CN110190139A - 一种无机钙钛矿薄膜的制备方法及其应用 - Google Patents
一种无机钙钛矿薄膜的制备方法及其应用 Download PDFInfo
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Abstract
本发明公开了一种无机钙钛矿薄膜的制备方法及其应用,所述制备方法包括如下步骤:(1)按通式(CsX)nPbX2的配比,在溶剂中加入CsX和PbX2,配置得到无机钙钛矿前驱体溶液,前驱体的质量浓度为50~150 mg/ml,其中,0.8<n<1.5,X为Br、I、Cl中的至少一种;(2)在步骤(1)得到的前驱体溶液中加入甜菜碱,以质量计,甜菜碱的用量为钙钛矿的0.5%~5%;(3)将步骤(2)得到的溶液在衬底上进行旋涂,退火,得到无机钙钛矿薄膜。该方法得到的无机钙钛矿薄膜致密平整,载流子缺陷较少,可应用于发光二极管、太阳能电池等光电器件。
Description
技术领域
本发明属于光电材料与半导体器件领域,涉及一种用于太阳能电池的无机钛矿薄膜,具体涉及一种利用甜菜碱辅助制备无机钙钛矿薄膜的方法。
背景技术
钙钛矿材料是一类有着与钛酸钙(CaTiO3)相同晶体结构的材料,是 Gustav Rose在1839年发现,后来由俄罗斯矿物学家L. A. Perovski命名。钙钛矿材料结构式一般为ABX3,其中A和B是两种阳离子,X是阴离子。这种奇特的晶体结构让它具备了很多独特的理化性质,比如吸光性、电催化性等等,在化学、物理领域有不小的应用。钙钛矿大家族里现已包括了数百种物质,从导体、半导体到绝缘体,范围极为广泛,其中很多是人工合成的。太阳能电池中用到的钙钛矿(CH3NH3PbI3、CH3NH3PbBr3和CH3NH3PbCl3等)属于半导体,有良好的吸光性。全无机的钙钛矿材料的分子式为CsPbX3,其中Cs是铯,Pb是铅,X是碘(I)、氯(Cl)、溴(Br)中的一种。这种无机钙钛矿具有热稳定性好、易于制备等特点,在太阳能电池、发光二极管等领域中具有很大的应用前景和研究价值。
为改善成膜性,现有技术中,对有机无机杂化钙钛矿的制备进行了较多研究。例如,中国发明专利CN106159097A公开了一种改善钙钛矿薄膜质量的新方法,钙钛矿结构式为ABX 3,式中A 为CH3NH3、NH2-CH=NH2中的一种或两种的复合物,B 为Pb,X 为I、Br、Cl 中的一种或两种的复合物,主要步骤为:在一定温度下,将钙钛矿薄膜经有机胺气体或者有机胺溶液处理一定时间,来改善钙钛矿薄膜的质量。中国发明专利申请CN108922972A公开了一种钙钛矿薄膜,所述钙钛矿薄膜包括钙钛矿型ABX3有机-无机杂化材料和聚合物,所述聚合物由丙烯酸酯单体聚合得到。聚合物含有C=O官能团和C=C官能团,其中C=O官能团可与钙钛矿晶界处的B离子(如Pb2+、Sn2+、Ge2+等)通过配位键发生弱相互作用,可以有效调节钙钛矿薄膜的生长。
而对于全无机的钙钛矿材料,采用例如在溶剂中添加二甲基亚砜或者***等作为反溶剂,使钙钛矿材料快速从原溶剂中析出的方法制备的钙钛矿薄膜,在薄膜晶相、颗粒形貌及覆盖率等方面仍达不到所需效果,如何提升薄膜形貌质量仍然是当前研究的关键。
发明内容
本发明的发明目的是提供一种无机钙钛矿薄膜的制备方法,以获得平整致密的薄膜。本发明的另一发明目的是提供采用该方法制备的薄膜的应用。
为达到上述发明目的,本发明采用的技术方案是:一种无机钙钛矿薄膜的制备方法,包括如下步骤:
(1) 按通式 (CsX)nPbX2的配比,在溶剂中加入CsX和PbX2,配置得到无机钙钛矿前驱体溶液,前驱体的质量浓度为50~150 mg/ml,其中,0.8<n<1.5,X为Br、I、Cl中的至少一种;
(2) 在步骤(1)得到的前驱体溶液中加入甜菜碱,以质量计,甜菜碱的用量为钙钛矿的0.5%~5%;
(3) 将步骤(2)得到的溶液在衬底上进行旋涂,退火,得到无机钙钛矿薄膜。
上述技术方案中,步骤(1)中,所述溶剂为DMF、DMSO中的一种或两种。
上述技术方案中,步骤(2)中,所述甜菜碱选自烷基甜菜碱、硫代甜菜碱、烷基酰胺甜菜碱、磺丙基甜菜碱和磷酸脂甜菜碱中的一种或两种以上的混合物。
步骤(3)中,旋涂的转速为2000~10000 rpm。
优选地,1≤n≤1.4。
优选地,前驱体的质量浓度为90~150 mg/ml。
优选地,以质量计,甜菜碱的用量为钙钛矿的1%~2%。
采用上述制备方法得到的无机钙钛矿薄膜,可以应用于制备钙钛矿发光二极管的发光层或者太阳能电池的光吸收层。
由于上述技术方案运用,本发明与现有技术相比具有下列优点:
1、本发明通过在前驱体溶液中引入甜菜碱,以甜菜碱起到表面活性剂的作用,极大地减少了钙钛矿晶粒的尺寸,有利于形成平整致密的薄膜。
2、本发明的方法制备工艺简单。
附图说明
图1为本发明实施例一提供的CsPbBr3薄膜的扫描电镜图。
图2为前驱体溶液中未加入硫代甜菜碱所制备的CsPbBr3薄膜的扫描电镜图。
图3为本发明实施例一提供的CsPbBr3薄膜的原子力显微镜图。
图4为本发明实施例一提供的发光二极管的外量子效率随电压变化的函数曲线。
图5为本发明实施例二提供的CsPbBr3薄膜的扫描电镜图。
具体实施方式
下面结合附图及实施例对本发明作进一步描述:
实施例一:一种甜菜碱辅助制备无机钙钛矿薄膜的方法,包括以下步骤:
(1) 配置无机钙钛矿前驱体溶液。按1:1的摩尔比向DMSO溶液中加入CsBr和PbBr2,前驱体的质量浓度为100 mg/ml。
(2) 在步骤(1)得到的前驱体溶液中加入硫代甜菜碱,甜菜碱与钙钛矿的质量比为1.5%。
(3) 将步骤(2)得到的溶液在衬底上进行旋涂,退火,得到CsPbBr3无机钙钛矿薄膜。
获得的CsPbBr3薄膜的扫描电镜图如附图1所示。
不加入硫代甜菜碱,采用同样的旋涂、退火方法制备薄膜作为对比例,得到的薄膜的扫描电镜图如附图2所示。
对比图1和图2可见,本发明实施例获得的薄膜更加的致密,覆盖率更高,晶粒尺寸更小。
图3为本发明实施例提供的CsPbBr3薄膜的原子力显微镜图。从图中可以看出薄膜的表面较为光滑平整。
将本实施例获得的上述CsPbBr3无机钙钛矿薄膜应用到ITO/Pvk/ CsPbBr3/TPBi/Liq/Al的光电器件结构中,制备发光二极管。图4为发光二极管的外量子效率随电压变化的函数曲线。可见,外量子效率达到2.3%。
实施例二:一种甜菜碱辅助制备无机钙钛矿薄膜的方法,包括以下步骤:
(1) 配置无机钙钛矿前驱体溶液。按1.4:1的摩尔比向DMSO溶液中加入CsBr和PbBr2,前驱体的质量浓度为140 mg/ml。
(2) 在步骤(1)得到的前驱体溶液中加入硫代甜菜碱,甜菜碱与钙钛矿的质量比为5%。
(3) 将步骤(2)得到的溶液在衬底上进行旋涂,退火,得到CsPbBr3无机钙钛矿薄膜。
获得的CsPbBr3薄膜的扫描电镜图如附图5所示。可见,本发明实施例获得的薄膜致密平整,表面光滑。
Claims (8)
1.一种无机钙钛矿薄膜的制备方法,其特征在于,包括如下步骤:
(1) 按通式 (CsX)nPbX2的配比,在溶剂中加入CsX和PbX2,配置得到无机钙钛矿前驱体溶液,前驱体的质量浓度为50~150 mg/ml,其中,0.8<n<1.5,X为Br、I、Cl中的至少一种;
(2) 在步骤(1)得到的前驱体溶液中加入甜菜碱,以质量计,甜菜碱的用量为钙钛矿的0.5%~5%;
(3) 将步骤(2)得到的溶液在衬底上进行旋涂,退火,得到无机钙钛矿薄膜。
2.根据权利要求1所述的无机钙钛矿薄膜的制备方法,其特征在于:步骤(1)中,所述溶剂为DMF、DMSO中的一种或两种。
3.根据权利要求1所述的无机钙钛矿薄膜的制备方法,其特征在于:步骤(2)中,所述甜菜碱选自烷基甜菜碱、硫代甜菜碱、烷基酰胺甜菜碱、磺丙基甜菜碱和磷酸脂甜菜碱中的一种或两种以上的混合物。
4. 根据权利要求1所述的无机钙钛矿薄膜的制备方法,其特征在于:步骤(3)中,旋涂的转速为2000~10000 rpm。
5.根据权利要求1所述的无机钙钛矿薄膜的制备方法,其特征在于:1≤n≤1.4。
6. 根据权利要求1所述的无机钙钛矿薄膜的制备方法,其特征在于:前驱体的质量浓度为90~150 mg/ml。
7.根据权利要求1所述的无机钙钛矿薄膜的制备方法,其特征在于:以质量计,甜菜碱的用量为钙钛矿的1%~2%。
8.采用权利要求1至7中任一项所述制备方法得到的无机钙钛矿薄膜在制备钙钛矿发光二极管的发光层或者太阳能电池的光吸收层中的应用。
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CN111403547A (zh) * | 2020-03-11 | 2020-07-10 | 武汉理工大学 | 一种钙钛矿太阳能电池及其制备方法 |
CN111463355A (zh) * | 2020-04-13 | 2020-07-28 | 苏州大学 | 一种蓝光钙钛矿膜及其应用 |
CN111733401A (zh) * | 2020-06-18 | 2020-10-02 | 浙江大学 | 一种高导热性无机铅卤钙钛矿复合薄膜的制备方法 |
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Cited By (6)
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CN111403547A (zh) * | 2020-03-11 | 2020-07-10 | 武汉理工大学 | 一种钙钛矿太阳能电池及其制备方法 |
CN111463355A (zh) * | 2020-04-13 | 2020-07-28 | 苏州大学 | 一种蓝光钙钛矿膜及其应用 |
CN111733401A (zh) * | 2020-06-18 | 2020-10-02 | 浙江大学 | 一种高导热性无机铅卤钙钛矿复合薄膜的制备方法 |
CN111733401B (zh) * | 2020-06-18 | 2021-10-22 | 浙江大学 | 一种高导热性无机铅卤钙钛矿复合薄膜的制备方法 |
CN112038449A (zh) * | 2020-08-27 | 2020-12-04 | 上海应用技术大学 | 一种采用溶液喷涂法制得的CsPbX3薄膜及其制备和应用 |
WO2023098926A3 (zh) * | 2021-12-01 | 2023-07-20 | 浙江大学 | 双极性分子稳定的钙钛矿材料及光电器件 |
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