无镉的铜铟镓硒太阳能电池制备与性能研究
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摘要
黄铜矿型铜铟镓硒(CuIn1-xGaxSe2, CIGS)薄膜太阳能电池具有光电转换效率高、成本低、稳定性好等优点,是最有发展前景的薄膜太阳能电池之一,但其多层薄膜制作工艺复杂,包括钼(Mo)背电极层、CIGS光吸收层、硫化镉(CdS)缓冲层、本征氧化锌(i-ZnO)和掺铝氧化锌(AZO)窗口层,任何一层薄膜质量不好都将影响太阳能电池的的光电性能,因此工艺控制至关重要,本论文重点在CIGS吸收层和无镉缓冲层制备工艺控制研究。
CIGS薄膜是太阳能电池的核心材料。本论文研究了一种工艺简单、可控的CIGS薄膜制备技术：首先,在钠钙玻璃衬底上溅射制备厚度约1微米的钼电极,然后采用双室多靶位磁控溅射沉积系统,通过交替直流溅射CuGa靶(原子比3：1；纯度99.999%)和纯In靶(纯度99.999%),选择不同的叠层方式在钼电极上制备铜铟镓前驱膜；再将前驱膜放入特制的真空炉中选择不同的升温方式进行硒化退火,得到四元化合物铜铟镓硒半导体纳米薄膜,对薄膜进行各项表征(SEM、AFM、XPS、XRD等),分析了前驱膜叠层及硒化升温方式对铜铟镓硒薄膜性能的影响,优化了制备条件：In/CuGa/In多层前驱膜先在250℃恒温20分钟加热预处理,再升温至560℃硒化温度30分钟,制备出致密的黄铜矿结构的多晶铜铟镓硒薄膜,薄膜颗粒直径约1μm,有较好的结晶质量,膜厚2μm,方块电阻为0.11Ω/□,薄膜在波长500-1100nm之间,对可见光及近红外线有很好的吸收。
缓冲层是位于CIGS吸收层和透明导电窗口层之间的薄膜,用以缓冲吸收层和透明导电层之间的带隙差。传统采用的缓冲层CdS对人体有害,而且带隙偏窄,造成太阳光的短波损失,且CdS的传统化学浴制备方法都是湿法工艺,破坏了溅射后硒化或共蒸发中的真空和干法制造流程,因而无镉缓冲层的干法制备具有重要意义。在CIGS电池中的缓冲层材料很薄,原子层沉积方式是最理想的选择,本文采用原子层沉积ZnO(ALD-ZnO)代替CdS做缓冲层,它是没有采用等离子体的软沉积法,可以避免采用磁控溅射的方法制备ZnO时对CIGS膜的损伤；还可以方便地避免现有CIGS工艺流程中唯一的液相化学浴(CBD)工艺,ALD设备可以与现有CIGS生产线其它真空工艺无缝对接,基底在大气中的暴露将很少；ALD-ZnO还提高了短波和近红外范围的量子效率,具有工业化应用价值。
本文研究了ALD制备ZnO缓冲层时薄膜厚度与锌源(DEZn)脉冲时间的关系、薄膜表面粗糙度与锌源脉冲时间的关系和温度对薄膜质量的影响、携带DEZn气体流量与平均生长的薄膜厚度关系、不同锌源脉冲时间下ZnO薄膜的光学特性等,在我们的实验范围得出了最佳工艺条件为：DEZn脉冲时间0.1秒,清洗时间3秒；H2O脉冲时间0.1秒,清洗时间4秒,携带气体为高纯N2,DEZn的携带气体流量为150sccm, H2O的携带气体流量为200sccm,衬底温度为250℃,真空度为20hPa时沉积开始,薄膜生长200个周期。
用原子层沉积法在钠钙玻璃上沉积厚度仅为56.8nm的氧化锌薄膜,利用场发射扫描电镜、AFM和X射线衍射(XRD)、XPS等对样品表面形貌和物相进行分析,得到的ZnO纳米颗粒为六角纤锌矿结构,颗粒的大小约在30-60nm之间；薄膜在波长400-900nm可见光区域透射率达90%以上；使用该原子层沉积氧化锌薄膜做铜铟镓硒太阳能电池的缓冲层,透射电镜TEM显示氧化锌层致密地覆盖在CIGS薄膜上,得到的电池的光电转换效率较高,完全可以替代有毒的CdS做缓冲层。本工艺技术路线环保,简单可控,将有助于无镉的CIGS太阳电池的产业化。
研究制备了的结构为Glass/Mo/CIGS/ALD-ZnO/i-ZnO/n-ZnO:Al无镉的铜铟镓硒太阳能电池。该电池的开路电压为Voc=0.46V,短路电流密度Jsc=13.8mA/cm2,填充因子FF=0.59,样品在没减反射膜情况下的光电转换效率达到3.84%。
Chalcopyrite CuIn1-xGaxSe2(CIGS) thin-film solar cells has advantages of high photoelectric conversion efficiency, low cost and good stability etc., which is one of the most promising thin film solar cells, But the multilayer film production process is complex, including molybdenum (Mo) back electrode layer, CIGS optical absorbing layer, CdS buffer layer, intrinsic ZnO (i-ZnO) window layer and ZnAlO (AZO) film, any one layer of poor quality will affect the photoelectric properties of the solar cells, so the process control is very important, This paper focuses on the CIGS absorption layer and Cd-free buffer layer preparation process control research.
CIGS thin film is the core material of solar cells. In this paper, a kind of simple, controllable technology of the CIGS film fabrication is studied, First, sputter about1micron Mo electrodes on the substrate of the soda-lime glass, and then use dual chamber multi-target magnetron sputtering deposition system, by alternately DC sputtering CuGa target (atomic ratio is3:1; purity is99.999%) and pure In target (purity is99.999%), select a different stack method to prepare precursor film of CIGS on Mo electrode layer; and then, place precursor film into a special vacuum furnace to do selenium annealing by different heating mode to obtain quaternary compounds of CIGS semiconductor nanometer thin films. Based on the characterization of the films (SEM、AFM、XPS、XRD), the effect of precursor film lamination and selenizing heating method to the performance of CIGS thin film is analyzed, preparation conditions are optimizatized:In/CuGa/In multiple precursor film is pretreated when heat20minutes at250℃and then keep30minutes selenizing temperature of560℃, poly crystalline CIGS thin-film can be prepared with dense chalcopyrite structure, thin film particle diameter is about1μm, have good crystalline quality, film thickness is2μm, square resistance is0.11Ω/□. Between the wavelength of500-1100nm, film has good absorption to the visible and near infrared.
The buffer layer is located on the CIGS absorbing layer and transparent conductive window layer, buffer the band gap difference of these two layers. The traditional buffer layer of CdS is harmful to person, and the band gap is narrow resulting in the loss of the short wave of Sunlight. Traditional CdS chemical bath preparation methods are wet technology which destroyed the vacuum after sputtering selenization or co-evaporation and dry manufacturing process, so the development of dry technology of cadmium free (Cd-free) buffer layer has the vital significance. In CIGS cells, the buffer layer material is very thin, the atomic layer deposition method is the best choice, this paper adopts atomic layer deposition of ZnO(ALD-ZnO)to replace CdS to be a buffer layer, it is soft deposition which is no use plasma, so it can avoid the damage of CIGS film when we prepared ZnO film using magnetron sputtering method. ALD technique can easily avoid the only liquid phase chemical bath (CBD) technology of the existing CIGS process, ALD equipment can joint with other vacuum process of the existing production lines seamlessly, the substrate is rarely exposed in the atmosphere; ALD-ZnO also enhances the quantum efficiency of the short wave and near infrared range, it has industrial application value.
This paper studies the relationship between film thickness and zinc source (DEZn) pulse time; the film roughness degree and zinc source pulse time; temperature and the quality of the films; the thickness per growth cycle and carrying the DEZn gas flow; the optical properties of ZnO thin films with different zinc sources pulse, et al; the optimum technological conditions are obtained in our experimental range:DEZn pulse time is0.1seconds,DEZn cleaning time is3seconds; H2O pulse time is0.1seconds, H2O cleaning time is4seconds, carrying gas is high purity N2, carrying DEZn gas flow rate is150sccm, carrying H2O gas flow rate is200sccm, substrate temperature is250℃deposition vacuum is20hPa, thin film growth200cycle.
Zinc oxide thin film which thickness of only56.8nm was deposited on soda-lime glass by the means of atomic layer deposition method, the sample surface morphology and phase are analyzed in the use of field emission scanning electron microscopy、AFM and X-ray diffraction (XRD)、XPS, it shows that the obtained ZnO nano-particles are of hexagonal fiber zinc structure, the particle's diameter is between30nm and60nm; transmittance of the thin film Between the wavelength of400-900nm (in the visible region) is90%or more; and use zinc oxide thin film of atomic layer deposition method as the buffer layer of CIGS solar cell, the TEM shows the zinc oxide layer covers the CIGS thin film densely, and the photoelectric conversion efficiency of the cell is higher, which can totally replace the toxic CdS as the buffer layer, the technology of advanced and environmental protection, simple and controllable, will help the Cd-free CIGS solar cell industrialization.
The structure of Glass/Mo/CIGS/ALD-ZnO/i-ZnO/n-ZnO:Al Cd-Free CIGS solar cells is prepared. The open circuit voltage of the cell is Voc-0.46V, Jsc (short circuit current density)=13.8mA/cm2, FF (fill factor)=0.59, the photoelectric conversion efficiency without antireflection coating reaches3.84%.
CIGS薄膜是太阳能电池的核心材料。本论文研究了一种工艺简单、可控的CIGS薄膜制备技术：首先,在钠钙玻璃衬底上溅射制备厚度约1微米的钼电极,然后采用双室多靶位磁控溅射沉积系统,通过交替直流溅射CuGa靶(原子比3：1；纯度99.999%)和纯In靶(纯度99.999%),选择不同的叠层方式在钼电极上制备铜铟镓前驱膜；再将前驱膜放入特制的真空炉中选择不同的升温方式进行硒化退火,得到四元化合物铜铟镓硒半导体纳米薄膜,对薄膜进行各项表征(SEM、AFM、XPS、XRD等),分析了前驱膜叠层及硒化升温方式对铜铟镓硒薄膜性能的影响,优化了制备条件：In/CuGa/In多层前驱膜先在250℃恒温20分钟加热预处理,再升温至560℃硒化温度30分钟,制备出致密的黄铜矿结构的多晶铜铟镓硒薄膜,薄膜颗粒直径约1μm,有较好的结晶质量,膜厚2μm,方块电阻为0.11Ω/□,薄膜在波长500-1100nm之间,对可见光及近红外线有很好的吸收。
缓冲层是位于CIGS吸收层和透明导电窗口层之间的薄膜,用以缓冲吸收层和透明导电层之间的带隙差。传统采用的缓冲层CdS对人体有害,而且带隙偏窄,造成太阳光的短波损失,且CdS的传统化学浴制备方法都是湿法工艺,破坏了溅射后硒化或共蒸发中的真空和干法制造流程,因而无镉缓冲层的干法制备具有重要意义。在CIGS电池中的缓冲层材料很薄,原子层沉积方式是最理想的选择,本文采用原子层沉积ZnO(ALD-ZnO)代替CdS做缓冲层,它是没有采用等离子体的软沉积法,可以避免采用磁控溅射的方法制备ZnO时对CIGS膜的损伤；还可以方便地避免现有CIGS工艺流程中唯一的液相化学浴(CBD)工艺,ALD设备可以与现有CIGS生产线其它真空工艺无缝对接,基底在大气中的暴露将很少；ALD-ZnO还提高了短波和近红外范围的量子效率,具有工业化应用价值。
本文研究了ALD制备ZnO缓冲层时薄膜厚度与锌源(DEZn)脉冲时间的关系、薄膜表面粗糙度与锌源脉冲时间的关系和温度对薄膜质量的影响、携带DEZn气体流量与平均生长的薄膜厚度关系、不同锌源脉冲时间下ZnO薄膜的光学特性等,在我们的实验范围得出了最佳工艺条件为：DEZn脉冲时间0.1秒,清洗时间3秒；H2O脉冲时间0.1秒,清洗时间4秒,携带气体为高纯N2,DEZn的携带气体流量为150sccm, H2O的携带气体流量为200sccm,衬底温度为250℃,真空度为20hPa时沉积开始,薄膜生长200个周期。
用原子层沉积法在钠钙玻璃上沉积厚度仅为56.8nm的氧化锌薄膜,利用场发射扫描电镜、AFM和X射线衍射(XRD)、XPS等对样品表面形貌和物相进行分析,得到的ZnO纳米颗粒为六角纤锌矿结构,颗粒的大小约在30-60nm之间；薄膜在波长400-900nm可见光区域透射率达90%以上；使用该原子层沉积氧化锌薄膜做铜铟镓硒太阳能电池的缓冲层,透射电镜TEM显示氧化锌层致密地覆盖在CIGS薄膜上,得到的电池的光电转换效率较高,完全可以替代有毒的CdS做缓冲层。本工艺技术路线环保,简单可控,将有助于无镉的CIGS太阳电池的产业化。
研究制备了的结构为Glass/Mo/CIGS/ALD-ZnO/i-ZnO/n-ZnO:Al无镉的铜铟镓硒太阳能电池。该电池的开路电压为Voc=0.46V,短路电流密度Jsc=13.8mA/cm2,填充因子FF=0.59,样品在没减反射膜情况下的光电转换效率达到3.84%。
Chalcopyrite CuIn1-xGaxSe2(CIGS) thin-film solar cells has advantages of high photoelectric conversion efficiency, low cost and good stability etc., which is one of the most promising thin film solar cells, But the multilayer film production process is complex, including molybdenum (Mo) back electrode layer, CIGS optical absorbing layer, CdS buffer layer, intrinsic ZnO (i-ZnO) window layer and ZnAlO (AZO) film, any one layer of poor quality will affect the photoelectric properties of the solar cells, so the process control is very important, This paper focuses on the CIGS absorption layer and Cd-free buffer layer preparation process control research.
CIGS thin film is the core material of solar cells. In this paper, a kind of simple, controllable technology of the CIGS film fabrication is studied, First, sputter about1micron Mo electrodes on the substrate of the soda-lime glass, and then use dual chamber multi-target magnetron sputtering deposition system, by alternately DC sputtering CuGa target (atomic ratio is3:1; purity is99.999%) and pure In target (purity is99.999%), select a different stack method to prepare precursor film of CIGS on Mo electrode layer; and then, place precursor film into a special vacuum furnace to do selenium annealing by different heating mode to obtain quaternary compounds of CIGS semiconductor nanometer thin films. Based on the characterization of the films (SEM、AFM、XPS、XRD), the effect of precursor film lamination and selenizing heating method to the performance of CIGS thin film is analyzed, preparation conditions are optimizatized:In/CuGa/In multiple precursor film is pretreated when heat20minutes at250℃and then keep30minutes selenizing temperature of560℃, poly crystalline CIGS thin-film can be prepared with dense chalcopyrite structure, thin film particle diameter is about1μm, have good crystalline quality, film thickness is2μm, square resistance is0.11Ω/□. Between the wavelength of500-1100nm, film has good absorption to the visible and near infrared.
The buffer layer is located on the CIGS absorbing layer and transparent conductive window layer, buffer the band gap difference of these two layers. The traditional buffer layer of CdS is harmful to person, and the band gap is narrow resulting in the loss of the short wave of Sunlight. Traditional CdS chemical bath preparation methods are wet technology which destroyed the vacuum after sputtering selenization or co-evaporation and dry manufacturing process, so the development of dry technology of cadmium free (Cd-free) buffer layer has the vital significance. In CIGS cells, the buffer layer material is very thin, the atomic layer deposition method is the best choice, this paper adopts atomic layer deposition of ZnO(ALD-ZnO)to replace CdS to be a buffer layer, it is soft deposition which is no use plasma, so it can avoid the damage of CIGS film when we prepared ZnO film using magnetron sputtering method. ALD technique can easily avoid the only liquid phase chemical bath (CBD) technology of the existing CIGS process, ALD equipment can joint with other vacuum process of the existing production lines seamlessly, the substrate is rarely exposed in the atmosphere; ALD-ZnO also enhances the quantum efficiency of the short wave and near infrared range, it has industrial application value.
This paper studies the relationship between film thickness and zinc source (DEZn) pulse time; the film roughness degree and zinc source pulse time; temperature and the quality of the films; the thickness per growth cycle and carrying the DEZn gas flow; the optical properties of ZnO thin films with different zinc sources pulse, et al; the optimum technological conditions are obtained in our experimental range:DEZn pulse time is0.1seconds,DEZn cleaning time is3seconds; H2O pulse time is0.1seconds, H2O cleaning time is4seconds, carrying gas is high purity N2, carrying DEZn gas flow rate is150sccm, carrying H2O gas flow rate is200sccm, substrate temperature is250℃deposition vacuum is20hPa, thin film growth200cycle.
Zinc oxide thin film which thickness of only56.8nm was deposited on soda-lime glass by the means of atomic layer deposition method, the sample surface morphology and phase are analyzed in the use of field emission scanning electron microscopy、AFM and X-ray diffraction (XRD)、XPS, it shows that the obtained ZnO nano-particles are of hexagonal fiber zinc structure, the particle's diameter is between30nm and60nm; transmittance of the thin film Between the wavelength of400-900nm (in the visible region) is90%or more; and use zinc oxide thin film of atomic layer deposition method as the buffer layer of CIGS solar cell, the TEM shows the zinc oxide layer covers the CIGS thin film densely, and the photoelectric conversion efficiency of the cell is higher, which can totally replace the toxic CdS as the buffer layer, the technology of advanced and environmental protection, simple and controllable, will help the Cd-free CIGS solar cell industrialization.
The structure of Glass/Mo/CIGS/ALD-ZnO/i-ZnO/n-ZnO:Al Cd-Free CIGS solar cells is prepared. The open circuit voltage of the cell is Voc-0.46V, Jsc (short circuit current density)=13.8mA/cm2, FF (fill factor)=0.59, the photoelectric conversion efficiency without antireflection coating reaches3.84%.
引文
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