近中性pH溶液双电位阶跃法电沉积CuInSe_2薄膜
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摘要
随着世界能源问题的日趋严重,作为太阳能电池吸收层的CuInSe_2薄膜越来越受到人们的重视,本文研究了温和化学条件下CuInSe_2薄膜的电沉积制备,实现了可在ZnO等耐酸碱性差的基底上沉积CuInSe_2薄膜的目的。课题在调查近中性pH温和条件下电沉积CuInSe_2薄膜体系的影响因素的基础上,首次采用双电位阶跃电沉积(DPSED)方法,并结合络合剂的辅助,克服了三元组分沉积电位不匹配的问题,在温和条件下电沉积制备出了接近化学剂量的黄铜矿CuInSe_2薄膜。
首先在ITO玻璃基底上,利用线性伏安法研究了不同络合剂、不同温度以及不同浓度对单一CuCl_2·2H_2O、InCl_3·4H_2O、SeO_2水溶液体系沉积电位的影响。实验得出,在温和条件下通过上述措施,难以实现CuInSe_2薄膜的常规电沉积;柠檬酸钠适合作温和条件下电沉积溶液的络合剂;在-800mV与-1400mV两个沉积电位下,沉积溶液中的三元素Cu、In、Se倾向于两两共沉积,由此提出了DPSED方法。
在DPSED沉积研究中,沉积溶液pH值为6-7的近中性条件,以CuCl_2·2H_2O、InCl_3·4H_2O、SeO_2为前驱体,以柠檬酸钠为络合剂,通过加入过量的柠檬酸钠方式,获得了稳定三元共混的电沉积溶液。考察了DPSED沉积体系、溶液Cu/In比以及阶跃参数对薄膜沉积结构、化学计量与光学性能的影响。通过XRD、XPS、SEM、UV-Vis表征了薄膜。
实验表明,双阶跃电位点分别为-800mV与-1400mV,持续时间分别为30s与60s,循环次数为5次。使用柠檬酸钠为15mM,Cu:In:Se=5:3:5时,得到了接近化学剂量比的无定形沉积膜,随后在氩气氛保护热处理,400℃保温1小时,无定形沉积膜进一步结晶,获得结晶良好,光学性能优异的CuInSe_2薄膜。Cu/In比变化显著影响薄膜形貌及半导体性质,阶跃参数的变化也会影响薄膜形貌。
DPSED沉积过程分析表明,在阶跃沉积样品的XRD衍射谱上出现了CuIn合金相,这可能为生成近化学剂量比的CuInSe_2薄膜提供了活性的两元金属成分。
As the energy problem becom more and more severe, CuInSe_2 as one of I–III–VI chalcopyrite materials, used as absorber layers in solar cells, has obtained widely attention, and it has also been proved to be a leading candidate for photovoltaic applications. This study focused on the electrodeposition of CuInSe_2 thin films using electrolyte with near neutral pH value (pH=6.5), which made the employ of ZnO substrate possible. In this paper, various parameters of mild electrolyte, such as complexing agents, concentrations and temperatures, were investigated as to obtaining CuInSe_2 films. Double potential step electrodeposite (DPSED) methods were creatively adopted in this experiment to prepare CuInSe_2 thin films for the first time.
Linear sweep voltammetry was used to study deposition potential of single raw material (CuCl2, InCl3 and SeO2, respectively) in aqueous solutions systems with different complexing agents, concentrations and temperatures. The results showed that CuInSe_2 couldn’t be obtained at single potential step electrodeposition under any condition with near neutral pH value, whereas binary compound (CuSe, CuIn etc.) could be deposited easily when sodium citrate (CitNa) were used as complexing agent in mild solutions. So DPSED method was proposed to synthesize CuInSe_2 material.
During the deposition of CuInSe_2 by DPSED method, the pH values of electrolyte were fixed between 6~7. CuCl_2·2H_2O, InCl_3·4H_2O, SeO_2 were used as raw materials, and CitNa was adopted as complexing agent. Effects of DPSED systems, such as Cu/In ratio and the step potential parameters, were investigated. XRD、XPS、SEM、UV-Vis were used to characterize films’structure, stoichiometric, morphology and optical properties.
When Cu/In/Se ratio was 5/3/5 with 15mM CitNa, and DPSED parameters was V1=800mV for 30s and V2=1400mV for 60s with 5cycles, as-deposited film were amorphous with near Cu:In:Se=1:1:2. After annealed at 400℃in Ar atmosphere for 60 min, CuInSe_2 films with chalcopyrite structure were obtained. Further studies showed that CuInSe_2 films’semiconductor properties and morphology could be affected when Cu/In ratios of electrolyte and step potential parameters were changed.
The reason for CuInSe_2 successful deposition by DPSED method can be deduced by XRD test. The characteristic peak of CuIn alloy appeared on the samples’XRD spectra , which indicated that active binary metal elements were formed and transformed to be CuInSe_2 films in later annealing process.
首先在ITO玻璃基底上,利用线性伏安法研究了不同络合剂、不同温度以及不同浓度对单一CuCl_2·2H_2O、InCl_3·4H_2O、SeO_2水溶液体系沉积电位的影响。实验得出,在温和条件下通过上述措施,难以实现CuInSe_2薄膜的常规电沉积;柠檬酸钠适合作温和条件下电沉积溶液的络合剂;在-800mV与-1400mV两个沉积电位下,沉积溶液中的三元素Cu、In、Se倾向于两两共沉积,由此提出了DPSED方法。
在DPSED沉积研究中,沉积溶液pH值为6-7的近中性条件,以CuCl_2·2H_2O、InCl_3·4H_2O、SeO_2为前驱体,以柠檬酸钠为络合剂,通过加入过量的柠檬酸钠方式,获得了稳定三元共混的电沉积溶液。考察了DPSED沉积体系、溶液Cu/In比以及阶跃参数对薄膜沉积结构、化学计量与光学性能的影响。通过XRD、XPS、SEM、UV-Vis表征了薄膜。
实验表明,双阶跃电位点分别为-800mV与-1400mV,持续时间分别为30s与60s,循环次数为5次。使用柠檬酸钠为15mM,Cu:In:Se=5:3:5时,得到了接近化学剂量比的无定形沉积膜,随后在氩气氛保护热处理,400℃保温1小时,无定形沉积膜进一步结晶,获得结晶良好,光学性能优异的CuInSe_2薄膜。Cu/In比变化显著影响薄膜形貌及半导体性质,阶跃参数的变化也会影响薄膜形貌。
DPSED沉积过程分析表明,在阶跃沉积样品的XRD衍射谱上出现了CuIn合金相,这可能为生成近化学剂量比的CuInSe_2薄膜提供了活性的两元金属成分。
As the energy problem becom more and more severe, CuInSe_2 as one of I–III–VI chalcopyrite materials, used as absorber layers in solar cells, has obtained widely attention, and it has also been proved to be a leading candidate for photovoltaic applications. This study focused on the electrodeposition of CuInSe_2 thin films using electrolyte with near neutral pH value (pH=6.5), which made the employ of ZnO substrate possible. In this paper, various parameters of mild electrolyte, such as complexing agents, concentrations and temperatures, were investigated as to obtaining CuInSe_2 films. Double potential step electrodeposite (DPSED) methods were creatively adopted in this experiment to prepare CuInSe_2 thin films for the first time.
Linear sweep voltammetry was used to study deposition potential of single raw material (CuCl2, InCl3 and SeO2, respectively) in aqueous solutions systems with different complexing agents, concentrations and temperatures. The results showed that CuInSe_2 couldn’t be obtained at single potential step electrodeposition under any condition with near neutral pH value, whereas binary compound (CuSe, CuIn etc.) could be deposited easily when sodium citrate (CitNa) were used as complexing agent in mild solutions. So DPSED method was proposed to synthesize CuInSe_2 material.
During the deposition of CuInSe_2 by DPSED method, the pH values of electrolyte were fixed between 6~7. CuCl_2·2H_2O, InCl_3·4H_2O, SeO_2 were used as raw materials, and CitNa was adopted as complexing agent. Effects of DPSED systems, such as Cu/In ratio and the step potential parameters, were investigated. XRD、XPS、SEM、UV-Vis were used to characterize films’structure, stoichiometric, morphology and optical properties.
When Cu/In/Se ratio was 5/3/5 with 15mM CitNa, and DPSED parameters was V1=800mV for 30s and V2=1400mV for 60s with 5cycles, as-deposited film were amorphous with near Cu:In:Se=1:1:2. After annealed at 400℃in Ar atmosphere for 60 min, CuInSe_2 films with chalcopyrite structure were obtained. Further studies showed that CuInSe_2 films’semiconductor properties and morphology could be affected when Cu/In ratios of electrolyte and step potential parameters were changed.
The reason for CuInSe_2 successful deposition by DPSED method can be deduced by XRD test. The characteristic peak of CuIn alloy appeared on the samples’XRD spectra , which indicated that active binary metal elements were formed and transformed to be CuInSe_2 films in later annealing process.
引文
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