time and the time of current jump anddrop region last are firstly studied. It is found that the decay time of photo excited current of CZTSdecreased from378s to0.341s with the electrical field reducing from1V to1×10~(-4)V, respectively.Under lower electrical fields, the "instantaneous" jump and drop of current appeared respectively when the light was turned on and off and their mechanism was investigated. The relationship betweenapplied voltage and decay time could be given by exponential function.
The CdS and ZnS emitter layers for the CZTS based solar cells were successfully prepared bychemical bath deposition. The properties of CdS and ZnS films were systematically researched byXRD, SEM, UV-Vis-IR. It is found that the prepared CdS and ZnS films are compact and the elementratios of these films are all close to the stiochiometric. The band gap energy of CdS and ZnS are about2.5and3.9eV, respectively. The unoptimized prepared CZTS/CdS and CZTS/ZnS heterojunction thinfilm solar cells all showed obvious PV performance.
Cd free completely nontoxic novel SnS/a-Si and CZTS/a-Si thin film heterojunction solar cellswere firstly fabricated and reported in this thesis. All the PV performances of SnS/a-Si and CZTS/a-Sisolar cells are very obviously. The open circuit voltage, the short circuit current density, the filledfactor and the conversion efficiency of SnS/a-Si solar cell are289m,1.55mA/cm2,38%and0.17%,respectively. The effect of i-a-Si layer on the CZTS/a-Si thin film solar cells was researched. It isfound that i-a-Si layer can obviously improve the PV performance of CZTS/a-Si solar cells. The opencircuit voltage, short circuit current density and fill factor of this solar cell all increased obviously byinserting intrinsic a-Si film (i-a-Si), and the conversion efficiency increased about139%by insertingi-a-Si film. The open circuit voltage, short circuit current density, fill factor and conversion efficiencyof CZTS/i-a-Si/n-a-Si solar cell reached562mV,12.3mA/cm2,43.8%and3.03%, respectively.
Cu_2ZnSnS_4(CZTS)和高度成熟的CIGS和CuInS3材料类似，是薄膜光伏器件领域极富前景的竞争者。CZTS电池因为其组成元素储量丰富价格低廉，具有降低未来电池商业成本的潜在能力。
在制备和研究CZTS薄膜及其电池之前，本文首先研究了SnS薄膜的硫化法制备工艺。硫化法制备SnS薄膜的过程通过二步过程完成，这个过程包括：首先用溅射法制备金属Sn预制层，然后将金属预制层在硫气氛中进行加热硫化。实验中得到的高质量的制备态的SnS薄膜表明本论文实验中选择的硫化法工艺非常适合制备硫化物光伏薄膜。SnS薄膜的硫化法制备工艺和研究方法为后续硫化法制备CZTS薄膜提供了极为实用的研究基础和借鉴。
在二步法制备SnS薄膜及其研究基础之上，本文运用了二步法同样成功制备了CZTS薄膜。二步法制备CZTS薄膜的过程为：首先溅射法制备了Cu, Zn和Sn金属预制层，然后在充有硫气氛的加热炉中通过加热方式进行硫化。
CZTS薄膜的硫化反应、形貌、元素比例、光学、电学以及光响应电流性能与CZTS薄膜的硫化温度、硫化时间和金属预制层中各单层的排列顺序之间的关系通过XRD、Raman光谱、SEM、EDS、UV-VIS-IR分光光度计和Keithely2400数字源表等手段和仪器进行了一系列的研究。研究发现最佳硫化温度为500℃,最佳硫化时间为2h,而最佳金属预制层中各单层的排列顺序为glass/Zn/Sn/Cu。制备的CZTS薄膜表面致密均匀，元素比例非常接近标准化学计量比。
CZTS薄膜具有明显的光响应电流和持续光电导现象。本文首次研究了外加电压对CZTS薄膜光电流衰减时间以及光电流的瞬态跃迁和陡然下降过程持续时间的影响。结果发现CZTS薄膜光生电流的衰减时间随着外加电压从1V下降到1×10~(-4)V的过程中由378s下降到0.341s。在较低的外加电压下即较低的电场强度下，光照时光生电流的瞬态跃迁和在关闭光照时电流的陡然下降过程明显。同时，外加电压和CZTS薄膜光电流的衰减时间之间的关系可以通过e指数函数来表示。
本文运用化学浴的方法成功制备了用于CZTS太阳电池发射极的CdS和ZnS薄膜。CdS和ZnS薄膜的性能通过XRD、SEM、紫外-可见-近红外分光光度计等手段进行了一系列的研究。.测试发现制备态的CdS和ZnS薄膜表面致密，且薄膜中元素比例都接近标准化学计量比。CdS和ZnS的光学带隙值为2.5和3.9eV。制备态的CZTS/CdS和CZTS/ZnS异质结薄膜太阳电池都具有明显的光伏性能。
本文首次制备了无Cd的完全无毒的新型环保型SnS/a-Si和CZTS/a-Si异质结薄膜太阳电池。SnS/a-Si和CZTS/a-Si异质结薄膜太阳电池都具有明显的光伏性能。SnS/a-Si异质结薄膜太阳电池的开路电压，短路电流密度，填充因子和光电转换效率分别为289mV,1.55mA/cm2,38%和0.17%。同时研究了本征非晶硅薄膜即i-a-Si对CZTS/a-Si薄膜太阳电池的影响。结果发现本征非晶硅薄膜即i-a-Si能够明显提升CZTS/a-Si薄膜太阳电池的光伏性能。引入本征非晶硅薄膜即i-a-Si后CZTS/a-Si电池的开路电压，短路电流密度，填充因子和光电转换效率都明显提升，其中光电转换效率更是提升了将近139%。引入本征非晶硅薄膜即i-a-Si后制备的CZTS/i-a-Si/n-a-Si薄膜太阳电池的开路电压，短路电流密度，填充因子和光电转换效率分别为562mV,12.3mA/cm2,43.8%和3.03%。
The most promising renewable energy is solar energy, as it can potentially cover the world’s energyconsumption So far, three thin film materials have been used for industrial production of solar cells:a-Si, CdTe and Cu(In,Ga)(S,Se)2(CIGS), in which CIGS solar cell reached the highest efficienciy andcan compete with polycrystalline silicon. Admittedly CIGS will also have to face some difficulties.One problem is that indium is a rare element and could run low within the next10～20years, whilethe price of indium is already now increasing rapidly.
Cu_2ZnSnS_4(CZTS), similar to the highly successful Cu(In,Ga)(S,Se)2and CuInS2materials, is apromising candidate for thin film photovoltaic devices. It has advantages such as containing no rare orexpensive elements, and cost-reduction potential for commercial systems.
Before the preparation and research of CZTS thin film, SnS film’s preparation by sulfurization wasfirstly carried out in this thesis. A two-stage process for fabrication of SnS films is presented, whichincludes sputtering of Sn layers and a succeeded heat treatment in the presence of S vapour(‘sulfurisation’). The high property of prepared SnS film shows that the sulfurization method issuitable for the preparation of chalcogenide photovoltaic thin films. The research method and thesulfurization process of SnS are useful for the preparation and research of the CZTS thin film.
Based on the successful two-stage process preparation and research on the SnS film, CZTS filmswere successful prepared by a two-stage process which consists of sequential sputtering of Cu, Sn andZn layers followed by a heat treatment in the presence of S vapour (‘sulfurisation’) too.
The sulfurisation reaction and morphology, element ratio, optical, electrical and photoresponsecurrent of CZTS were studied by XRD, Raman spectroscopy, SEM, EDS, UV-VIS-IRspectrophotometer and Keithely2400source meter as a function of temperature, sulfurization timeand the sort order of precursors. It is shown that the best sulfurisation temperature, the bestsulfurization time and the best precursor are500℃,2h, and glass/Zn/Sn/Cu respectively. The surfaceof the prepared CZTS film is compact and the element ratio is close to the stoichiometric.
The CZTS film shows obvious photo response current and persistent photoconductivityphenomenon. The effect of applied voltage on the current decay time and the time of current jump anddrop region last are firstly studied. It is found that the decay time of photo excited current of CZTSdecreased from378s to0.341s with the electrical field reducing from1V to1×10~(-4)V, respectively.Under lower electrical fields, the "instantaneous" jump and drop of current appeared respectively when the light was turned on and off and their mechanism was investigated. The relationship betweenapplied voltage and decay time could be given by exponential function.
The CdS and ZnS emitter layers for the CZTS based solar cells were successfully prepared bychemical bath deposition. The properties of CdS and ZnS films were systematically researched byXRD, SEM, UV-Vis-IR. It is found that the prepared CdS and ZnS films are compact and the elementratios of these films are all close to the stiochiometric. The band gap energy of CdS and ZnS are about2.5and3.9eV, respectively. The unoptimized prepared CZTS/CdS and CZTS/ZnS heterojunction thinfilm solar cells all showed obvious PV performance.
Cd free completely nontoxic novel SnS/a-Si and CZTS/a-Si thin film heterojunction solar cellswere firstly fabricated and reported in this thesis. All the PV performances of SnS/a-Si and CZTS/a-Sisolar cells are very obviously. The open circuit voltage, the short circuit current density, the filledfactor and the conversion efficiency of SnS/a-Si solar cell are289m,1.55mA/cm2,38%and0.17%,respectively. The effect of i-a-Si layer on the CZTS/a-Si thin film solar cells was researched. It isfound that i-a-Si layer can obviously improve the PV performance of CZTS/a-Si solar cells. The opencircuit voltage, short circuit current density and fill factor of this solar cell all increased obviously byinserting intrinsic a-Si film (i-a-Si), and the conversion efficiency increased about139%by insertingi-a-Si film. The open circuit voltage, short circuit current density, fill factor and conversion efficiencyof CZTS/i-a-Si/n-a-Si solar cell reached562mV,12.3mA/cm2,43.8%and3.03%, respectively.
引文
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