CN110190195A - 一种基于复合界面传输材料的钙钛矿光伏-发光-光探测多功能器件及其制备方法 - Google Patents
一种基于复合界面传输材料的钙钛矿光伏-发光-光探测多功能器件及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种基于复合界面传输材料的钙钛矿光伏‑发光‑光探测多功能器件及其制备方法。所述多功能器件包括从下至上依次层叠设置的透明导电玻璃、复合电子传输层、钙钛矿活性层、复合空穴传输层和金属电极层。本发明是利用多元界面传输材料的复合调整界面传输层的功函数,让电子传输层和空穴传输层的功函数分别与钙钛矿活性层的导带和价带位置拉平。经实验结果对比,能带调控后的钙钛矿多功能器件光电转换效率和发光效率都有了明显的提升。
Description
技术领域
本发明所属钙钛矿光电领域,具体涉及一种基于复合界面传输材料的钙钛矿光伏-发光-光探测多功能器件及其制备方法。
背景技术
近年来,有机无机卤化钙钛矿材料具有吸光系数高、载流子寿命长、禁带宽度可调和低成本等诸多优点而成为光电领域的研究热点。由该材料制备得到的太阳能电池和发光二极管都取得了巨大进展,逐渐展现出很好的应用前景。根据美国国家可再生能源实验室(NREL)统计,钙钛矿太阳能电池的最高认证能量转换效率已经达到23.7%。而作为电致发光材料,最新《自然》报道,钙钛矿发光二极管的外量子效率突破了20%。并且器件可以实现光探测功能,能否把多重功能统一起来,即在一个器件上实现多功能,制备出兼具光伏、发光和光探测的钙钛矿多功能器件,使其能够敏感响应光信号,在太阳光照下高效发电,黑暗情况下低能耗发光,是一个极具意义的研究课题。
虽然钙钛矿太阳能电池和发光二极管具有类似的器件结构,但在工作条件下具有相反的光电转换过程。图2b和2c比较了太阳能电池(图2b)、发光二极管(图2c)的能带排布。太阳能电池采用的是交错式能带排列,即钙钛矿活性层的导带高于电子传输层的导带(最低非占有轨道),价带低于空穴传输层的价带(最高占有轨道),见图2b,这种能带结构有利于活性层中的光生载流子有效分离至电子传输层和空穴传输层。而对于发光二极管,能带排列采用的是跨越式排布,即钙钛矿活性层的导带低于电子传输层的导带(最低非占有轨道),价带高于空穴传输层的价带(最高占有轨道),见图2c,这种能带结构有利于电子传输层和空穴传输层向活性层中的注入电荷到钙钛矿活性层,在活性层实现辐射复合发光。对于光探测器,需要降低暗电流等。因此,从能带排布来看,这两种器件的能带排布要求是不太相同的。制备高光电转换效率、高发光效率和高探测灵敏度于一体的钙钛矿多功能器件成为了挑战。
发明内容
针对异质结结构的太阳能电池,发光二极管,光电探测器中,由于不同器件中各个功能层不同的能带排布方式,导致难以在同一器件上同时实现高性能的光伏,发光,光探测性能的问题,本发明旨在提出一种基于复合界面传输材料的钙钛矿光伏-发光-光探测多功能器件及其制备方法,通过能带工程消除钙钛矿活性层和传输层的势垒,设计得到如图2a所示的能带结构。该能带结构可以同时有效地提高钙钛矿多功能器件的光伏效率、发光效率和光探测灵敏度。
本发明的目的至少通过以下技术方案之一实现。
一种基于复合界面传输材料的钙钛矿的光伏-发光-光探测多功能器件,所述多功能器件包括从下至上依次层叠设置的透明导电玻璃、复合电子传输层、钙钛矿活性层、复合空穴传输层和金属电极层。
进一步的,所述透明导电电极层为ITO或FTO透明导电玻璃;具体的,透明导电电极的方块电阻为8~15Ω,透光率为85~90%,透明导电玻璃的厚度为1.1~2.2mm。
进一步的,所述金属电极层为金、银、铜或铝。具体通过热蒸镀的方法沉积在空穴传输层上,且其厚度为0.1~1000nm。
进一步的,所述复合电子传输层厚度为5~120nm,所述复合电子传输层为SnO2(Cl):GQDs或TiO2(Cl):GQDs薄膜,具体是包括氨基化的石墨烯量子点,且还包括氯盐制备的二氧化锡或的二氧化钛,且所述氯盐与氨基化的石墨烯量子点的质量比为10:1到1000:1。所述氯盐制备的二氧化锡或二氧化钛是部分Cl残留在SnO2或TiO2。且所述复合电子传输层的厚度为5-120nm。
进一步的,所述的钙钛矿活性层为CH3NH3PbX3、NH2CH2NH3PbX3或CsPbX3中一种或两种以上,且X为I或Br,其厚度为50~600nm。
进一步的,所述的复合空穴传输层为四[N,N-二(4-甲氧基苯基)氨基]-9,9'-螺二芴(spiro-OMeTAD)和2,7-二溴-9,9-双[3-(二甲氨基)丙基]芴(FN-Br)复合构成的spiro-OMeTAD:FN-Br,且spiro-OMeTAD与FN-Br的质量比为10-1000:1,且复合空穴传输层厚度为20~200nm。
进一步的,FN-Br可以被功函数大于5.4的TFB或F8BT取代。
本发明还提供了上述多功能器件的制备方法,包括以下步骤:
(1)透明导电玻璃的清洗
导电玻璃超声清洗,用氮气或者压缩空气将导电玻璃吹干,然后采用紫外光表面清洗处理去除有机物和增加成膜性;
(2)复合电子传输层的制备
制备二氯化锡、四氯化锡或四氯化钛制备前驱体溶液,然后加入氨基化的石墨烯量子点进行混合,将混合溶液旋涂在导电透明玻璃上,然后热处理,待冷却后进行紫外臭氧处理;所述紫外抽样处理形成悬挂键,可以增强后续成膜性;
(3)钙钛矿活性层的制备
将钙钛矿前驱体溶液旋涂在复合电子传输层上,在溶剂未干时滴加反型溶剂继续旋涂,将旋涂好的钙钛矿薄膜热处理;
(4)复合空穴传输层的制备
将spiro-OMeTAD和FN-Br混合溶液旋涂在钙钛矿活性层表面;
(5)金属电极的制备
在真空条件下,在复合空穴传输层上蒸镀金或银,得到所述基于钙钛矿的光伏-发光-光探测多功能器件。
进一步的,在步骤(1)中,导电玻璃依次在去离子水、洗洁精、丙酮、乙醇溶液中超声清洗5~10min,然后用氮气或者压缩空气将ITO或FTO导电玻璃吹干,采用紫外臭氧清洗机处理10~30min。
进一步的,步骤(2)中,具体是将混合溶液涂在导电透明玻璃基底上,转速为2000~5000rpm,旋涂时间为30~60s。最后,将旋涂好的薄膜放在加热台上180~270℃加热0.5~2h,待冷却后放入紫外臭氧中处理5~15min;混合溶液的溶剂为乙醇,且二氯化锡或四氯化锡的浓度为0.1%-10wt%,氨基化的石墨烯量子点的浓度为0.01~1wt%。
进一步的,步骤(3)中,将PbI2、NH2CH2NH3I(或者CH3NH3I等)和DMSO按1:1:1的摩尔比溶解在DMF溶液中,浓度为1.25~1.6mol/ml。溶解后,将钙钛矿前驱体溶液滴在复合电子传输层上,在3000~5000rpm下旋涂,在第20~25s时滴加100~1000μL的乙醚。将旋涂好的钙钛矿薄膜放在100~120℃的加热台上热处理5~30min。
进一步的,步骤(4)中,所述spiro-OMeTAD和FN-Br混合溶液是将spiro-OMeTAD和FN-Br粉末溶解于氯苯中,且spiro-OMeTAD的质量浓度为1~10wt%,FN-Br的质量浓度为0.01~1wt%。且旋涂条件为以3000~5000rpm转速旋涂35-60s。
进一步的,所述反型溶剂为甲苯、氯苯或乙醚。
本发明中的复合电子传输层、钙钛矿活性层和复合空穴传输层能带排布形成如图2a所示,其具体调控思路见图3,核心思路为利用功函数比较大的电子传输材料搭配功函数小的电子传输材料,得到和钙钛矿导带准费米能级拉平,消除复合电子传输层与钙钛矿发光层接触界面的电荷转移势垒,即使该接触界面电子转移势垒为零(见图3虚框),既可以向钙钛矿层注入电子又可以提取电子,其电子、空穴转移界面势垒为零,可以实现电荷注入和提取;还利用功函数比较大的空穴传输材料(如FN-Br)搭配功函数小的空穴传输材料(如spiro-OMeTAD),调整复合材料的功函数,使之与钙钛矿价带准费米能级拉平,消除复合空穴传输层与钙钛矿发光层接触界面的电荷转移势垒,即使该接触界面空穴转移势垒为零(见图3虚框),既可以向钙钛矿层注入空穴又可以提取空穴。这种由多种传输材料复合得到复合电子传输层和复合空穴传输层,搭配上钙钛矿活性层,获得高综合性能钙钛矿多功能器件,使器件形成了如图2a所示的接近电荷转移零势垒的能带结构排布,从而抑制了非辐射复合,最终大幅度提高了钙钛矿多功能器件的光电转换效率、发光效率和光探测性能。
与现有技术相比,本发明具有以下有益的技术效果:
和普通的钙钛矿太阳能电池和发光二极管相比,本发明的不同之处在于通过消除钙钛矿活性层和传输层之间的能带势垒,从而可以在外加电压下实现电荷注入到活性层,也可以在光照条件下实现从活性层提取电荷,制备出高光电转换效率、高发光效率、高探测灵敏度于一体的钙钛矿多功能器件。
关键技术在于利用复合电子/空穴材料实现能带调控,分别通过对多元电子传输材料和空穴传输材料进行掺杂复合,有效地调控电子传输层和空穴传输层的功函数,从而有效地消除了钙钛矿和传输层之间的界面势垒,抑制界面处的非辐射复合。经实验结果对比,能带调控后的钙钛矿多功能器件光电转换效率(20.45%)和发光效率(EQE,4.3%)都有了明显的提升。
附图说明
图1为本发明中基于复合界面传输材料的钙钛矿光伏-发光-光探测多功能器件的结构图;
图2a为本发明中钙钛矿多功能器件能带结构原理图;
图2b为太阳能电池的能带结构原理图;
图2c为发光二极管的能带结构原理图;
图3为本发明实施1例中所述的钙钛矿多功能器件结构和工作原理图;
图4为本发明实施1例中所述的钙钛矿多功能器件电子传输层和空穴传输层的能带图;
图5为本发明实施1例中所述的钙钛矿多功能器件在AM1.5光照下的I-V曲线图;
图6为本发明实施1例中所述的钙钛矿多功能器件在AM1.5光照下的光响应图。
具体实施方式
下面结合具体的实施例对本发明做进一步的详细说明,所述是对本发明的解释但不限于此。
实施例1
如图1所示,一种基于钙钛矿的光的光伏-发光-光探测多功能器件包括从下至上依次层叠的透明导电玻璃、复合电子传输层、钙钛矿活性层、复合空穴传输层和金属电极层。
所述基于钙钛矿的光的光伏-发光-光探测多功能器件的制备方法包括以下步骤:
(1)ITO玻璃的清洗:选择方块电阻为10Ω,透光率90%,厚度为1.1mm的ITO玻璃,将ITO导电玻璃依次在去离子水、洗洁精、丙酮、乙醇溶液中超声清洗5min,然后用氮气将ITO玻璃吹干,采用紫外臭氧清洗机处理20min。
(2)复合电子传输层的制备:将23mg的SnCl2·2H2O和0.4mg的氨基化石墨烯量子点溶解在1mL的乙醇溶液中(氨基化石墨烯量子点的浓度为0.05wt%,氯化亚锡的浓度为2.4wt%,二氯化锡与氨基化石墨烯量子点的质量比为190:4),溶解完全后将溶液旋涂在ITO基底上,转速为3000rpm,旋涂时间为30s。最后,将旋涂好的薄膜放在加热台上230℃加热1小时,待冷却后放入紫外臭氧中处理5min形成所述复合电子传输层,所述复合电子传输层的厚度为40nm;
(3)钙钛矿薄膜的制备:将PbI2、CH3NH3I和DMSO按1:1:1的摩尔比溶解在DMF中得到浓度为1.45mol/ml的钙钛矿前驱体溶液。待完全溶解后,将钙钛矿前驱体溶液滴在SnO2上。在1000rpm下旋涂10s后加速至5000rpm,在第20~22s时滴加600μL的乙醚。将旋涂好的钙钛矿薄膜放在100℃的加热台上热处理10min。
(4)复合空穴传输层的制备:将24mg spiro-OMeTAD、0.05mg FK209和1mg FN-Br粉末溶解于1mL的氯苯溶剂中(spiro-OMeTAD的质量浓度为2.1%,FN-Br的质量浓度为0.09%,spiro-OMeTAD与FN-Br的质量比为24:1,)。最后将spiro-OMeTAD混合溶液滴在钙钛矿薄膜表面,以3000rpm转速旋涂35s,所述复合空穴传输层的厚度为60nm;
(5)金属电极的制备:在1.0×10-3Pa的真空条件下,在spiro-OMeTAD薄膜上蒸镀金,制得厚度为100nm的金属电极;
完成上述步骤后得到所述基于钙钛矿的光的光伏-发光-光探测多功能器件。
在本实例中得到的钙钛矿多功能器件的性能如图4所示。图4中的(a)为复合电子传输层的能带图,图4中的(b)为复合空穴传输层的能带图,掺入氨基化石墨烯量子点后,SnO2电子传输层的功函数从4.45eV降低至4.25eV。掺入FN-Br后,spiro-OMeTAD的功函数从4.5eV提高至5.1eV。该多功能器件的光电效率反扫为21.54%,正扫为20.88%,如图所示5。优化前后器件的发光效率分别为0.2%和4.3%,如图6中的(a)所示,图6中的(b)为多功能器件的荧光发光谱,发光峰位为772nm。
实施例2
本实施例中,所用透明电极为FTO导电玻璃。其他步骤与实施例1相同,光电效率反扫为20.8%,正扫为20.2%。发光效率为1.8%。
实施例3
一种基于钙钛矿的光的光伏-发光-光探测多功能器件,其制备方法包括以下步骤:
(1)ITO玻璃的清洗:选择方块电阻为10Ω,透光率90%,厚度为1.1mm的ITO玻璃,将ITO导电玻璃依次在去离子水、洗洁精、丙酮、乙醇溶液中超声清洗5min,然后用氮气将ITO玻璃吹干,采用紫外臭氧清洗机处理20min。
(2)复合电子传输层的制备:将23mg的SnCl2·2H2O,0.5mg的氨基化的石墨烯量子点溶解在1mL的乙醇溶液中(氨基化石墨烯量子点的浓度为0.06wt%,氯化亚锡的浓度为2.4wt%,二氯化锡与氨基化石墨烯量子点的质量比为38:1),溶解完全后将溶液旋涂在ITO基底上,转速为3000rpm,旋涂时间为30s。最后,将旋涂好的薄膜放在加热台上200℃加热1小时,待冷却后放入紫外臭氧中处理5min,所述复合电子传输层的厚度为40nm;
(3)钙钛矿薄膜的制备:将PbI2、NH2CH2NH3I(或者CH3NH3I等)和DMSO按1:1:1的摩尔比溶解在DMF溶液中,浓度为1.45mol/ml。待溶液完全溶解后,将钙钛矿前驱体溶液滴在SnO2上。在1000rpm下旋涂10s后加速至5000rpm,在第20~22s时滴加600μL的乙醚。将旋涂好的钙钛矿薄膜放在100℃的加热台上热处理10min。
(4)复合空穴传输层的制备:将75mg spiro-OMeTAD,0.05mg FK209和2mg FN-Br粉末溶解于1mL的氯苯溶剂中(spiro-OMeTAD的质量浓度为6.3%,FN-Br的质量浓度为0.17%,spiro-OMeTAD与FN-Br的质量比为75:2)。最后将Spiro-OMeTAD混合溶液滴在钙钛矿薄膜表面,以3000rpm转速旋涂35s,所述复合空穴传输层的厚度为200nm;
(5)金属电极的制备:在1.0×10-3Pa的真空条件下,在spiro-OMeTAD薄膜上蒸镀金,制得厚度为100nm的金属电极;
完成上述步骤后得到所述基于钙钛矿的光的光伏-发光-光探测多功能器件。
在本实例中得到的钙钛矿多功能器件的光电效率反扫为20.7%,正扫为20.4%。发光效率为4.2%。
实施例4
本实施例中,SnO2的热处理温度为230℃。其他步骤与实施例3相同,在本实例中得到的钙钛矿多功能器件的光电效率反扫为21.1%,正扫为20.7%,发光效率为2.9%。
实施例5
本实施例中,将75mg spiro-OMeTAD,0.05mg FK209和0.75mg FN-Br粉末溶解于1mL的氯苯溶剂中(经计算,spiro-OMeTAD的质量浓度为6.3%,FN-Br的质量浓度为0.063%,spiro-OMeTAD与FN-Br的质量比为100:1)。其他步骤与实施例3相同,在本实例中得到的钙钛矿多功能器件的光电效率反扫为21.3%,正扫为20.1%,发光效率为2.2%。
实施例6
本实施例中,将10mg氨基化石墨烯量子点和100mg二氯化锡溶于1mL乙醇溶液中。将2mg FN-Br和100mg spiro-OMeTAD溶于1mL氯苯(计算得出氨基化石墨烯的浓度为0.01wt%,二氯化锡的浓度为0.1wt%,二氯化锡与氨基化石墨烯量子点的质量比为10:1,FN-Br的浓度为0.16wt%,spiro-OMeTAD的浓度为8.3wt%,且spiro-OMeTAD与FN-Br的质量比为50:1)。其他步骤与实施例3相同,在本实例中得到的钙钛矿多功能器件的光电效率反扫为20.4%,正扫为19.6%,发光效率为2.8%。
实施例7
本实施例中,将0.09mg氨基化石墨烯量子点和910mg二氯化锡溶于1mL乙醇溶液中,将12.3mgFN-Br和123mg spiro-OMeTAD溶于1mL氯苯(经计算,该实施例中氨基化石墨烯的浓度为0.01wt%,二氯化锡的浓度为10wt%,二者的质量比为1:1000,spiro-OMeTAD的浓度为10wt%,FN-Br的浓度为1wt%,二者的质量比为10:1),其他步骤与实施例3相同,在本实例中得到的钙钛矿多功能器件的光电效率反扫为20.1%,正扫为19.3%,发光外量子效率为2.1%。。
实施例8
本实施例中,将9mg氨基化石墨烯量子点和91mg二氯化锡溶于1mL乙醇溶液中,将0.123mg FN-Br和123mg spiro-OMeTAD溶于1mL氯苯(经计算,该实施例中氨基化石墨烯的浓度为1wt%,二氯化锡的浓度为10wt%,二者的质量比为1:10,spiro-OMeTAD的浓度为10wt%,FN-Br的浓度为0.01wt%,二者的质量比为1000:1),其他步骤与实施例3相同,在本实例中得到的钙钛矿多功能器件的光电效率反扫为19.8%,正扫为19.0%,发光效率为1.9%。
对比例1
本实施例中,在空穴传输层制备中不添加FN-Br,其他步骤与实施例1相同。所得到器件的性能结果见图5和6,光电效率反扫为17.4%,正扫为低于15%,发光效率仅为0.2%。
对比例2
本实施例中,在电子传输层制备中不添加石墨烯量子点,其他步骤与实施例1相同。所得到器件的性能结果见图5和6,光电效率反扫为20.2%,正扫为低于19.5%,发光效率仅为1.7%。
以上所述的具体实施例,对本发明的技术方案和有益效果进行了详细说明,所应理解的是,所述仅为本发明的具体实施例而已,并不用于限制本发明,凡在本发明精神和原则之内,所做的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。
Claims (9)
1.一种基于复合界面传输材料的钙钛矿的光伏-发光-光探测多功能器件,其特征在于,所述多功能器件包括从下至上依次层叠设置的透明导电电极层、复合电子传输层、钙钛矿活性层、复合空穴传输层和金属电极层。
2.如权利要求1所述多功能器件,其特征在于,所述透明导电电极层为ITO或FTO透明导电玻璃;所述金属电极层为金、银、铜或铝。
3.如权利要求1所述多功能器件,其特征在于,所述复合电子传输层厚度为5~120 nm,所述复合电子传输层材料为氨基化的石墨烯量子点,且还包括氯盐制备的二氧化锡或二氧化钛,且所述氯盐与氨基化的石墨烯量子点的质量比为10:1到1000:1。
4.如权利要求1所述多功能器件,其特征在于,所述钙钛矿活性层为CH3NH3PbX3、NH2CH2NH3PbX3或CsPbX3中一种或两种以上,且X为I或Br;所述钙钛矿活性层的厚度为50-600nm。
5.如权利要求1所述多功能器件,其特征在于,所述复合空穴传输层厚度为20~200 nm,且所述复合空穴传输层为spiro-OMeTAD和FN-Br复合构成的spiro-OMeTAD:FN-Br,且spiro-OMeTAD与FN-Br的质量比为10-1000:1。
6.如权利要求5所述多功能器件,其特征在于,所述复合空穴传输层材料中FN-Br被功函数大于5.4 eV的TFB或F8BT取代。
7.权利要求1-6任一项所述多功能器件的制备方法,其特征在于,包括以下步骤:
(1)透明导电玻璃的清洗
导电玻璃超声清洗,用氮气或者压缩空气将导电玻璃吹干,然后采用紫外光表面清洗处理去除有机物和增加成膜性;
(2)复合电子传输层的制备
将二氯化锡、四氯化锡或四氯化钛制备前驱体溶液,然后加入氨基化的石墨烯量子点进行混合,将混合溶液旋涂在导电透明玻璃上,然后热处理,待冷却后进行紫外臭氧处理,臭氧处理形成悬挂键可以增强后续成膜性;
(3)钙钛矿活性层的制备
将钙钛矿前驱体溶液旋涂在复合电子传输层上,在溶剂未干时滴加反型溶剂继续旋涂,将旋涂好的钙钛矿薄膜热处理;
(4)复合空穴传输层的制备
将spiro-OMeTAD和FN-Br的混合溶液旋涂在钙钛矿活性层表面;
(5)金属电极的制备
在真空条件下,在复合空穴传输层上蒸镀金或银,得到所述基于钙钛矿的光伏-发光-光探测多功能器件。
8.如权利要求7所述的制备方法,其特征在于,所述前驱体溶液中溶剂为乙醇,且二氯化锡或四氯化锡的浓度为0.1%-10wt%,氨基化的石墨烯量子点的浓度为0.01~1wt%;且步骤(2)中热处理为180~270 °C加热0.5~2 h,紫外臭氧处理5~15 min。
9.如权利要求7所述的制备方法,其特征在于,所述spiro-OMeTAD和FN-Br混合溶液是将spiro-OMeTAD和FN-Br粉末溶解于氯苯中,且spiro-OMeTAD的浓度为1~10wt%,FN-Br的浓度为0.01~1wt%。
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