CN110230108A - 一种钙钛矿复合纳米纤维膜及其制备方法和应用 - Google Patents
一种钙钛矿复合纳米纤维膜及其制备方法和应用 Download PDFInfo
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明属于钙钛矿复合材料技术领域，具体涉及一种钙钛矿复合纳米纤维膜及其制备方法和应用；其制备方法包括以下步骤：在有机溶剂中配制聚合物溶液，所述聚合物包括聚乙烯吡咯烷酮、聚丙烯腈、聚氨酯中的至少一种；将卤化铅加入所述聚合物溶液中得到纺丝液，将纺丝液进行静电纺丝，得到卤化铅/聚合物纳米纤维膜；将卤化铯溶液或甲基卤化胺溶液涂覆于卤化铅/聚合物纳米纤维膜之上，制得钙钛矿复合纳米纤维膜。本发明采用静电纺丝技术结合溶液法制备了钙钛矿复合纳米纤维膜，实现钙钛矿与聚合物纤维的结合，获得一维柔性钙钛矿材料，并使钙钛矿材料分布在纳米纤维的表面，有利于钙钛矿材料的光吸收和电荷的分离；且制备方法简单。
Description
技术领域
本发明属于钙钛矿复合材料技术领域，具体涉及一种钙钛矿复合纳米纤维膜及其制备方法和应用。
背景技术
能源是人类赖以生存的战略性基础资源。太阳能电池将取之不尽、用之不竭的绿色太阳能转换成电能备受关注。随着纳米材料科学的发展，一类新型的太阳能电池，即钙钛矿太阳能电池(Perovskite solar cells，PSCs)应运而生。经过几年的研究发展，钙钛矿太阳能电池的光电转换效率已超过23％，应用潜力巨大。
钙钛矿光吸收层是钙钛矿太阳能电池的核心组成部分。钙钛矿晶体为ABX3结构，在钙钛矿晶体中，A离子通常指的是有机阳离子CH3NH3 +和无机阳离子Cs+位于立方晶胞的中心，被12个X离子(通常为Cl、Br或I)包围成配位立方八面体；B离子通常为Pb2+位于立方晶胞的角顶，被6个X离子包围成配位八面体，配位数为6。
目前最常用的钙钛矿光吸收层薄膜的制备方法为溶液旋涂法和双源共蒸发法。溶液旋涂法包括配料、高速旋转、溶剂挥发成膜三个步骤，通过控制匀胶的时间、转速加速度、滴液量以及所用溶液的浓度、粘度来控制成膜的厚度。旋涂法是依靠衬底旋转时产生的离心力及重力作用，将落在衬底上的涂料液滴全面流布于衬底表面的涂覆过程。然而，旋涂法只适用于在平面状衬底上制备单侧涂层，且一般旋涂衬底面积不宜过大。双源共蒸发法制备的钙钛矿薄膜厚度比较均一。但是双源共蒸发法的制备工艺比较复杂、能耗较高。另外，无论是旋涂法还是双源共蒸发法，钙钛矿薄膜的制备过程中必须沉积在特定的基底上。
静电纺丝是一种简便易行的制备连续纳米纤维的方法，其制备的纳米纤维的直径小，形貌结构可控，表面积大。因此，静电纺丝技术在能源、催化和环境等领域具有广泛的应用。因此，静电纺制备钙钛矿纳米纤维膜备受关注。如申请号为201510221419.4的专利文献公开了一种钙钛矿纳米纤维膜太阳能电池及其制备方法，其中制备方法包括：通过高分子为络合剂，将钙钛矿前驱体溶液直接静电纺丝制备得到有机-无机杂化铅卤基纳米纤维膜，作为钙钛矿太阳电池光吸收层。如Chen等采用同轴静电纺丝以钙钛矿为核、高聚物为皮的皮芯结构复合纳米纤维膜，然而其制备的复合纳米纤维中，钙钛矿位于纳米纤维内部，由于聚合物的遮挡，抑制其光捕获效率，从而降低了光生载流子的产生效率；并且聚合物完全阻挡钙钛矿与电荷传输层的有效接触，抑制电荷的转移，限制其在太阳能电池等领域的应用。利用共混静电纺丝法，如申请号为201810359252.1的专利文献公开了一种复合荧光纳米纤维膜的制备方法，其制得的复合荧光纳米纤维膜，依然会造成钙钛矿位于纤维内部。因此，钙钛矿在纳米纤维表面结晶的形成一维结构的钙钛矿纳米纤维膜成为钙钛矿纳米纤维膜研究的重点。
发明内容
基于现有技术中存在的上述不足，本发明提供一种钙钛矿复合纳米纤维膜及其制备方法和应用。
为了达到上述发明目的，本发明采用以下技术方案：
一种钙钛矿复合纳米纤维膜的制备方法，包括以下步骤：
S1、在有机溶剂中配制聚合物溶液，所述聚合物包括聚乙烯吡咯烷酮、聚丙烯腈、聚氨酯中的至少一种；
S2、将卤化铅加入所述聚合物溶液中得到纺丝液，将纺丝液进行静电纺丝，得到卤化铅/聚合物纳米纤维膜；
S3、将卤化铯溶液或甲基卤化胺溶液涂覆于卤化铅/聚合物纳米纤维膜之上，制得钙钛矿复合纳米纤维膜。
作为优选方案，所述聚合物与有机溶剂的质量比为0.09～0.2：1。
作为优选方案，所述有机溶剂为N，N-二甲基甲酰胺和二甲基亚砜中的至少一种。
作为优选方案，所述卤化铅与有机溶剂的质量比小于或等于1：1。
作为优选方案，所述卤化铯或甲基卤化胺与卤化铅/聚合物纳米纤维膜中的卤化铅的摩尔比小于或等于5：1。
作为优选方案，所述静电纺丝的工艺条件包括：挤出速率为0.1～2mL/h，电压为10～40kV，环境温度为0～50℃，湿度为50％以下。
本发明还提供一种钙钛矿复合纳米纤维膜，由如上任一方案所述的制备方法制得。
作为优选方案，所述钙钛矿复合纳米纤维膜为以聚合物为载体，钙钛矿包覆聚合物的复合纳米纤维膜。
本发明还提供钙钛矿复合纳米纤维膜的应用，所述钙钛矿复合纳米纤维膜应用于钙钛矿太阳能电池。
作为优选方案，所述钙钛矿复合纳米纤维膜作为钙钛矿太阳能电池的光吸收层。
本发明与现有技术相比，有益效果是：
本发明采用简单静电纺丝技术结合溶液法制备了钙钛矿复合纳米纤维膜，实现钙钛矿与聚合物纤维的结合，获得一维柔性钙钛矿材料，并使钙钛矿材料分布在纳米纤维的表面，有利于钙钛矿材料的光吸收，并使钙钛矿与电荷传输层有效接触，促进电荷的传输；同时，模块化的柔性钙钛矿纳米纤维膜在器件的组装时操作简单方便。此外，钙钛矿复合纳米纤维膜不受基底的限制，能大面积制备，制备过程简单，这使其在钙钛矿太阳能电池的应用潜力巨大。
附图说明
图1是本发明实施例1的钙钛矿复合纳米纤维膜的扫描电镜SEM照片；
图2是本发明实施例1的钙钛矿复合纳米纤维膜的X射线衍射XRD图；
图3是利用本发明实施例1的钙钛矿复合纳米纤维膜构筑的钙钛矿太阳能电池的结构示意图；
图4是利用本发明实施例的钙钛矿复合纳米纤维膜构筑的钙钛矿太阳能电池的光电流电压曲线，其中(a～d)依次为实施例1-4的实施例的电池的光电流电压曲线，(e、f)分别为对比例1和2的电池的光电流电压曲线。
具体实施方式
下面通过具体实施例对本发明的技术方案作进一步描述说明。
实施例1：
本实施例的钙钛矿复合纳米纤维膜的具体制备过程如下：
将0.08克PVP、0.1克PAN和0.2克PbBr2加入到2克二甲基亚砜DMSO中，经过磁力搅拌获得纺丝液；
将纺丝液装入到注射器中，喷丝头和接收装置间加20kV的高电压，喷丝头与接收板的距离是20cm，挤出速率为0.6mL/h，纺丝环境温度为10℃，湿度为30％，使溶液以无序状态直接沉积在接收板上，形成含碘化铅的纳米纤维膜，即碘化铅/聚合物纳米纤维膜；
随后，将含有0.06克溴化铯CsBr的甲醇溶液涂敷在碘化铅/聚合物纳米纤维膜上，从而获得了钙钛矿复合纳米纤维膜。
以下将对本实施例的钙钛矿复合纳米纤维膜进行结构和性能的表征：
如图1所示，为钙钛矿复合纳米纤维膜的SEM照片，可以发现纳米纤维上有大量的纳米颗粒连接，且钙钛矿包覆纳米纤维。图2为本实施例的钙钛矿复合纳米纤维膜的X射线衍射谱图，说明钙钛矿CsPbBr3的形成。另外，本实施例的钙钛矿复合纳米纤维膜可以弯曲成圆形，具有良好的柔韧性。
将本实施例的钙钛矿复合纳米纤维膜应用在钙钛矿太阳能电池中，按图3所示的组装器件，包括自下而上依次叠层的导电衬底1、电荷传输层2、本实施例的钙钛矿复合纳米纤维膜3、电荷传输层4和顶层电极5；其中，电荷传输层2和电荷传输层4分别作为电子传输层或空穴传输层，电荷传输层可以是TiO2、ZnO、SnO2、Al2O3或富勒烯衍生物中的一种或多种，空穴传输层可以是含三苯胺结构的小分子、含噻吩结构的小分子、含苯胺结构的聚合物、含噻吩结构的聚合物、镍的化合物、铜的化合物和钼的化合物中的一种或多种混合；导电衬底1可以是如ITO、FTO、金属纳米线或导电高分子等的导电材料沉积在玻璃或聚合物基底上；顶层电极5，即背电极，采用贵金属或碳材料。首先，将空穴传输层聚(3,4-乙烯二氧噻吩)-聚苯乙烯磺酸(PEDOT:PSS)涂敷在ITO导电基底上，再将本实施例的钙钛矿复合纳米纤维膜放置在空穴传输层之间，随后旋涂富勒烯衍生物PCBM电子传输层，最后，蒸镀金电极从而组成钙钛矿太阳能电池。
本实施例的钙钛矿太阳能电池的光电转换效率为1.72％，如图4(a)所示。
本实施例采用简单静电纺丝技术结合溶液法制备了钙钛矿复合纳米纤维膜，实现钙钛矿与聚合物纤维的结合，获得一维柔性钙钛矿材料，并使钙钛矿材料分布在纳米纤维的表面，这有利于钙钛矿材料的光吸收和电荷的分离；同时，模块化的柔性钙钛矿纳米纤维膜在器件的组装时操作简单方便。此外，钙钛矿纳米纤维膜不受基底的限制，能大面积制备，制备过程简单，这使其在钙钛矿太阳能电池应用潜力巨大。
实施例2：
本实施例的钙钛矿复合纳米纤维膜的具体制备过程如下：
将0.15克PU、0.05克PVP、0.05克PAN、0.028克PbCl2和0.037克PbBr2加入到2克混合溶剂中(1克DMSO和1克DMF)，经过磁力搅拌获得纺丝液；
将纺丝液装入到注射器中，喷丝头和接收装置间加10kV的高电压，喷丝头与接收板的距离是20cm，挤出速率为0.1mL/h，纺丝环境温度为50℃，湿度为50％，使溶液以无序状态直接沉积在接收板上，形成含卤化铅的纳米纤维膜；
随后，将含有0.08克溴化铯CsBr的甲醇溶液涂敷在上述含卤化铅的纳米纤维膜上，从而获得了钙钛矿复合纳米纤维膜。
以下将对本实施例的钙钛矿复合纳米纤维膜进行结构和性能的表征：
本实施例的钙钛矿复合纳米纤维膜的形貌、XRD图与实施例1类似，即意味着本实施例的钙钛矿复合纳米纤维膜的晶体结构、外观形貌以及柔韧性与实施例1相似。
本实施例的钙钛矿复合纳米纤维膜在钙钛矿太阳能电池中的应用，与实施例1类似，其组装的太阳能电池的光电转换效率达到了1.98％，如图4(b)所示。
实施例3：
本实施例的钙钛矿复合纳米纤维膜的具体制备过程如下：
将0.15克PU、0.2克PVP、1.01克PbBr2和0.92克PbI2加入到2克混合溶剂中(1.5克DMSO和0.5克DMF)，经过磁力搅拌获得纺丝液；
将纺丝液装入到注射器中，喷丝头和接收装置间加40kV的高电压，喷丝头与接收板的距离是20cm，挤出速率为1.2mL/h，纺丝环境温度为5℃，湿度为10％，使溶液以无序状态直接沉积在接收板上，形成含卤化铅的纳米纤维膜；
随后，将含有2克甲基碘化胺(CH3NH3I)的溶液涂敷在上述含卤化铅的纳米纤维膜上，从而获得了钙钛矿复合纳米纤维膜。
以下将对本实施例的钙钛矿复合纳米纤维膜进行结构和性能的表征：
本实施例的钙钛矿复合纳米纤维膜的形貌、XRD图与实施例1类似，即意味着本实施例的钙钛矿复合纳米纤维膜的晶体结构、外观形貌以及柔韧性与实施例1相似。
本实施例的钙钛矿复合纳米纤维膜在钙钛矿太阳能电池中的应用，与实施例1类似，其组装的太阳能电池的光电转换效率为3.58％，如图4(c)所示。
实施例4：
本实施例的钙钛矿复合纳米纤维膜的具体制备过程如下：
本实施例的钙钛矿复合纳米纤维膜的具体制备过程如下：
将0.2克PU、0.1克PVP、0.1克PAN、0.56克PbCl2、0.73克PbBr2和0.46克PbI2加入到2克DMF，经过磁力搅拌获得纺丝液；
将纺丝液装入到注射器中，喷丝头和接收装置间加40kV的高电压，喷丝头与接收板的距离是20cm，挤出速率为2mL/h，纺丝环境温度为30℃，湿度为10％，使溶液以无序状态直接沉积在接收板上，形成含卤化铅的纳米纤维膜；
随后，将含有4克甲基碘化胺(CH3NH3I)的溶液涂敷在上述含卤化铅的纳米纤维膜上，从而获得了钙钛矿复合纳米纤维膜。
以下将对本实施例的钙钛矿复合纳米纤维膜进行结构和性能的表征：
本实施例的钙钛矿复合纳米纤维膜的形貌、XRD图与实施例1类似，即意味着本实施例的钙钛矿复合纳米纤维膜的晶体结构、外观形貌以及柔韧性与实施例1相似。
本实施例的钙钛矿复合纳米纤维膜在钙钛矿太阳能电池中的应用，与实施例1类似，其组装的太阳能电池的光电转换效率为3.25％，如图4(d)所示。
对比例1：
按实施例1的钙钛矿太阳能电池的结构组成，利用相同的工艺，采用聚合物包覆钙钛矿的复合纳米纤维膜为吸光层组成钙钛矿太阳电池，其光电转换效率只有0.02％，如图4(e)所示；
其中，聚合物包覆钙钛矿的复合纳米纤维膜的过程为：先将0.228克PbBr2、和0.101克CsBr加到2克DMSO中，在温度为80℃下经磁力搅拌3h获得清澈溶液，之后在溶液中加入0.15克PVP和0.15克PAN，在室温下经磁力搅拌搅拌6h获得CsPbBr3的前驱体纺丝液，将前驱体纺丝液装入到注射器中，进行静电纺丝获得聚合物包覆CsPbBr3无机钙钛矿的复合纳米纤维膜。
对比例2：
按实施例1的钙钛矿太阳能电池的结构组成，利用相同的工艺，采用一步静电纺丝法制备的钙钛矿/聚合物纳米纤维膜为吸光层组成钙钛矿太阳电池，其光电转换效率为1.12％，如图4(f)所示；
其中一步法制备钙钛矿/聚合物纳米纤维膜的过程为：先将0.1克PU、0.1克PVP和0.1克PAN加入到2克DMSO中，在室温下经磁力搅拌2h获得清澈溶液，之后在溶液中加入0.32克PbBr2和0.24克CsI，在温度为80℃下经磁力搅拌搅拌6h获得CsPbX3(X＝Br或I)的前驱体纺丝液，将前驱体纺丝液装入到注射器中进行静电纺丝，形成CsPbX3(X＝Br-或I-)无机钙钛矿/聚合物纳米纤维膜。
在上述实施例及其替换方案中，聚合物与有机溶剂的质量比还可以为0.1：1、0.12：1、0.13：1、0.16：1、0.18：1、0.19：1等。
在上述实施例及其替换方案中，有机溶剂还可以为N，N-二甲基甲酰胺或任意比例混合的N，N-二甲基甲酰胺和二甲基亚砜。
在上述实施例及其替换方案中，聚合物还可以包括聚乙烯吡咯烷酮、聚丙烯腈、聚氨酯中的至少一种(除上述实施例公开的之外)；当至少包括两种时，相应的聚合物的种类为任意质量比。
在上述实施例及其替换方案中，卤化铅与有机溶剂的质量比还可以为0.2：1、0.3：1、0.5：1、0.6：1、0.9：1等。
在上述实施例及其替换方案中，卤化铯或甲基卤化胺与卤化铅/聚合物纳米纤维膜中的卤化铅的摩尔比还可以为0.5：1、1：1、2：1、3：1、4：1、5：1等。
在上述实施例及其替换方案中，静电纺丝的工艺条件中：
挤出速率还可以为0.5mL/h、0.8mL/h、1.5mL/h、1.8mL/h等；
电压还可以为15kV、25kV、30kV、35kV等；
纺丝环境温度还可以为0℃、15℃、25℃、35℃、40℃、45℃等；
湿度还可以为5％、15％、25％、35％、40％、45％等。
以上所述仅是对本发明的优选实施例及原理进行了详细说明，对本领域的普通技术人员而言，依据本发明提供的思想，在具体实施方式上会有改变之处，而这些改变也应视为本发明的保护范围。
Claims (10)
1.一种钙钛矿复合纳米纤维膜的制备方法，其特征在于，包括以下步骤：
S1、在有机溶剂中配制聚合物溶液，所述聚合物包括聚乙烯吡咯烷酮、聚丙烯腈、聚氨酯中的至少一种；
S2、将卤化铅加入所述聚合物溶液中得到纺丝液，将纺丝液进行静电纺丝，得到卤化铅/聚合物纳米纤维膜；
S3、将卤化铯溶液或甲基卤化胺溶液涂覆于卤化铅/聚合物纳米纤维膜之上，制得钙钛矿复合纳米纤维膜。
2.根据权利要求1所述的一种钙钛矿复合纳米纤维膜的制备方法，其特征在于，所述聚合物与有机溶剂的质量比为0.09～0.2：1。
3.根据权利要求1所述的一种钙钛矿复合纳米纤维膜的制备方法，其特征在于，所述有机溶剂为N，N-二甲基甲酰胺和二甲基亚砜中的至少一种。
4.根据权利要求1所述的一种钙钛矿复合纳米纤维膜的制备方法，其特征在于，所述卤化铅与有机溶剂的质量比小于或等于1：1。
5.根据权利要求1所述的一种钙钛矿复合纳米纤维膜的制备方法，其特征在于，所述卤化铯或甲基卤化胺与卤化铅/聚合物纳米纤维膜中的卤化铅的摩尔比小于或等于5：1。
6.根据权利要求1所述的一种钙钛矿复合纳米纤维膜的制备方法，其特征在于，所述静电纺丝的工艺条件包括：挤出速率为0.1～2mL/h，电压为10～40kV，环境温度为0～50℃，湿度为50％以下。
7.一种钙钛矿复合纳米纤维膜，其特征在于，由如权利要求1-6任一项所述的制备方法制得。
8.根据权利要求7所述的一种钙钛矿复合纳米纤维膜，其特征在于，所述钙钛矿复合纳米纤维膜为以聚合物为载体，钙钛矿包覆聚合物的复合纳米纤维膜。
9.如权利要求7所述的钙钛矿复合纳米纤维膜的应用，其特征在于，所述钙钛矿复合纳米纤维膜应用于钙钛矿太阳能电池。
10.如权利要求9所述的钙钛矿复合纳米纤维膜的应用，其特征在于，所述钙钛矿复合纳米纤维膜作为钙钛矿太阳能电池的光吸收层。
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