CN111952383A - 一种CsPbBr3-CsPb2Br5全无机混合钙钛矿薄膜的自驱动可见光光电探测器 - Google Patents
一种CsPbBr3-CsPb2Br5全无机混合钙钛矿薄膜的自驱动可见光光电探测器 Download PDFInfo
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Abstract
本发明提出了一种CsPbBr3‑CsPb2Br5混合钙钛矿薄膜的自驱动可见光光电探测器。器件的结构为透明导电玻璃/氧化锡电子传输层/CsPbBr3‑CsPb2Br5混合钙钛矿薄膜/碳电极,其中混合钙钛矿薄膜是使用CsPb2Br5钙钛矿前驱体配合多次旋涂CsBr并退火的旋涂法制备的。该器件具有较好的自驱动特性和很好的水氧稳定性。本发明避免了传统一步法制备CsPbBr3薄膜所导致的多针孔缺陷,极大的提高了器件的性能和稳定性。用其制备的光电探测器性能稳定,制作周期短,具有高的响应度和探测灵敏度。该器件制作工艺简单、成本低廉,适用于大批量大面积产业化生产。同时其自驱动特性有利于节约能源。
Description
技术领域
本发明涉及半导体纳米材料以及光电探测器技术领域,特别是一种 CsPbBr3-CsPb2Br5全无机混合钙钛矿薄膜的自驱动可见光光电探测器,它使用高 溶解度的CsPb2Br5钙钛矿前驱体配合多次旋涂CsBr并退火的方法来制备具有致 密、稳定、高效吸光能力的CsPbBr3-CsPb2Br5混合钙钛矿薄膜。用该混合钙钛矿 薄膜来制备高性能的光电探测器。
背景技术
近年来,卤化物钙钛矿材料由于禁带可调、高的载流子迁移率与扩散长度等 优点,在光电器件领域受到了极大的关注[1]。对于光电探测器来说,卤化物钙钛 矿具有制备工艺简单、高的光电转换能力等优点而受到青睐。卤化物钙钛矿通过 结合N型材料和P型材料,组成PIN结构的自驱动光电探测器,具有极高的探 测度和响应速度;但有机无机杂化的卤化物钙钛矿由于存在有机阳离子MA+ (FA+)等,在空气和紫外(UV)光环境下易受水氧的影响而导致分解,使得其 性能不能长久保持。
全无机卤化铅钙钛矿CsPbX3(X=I,Br,Cl)因为带隙可调,稳定性好,性 能强的原因,被认为是有机无机杂化钙钛矿最适合的替代品[2]。经过不断的发展, 以全无机钙钛矿为基础的光电探测器光电性能已经提高到了新的水平。以 CsPbBr3钙钛矿为吸光层的器件光暗态开关比可以达到106,而响应时间仅为微秒 级别[3]。其稳定性更是远远超过了有机无机杂化卤化物钙钛矿探测器。
由于在一步法制备CsPbBr3钙钛矿材料常常要用到CsBr,但是CsBr在目前 已发现的有机溶剂二甲基亚砜,N,N-二甲基甲酰胺中溶解度较低,使得一步法做 出来的薄膜充满针孔,从而导致大量的缺陷,最终会严重影响器件的性能[4]。我 们利用CsPb2Br5钙钛矿的高溶解度来制备致密的CsPb2Br5薄膜,再通过多次旋 涂CsBr甲醇溶液并退火的方法使得其转变为致密、具有极强的可见光吸收能力 的CsPbBr3-CsPb2Br5混和钙钛矿薄膜。避免了缺陷的产生,极大的提高了光电探 测器的性能。实验发现一定量的CsPb2Br5在CsPbBr3薄膜中具有钝化作用,能够 提高CsPbBr3钙钛矿的稳定性和光电性能。且其顶电极采用刮涂碳浆的方法,成 本低廉、易操作,便于产业化生产。同时碳具有一定的保护作用,提高了器件的 耐水氧和紫外线能力。
参考文献
[1]Saini,H.,Li-Fi(Light Fidelity)-The Future Technology In WirelessCommunication.J.Comput.Appl 2016,7(1),13-15.
[2]Zhou,W.;Zhao,Y.;Zhou,X.;Fu,R.;Li,Q.;Zhao,Y.;Liu,K.;Yu,D.;Zhao,Q.Light-Independent IonicTransport in Inorganic Perovskite and UltrastableCs-Based Perovskite Solar Cells.The Journal of Physical Chemistry Letters2017,8(17), 4122-4128.
[3]Yang,B.;Zhang,F.;Chen,J.;Yang,S.;Xia,X.;Pullerits,T.;Deng,W.;Han,K.Ultrasensitive and Fast All-Inorganic Perovskite-Based Photodetector ViaFast Carrier Diffusion.Advanced Materials 2017,29(40),1703758.
[4]Fu,Y.;Zhu,H.;Stoumpos,C.C.;Ding,Q.;Wang,J.;Kanatzidis,M.G.;Zhu,X.;Jin,S.Broad Wavelength Tunable Robust Lasing from Single-Crystal Nanowiresof Cesium Lead Halide Perovskites (CsPbX3, X=Cl, Br, I). ACS Nano 2016, 10(8), 7963-7972.
发明内容
基于上述技术背景,本发明提供一种基于CsPbBr3-CsPb2Br5全无机混合钙钛 矿的自驱动光电探测器,其结构为透明导电玻璃/氧化锡/CsPbBr3-CsPb2Br5钙钛 矿薄膜/碳电极的结构。此探测器的制备步骤简单,实验成本低廉,且所制备的 CsPbBr3-CsPb2Br5薄膜整体结构致密,钙钛矿晶粒大。制备的探测器具有高的响 应度和探测度,极快的响应速度以及较好的稳定性。
本发明是这样实现的。它主要由透明导电玻璃、氧化锡种子层、钙钛矿吸光 层、碳电极组成。
本发明的具体制备流程和工艺如下:
(1)分别用去离子水、丙酮、酒精超声透明导电玻璃衬底各20分钟,然后 用紫外臭氧环境处理30分钟;
(2)通过旋涂法制备氧化锡电子传输层
采用3000转/分,旋涂30秒的速度旋涂氧化锡水溶液浆料。然后100℃烘 干,冷却至室温后用紫外臭氧环境处理30分钟。
(3)用旋涂法制备致密的CsPbBr3-CsPb2Br5全无机混合钙钛矿薄膜
a)、1毫摩尔CsPb2Br5粉末溶解在1毫升DMSO(二甲基亚砜)中,70℃ 下保温搅拌12小时使其充分溶解,然后过滤备用;
b)、将CsBr(10毫克/毫升)溶解在甲醇溶液中搅拌40分钟备用;
c)、将CsPb2Br5溶液采用4000转/分,旋涂40秒的速度旋涂在处理后的透 明导电玻璃上,在剩余时间10秒时滴加150微升反溶剂氯苯,然后在250℃下 烘烤20分钟,取下自然冷却至室温后,再旋涂配好的CsBr甲醇溶液,速度为 2000~4000转/分,旋涂40秒,每次旋涂120微升。每次旋涂完后重复250℃ 烘烤及自然冷却过程,重复2~6次,得到致密的CsPbBr3-CsPb2Br5全无机混合 钙钛矿薄膜;
(4)制备碳电极
使用掩膜版在制备好的钙钛矿薄膜上刮涂碳浆,然后用100℃加热20分钟 使得碳浆干燥;
(5)检测样品性能
所制备样品在300-450nm范围的可见光照射下具有明显的光电效应。在 468mWcm-2的473nm激光照射下产生1.26V的开路电压。
至此,即可制作成一个完整的可见光自驱动结构的光电探测器。
形貌和晶体结构测试采用紫外可见光分光光度计(MPC-3100SHIMADZU), 场致发射扫描电子显微镜(SEM)(JSM-7100F)和X射线衍射(XRD)(Bruker D8 Advance CuKaradiation);光电性能(I-V,I-t)由半导体性能测试仪(Agilent Technologies B1500A)测试。这些测试分析结果分别列于附图中。
本发明的器件结构为透明导电玻璃/氧化锡/CsPbBr3-CsPb2Br5全无机混合 钙钛矿薄膜/碳电极(如图1所示),该器件在0V偏压468mW cm-2可见光照 射下开关比达到了106。同时,此器件展示了很强的水氧稳定性,在平均温度 30℃,相对湿度70%的大气环境下放置30天,其光电流衰减幅度小于3%;在 100mW cm-2强度的473nm激光照射下3000s后光暗电流几乎没有衰减。该探 测器光电探测范围为300-540nm的可见光。本发明制作的探测器具有高的响应 度和探测灵敏度。此器件展示了高的光电响应性能,在0V偏压下达110mA W-1;探测度高达1.4×1012Jones。另外,此器件的光响应上升和下降时间仅为6/64μs, 具有很快的响应速度。此器件制作工艺简单,成本低,适合于大批量、大面积 产业化生产。
本发明的优点和特色之处在于:
(1)本发明中制作的光电探测器,制作工艺简单、成本低廉,制作周期短, 适合大面积大规模工业化生产。
(2)本发明解决了全无机CsPbBr3钙钛矿薄膜针孔多,性能差的问题。制备 了高稳定性和高性能,响应速度快的可见光光电探测器。
附图说明
图1是本发明的器件结构图。
其中1---碳电极,2---CsPbBr3-CsPb2Br5全无机混合钙钛矿薄膜,3---/氧化锡 电子传输层,4透明导电玻璃;
图2旋涂四次CsBr溶液后的XRD(a)和SEM(b);
图3是是本发明的探测器在不同光强下的I-T曲线;
图4是是本发明的探测器在暗态和光照下的I-V特性曲线;
图5是本发明的探测器的响应度曲线。
具体实施方式
下面通过实施例将能够更好地理解本发明。
实施例1:不同CsBr旋涂次数的CsPbBr3-CsPb2Br5混和钙钛矿光电探测器的 制备:
(1)分别用去离子水、丙酮、酒精超声透明玻璃衬底各20分钟,然后用紫 外臭氧环境处理30分钟;
(2)通过旋涂法制备氧化锡电子传输层
采用3000转30秒的速度旋涂氧化锡水溶液浆料。然后100℃烘干,冷却至 室温后用紫外臭氧环境处理30分钟;
(3)用旋涂法制备致密的CsPbBr3-CsPb2Br5全无机混合钙钛矿薄膜
1毫摩尔CsPb2Br5粉末溶解在1毫升DMSO(二甲基亚砜)中,70℃下保温 搅拌12小时使其充分溶解,然后过滤备用;将CsBr(10毫克/毫升)溶解在甲 醇溶液中搅拌40分钟备用。CsPb2Br5溶液采用4000转/分,旋涂40秒的速度旋 涂在(2)中处理后的透明导电玻璃上,在剩余时间10秒时滴加150微升反溶剂 氯苯。然后在250℃下烘烤20分钟,取下自然冷却至室温后,旋涂配好的CsBr 甲醇溶液,速度为4000转40秒,每次旋涂120微升。每次旋涂完后重复250℃ 烘烤及自然冷却过程,旋涂次数为一到六次,得到致密的不同比率的 CsPbBr3-CsPb2Br5全无机混合钙钛矿薄膜。
(4)制备碳电极
使用掩膜版在(3)中制备好的钙钛矿薄膜上刮涂碳浆,然后用100℃加热 20分钟使得碳浆干燥。
(5)检测样品性能
将得到的薄膜进行XRD、SEM等表征分析,并对组装好的光电探测器测试I-t 和I-V特性曲线、光电响应曲线和响应速度等性能。这些测试分析结果分别列于 附图中。
实施例2:不同退火温度下的CsPbBr3-CsPb2Br5混和钙钛矿光电探测器的制 备:
(1)分别用去离子水、丙酮、酒精超声透明玻璃衬底各20分钟,然后用紫 外臭氧环境处理30分钟;
(2)通过旋涂法制备氧化锡电子传输层
采用3000转30秒的速度旋涂氧化锡水溶液浆料。然后100℃烘干,冷却至 室温后用紫外臭氧环境处理30分钟;
(3)用旋涂法制备致密的CsPbBr3-CsPb2Br5全无机混合钙钛矿薄膜
1毫摩尔CsPb2Br5粉末溶解在1毫升DMSO(二甲基亚砜)中,70℃下保温 搅拌12小时使其充分溶解,然后过滤备用;将CsBr(10毫克/毫升)溶解在甲 醇溶液中搅拌40分钟备用。CsPb2Br5溶液采用4000转,40秒的速度旋涂在(2) 中处理后的透明导电玻璃上,在剩余时间10秒时滴加150微升反溶剂氯苯。然 后在200℃,220℃,250℃下烘烤20分钟,取下自然冷却至室温后,旋涂配好的 CsBr甲醇溶液,速度为4000转/分,旋涂40秒,每次旋涂120微升。每次旋涂 完后重复250℃烘烤及自然冷却过程,旋涂次数为四次,得到致密的 CsPbBr3-CsPb2Br5全无机混合钙钛矿薄膜。
(4)制备碳电极
使用掩膜版在(3)中制备好的钙钛矿薄膜上刮涂碳浆,然后用100℃加热 20分钟使得碳浆干燥。
(5)检测样品性能
将得到的薄膜进行XRD、SEM等表征分析,并对组装好的光电探测器测试I-t 和I-V特性曲线、光电响应曲线和响应速度等性能。这些测试分析结果分别列于 附图中。
实施例3:不同转速下的CsPbBr3-CsPb2Br5混和钙钛矿光电探测器的制备:
(1)分别用去离子水、丙酮、酒精超声透明玻璃衬底各20分钟,然后用紫 外臭氧环境处理30分钟;
(2)通过旋涂法制备氧化锡电子传输层
采用3000转30秒的速度旋涂氧化锡水溶液浆料。然后100℃烘干,冷却至 室温后用紫外臭氧环境处理30分钟;
(3)用旋涂法制备致密的CsPbBr3-CsPb2Br5全无机混合钙钛矿薄膜
1毫摩尔CsPb2Br5粉末溶解在1毫升DMSO(二甲基亚砜)中,70℃下保温 搅拌12小时使其充分溶解,然后过滤备用;将CsBr(10毫克/毫升)溶解在甲 醇溶液中搅拌40分钟备用。CsPb2Br5溶液采用4000转每分钟,旋涂40秒的条件 下旋涂在(2)中处理后的透明导电玻璃上,在剩余时间10秒时滴加150微升反 溶剂氯苯。然后在250℃下烘烤20分钟,取下自然冷却至室温后,旋涂配好的 CsBr甲醇溶液,速度为2000/3000/4000转/分,旋涂40秒;每次旋涂120微升。 每次旋涂完后重复250℃烘烤及自然冷却过程,旋涂次数为四次,得到致密的CsPbBr3-CsPb2Br5全无机混合钙钛矿薄膜。
(4)制备碳电极
使用掩膜版在(3)中制备好的钙钛矿薄膜上刮涂碳浆,然后用100℃加热 20分钟使得碳浆干燥。
(5)检测样品性能
将得到的薄膜进行XRD、SEM等表征分析,并对组装好的光电探测器测试I-t 和I-V特性曲线、光电响应曲线和响应速度等性能。这些测试分析结果分别列于 附图中。
Claims (2)
1.一种CsPbBr3-CsPb2Br5全无机混合钙钛矿薄膜的自驱动可见光光电探测器。其主要由透明导电玻璃、氧化锡电子传输层、钙钛矿吸光层、碳电极组成,其特征在于钙钛矿吸光层是由致密的CsPbBr3-CsPb2Br5全无机混和钙钛矿薄膜构成;
所述致密的CsPbBr3-CsPb2Br5全无机混和钙钛矿薄膜是用下述旋涂方法制备的:
a)、1毫摩尔CsPb2Br5粉末溶解在1毫升DMSO(二甲基亚砜)中,70℃下保温搅拌12小时使其充分溶解,然后过滤备用;
b)、将CsBr(10毫克/毫升)溶解在甲醇溶液中搅拌40分钟备用;
c)、将CsPb2Br5溶液采用4000转/分,旋涂40秒的速度旋涂在处理后的透明导电玻璃上,在剩余时间10秒时滴加150微升反溶剂氯苯,然后在250℃下烘烤20分钟,取下自然冷却至室温后,再旋涂配好的CsBr甲醇溶液,速度为2000~4000转/分,旋涂40秒,每次旋涂120微升。每次旋涂完后重复250℃烘烤及自然冷却过程,重复2~6次,得到致密的CsPbBr3-CsPb2Br5全无机混合钙钛矿薄膜。
2.一种CsPbBr3-CsPb2Br5全无机混合钙钛矿薄膜的自驱动可见光光电探测器制备方法,其特征在于步骤为:
(1)分别用去离子水、丙酮、酒精超声透明导电玻璃衬底各20分钟,然后用紫外臭氧环境处理30分钟;
(2)通过旋涂法制备氧化锡电子传输层
采用3000转/分,旋涂30秒的速度旋涂氧化锡水溶液浆料。然后100℃烘干,冷却至室温后用紫外臭氧环境处理30分钟;
(3)用旋涂法制备致密的CsPbBr3-CsPb2Br5全无机混合钙钛矿薄膜
a)、1毫摩尔CsPb2Br5粉末溶解在1毫升DMSO(二甲基亚砜)中,70℃下保温搅拌12小时使其充分溶解,然后过滤备用;
b)、将CsBr(10毫克/毫升)溶解在甲醇溶液中搅拌40分钟备用;
c)、将CsPb2Br5溶液采用4000转/分,旋涂40秒的速度旋涂在处理后的透明导电玻璃上,在剩余时间10秒时滴加150微升反溶剂氯苯,然后在250℃下烘烤20分钟,取下自然冷却至室温后,再旋涂配好的CsBr甲醇溶液,速度为2000~4000转/分,旋涂40秒,每次旋涂120微升。每次旋涂完后重复250℃烘烤及自然冷却过程,重复2~6次,得到致密的CsPbBr3-CsPb2Br5全无机混合钙钛矿薄膜;
(4)制备碳电极
使用掩膜版在(3)中制备好的钙钛矿薄膜上刮涂碳浆,然后用100℃加热20分钟使得碳浆干燥;
(5)检测样品性能
至此,即可制作成一个完整的自驱动结构的可见光光电探测器。
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