CN113540270A - 一种获得平整、均匀、致密钙钛矿薄膜的方法 - Google Patents
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Abstract
本发明公开了一种获得平整、均匀、致密钙钛矿薄膜的方法,本发明先采用旋涂法制备CsPbBr3钙钛矿薄膜,将制备CsPbBr3钙钛矿薄膜放入压印腔内的样品台,压印降温得到钙钛矿薄膜;本发明使旋涂法制备的各种组份的钙钛矿薄膜在不改变晶相结构的前提下显著提高平整度、均匀度、致密度等方面有较大的提高。
Description
技术领域
本发明属于材料热压印处理方法,具体涉及一种获得平整、均匀、致密钙钛矿薄膜的方法。
背景技术
在过去十年内,由于出色的光电特征和低成本,钙钛矿薄膜极其器件研究得到了广泛的关注。比如,钙钛矿薄膜在光伏电池、LEDs等方面展现了极大潜力。在这些器件研究中,最广泛的钙钛矿薄膜制备方法是旋涂法,具有操作简单、成本低、大面积等优点。然而,该方面制备的钙钛矿薄膜在平整性、均匀性、致密性方面具有显著的缺点,影响了光电器件的性能。
发明内容
本发明针对现有技术的不足,提出了一种获得平整、均匀、致密钙钛矿薄膜的方法。
一种获得平整、均匀、致密钙钛矿薄膜的方法,该方法具体包括以下步骤:
步骤一:采用旋涂法制备CsPbBr3钙钛矿薄膜;
用丙酮、乙醇和去离子水依次对衬底进行超声波清洗;
将PbBr2和N,N-二甲基甲酰胺混合溶液以2000-3500rpm的转速旋涂在衬底表面30-40秒,衬底表面生成第一层膜;其中混合溶液中PbBr2的含量为1-1.5M;
将PbBr2和N,N-二甲基甲酰胺混合溶液以3500-4000rpm的转速旋涂在第一层膜上20-30秒,其中混合溶液中PbBr2的含量为0.8-1M;
将制备好的膜浸于CsBr和甲醇的混合溶液中10-15分钟,用异丙醇漂洗,在空气中旋转干燥,在热板上加热至200~250℃,保持5-8分钟,形成CsPbBr3薄膜层;其中CsBr和甲醇的混合溶液中CsBr的浓度为0.07-0.09M;
步骤二:将步骤一得到的CsPbBr3薄膜层放入压印腔内的样品台上,将压印腔抽真空至(1~5)*10-5Pa;将CsPbBr3薄膜层加热到在30-60摄氏度,通过移动活动压柱及施加压力到CsPbBr3薄膜层上;压力范围为20000-45000牛顿;压印时间为10-20分钟;
步骤三:将CsPbBr3薄膜层降温到常温后,取出,获得平整、均匀、致密钙钛矿薄膜。
作为优选,所述的PbBr2和N,N-二甲基甲酰胺混合溶液中PbBr2的含量为1.3M。
作为优选,所述的CsBr和甲醇的混合溶液中CsBr的浓度为0.08M。
作为优选,压印腔抽真空度为3*10-55Pa。
作为优选,活动压柱的压力为32000牛顿。
作为优选,所述的衬底为玻璃衬底。
本发明相对于现有技术具有的效果:通过本发明的方法,可以使旋涂法制备的各种组份的钙钛矿薄膜在不改变晶相结构的前提下显著提高平整度、均匀度、致密度等方面有较大的提高。这种改善有助于钙钛矿器件性能的提升。通过本方法,可以获得更致密的钙钛矿薄膜,能够降低薄膜内的孔洞;其受益是可以提高钙钛矿电池的转换效率。
附图说明
图1钙钛矿薄膜样品压印处理示意图;
图2为钙钛矿薄膜扫描电镜图,上半部分为原始未压印钙钛矿薄膜区域,下半部分为经过本发明方法处理的区域;
图3钙钛矿薄膜扫描电镜图,上半区域为原始未压印钙钛矿薄膜,下半区域为压印处理的钙钛矿薄膜;
图4放大的、局部的钙钛矿薄膜扫描电镜图,右半区域为原始未压印钙钛矿薄膜,左半区域为压印处理的钙钛矿薄膜。
具体实施方式
实施例一:
步骤一:采用旋涂法制备CsPbBr3钙钛矿薄膜;
用丙酮、乙醇和去离子水依次对玻璃衬底进行超声波清洗;
将PbBr2和N,N-二甲基甲酰胺混合溶液以2000rpm的转速旋涂在玻璃表面30秒,玻璃表面生成第一层膜;其中混合溶液中PbBr2的含量为1M;
将PbBr2和N,N-二甲基甲酰胺混合溶液以3500rpm的转速旋涂在第一层膜上20秒,其中混合溶液中PbBr2的含量为0.8M;
将制备好的膜浸于CsBr和甲醇的混合溶液中10分钟,用异丙醇漂洗,在空气中旋转干燥,在热板上加热至200℃,保持5分钟,形成CsPbBr3薄膜层;其中CsBr和甲醇的混合溶液中CsBr的浓度为0.07M;
步骤二:将步骤一得到的CsPbBr3薄膜层放入压印腔内的样品台上,将压印腔抽真空至1*10-55Pa;将CsPbBr3薄膜层加热到在30摄氏度,通过移动活动压柱及施加压力到CsPbBr3薄膜层上;压力范围为20000牛顿;压印时间为10分钟;如图1所示;
步骤三:将CsPbBr3薄膜层降温到常温后,取出,获得平整、均匀、致密钙钛矿薄膜。
实施例一处理的钙钛矿电池和无压印处理的钙钛矿电池的光伏参数测量比较,如表1所示:
表1
实施例一处理后的钙钛矿薄膜区域的扫描电镜图,如图2、图3、图4所示;
实施例二:
步骤一:采用旋涂法制备CsPbBr3钙钛矿薄膜;
用丙酮、乙醇和去离子水依次对玻璃衬底进行超声波清洗;
将PbBr2和N,N-二甲基甲酰胺混合溶液以3000rpm的转速旋涂在玻璃表面35秒,玻璃表面生成第一层膜;其中混合溶液中PbBr2的含量为1.2M;
将PbBr2和N,N-二甲基甲酰胺混合溶液以3800rpm的转速旋涂在第一层膜上25秒,其中混合溶液中PbBr2的含量为0.9M;
将制备好的膜浸于CsBr和甲醇的混合溶液中12分钟,用异丙醇漂洗,在空气中旋转干燥,在热板上加热至230℃,保持7分钟,形成CsPbBr3薄膜层;其中CsBr和甲醇的混合溶液中CsBr的浓度为0.08M;
步骤二:将步骤一得到的CsPbBr3薄膜层放入压印腔内的样品台上,将压印腔抽真空至3*10-55Pa;将CsPbBr3薄膜层加热到在50摄氏度,通过移动活动压柱及施加压力到CsPbBr3薄膜层上;压力范围为32000牛顿;压印时间为16分钟;
步骤三:将CsPbBr3薄膜层降温到常温后,取出,获得平整、均匀、致密钙钛矿薄膜。
实施例三:
步骤一:采用旋涂法制备CsPbBr3钙钛矿薄膜;
用丙酮、乙醇和去离子水依次对玻璃衬底进行超声波清洗;
将PbBr2和N,N-二甲基甲酰胺混合溶液以3500rpm的转速旋涂在玻璃表面30-40秒,玻璃表面生成第一层膜;其中混合溶液中PbBr2的含量为1.5M;
将PbBr2和N,N-二甲基甲酰胺混合溶液以4000rpm的转速旋涂在第一层膜上30秒,其中混合溶液中PbBr2的含量为1M;
将制备好的膜浸于CsBr和甲醇的混合溶液中15分钟,用异丙醇漂洗,在空气中旋转干燥,在热板上加热至250℃,保持8分钟,形成CsPbBr3薄膜层;其中CsBr和甲醇的混合溶液中CsBr的浓度为0.09M;
步骤二:将步骤一得到的CsPbBr3薄膜层放入压印腔内的样品台上,将压印腔抽真空至5*10-55Pa;将CsPbBr3薄膜层加热到在60摄氏度,通过移动活动压柱及施加压力到CsPbBr3薄膜层上;压力范围为45000牛顿;压印时间为20分钟;
步骤三:将CsPbBr3薄膜层降温到常温后,取出,获得平整、均匀、致密钙钛矿薄膜。
Claims (6)
1.一种获得平整、均匀、致密钙钛矿薄膜的方法,其特征在于,该方法具体包括以下步骤:
步骤一:采用旋涂法制备CsPbBr3钙钛矿薄膜;
用丙酮、乙醇和去离子水依次对衬底进行超声波清洗;
将PbBr2和N,N-二甲基甲酰胺混合溶液以2000-3500rpm的转速旋涂在衬底表面30-40秒,衬底表面生成第一层膜;其中混合溶液中PbBr2的含量为1-1.5M;
将PbBr2和N,N-二甲基甲酰胺混合溶液以3500-4000rpm的转速旋涂在第一层膜上20-30秒,其中混合溶液中PbBr2的含量为0.8-1M;
将制备好的膜浸于CsBr和甲醇的混合溶液中10-15分钟,用异丙醇漂洗,在空气中旋转干燥,在热板上加热至200~250℃,保持5-8分钟,形成CsPbBr3薄膜层;其中CsBr和甲醇的混合溶液中CsBr的浓度为0.07-0.09M;
步骤二:将步骤一得到的CsPbBr3薄膜层放入压印腔内的样品台上,将压印腔抽真空至(1~5)*10-5Pa;将CsPbBr3薄膜层加热到在30-60摄氏度,通过移动活动压柱及施加压力到CsPbBr3薄膜层上;压力范围为20000-45000牛顿;压印时间为10-20分钟;
步骤三:将CsPbBr3薄膜层降温到常温后,取出,获得平整、均匀、致密钙钛矿薄膜。
2.根据权利要求1所述的一种获得平整、均匀、致密钙钛矿薄膜的方法,其特征在于:所述的PbBr2和N,N-二甲基甲酰胺混合溶液中PbBr2的含量为1.3M。
3.根据权利要求1所述的一种获得平整、均匀、致密钙钛矿薄膜的方法,其特征在于:所述的CsBr和甲醇的混合溶液中CsBr的浓度为0.08M。
4.根据权利要求1所述的一种获得平整、均匀、致密钙钛矿薄膜的方法,其特征在于:压印腔抽真空度为3*10-5Pa。
5.根据权利要求1所述的一种获得平整、均匀、致密钙钛矿薄膜的方法,其特征在于:活动压柱的压力为32000牛顿。
6.根据权利要求1所述的一种获得平整、均匀、致密钙钛矿薄膜的方法,其特征在于:所述的衬底为玻璃衬底。
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