CN109411608A - 一种具有补丁结构钙钛矿薄膜的制备方法 - Google Patents
一种具有补丁结构钙钛矿薄膜的制备方法 Download PDFInfo
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Abstract
本发明涉及一种具有补丁结构钙钛矿薄膜的制备方法,属于有机‑无机杂化钙钛矿材料技术领域。本发明所述方法主要是利用甲巯咪唑的有机溶液处理钙钛矿薄膜,将钙钛矿薄膜中残留的碘化铅转化成MMI‑PbI2配合物,该配合物位于晶界处,能连接毗连的晶粒,钝化晶界,有利于增大钙钛矿薄膜中的晶体尺寸,有效地抑制离子迁移和金属电极扩散,延长载流子的寿命,从而大幅提升太阳能电池器件的稳定性。
Description
技术领域
本发明涉及一种具有补丁结构钙钛矿薄膜的制备方法,属于有机-无机杂化钙钛矿材料技术领域。
背景技术
随着人类社会的进步与发展,人类对能源的需求大幅增长,大量化石能源的使用造成了严重的环境污染,而且化石能源日益枯竭,使得能源危机成为全人类面临的问题。太阳能是一种清洁、安全的可再生能源,有效利用太阳能对于缓解能源危机、保护地球环境以及推动经济发展具有重要的意义。
基于有机-无机杂化钙钛矿太阳能电池以其制备成本低、制备工艺简单等优点受到了全世界科研工作者的广泛关注,其优越的光电性能使其有很大的潜力去取代昂贵的硅基太阳能电池。近几年,有机-无机杂化钙钛矿材料作为一种新型的吸光材料,在太阳能电池领域取得重大进展,其光电转化效率记录不断被刷新。但是,太阳能电池器件的稳定性依然是个重大挑战。一方面是由于材料本身引起的:例如薄膜表面和晶界处存在很多缺陷,这些缺陷很容易吸附其他的物质引发分解;此外,作为主要的离子迁移途径,晶界和迟滞密切相关。另一方面,太阳能电池器件中的金属电极很容易扩散,和钙钛矿中的碘反应,降低器件效率。
发明内容
为了解决离子迁移和金属电极扩散引发的太阳能电池器件稳定性问题,本发明提供了一种具有补丁结构钙钛矿薄膜的制备方法,该方法主要是利用甲巯咪唑的有机溶液处理钙钛矿薄膜,与钙钛矿薄膜中残留的碘化铅形成配合物,该配合物位于晶界处,能连接毗连的晶粒,钝化晶界,有效地抑制离子迁移和金属电极扩散,从而大幅提升太阳能电池器件的稳定性。
本发明的目的是通过以下技术方案实现的。
一种具有补丁结构钙钛矿薄膜的制备方法,所述方法步骤如下:
(1)将甲基碘化铵(MAI)和碘化铅(PbI2)溶解在二甲基甲酰胺(DMF)中,得到前驱体溶液;
(2)将前驱体溶液涂覆在基底上,并打反溶剂,再进行退火处理,得到钙钛矿薄膜;
所述反溶剂是不溶于前驱体溶液的溶剂,优选乙醚、甲苯、氯苯或二氯甲烷;
(3)在钙钛矿薄膜上涂覆20μL~50μL浓度为1mg/mL~10mg/mL的甲巯咪唑(MMI)的有机溶液,再进行退火处理,得到具有补丁结构钙钛矿薄膜。
步骤(2)步骤(3)中,所述退火处理的温度分别独立为80℃~120℃,退火处理时间分别独立为5min~20min。
所述涂覆包括旋涂、狭缝挤出或者刮涂。
甲巯咪唑的有机溶液中,其溶剂能够微溶钙钛矿薄膜,优选异丙醇(IPA)、乙酸乙酯或乙腈。
有益效果:
本发明所述方法主要是利用甲巯咪唑的有机溶液处理钙钛矿薄膜,将钙钛矿薄膜中残留的碘化铅转化成MMI-PbI2配合物,该配合物位于晶界处,能连接毗连的晶粒,钝化晶界,有利于增大钙钛矿薄膜中的晶体尺寸,有效地抑制离子迁移和金属电极扩散,延长载流子的寿命,从而大幅提升太阳能电池器件的稳定性。
附图说明
图1为对比例1中制备的钙钛矿薄膜的扫描电子显微镜(SEM)图。
图2为实施例1中制备的具有补丁结构钙钛矿薄膜的SEM图。
图3是基于对比例1中制备的钙钛矿薄膜的太阳能电池的元素分布线扫图。
图4是基于实施例1中制备的具有补丁结构钙钛矿薄膜的太阳能电池的元素分布线扫图。
图5是基于对比例1中制备的钙钛矿薄膜的太阳能电池的截面元素分布面扫图。
图6是基于实施例1中制备的具有补丁结构钙钛矿薄膜的太阳能电池的截面元素分布面扫图。
具体实施方式
下面结合附图和具体实施方式对本发明作进一步阐述,其中,所述方法如无特别说明均为常规方法,所述原材料如无特别说明均能从公开商业途径而得。
以下实施例中:
SEM表征采用的是S-4800型扫描电子显微镜;
太阳能电池的元素分布表征采用的是高角环形暗场像-扫描透射电子显微镜(HAADF-STEM)以及球差校正高分辨透射电子显微镜(FEI Titan G2);
太阳能电池性能测试:采用Newport Thermal Oriel 91192 1000W太阳光模拟器,模拟太阳光光照强度AM1.5G,100mW cm-2,并使用KG-5电池对太阳光进行光强校准,采用Keithley 2400源表进行测试,电压扫描范围1.2V~-0.2V,扫描步长0.02V。
钙钛矿太阳能电池的制备:将SnO2溶液在3000rpm条件下旋涂在洁净的ITO导电玻璃基底上,旋涂30s,再将旋涂SnO2后的ITO导电玻璃置于150℃下退火30min,在ITO导电玻璃上形成SnO2电子传输层;采用实施例或对比例中的方法在SnO2电子传输层制备钙钛矿薄膜;将spiro-OMeTAD溶液在3000rpm条件下旋涂在钙钛矿薄膜上,旋涂30s,在钙钛矿薄膜上形成空穴传输层;再在空穴传输层上蒸镀100nm银作为电极,得到平板异质结钙钛矿太阳能电池;
其中,将质量分数为15%的SnO2水溶液与超纯水按照1:5的体积比进行稀释,混合均匀,得到SnO2溶液;将80mg spiro-OMeTAD(2,2',7,7'-四[N,N-二(4-甲氧基苯基)氨基]-9,9'-螺二芴)溶于1mL氯苯中,并添加35μL浓度为260mg mL-1的双三氟甲烷磺酰亚胺锂/乙腈溶液和30μL 4-叔丁基吡啶,混合均匀,得到spiro-OMeTAD溶液。
实施例以及对比例中所述钙钛矿前驱体溶液的配制:将461mg碘化铅和159mg甲基碘化铵加入600μL N,N-二甲基甲酰胺中,并在70℃下加热10min使混合溶液变澄清,再在常温下搅拌12h,得到钙钛矿前驱体溶液。
实施例1
(1)将钙钛矿前驱体溶液旋涂在氧化锡基底上,3000rpm下旋涂20s后,打反溶剂乙醚1mL,再置于100℃下退火5min,得到CH3NH3PbI3钙钛矿薄膜;
(2)将50μL浓度为1mg/mL的MMI/IPA溶液旋涂在CH3NH3PbI3钙钛矿薄膜上,3000rpm下旋涂30s后,再置于100℃下退火10min,得到具有补丁结构CH3NH3PbI3钙钛矿薄膜。
实施例2
(1)将钙钛矿前驱体溶液旋涂在氧化锡基底上,3000rpm下旋涂20s后,打反溶剂乙醚1mL,再置于100℃下退火5min,得到CH3NH3PbI3钙钛矿薄膜;
(2)将50μL浓度为2mg/mL的MMI/IPA溶液旋涂在CH3NH3PbI3钙钛矿薄膜上,3000rpm下旋涂30s后,再置于100℃下退火10min,得到具有补丁结构CH3NH3PbI3钙钛矿薄膜。
实施例3
(1)将钙钛矿前驱体溶液旋涂在氧化锡基底上,3000rpm下旋涂20s后,打反溶剂乙醚1mL,再置于100℃下退火5min,得到CH3NH3PbI3钙钛矿薄膜;
(2)将50μL浓度为3mg/mL的MMI/IPA溶液旋涂在CH3NH3PbI3钙钛矿薄膜上,3000rpm下旋涂30s后,再置于100℃下退火5min,得到具有补丁结构CH3NH3PbI3钙钛矿薄膜。
对比例1
(1)将钙钛矿前驱体溶液旋涂在氧化锡基底上,3000rpm下旋涂20s后,打反溶剂乙醚1mL,再置于100℃下退火5min,得到CH3NH3PbI3钙钛矿薄膜;
(2)将50μL IPA旋涂在CH3NH3PbI3钙钛矿薄膜上,3000rpm下旋涂30s后,再置于100℃下退火10min,得到IPA处理的CH3NH3PbI3钙钛矿薄膜。
性能表征
(1)根据图1和图2可知,对比例1中经过IPA处理的CH3NH3PbI3钙钛矿薄膜晶界处含有很多颗粒状的物质;实施例1中经过MMI/IPA处理的CH3NH3PbI3钙钛矿薄膜表面的颗粒状物质消失了,在晶界处形成了类似于补丁的配合物,而且晶粒尺寸较大。实施例2和实施例3所制备的CH3NH3PbI3钙钛矿薄膜与实施例1中制备的CH3NH3PbI3钙钛矿薄膜具有类似的补丁结构,而且晶粒尺寸比对比例1中制备的CH3NH3PbI3钙钛矿薄膜的晶粒尺寸大。
(2)分别基于实施例1~3以及对比例1中的CH3NH3PbI3钙钛矿薄膜制备钙钛矿太阳能电池,并对其进行性能测试。根据表1中的测试结果可知,与基于对比例1中CH3NH3PbI3钙钛矿薄膜制备的太阳能电池相比,基于实施例1~3中CH3NH3PbI3钙钛矿薄膜制备的太阳能电池的效率提高了。
表1
(3)将基于实施例1以及对比例1中的CH3NH3PbI3钙钛矿薄膜制备的钙钛矿太阳能电池分别置于太阳光模拟器(模拟太阳光光照强度AM1.5G)下照射1个月,再对照射后的钙钛矿太阳能电池分别进行元素线扫描(如图3和图4所示)以及截面的元素面扫描(如图5和图6所示)。
从图3和图5的表征结果可知,基于对比例1中CH3NH3PbI3钙钛矿薄膜的钙钛矿太阳能电池的碘元素分布不均匀,经过光照之后碘发生了明显的迁移,甚至扩散到了空穴传输层;此外,银电极也发生了迁移,扩散到了CH3NH3PbI3钙钛矿薄膜层。从图4和图6的表征结果可知,基于实施例1中CH3NH3PbI3钙钛矿薄膜的钙钛矿太阳能电池的碘元素分布则更均匀,在相同的条件下照射后,碘以及银电极都未见明显的迁移,表明经过MMI处理的CH3NH3PbI3钙钛矿薄膜中所形成的补丁结构能够抑制碘的迁移和金属电极的扩散。
综上所述,以上仅为本发明的较佳实施例而已,并非用于限定本发明的保护范围。凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。
Claims (5)
1.一种具有补丁结构钙钛矿薄膜的制备方法,其特征在于:所述方法步骤如下:
(1)将甲基碘化铵和碘化铅溶解在二甲基甲酰胺中,得到前驱体溶液;
(2)将前驱体溶液涂覆在基底上,并打反溶剂,再进行退火处理,得到钙钛矿薄膜;
(3)在钙钛矿薄膜上涂覆20μL~50μL浓度为1mg/mL~10mg/mL的甲巯咪唑的有机溶液,再进行退火处理,得到具有补丁结构钙钛矿薄膜;
其中,所述反溶剂是不溶于前驱体溶液的溶剂,甲巯咪唑的有机溶液的溶剂微溶钙钛矿薄膜。
2.根据权利要求1所述的一种具有补丁结构钙钛矿薄膜的制备方法,其特征在于:所述反溶剂为乙醚、甲苯、氯苯或二氯甲烷。
3.根据权利要求1所述的一种具有补丁结构钙钛矿薄膜的制备方法,其特征在于:步骤(2)步骤(3)中,所述退火处理的温度分别独立为80℃~120℃,退火处理时间分别独立为5min~20min。
4.根据权利要求1所述的一种具有补丁结构钙钛矿薄膜的制备方法,其特征在于:所述涂覆包括旋涂、狭缝挤出或者刮涂。
5.根据权利要求1所述的一种具有补丁结构钙钛矿薄膜的制备方法,其特征在于:甲巯咪唑的有机溶液的溶剂为异丙醇、乙酸乙酯或乙腈。
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