CN114988461A - 一种无机CsPbI3钙钛矿薄膜及其制备方法 - Google Patents
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Abstract
本发明涉及一种无机CsPbI3钙钛矿薄膜及其制备方法,所述无机CsPbI3钙钛矿薄膜晶粒尺寸均匀,无孔洞,其制备方法步骤如下:1)将制备CsPbI3钙钛矿的粉体原料及1‑萘甲酸溶于N,N‑二甲基甲酰胺中,配制得到钙钛矿前驱体溶液;2)将表面制备有TiO2电子传输层的FTO导电玻璃进行紫外臭氧处理,然后在其表面涂覆钙钛矿前驱体溶液,再进行退火处理得到无机CsPbI3钙钛矿薄膜。本发明提供的无机CsPbI3钙钛矿薄膜晶粒尺寸均匀,结晶性好,薄膜表面无孔洞存在,薄膜的光学性能和湿度稳定性明显得到改善。
Description
技术领域
本发明属于半导体器件材料的选择技术领域,具体涉及一种无机CsPbI3钙钛矿薄膜及其制备方法。
背景技术
金属卤化物钙钛矿(ABX3)太阳能电池如今已经取得了25.5%的认证效率(Nature,2021,598,444–450)。预计到2026年,钙钛矿太阳能电池(PSC)的市场价值将达到23.5亿美元,市场增长率为每年32.0%(Energy Environ.Sci.,2021,14,1286-1325)。然而,有机A位阳离子(如:甲胺,甲脒等)在热、氧、湿气和光照条件下不稳定,阻碍了钙钛矿走向商业化应用,而无机Cs+可以代替挥发性和吸湿性有机阳离子,大大提高钙钛矿的热稳定性。
其中,带隙1.68-1.73eV范围内的CsPbI3是应用在钙钛矿-硅叠层太阳能电池中作为顶部电池的理想候选者(Science,2020,370,1300-1309;Joule,2021,5,183-196)。但是,无机钙钛矿CsPbI3目前存在两个问题,一是空气稳定性差,由于CsPbI3非光学活性的黄相形成能低于光学活性的黑相,所以钙钛矿薄膜置于空气中易相变为非光学活性的黄相;二是CsPbI3在低温下无法形成黑相,所以只能用高温进行退火,不过高温退火又会诱发薄膜形貌粗糙且存在孔洞等问题,大大降低了无机钙钛矿CsPbI3的薄膜性能,进而阻碍其应用。
本发明针对现有全无机CsPbI3薄膜表面粗糙的问题,提供了一种结晶性好且无孔洞的全无机CsPbI3钙钛矿薄膜及其制备方法,对钙钛矿太阳能电池的发展具有重要意义。
发明内容
针对现有技术中存在的上述不足,本发明的目的之一是提供一种无机CsPbI3钙钛矿薄膜。
为实现上述发明目的,具体技术方案如下:
一种无机CsPbI3钙钛矿薄膜,所述无机CsPbI3钙钛矿薄膜晶粒尺寸均匀,无孔洞,其制备方法步骤如下:
1)将制备CsPbI3钙钛矿的粉体原料及1-萘甲酸溶于N,N-二甲基甲酰胺中,配制得到钙钛矿前驱体溶液;
2)将表面制备有TiO2电子传输层的FTO导电玻璃进行紫外臭氧处理(将基底表面的油脂和有机物氧化去除,并改变基底表面的亲疏水性,有利于钙钛矿前驱体溶液在基底上铺展),然后在其表面涂覆步骤1)所得钙钛矿前驱体溶液,再进行退火处理得到无机CsPbI3钙钛矿薄膜。
按上述方案,步骤1)所述制备CsPbI3钙钛矿的粉体原料为碘化铯(CsI)、碘化铅(PbI2)、二甲胺氢碘酸盐(DMAI),所述碘化铯、碘化铅与二甲胺氢碘酸盐的摩尔比为1:1:1。
按上述方案,步骤1)所述碘化铯与1-萘甲酸的摩尔比为1:0.01~0.02。优选为1:0.02。
按上述方案,步骤1)所述粉体原料与N,N-二甲基甲酰胺的摩尔体积比为0.6~0.7mmol/mL。即0.6~0.7mmol的粉体原料溶于1毫升的N,N-二甲基甲酰胺溶剂中。
按上述方案,步骤2)在FTO导电玻璃表面涂覆钙钛矿前驱体溶液的工艺条件为:以3000rpm/min的转速旋涂30s。
按上述方案,步骤2)退火处理工艺条件为:210℃下退火5min。
本发明的目的之二在于提供一种上述无机CsPbI3钙钛矿薄膜的制备方法。
具体技术方案如下:
一种上述无机CsPbI3钙钛矿薄膜的制备方法,具体步骤如下:
1)将制备CsPbI3钙钛矿的粉体原料及1-萘甲酸溶于N,N-二甲基甲酰胺中,配制得到钙钛矿前驱体溶液;
2)将表面制备有TiO2电子传输层的FTO导电玻璃进行紫外臭氧处理,然后在其表面涂覆步骤1)所得钙钛矿前驱体溶液,再进行退火处理得到无机CsPbI3钙钛矿薄膜。
本发明的目的之三为提供上述无机CsPbI3钙钛矿薄膜的应用。
具体技术方案如下:
一种上述无机CsPbI3钙钛矿薄膜在钙钛矿太阳能电池中的应用。
本发明的原理如下:本发明在钙钛矿前驱体溶液中引入1-萘甲酸,促使了DMF溶剂的水解,在前驱体溶液种形成了更多的DMAI物质,进而调控了钙钛矿的成核结晶过程,当引入量为碘化铯摩尔量的1~2%时,获得的钙钛矿薄膜粒径均匀,结晶性得到明显改善,同时光学性能和湿度稳定性得到明显改善。
本发明的有益效果在于:1、本发明提供的无机CsPbI3钙钛矿薄膜晶粒尺寸均匀,结晶性好,薄膜表面无孔洞存在,薄膜的光学性能和湿度稳定性明显得到改善。2、本发明提供的制备方法操作简便,成本低,重复性好,适于规模化生产。
附图说明
图1为本发明实施例1前驱体溶液中不同1-萘甲酸含量所制备的五种无机CsPbI3钙钛矿薄膜的扫描电子显微镜图;
图2为实施例1前驱体溶液中不同1-萘甲酸含量所制备的五种无机CsPbI3钙钛矿薄膜的X射线衍射图谱;
图3为实施例1前驱体溶液中不同1-萘甲酸含量所制备的无机CsPbI3钙钛矿薄膜的光致发光光谱;
图4为实施例1前驱体溶液中添加与不添加1-萘甲酸所制备的无机CsPbI3钙钛矿薄膜的湿度稳定性图。
具体实施方式
为使本领域技术人员更好地理解本发明的技术方案,下面结合附图对本发明作进一步详细描述。
本发明实施例所用原料均在手套箱中称取,搅拌过程在手套箱中采用震荡搅拌。
实施例1
一种无机CsPbI3钙钛矿薄膜,其制备方法包括以下步骤:
1)对FTO导电玻璃基底分别用清洗剂、超纯水和酒精进行清洗,对清洗好的FTO导电玻璃基底进行紫外臭氧处理15分钟后,通过旋涂法将浓度为0.2M的双(乙酰丙酮基)二异丙基钛酸酯溶液(商购原料)旋涂在预处理后的FTO导电玻璃表面,以4000rpm/s的速率旋涂30s,并在100℃下退火10min,在FTO导电玻璃表面制备得到TiO2电子传输层;
2)将碘化铯、碘化铅、二甲胺氢碘酸盐和1-萘甲酸按1:1:1:x(x=0,0.5%,1.0%,2.0%,4.0%)的摩尔比溶于1mL的N,N-二甲基甲酰胺溶剂中,碘化铯、碘化铅和二甲胺氢碘酸盐的物质的量总计0.6mmol,配置成五种钙钛矿前驱体溶液;
3)将步骤1)所得表面覆有TiO2电子传输层的FTO导电玻璃进行紫外臭氧处理15分钟,之后在FTO导电玻璃上利用旋涂法分别旋涂步骤2)配制的五种钙钛矿前驱体溶液中的一种,按3000rpm/min的转速旋涂30s,然后进行退火处理,210℃下退火5min,制得五种无机CsPbI3钙钛矿薄膜。
图1为本实施例前驱体溶液中不同1-萘甲酸含量所制备的五种无机CsPbI3钙钛矿薄膜的扫描电子显微镜图,从图中对比来看,前驱体溶液中不添加1-萘甲酸时,钙钛矿薄膜中出现大量孔洞,且薄膜致密性差,随着1-萘甲酸的含量提高至2.0%,钙钛矿晶体均匀性逐渐得到改善,膜内孔洞也逐渐消失,薄膜形貌得到明显改善,但进一步将1-萘甲酸含量的提高至4.0%时,薄膜内孔洞重新出现。这说明通过对1-萘甲酸的比例调控可以在一定程度上影响全无机钙钛矿成核结晶,进而影响钙钛矿薄膜形貌,优选的1-萘甲酸添加范围为1.0~2.0%。
图2为本实施例前驱体溶液中不同1-萘甲酸含量所制备的五种无机CsPbI3钙钛矿薄膜的X射线衍射图谱,从图中对比来看,随着1-萘甲酸的含量提高至2.0%,钙钛矿晶体的衍射峰的强度逐渐提高,且择优取向也越来越明显,说明钙钛矿的结晶性逐渐得到改善,但进一步将1-萘甲酸含量的提高至4.0%时,衍射峰的强度明显下降,且择优取向也相对变弱。这一变化趋势与图1结果相吻合。
图3为本实施例前驱体溶液中不同1-萘甲酸含量所制备的无机CsPbI3钙钛矿薄膜(1-萘甲酸掺入量分别为0,1.0%,2.0%,4.0%)的光致发光光谱,图中对比来看,随着1-萘甲酸的含量提高至2.0%,钙钛矿薄膜内的非辐射复合过程得到抑制,所以薄膜显示的光致发光强度越来越强,不过,进一步将1-萘甲酸含量的提高至4.0%时,光致发光强度明显下降,说明薄膜质量开始下降。此外,1-萘甲酸的添加并没有明显改变钙钛矿的带隙宽度。
图4为本实施例前驱体溶液中添加与不添加1-萘甲酸所制备的无机CsPbI3钙钛矿薄膜(1-萘甲酸掺入量分别为0,2.0%)的湿度稳定性图,将无机CsPbI3钙钛矿薄膜样品置于室温、相对湿度60~70%条件下,用UV-Vis法测试两种无机CsPbI3钙钛矿薄膜样品的湿度稳定性情况,图中对比来看,不添加1-萘甲酸的薄膜置于相对湿度60~70%条件下1h后,迅速由光活性钙钛矿的黑相降解为非光活性钙钛矿的黄相(见插图),且薄膜的UV-Vis吸光度下降明显;而添加1-萘甲酸后薄膜置于环境中1h后,薄膜还能以光活性钙钛矿的黑相形式存在(见插图),且UV-Vis的吸光度和薄膜吸收起始点(~735nm)无明显下降,表明薄膜的湿度稳定性得到改善。
对于本领域的技术人员来说,可以根据以上的技术方案和构思,给出各种相应的改变和变形,而所有的这些改变和变形,都应该包括在本发明权利要求的保护范围之内。
Claims (9)
1.一种无机CsPbI3钙钛矿薄膜,其特征在于,所述无机CsPbI3钙钛矿薄膜晶粒尺寸均匀,无孔洞,其制备方法步骤如下:
1)将制备CsPbI3钙钛矿的粉体原料及1-萘甲酸溶于N,N-二甲基甲酰胺中,配制得到钙钛矿前驱体溶液;
2)将表面制备有TiO2电子传输层的FTO导电玻璃进行紫外臭氧处理,然后在其表面涂覆步骤1)所得钙钛矿前驱体溶液,再进行退火处理得到无机CsPbI3钙钛矿薄膜。
2.根据权利要求1所述的无机CsPbI3钙钛矿薄膜,其特征在于,步骤1)所述制备CsPbI3钙钛矿的粉体原料为碘化铯、碘化铅、二甲胺氢碘酸盐,所述碘化铯、碘化铅与二甲胺氢碘酸盐的摩尔比为1:1:1。
3.根据权利要求1所述的无机CsPbI3钙钛矿薄膜,其特征在于,步骤1)所述碘化铯与1-萘甲酸的摩尔比为1:0.01~0.02。
4.根据权利要求3所述的无机CsPbI3钙钛矿薄膜,其特征在于,步骤1)所述碘化铯与1-萘甲酸的摩尔比为1:0.02。
5.根据权利要求1所述的无机CsPbI3钙钛矿薄膜,其特征在于,步骤1)所述粉体原料与N,N-二甲基甲酰胺的摩尔体积比为0.6~0.7mmol/mL。
6.根据权利要求1所述的无机CsPbI3钙钛矿薄膜,其特征在于,步骤2)在FTO导电玻璃表面涂覆钙钛矿前驱体溶液的工艺条件为:以3000rpm/min的转速旋涂30s。
7.根据权利要求1所述的无机CsPbI3钙钛矿薄膜,其特征在于,步骤2)退火处理工艺条件为:210℃下退火5min。
8.一种权利要求1-7任一项所述的无机CsPbI3钙钛矿薄膜的制备方法,其特征在于,具体步骤如下:
1)将制备CsPbI3钙钛矿的粉体原料及1-萘甲酸溶于N,N-二甲基甲酰胺中,配制得到钙钛矿前驱体溶液;
2)将表面制备有TiO2电子传输层的FTO导电玻璃进行紫外臭氧处理,然后在其表面涂覆步骤1)所得钙钛矿前驱体溶液,再进行退火处理得到无机CsPbI3钙钛矿薄膜。
9.一种权利要求1-7任一项所述的无机CsPbI3钙钛矿薄膜在钙钛矿太阳能电池中的应用。
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