CN113346024A - 一种钙钛矿晶体薄膜以及钙钛矿太阳能电池的制备方法 - Google Patents
一种钙钛矿晶体薄膜以及钙钛矿太阳能电池的制备方法 Download PDFInfo
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- CN113346024A CN113346024A CN202010137011.XA CN202010137011A CN113346024A CN 113346024 A CN113346024 A CN 113346024A CN 202010137011 A CN202010137011 A CN 202010137011A CN 113346024 A CN113346024 A CN 113346024A
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Abstract
本发明涉及一种钙钛矿晶体薄膜的制备方法,包括步骤:配制含碳酸氢铵的金属卤化物溶液;在基底表面涂布或沉积步骤1制备的含碳酸氢铵的金属卤化物溶液,得到金属卤化物薄膜;将含氮卤化物扩散进入金属卤化物薄膜,反应得到钙钛矿晶体薄膜层。本发明还公开一种使用该方法进行钙钛矿太阳能电池的制备方法。本发明通过适量碳酸氢铵添加剂的引入,促进了两步法制备钙钛矿薄膜的过程中,钙钛矿组分的充分扩散、反应,易于大面积制备均匀且厚的钙钛矿晶体薄膜。
Description
技术领域
本发明涉及一种钙钛矿晶体薄膜以及钙钛矿太阳能电池的制备方法。
背景技术
钙钛矿光吸收材料是一类具有ABX3结构的化合物,一般地,A位主要是一价的金属离子,包括Li+、Na+、K+、Rb+、Cs+等,以及一些含氮的有机阳离子,比如甲胺阳离子、二甲胺阳离子、乙胺阳离子、正丁胺阳离子、苯甲胺阳离子、甲脒阳离子、胍阳离子。B位主要二价的铅离子和锡离子。X位主要是卤素阴离子和硫氰酸根阴离子,以及醋酸根阴离子。这些离子组成具有钙钛矿晶体结构的材料具有良好的光电性能,非常适合应用在光伏、发光和光电探测等多个领域。
采用溶液两步法的方式制备钙钛矿薄膜具有成本低,易于大面积生长的特点。在两步法中,先在基底上沉积一层金属卤化物薄膜,然后将含氮卤化物扩散进入金属卤化物膜层,加热反应制得钙钛矿薄膜。这种方法有一个明显的局限,即金属卤化物薄膜不能太厚,否则,含氮卤化物难以充分扩散进入反应,导致薄膜中出现大量的缺陷,从而器件性能低下。研究表明,在钙钛矿晶体的生长过程中,引入少量的溶剂气体,可以有效的促进含氮卤化物的扩散,调节晶体的生长,获得缺陷少、晶粒大,膜层更厚的钙钛矿晶体。而采用溶剂辅助晶体生长的方法仍然存在不足,溶剂气体由表及里的作用过程中,表面或晶界的钙钛矿材料经受了大量的溶剂侵袭,会导致缺陷增多。而受限于气体缓慢的的扩散过程,特别是对于厚的钙钛矿前驱体膜层,内部的钙钛矿并不能充分的与溶剂作用。因此,如何充分且均匀的制备厚的钙钛矿晶体膜层是亟待改善的问题。
发明内容
本发明所要解决的技术问题在于,提供一种钙钛矿晶体薄膜以及钙钛矿太阳能电池的制备方法,解决了常规使用两步法制备钙钛矿薄膜的过程中,因钙钛矿组分的扩散过程受限,难以制得大面积、均匀且厚的钙钛矿晶体薄膜,工艺重复性不佳等问题,易于制得厚的、结晶质量高的钙钛矿薄膜。
本发明是这样实现的,提供一种钙钛矿晶体薄膜的制备方法,包括如下步骤:
步骤1:配制含碳酸氢铵的金属卤化物溶液;
步骤2:在基底表面涂布或沉积步骤1制备的含碳酸氢铵的金属卤化物溶液,得到金属卤化物薄膜;
步骤3:将含氮卤化物扩散进入金属卤化物薄膜,反应得到钙钛矿晶体薄膜层。
本发明将适量的碳酸氢铵加入到钙钛矿的前驱体薄膜中,当退火时,碳酸氢铵逐渐分解出氨气和水,它们与钙钛矿前驱体材料短暂结合,促进钙钛矿组分的相互作用和扩散,使钙钛矿晶体的生长过程充分且均匀。因此,通过碳酸氢铵的加入,可以实现自溶剂退火。相比外源溶剂气体的引入,自溶剂退火具有明显的优势,可以诱导钙钛矿晶体自基底均匀、致密的生长,从而易于制得厚的、结晶质量高的钙钛矿薄膜。
本发明是这样实现的,提供一种钙钛矿太阳能电池的制备方法,在所述钙钛矿太阳能电池中含有钙钛矿薄膜层,所述钙钛矿薄膜层采用如前所述的钙钛矿晶体薄膜的制备方法制备。
与现有技术相比,本发明的一种钙钛矿晶体薄膜以及钙钛矿太阳能电池的制备方法,通过适量碳酸氢铵添加剂的引入,促进了两步法制备钙钛矿薄膜的过程中,钙钛矿组分的充分扩散、反应,易于大面积制备均匀且厚的钙钛矿晶体薄膜。
附图说明
图1为本发明的三种实施例制备的钙钛矿太阳能电池的电流-电压曲线性能示意图。
具体实施方式
为了使本发明所要解决的技术问题、技术方案及有益效果更加清楚明白,以下结合附图及实施例,对本发明进行进一步详细说明。应当理解,此处所描述的具体实施例仅仅用以解释本发明,并不用于限定本发明。
请参照图1所示,本发明钙钛矿晶体薄膜的制备方法的较佳实施例,包括如下步骤:
步骤1:配制含碳酸氢铵的金属卤化物溶液。
步骤2:在基底表面涂布或沉积步骤1制备的含碳酸氢铵的金属卤化物溶液,得到金属卤化物薄膜。
步骤3:将含氮卤化物扩散进入金属卤化物薄膜,反应得到钙钛矿晶体薄膜层。
具体地,在所述步骤1中,配制含碳酸氢铵的金属卤化物溶液的方法是将卤化铅粉末溶解在溶剂中配制成溶液,在该溶液中含有适量的添加剂,所述添加剂为碳酸氢铵。所用的溶剂是混合溶剂,所述混合溶剂包括酰胺类溶剂、砜类/亚砜类溶剂、酯类溶剂、烃类、卤代烃类溶剂、醇类溶剂、酮类溶剂、醚类溶剂、芳香烃溶剂中至少一种。在含碳酸氢铵的金属卤化物溶液中,阳离子中二价金属铅的摩尔百分数不低于80%,阴离子包括负一价氯离子、溴离子、碘离子、硫氰酸根、乙酸根中的至少一种,阴离子中碘离子的摩尔百分数不低于80%。
具体地,在金属卤化物溶液中还有掺杂剂,所述掺杂剂包括含胺基、脒基、胍基中至少一种有机化合物,或者含锂、钠、钾、铷、铯、硼、硅、锗、砷、锑、铍、镁、钙、锶、钡、铝、铟、镓、锡、铊、铅、铋、镧、铈、镨、钕、钐、铕、钆、铽、镝、钬、铒、铥、镱、镥、钪、钛、钒、铬、锰、铁、钴、镍、铜、锌、钇、锆、铌、钼、钌、铑、钯、银、镉、铪、钽、钨、铼、锇、铱、铂、金中至少一种无机化合物。
具体地,所述溶剂为N,N-二甲基甲酰胺(DMF)、己内酰胺、二甲基亚砜(DMSO)、N-甲基吡咯烷酮(NMP)、γ-丁内酯(GBL)中至少一种。
具体地,在步骤2中,所述基底包括透明导电层和半导体材料层,其在波长为350nm~800nm范围光透过率不低于80%。所述透明导电层包括相互复合的支撑层与功能层,所述支撑层的材料包括玻璃、聚对苯二甲酸乙二醇酯(PET)、聚萘二甲酸乙二醇酯(PEN)及聚酰亚胺(PI)中任意一种,所述功能层的材料包括氧化铟锡(ITO)、掺氟氧化锡(FTO)、掺铝氧化锌(AZO)中任意一种。所述半导体材料层的材料包括空穴传输材料或电子传输材料,所述空穴传输材料包括氧化镍、氧化钒、氧化钼、硫化铜、硫氰酸亚铜、氧化铜、氧化亚铜、氧化钴、PTAA、PEDOT、Spiro-MeOTAD和它们的掺杂物中的至少一种,该层厚度为5nm~200nm;所述电子传输材料包括二氧化钛、氧化锌、硫化镉、二氧化锡、三氧化二铟、氧化钨、氧化铈、C60、C70、PCBM以及它们的衍生物或掺杂物中的至少一种,该层厚度为5nm~300nm。
具体地,在步骤2中,所述涂布或沉积方法包括狭缝涂(slot die)、刮涂、旋涂、喷涂、丝网印刷、蒸镀中任意一种加工方式。
具体地,在步骤2的金属卤化物薄膜和步骤3的钙钛矿晶体薄膜的制备过程中,处理温度不超过200℃。
下面结合具体实施例说明本发明的钙钛矿太阳能电池的制备方法。
实施例1
本发明的第一种钙钛矿太阳能电池的制备方法,包括如下步骤:
(11).称取碘化铅粉末溶解在N,N-二甲基甲酰胺中,碘化铅的浓度为0.5mol/L,充分溶解后,再加入碳酸氢铵粉末,溶解后的浓度为2g/L。
(12).将步骤(11)得到的溶液在热风辅助下均匀喷涂在PEN/ITO/PEDOT:PSS基底上,60℃烘烤5分钟,得到厚度为300纳米的碘化铅薄膜。
(13).将甲胺氢碘酸盐蒸镀到步骤(12)制备的碘化铅薄膜上,厚度为50纳米。
(14).将经步骤(13)处理得到的基底置于氮气氛围中,100℃保持30分钟。
(15).待反应完成,冷却至室温,用异丙醇快速冲洗基底上制备的碘化铅薄膜表面,去除其上残余的甲胺氢碘酸盐,100℃保持10分钟,得到结晶良好的钙钛矿晶体薄膜层。
(16).依次在钙钛矿晶体薄膜层上蒸镀20纳米C60,5纳米BCP,100纳米金属银,完成钙钛矿太阳能电池的制备。
实施例2
本发明的第二种钙钛矿太阳能电池的制备方法,包括如下步骤:
(21).按质量比18:2:1分别称取碘化铅粉末、溴化铅粉末、碘化铯粉末,溶解在N,N-二甲基甲酰胺与二甲基亚砜的混合溶剂里,其中,碘化铅的浓度为1.1mol/L,N,N-二甲基甲酰胺与二甲基亚砜的体积比为4:1;充分溶解后,再加入碳酸氢铵粉末,溶解后浓度的为0.5g/L。
(22).按质量比10:1.5:1分别称取甲脒氢碘酸盐粉末、甲胺氢溴酸盐粉末、甲胺氢氯酸盐粉末,溶解在异丙醇溶液里,其中甲脒氢碘酸盐的浓度为60mg/mL。
(23).将步骤(21)得到的溶液均匀旋涂在ITO玻璃/SnO2基底上,80℃烘烤2分钟,然后将步骤(22)得到的溶液均匀旋涂其上。
(24).将经步骤(23)处理得到的基底置于湿度不超过50%的空气氛围中,100℃保持10分钟,然后150℃保持10分钟,得到结晶良好的钙钛矿晶体薄膜层。
(25).依次在钙钛矿晶体薄膜层上沉积20纳米PTAA,5纳米MoO3,80纳米金,完成钙钛矿太阳能电池的制备。
实施例3
本发明的第三种钙钛矿太阳能电池的制备方法,包括如下步骤:
(31).按质量之比10:1,称取碘化铅粉末和碘化铯粉末,溶解在N,N-二甲基甲酰胺与二甲基亚砜以及N-甲基吡咯烷酮的混合溶剂里,其中,碘化铅的浓度为1.5mol/L,N,N-二甲基甲酰胺与二甲基亚砜以及N-甲基吡咯烷酮的体积比为16:3:1;充分溶解后,再加入碳酸氢铵粉末,溶解后的浓度为0.1g/L。
(32).按质量比10:1分别称取甲脒氢碘酸盐粉末和甲胺氢氯酸盐粉末,溶解在异丙醇溶液里,其中,甲脒氢碘酸盐的浓度为30mg/mL。
(33).将步骤(31)得到的溶液均匀刮涂在预热的FTO玻璃/TiO2基底上,迅速置于密闭容器,抽真空2分钟~10分钟,适用的真空度范围为1×10-3Pa~1×103Pa,然后将步骤(32)得到的溶液均匀刮涂其上。
(34).将经步骤(33)处理得到的基底置于氮气氛围中,150℃保持30分钟,得到结晶良好的钙钛矿晶体薄膜层。
(35).依次在钙钛矿晶体薄膜层上沉积100纳米Spiro-MeOTAD(掺杂双三氟甲烷磺酰亚胺锂,叔丁基吡啶),80纳米金,完成钙钛矿太阳能电池的制备。
将上述三个实施例制备的钙钛矿太阳能电池分别进行性能测试,得到附图1所示的电流-电压曲线以及下表所示的性能测试数据。
以上所述仅为本发明的较佳实施例而已,并不用以限制本发明,凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等,均应包含在本发明的保护范围之内。
Claims (10)
1.一种钙钛矿晶体薄膜的制备方法,其特征在于,包括如下步骤:
步骤1:配制含碳酸氢铵的金属卤化物溶液;
步骤2:在基底表面涂布或沉积步骤1制备的含碳酸氢铵的金属卤化物溶液,得到金属卤化物薄膜;
步骤3:将含氮卤化物扩散进入金属卤化物薄膜,反应得到钙钛矿晶体薄膜层。
2.如权利要求1所述的钙钛矿晶体薄膜的制备方法,其特征在于,在所述步骤1中,配制含碳酸氢铵的金属卤化物溶液的方法是将卤化铅粉末溶解在溶剂中配制成溶液,在该溶液中含有添加剂,所述添加剂为碳酸氢铵,所用的溶剂包括酰胺类溶剂、砜类/亚砜类溶剂、酯类溶剂、烃类、卤代烃类溶剂、醇类溶剂、酮类溶剂、醚类溶剂、芳香烃溶剂中至少一种;在含碳酸氢铵的金属卤化物溶液中,阳离子中二价金属铅的摩尔百分数不低于80%,阴离子包括负一价氯离子、溴离子、碘离子、硫氰酸根、乙酸根中的至少一种,阴离子中碘离子的摩尔百分数不低于80%。
3.如权利要求2所述的钙钛矿晶体薄膜的制备方法,其特征在于,在金属卤化物溶液中还有掺杂剂,所述掺杂剂包括含胺基、脒基、胍基中至少一种有机化合物,或者含锂、钠、钾、铷、铯、硼、硅、锗、砷、锑、铍、镁、钙、锶、钡、铝、铟、镓、锡、铊、铅、铋、镧、铈、镨、钕、钐、铕、钆、铽、镝、钬、铒、铥、镱、镥、钪、钛、钒、铬、锰、铁、钴、镍、铜、锌、钇、锆、铌、钼、钌、铑、钯、银、镉、铪、钽、钨、铼、锇、铱、铂、金中至少一种无机化合物。
4.如权利要求2所述的钙钛矿晶体薄膜的制备方法,其特征在于,所述溶剂为N,N-二甲基甲酰胺(DMF)、己内酰胺、二甲基亚砜(DMSO)、N-甲基吡咯烷酮(NMP)、γ-丁内酯(GBL)中至少一种。
5.如权利要求1所述的钙钛矿晶体薄膜的制备方法,其特征在于,在步骤2中,所述基底包括透明导电层和半导体材料层,其在波长为350nm~800nm范围光透过率不低于80%;所述透明导电层包括相互复合的支撑层与功能层,所述支撑层的材料包括玻璃、聚对苯二甲酸乙二醇酯(PET)、聚萘二甲酸乙二醇酯(PEN)及聚酰亚胺(PI)中任意一种,所述功能层的材料包括氧化铟锡(ITO)、掺氟氧化锡(FTO)、掺铝氧化锌(AZO)中任意一种;所述半导体材料层的材料包括空穴传输材料或电子传输材料,所述空穴传输材料包括氧化镍、氧化钒、氧化钼、硫化铜、硫氰酸亚铜、氧化铜、氧化亚铜、氧化钴、PTAA、PEDOT、Spiro-MeOTAD和它们的掺杂物中的至少一种,该层厚度为5nm~200nm;所述电子传输材料包括二氧化钛、氧化锌、硫化镉、二氧化锡、三氧化二铟、氧化钨、氧化铈、C60、C70、PCBM以及它们的衍生物或掺杂物中的至少一种,该层厚度为5nm~300nm。
6.如权利要求1所述的钙钛矿晶体薄膜的制备方法,其特征在于,在步骤2的金属卤化物薄膜和步骤3的钙钛矿晶体薄膜的制备过程中,处理温度不超过200℃。
7.如权利要求1所述的钙钛矿晶体薄膜的制备方法,其特征在于,包括如下步骤:
(11).称取碘化铅粉末溶解在N,N-二甲基甲酰胺中,碘化铅的浓度为0.5mol/L,再加入碳酸氢铵粉末,溶解后的浓度为2g/L;
(12).将步骤(11)得到的溶液在热风辅助下均匀喷涂在PEN/ITO/PEDOT:PSS基底上,60℃烘烤5分钟,得到厚度为300纳米的碘化铅薄膜;
(13).将甲胺氢碘酸盐蒸镀到步骤(12)制备的碘化铅薄膜上,厚度为50纳米;
(14).将经步骤(13)处理得到的基底置于氮气氛围中,100℃保持30分钟;
(15).待反应完成,冷却至室温,用异丙醇快速冲洗基底上制备的碘化铅薄膜表面,去除其上残余的甲胺氢碘酸盐,100℃保持10分钟,得到结晶良好的钙钛矿晶体薄膜层。
8.如权利要求1所述的钙钛矿晶体薄膜的制备方法,其特征在于,包括如下步骤:
(21).按质量比18:2:1分别称取碘化铅粉末、溴化铅粉末、碘化铯粉末,溶解在N,N-二甲基甲酰胺与二甲基亚砜的混合溶剂里,其中,碘化铅的浓度为1.1mol/L,N,N-二甲基甲酰胺与二甲基亚砜的体积比为4:1;再加入碳酸氢铵粉末,溶解后的浓度为0.5g/L;
(22).按质量比10:1.5:1分别称取甲脒氢碘酸盐粉末、甲胺氢溴酸盐粉末、甲胺氢氯酸盐粉末,溶解在异丙醇溶液里,其中甲脒氢碘酸盐的浓度为60mg/mL;
(23).将步骤(21)得到的溶液均匀旋涂在ITO玻璃/SnO2基底上,80℃烘烤2分钟,然后将步骤(22)得到的溶液均匀旋涂其上;
(24).将经步骤(23)处理得到的基底置于湿度不超过50%的空气氛围中,100℃保持10分钟,然后150℃保持10分钟,得到结晶良好的钙钛矿晶体薄膜层。
9.如权利要求1所述的钙钛矿晶体薄膜的制备方法,其特征在于,包括如下步骤:
(31).按质量之比10:1,称取碘化铅粉末和碘化铯粉末,溶解在N,N-二甲基甲酰胺与二甲基亚砜以及N-甲基吡咯烷酮的混合溶剂里,其中,碘化铅的浓度为1.5mol/L,N,N-二甲基甲酰胺与二甲基亚砜以及N-甲基吡咯烷酮的体积比为16:3:1;再加入碳酸氢铵粉末,溶解后的浓度为0.1g/L;
(32).按质量比10:1分别称取甲脒氢碘酸盐粉末和甲胺氢氯酸盐粉末,溶解在异丙醇溶液里,其中,甲脒氢碘酸盐的浓度为30mg/mL;
(33).将步骤(31)得到的溶液均匀刮涂在预热的FTO玻璃/TiO2基底上,迅速置于密闭容器,抽真空2分钟~10分钟,适用的真空度范围为1×10-3Pa~1×103Pa,然后将步骤(32)得到的溶液均匀刮涂其上;
(34).将经步骤(33)处理得到的基底置于氮气氛围中,150℃保持30分钟,得到结晶良好的钙钛矿晶体薄膜层。
10.一种钙钛矿太阳能电池的制备方法,其特征在于,在所述钙钛矿太阳能电池中含有钙钛矿薄膜层,所述钙钛矿薄膜层采用如权利要求1至9中任意一项所述的钙钛矿晶体薄膜的制备方法制备。
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