CN112038490A - 一种改良蒸汽辅助制备钙钛矿太阳能电池的方法 - Google Patents
一种改良蒸汽辅助制备钙钛矿太阳能电池的方法 Download PDFInfo
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- CN112038490A CN112038490A CN202010961238.6A CN202010961238A CN112038490A CN 112038490 A CN112038490 A CN 112038490A CN 202010961238 A CN202010961238 A CN 202010961238A CN 112038490 A CN112038490 A CN 112038490A
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- Photovoltaic Devices (AREA)
Abstract
本发明公开了一种改良蒸汽辅助制备钙钛矿太阳能电池的方法，该方法包括在导电基底上制备第一传输层的步骤，制备钙钛矿前驱体薄膜的步骤，以及将钙钛矿前驱体薄膜与有机胺蒸汽接触反应转化成钙钛矿活性层的步骤，其特点在于，所述制备钙钛矿前驱体薄膜的步骤包括：将制备有第一传输层的导电基底置于真空镀膜装置中，采用铅盐作为钙钛矿前驱体源；抽真空至1×10‑3Pa以下；加热铅盐，使铅盐蒸发并在导电基底上沉积得到钙钛矿前驱体薄膜。与现有技术相比，采用本发明制备的钙钛矿薄膜致密、无针孔，晶粒粒径在500nm～1000nm之间，晶粒晶胞之间此时只有竖直的晶界，没有横向晶界，适应于制备大面积钙钛矿太阳能电池。
Description
技术领域
本发明属于太阳能电池领域，具体涉及一种改良蒸汽辅助制备钙钛矿太阳能电池的方法。
背景技术
太阳能是来自太阳的辐射能量，太阳能电池直接把太阳能转化为人们广泛使用的电能，是一种绿色环保和可持续利用的运作形式，近年来得到了迅速发展和推广。2009年，一种基于钙钛矿型有机金属卤化物ABX3太阳能电池引起了全世界的关注，其中A为CH3NH+，B为Pb2+，X为I-、Br-或Cl-的一种或多种。十年的时间里，钙钛矿太阳能电池的研究取得了重大进展。钙钛矿太阳电池的迅猛发展，预示着其作为一种高效的可再生能源器件，在未来拥有着广阔的应用前景。
钙钛矿太阳能电池的结构有正置结构和倒置结构，两种结构只是在电荷传输层的构建顺序上有不同，而主体钙钛矿层结构没有变化。
与硅电池相比，钙钛矿对绿光和蓝光的吸收明显更强。并且钙钛矿晶体的结晶度近乎完美，载流子复合得以大大减小，而载流子扩散长度随之增大，钙钛矿太阳电池突出的光电性能与这些特性密切相关。但钙钛矿型太阳能电池仍然存在着许多问题亟待解决，如电池的稳定性、电池的寿命、如何大面积制备等等。目前钙钛矿太阳能电池的制备工艺基于一步溶液旋涂法，实验室光电转化效率可达23.7％。但是旋涂法制备工艺只局限于小面积电池，且重现性差，无法向大面积工程化应用中推广。
2013年Yang yang课题组报道的蒸汽辅助沉积法，尽管蒸汽辅助沉积法制备得到的钙钛矿薄膜具有非常高的薄膜均匀性和结晶性以及完全的表面覆盖率。蒸汽辅助沉积法首先通过溶液或反溶剂旋涂法制备碘化铅等铅盐薄膜，然后使薄膜与碘甲胺等有机胺蒸汽反应，制得钙钛矿薄膜，然而目前蒸汽辅助沉积法制备的钙钛矿太阳能电池的工艺，无法面向大面积生产。因此，开发、设计一种适合大面积制备的有机胺蒸汽辅助钙钛矿太阳能电池制备方法具有重要意义。
发明内容
本发明的目的在于提供一种改良的蒸汽辅助制备钙钛矿太阳能电池的方法，以满足大面积生产的需要。
本发明为实现上述目的所采用的技术方案如下：
一种改良蒸汽辅助制备钙钛矿太阳能电池的方法，包括在导电基底上制备第一传输层的步骤，制备钙钛矿前驱体薄膜的步骤，以及将钙钛矿前驱体薄膜与有机胺蒸汽接触反应转化成钙钛矿活性层的步骤，其特点在于，所述制备钙钛矿前驱体薄膜的步骤包括：
将制备有第一传输层的导电基底置于真空镀膜装置中，采用铅盐作为钙钛矿前驱体源；
抽真空至1×10-3Pa以下；
加热铅盐，使铅盐蒸发并在导电基底上沉积得到钙钛矿前驱体薄膜。
在1×10-3Pa以下的气压下蒸镀铅盐是本发明的核心技术要点之一，只有在该气压条件的基础上才能获得高质量、高致密度、无针孔、大晶粒的钙钛矿薄膜，优选地，抽真空至4×10-4Pa。
优选地，所述铅盐选自碘化铅、溴化铅和氯化铅中的至少一种。
优选地，所述钙钛矿前驱体薄膜的厚度为20～300nm，更优选为50～150nm。
优选地，所述有机胺选自碳数为1～12的烷基卤化胺，或者苄胺。
所述碳数为1～12的烷基如甲基、乙基、丙基、丁基、戊基、己基、庚基、辛基、壬基、癸基、十一烷基、十二烷基。
更优选地，所述卤为氯、溴或碘。
优选地，钙钛矿前驱体薄膜与有机胺蒸汽在150～200℃和1Pa以下接触反应。
优选地，接触反应时间12min以上。
优选地，在170～200℃和0.1Pa以下接触反应。
更优选地，在接触反应之前，用惰性气体或氮气置换反应体系中的空气。
所述惰性气体如氦气、氖气、氩气。
优选地，所述导电基底为刚性或柔性透明导电基底。
所述刚性透明导电基底如FTO、ITO、AZO等导电玻璃。所述柔性透明导电基底如PEO(聚氧化乙烯)等导电聚合物。
优选地，所述钙钛矿太阳能电池的结构为正置结构，制备步骤包括在导电基底上制备第一传输层的步骤，制备钙钛矿前驱体薄膜的步骤，将钙钛矿前驱体薄膜与有机胺蒸汽接触反应转化成钙钛矿活性层的步骤，制备第二传输层的步骤，以及制备背电极的步骤，其中，所述第一传输层为电子传输层，所述第二传输层为空穴传输层。
优选地，所述电子传输层为TiO2致密层。
更优选地，TiO2致密层的制备过程包括在导电基底上旋涂或印刷一层有机钛，然后在120～200℃退火10～20min，接着在450～500℃退火30～60min。
所述的有机钛选自如双(乙酰丙酮基)钛酸二异丙酯、钛酸异丙酯等。
优选地，所述空穴传输层为Sprio-OMeTAD(2,2′,7,7′-四[N,N-二(4-甲氧基苯基)氨基]-9,9′-螺二芴)或CuSCN层，所述背电极为Au或Ag层。
更优选地，所述空穴传输层采用旋涂法、印刷法或热蒸镀法制备，所述背电极采用热蒸镀法制备。
优选地，在制备第一传输层后，先制备一层TiO2介孔层，再制备钙钛矿前驱体薄膜。
更优选地，TiO2介孔层的制备过程包括在第一传输层上旋涂TiO2介孔层浆料，然后在120～200℃退火10～20min，接着在550～600℃退火30～60min。
优选地，所述钙钛矿太阳能电池的结构为倒置结构，制备步骤包括在导电基底上制备第一传输层的步骤，制备钙钛矿前驱体薄膜的步骤，将钙钛矿前驱体薄膜与有机胺蒸汽接触反应转化成钙钛矿活性层的步骤，制备第二传输层的步骤，以及制备背电极的步骤，其中，所述第一传输层为空穴传输层，所述第二传输层为电子传输层。
优选地，所述空穴传输层为PEDOT:PSS(聚(3,4-乙烯二氧噻吩)-聚(苯乙烯磺酸))层。
更优选地，PEDOT:PSS层的制备过程包括在导电基底上旋涂或印刷一层PEDOT:PSS，然后对PEDOT:PSS进行退火处理，优选地，退火温度为120～200℃，时间为10～20min。
优选地，所述电子传输层为PC61BM([6,6]-苯基C61丁酸甲酯)、C60或BCP(2,9-二甲基-4,7-联苯-1,10-菲罗啉)层，所述背电极为Al或Ag层。
更优选地，所述电子传输层采用旋涂法、印刷法或热蒸镀法制备，所述背电极采用热蒸镀法制备。
本发明与背景技术相比，具有以下有益效果：
①溶液法制备的碘化铅薄膜重现很多针孔，没有形成均一的薄膜，和基底形成漏洞；而本发明在高真空度下蒸镀的铅盐薄膜，显示出均一，致密、无针孔的高质量薄膜，这为下一步在碘化铵蒸汽氛围下制备出高质量、高致密度、无针孔的钙钛矿薄膜奠定基础。
②一步反溶剂旋涂法制备的甲胺碘化铅基钙钛矿薄膜晶粒粒径在100nm～200nm之间，且显示出更多的针孔缺陷；与之相比，本发明改良后蒸汽辅助法制备的钙钛矿薄膜，晶粒粒径在500nm～1000nm之间，晶粒直径大于薄膜厚度，晶粒晶胞之间此时只有竖直的晶界，没有横向晶界。
附图说明
图1为改良后蒸汽辅助法所制备钙钛矿活性层表面扫描电镜图(SEM)。
图2为170℃MAI蒸汽辅助下时间变化对钙钛矿晶化转化的XRD变化。
图3为改良后蒸汽辅助法所制备的钙钛矿太阳能电池测试性能。
图4为不同条件下碘化铅的XRD图。
具体实施方式
下面结合具体实施例对本发明提供的蒸汽辅助法钙钛矿太阳能电池制备方法做进一步的阐述。
实施例一：正置结构的钙钛矿太阳能电池
①导电基底预处理：
用清洁剂清洗导电基底表面附着的灰尘颗粒和油脂，然后导电基底依次使用去离子水、丙酮、异丙醇分别超声清洗15min，然后在90℃烘箱中保存。导电基底采用FTO导电玻璃。
②电子传输层制备：
制备电极前使用氧等离子清洗仪将处理后的导电基底处理10min。将含有有机钛源(如双(乙酰丙酮基)钛酸二异丙酯、钛酸异丙酯等)的溶液铺成在处理好的导电基底上，以一定转速旋涂成膜，在120℃加热基板上退火10min，然后在马弗炉中程序升温至450℃，并维持此温度30min。
③TiO2介孔层制备：
将固含量3％TiO2介孔层浆料铺于②所得的电子传输层上，以一定转速旋涂成膜，在120℃加热基板上退火10min，然后在马弗炉中程序升温至550℃，并维持此温度30min。
④碘化铅薄膜的制备：
将第③步处理完的导电基底置于真空镀膜仪中，且在蒸发源上放置足量高纯碘化铅(PbI2)粉末。待整个真空系统抽至4.0×10-4Pa时，开启蒸发源及旋转导电基底，蒸镀碘化铅薄膜100nm左右。
⑤MAI蒸汽辅助促进碘化铅转化：
用高温双面胶将制备好碘化铅薄膜的导电基底粘在预先清洗好的玻璃培养皿的上盖下方(清洗步骤：将玻璃培养皿依次放在清洗液、蒸馏水、丙酮、蒸馏水、异丙醇中各超声清洗15分钟，在使用前用氮气吹干)，在玻璃培养皿内放置适量纯化后的甲基碘化胺(Methylammonium Iodide，CH3NH3I(MAI)粉末，盖好培养皿上盖，将整个装置放置真空干燥箱中，用高纯氮气进行三次置换，将真空干燥箱抽真空至0.09Pa，然后开启加热(整个装置安装与实验过程在手套箱中，N2气环境下进行，避免水氧对钙钛矿层形成的负面影响)，在甲基碘化胺蒸汽中，与PbI2薄膜反应(温度170℃，时间12min)，形成甲胺铅碘基钙钛矿薄膜，该钙钛矿活性层的SEM如图1所示。
⑥空穴传输层及背电极制备：
通过旋涂法或热蒸镀法将Sprio-OMeTAD或CuSCN等制备到甲胺铅碘基钙钛矿薄膜上，形成空穴传输层，然后将金属Au或Ag作为背电极通过热蒸镀法制备到空穴传输层上，背电极厚度为100nm，即完成整个电池的制备。
测试其光电转化性能。具体地，优选方案其短路电流为23.9mA/cm2，开路电压为1.03V，填充因子为0.67，且稳定光电转化效率可达16.7％(如图3所示)。与之相比，当碘化铅蒸镀条件为10-2Pa，其他条件不变时，其短路电流为21.8mA/cm2，开路电压为0.9V，填充因子为0.54，光电转化效率达10.6％。相应铅盐薄膜的XRD如图4所示。上述结果表明在本发明的真空范围内能明显提高铅盐薄膜的生长质量，从而显著提高电池的综合性能。
实施例二：反置结构的钙钛矿太阳能电池
①导电基底预处理：
用清洁剂清洗导电基底表面附着的灰尘颗粒和油脂，然后导电基底依次使用去离子水、丙酮、异丙醇分别超声清洗15min，然后在90度烘箱中保存。导电基底采用ITO导电玻璃。
②空穴传输层制备：
制备电极前使用氧等离子清洗仪将处理后的导电基底处理10min。将PEDOT：PSS水溶液通过旋涂法或卷对卷印刷法制备至导电基底上，厚度30nm左右，并在130度下进行退火20分钟。
③碘化铅薄膜制备：
将第②步处理完的导电基底置于真空镀膜仪中，且在蒸发源上放置足量高纯碘化铅(PbI2)粉末。待整个真空系统抽至4.0×10-4Pa时，开启蒸发源及旋转导电基底，蒸镀碘化铅薄膜100nm左右。
④MAI蒸汽辅助促进碘化铅转化：
用高温双面胶将制备好碘化铅薄膜的导电基底粘在预先清洗好的玻璃培养皿的上盖下方(清洗步骤：将玻璃培养皿依次放在清洗液、蒸馏水、丙酮、蒸馏水、异丙醇中各超声清洗15分钟，在使用前用氮气吹干)，在玻璃培养皿内放置适量纯化后的甲基碘化胺(Methylammonium Iodide，CH3NH3I(MAI)粉末，盖好培养皿上盖，将整个装置放置真空干燥箱中，用高纯氮气进行三次置换，将真空干燥箱抽真空至0.09Pa，然后开启加热(整个装置安装与实验过程在手套箱中，N2气环境下进行，避免水氧对钙钛矿层形成的负面影响)，根据实验条件，设置反应时间，在甲基碘化胺蒸汽中，与PbI2薄膜反应形成甲胺铅碘基钙钛矿薄膜，170℃下钙钛矿晶化随时间的变化如图2所示。
⑤电子传输层及背电极制备：
通过旋涂法或热蒸镀法将PC61BM、C60、BCP等阴极缓冲层制备到甲胺铅碘基钙钛矿薄膜上，形成电子传输层，然后将金属Al或Ag作为背电极通过热蒸镀法制备到电子传输层上，背电极厚度100nm，即完成整个电池的制备。
以上所述仅是本发明的优选实施方式，应当指出，对于本技术领域的技术人员来说，在不脱离本发明技术原理的前提下，若对前述各实施例所记载的技术方案进行修改，或者对其中部分技术特征进行等同替换，理应视为本发明的保护范围。
Claims (10)
1.一种改良蒸汽辅助制备钙钛矿太阳能电池的方法，包括在导电基底上制备第一传输层的步骤，制备钙钛矿前驱体薄膜的步骤，以及将钙钛矿前驱体薄膜与有机胺蒸汽接触反应转化成钙钛矿活性层的步骤，其特征在于，所述制备钙钛矿前驱体薄膜的步骤包括：
将制备有第一传输层的导电基底置于真空镀膜装置中，采用铅盐作为钙钛矿前驱体源；
抽真空至1×10-3Pa以下；
加热铅盐，使铅盐蒸发并在导电基底上沉积得到钙钛矿前驱体薄膜。
2.根据权利要求1所述的方法，其特征在于：抽真空至4×10-4Pa。
3.根据权利要求1所述的方法，其特征在于：所述铅盐选自碘化铅、溴化铅和氯化铅中的至少一种。
4.根据权利要求1所述的方法，其特征在于：所述钙钛矿前驱体薄膜的厚度为20～300nm，优选为50～150nm。
5.根据权利要求1所述的方法，其特征在于：所述有机胺选自碳数为1～12的烷基卤化胺，或者苄胺。
6.根据权利要求5所述的方法，其特征在于：所述卤为氯、溴或碘。
7.根据权利要求1所述的方法，其特征在于：钙钛矿前驱体薄膜与有机胺蒸汽在150～200℃和1Pa以下接触反应；
优选地，反应时间12min以上；
优选地，在170～200℃和0.1Pa以下接触反应；
在接触反应之前，用惰性气体或氮气置换反应体系中的空气。
8.根据权利要求1所述的方法，其特征在于：所述导电基底为刚性或柔性透明导电基底。
9.根据权利要求1～8任一所述的方法，其特征在于：所述钙钛矿太阳能电池的结构为正置结构，制备步骤包括在导电基底上制备第一传输层的步骤，制备钙钛矿前驱体薄膜的步骤，将钙钛矿前驱体薄膜与有机胺蒸汽接触反应转化成钙钛矿活性层的步骤，制备第二传输层的步骤，以及制备背电极的步骤，其中，所述第一传输层为电子传输层，所述第二传输层为空穴传输层；
优选地，所述电子传输层为TiO2致密层；
更优选地，TiO2致密层的制备过程包括在导电基底上旋涂或印刷一层有机钛，然后在120～200℃退火10～20min，接着在450～500℃退火30～60min；
优选地，所述空穴传输层为Sprio-OMeTAD或CuSCN层，所述背电极为Au或Ag层；
更优选地，所述空穴传输层采用旋涂法、印刷法或热蒸镀法制备，所述背电极采用热蒸镀法制备；
优选地，在制备第一传输层后，先制备一层TiO2介孔层，再制备钙钛矿前驱体薄膜；
更优选地，TiO2介孔层的制备过程包括在第一传输层上旋涂TiO2介孔层浆料，然后在120～200℃退火10～20min，接着在550～600℃退火30～60min。
10.根据权利要求1～8任一所述的方法，其特征在于：所述钙钛矿太阳能电池的结构为倒置结构，制备步骤包括在导电基底上制备第一传输层的步骤，制备钙钛矿前驱体薄膜的步骤，将钙钛矿前驱体薄膜与有机胺蒸汽接触反应转化成钙钛矿活性层的步骤，制备第二传输层的步骤，以及制备背电极的步骤，其中，所述第一传输层为空穴传输层，所述第二传输层为电子传输层；
优选地，所述空穴传输层为PEDOT:PSS层；
更优选地，PEDOT:PSS层的制备过程包括在导电基底上旋涂或印刷一层PEDOT:PSS，然后对PEDOT:PSS进行退火处理；
优选地，所述电子传输层为PC61BM、C60或BCP层，所述背电极为Al或Ag层；
更优选地，所述电子传输层采用旋涂法、印刷法或热蒸镀法制备，所述背电极采用热蒸镀法制备。
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