CN109881212B - 一种有机金属卤化物钙钛矿光阳极的制备方法 - Google Patents
一种有机金属卤化物钙钛矿光阳极的制备方法 Download PDFInfo
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Abstract
本发明提供一种具有优异稳定性的有机金属卤化物钙钛矿光阳极的制备方法。所制备的钙钛矿光阳极可用于光电化学分解水产氧。该光阳极以钙钛矿材料为主体,并将商用的导电碳浆和导电银浆用丝网印刷的方法封装在外层以保护钙钛矿免受电解液侵蚀。在无其他助催化剂的辅助下,该光阳极表现出良好的分解水产氧能力并有超长的稳定性。本发明提供的有机金属卤化物钙钛矿光阳极制备方法简单,成本低廉,并易于大面积操作,有效的将钙钛矿材料的优异光伏性能应用于光电催化分解水中,适用于新型高性能光电催化光阳极的开发和生产。
Description
发明人:许林陶然
技术领域
本发明属于光电催化技术领域,涉及一种有机金属卤化物钙钛矿光阳极的制备方法。
背景技术
随着能源危机和环境污染问题的日益加剧,开发利用清洁新能源受到了全世界的广泛关注。光电催化分解水技术作为太阳能利用的主要手段之一,可以将目前最丰富的能源太阳能直接转化为清洁能源氢能,为人类利用太阳能缓解能源危机和环境污染问题提供了可能性。然而历经了四十余年的努力,光电催化分解水技术的太阳能转化效率仍然较低,达不到大规模产业化的程度,这主要是由于该技术手段的核心组成部件半导体材料在光电催化分解水应用方面存在着诸多缺点。开发利用光催化稳定性好、太阳光响应范围宽、光生电子-空穴对分离和传输效率高以及表面水分解反应动力学快速的半导体催化剂材料是解决这些问题的关键因素。
近些年,新一代半导体材料——有机金属卤化物钙钛矿(CH3NH3PbX3,X=Cl,Br,I)因其具有窄带隙,高光吸收系数,双极性载流子传输性质,较长的载流子传输距离等优点而备受关注。尤其是以钙钛矿材料为光敏剂的太阳能电池更是取得了迅猛的发展,在全世界光伏领域掀起了巨大的研究浪潮。但是CH3NH3PbX3遇水即分解的缺点使得其优异的光伏性能在光电催化分解水领域难以应用,因此,如何使CH3NH3PbX3光电极直接浸入电解液中进行光电催化分解水成为现如今的一大难题。
发明内容
本发明的目的是提供一种可以在水中稳定工作的有机金属卤化物钙钛矿光阳极的制备方法,此法克服了钙钛矿难以作为光电极在光电催化分解水领域应用的技术难题。应用此种方法可使得光阳极在无其他催化剂辅助下,在对应可逆氢电极的1.23V处获得12.4mA/cm2的稳定光电流。其中钙钛矿的化学式为:(5-AVA)x(MA)1-xPbI3,5-AVA为5-氨基戊酸,化学式为: NH2(CH2)4CO2H;MA为甲胺阳离子,化学式为:CH3NH3 +。
本发明提供的钙钛矿光阳极可通过如下方法制备:
(一)介孔骨架的合成:
以FTO导电玻璃作为电极基底,首先用去离子水、丙酮、乙醇分别对FTO进行超声清洗,后在FTO上旋涂浓度为0.3mol/L的钛酸四异丙酯的乙醇溶液(转速为2500rpm,时间为60s),后放入马弗炉450℃烧结30分钟形成TiO2致密层。在TiO2致密层上丝网印刷一层TiO2介孔层(丝印浆料为:P25:松油醇=1:16;丝印网板孔径为300目),后在马弗炉中450℃烧结30分钟。然后在TiO2介孔层上依次丝网印刷介孔ZrO2层和介孔碳层(ZrO2浆料为:纳米ZrO2:乙基纤维素:松油醇=2:1:10;丝印ZrO2层网板孔径为300目;碳层浆料为:8000 目石墨粉:纳米碳粉:乙基纤维素:松油醇=4:1:16),后在马弗炉中400℃烧结30分钟。
(二)填充钙钛矿:
首先配制钙钛矿前驱液:取0.63gPbI2、0.212gCH3NH3I、0.015g5-AVA溶于1.4mL丁内酯中,60℃搅拌20分钟即合成为钙钛矿前驱液。取4.5μL前驱液滴在介孔骨架的碳层上,静置2小时,使钙钛矿前驱液填充整个结构,后50℃烘干两小时,形成钙钛矿。
(三)钙钛矿光阳极的制备:
在上述的含有钙钛矿的介孔骨架上,直接用100目的丝印网板丝网印刷两层导电碳浆(深圳东大来公司),而后80℃烘干20分钟,而后将约40μL的导电银胶(南京创益优电子科技公司)均匀地涂抹在之前印刷的导电碳浆上,而后50℃烘干30分钟。取用二甲酸酯稀释的导电碳浆约30μL涂抹在导电银浆之上,后80℃烘干20分钟。最后用环氧树脂对电极的四周进行封边处理,随即光阳极制备完成。
上述钙钛矿光阳极的结构示意图和制备过程示意图见附图1和附图2。钙钛矿的结构通过X射线粉末衍射(见附图3)进行表征。可以发现,在XRD谱图中,所合成的钙钛矿与标准钙钛矿的峰位置和峰强度均一致,这证明了用上述方法合成的材料确实为钙钛矿。此外,通过扫描电子显微镜的截面图像确定了该电极各层的厚度(见附图4a,附图4b),同时,通过扫面电子显微镜图像探究导电银浆层和导电碳浆层的微观平面形貌(见附图4c,附图4d)。
本发明提供的钙钛矿光阳极在光电化学分解水中的应用,其工作条件如下:
将制备好的钙钛矿光阳极用导线连接到电化学工作站的工作电极上,饱和甘汞电极作为参比电极,铂丝作为对电极,组成三电极系统(见附图1)。在工作电极和对电极之间施加可变的电压,在氙灯模拟自然光的照射下,测得随电压可变的光电流值。在光阳极表面和铂丝电极上均有气泡产生。
本发明中提供的钙钛矿光阳极具有以下特点:
1、该光阳极制备方法简单,主要使用可大面积操作得丝网印刷技术,并且电极构造不需要昂贵的空穴传输材料以及贵金属助催化剂。
2、该光阳极光电性能出色,在1.23V得光电流密度达到12.4mA/cm2,通过引入导电银胶(缩写为SC)在不影响性能的前提下能显著提高光阳极耐水性能,使其可连续工作12小时以上,并能在碱性电解液中可存放48小时以上。
附图说明
图1是钙钛矿光阳极的结构示意图以及所处三电极系统示意图。
图2是钙钛矿光阳极制作过程示意图。
图3是钙钛矿以及二氧化钛X射线粉末衍射图。
图4是钙钛矿光阳极的扫描电镜图。
图5是钙钛矿光阳极的光电性能测试以及电极表面析氧照片。
图6是钙钛矿光阳极的稳定性测试。
具体实施方式
为了进一步说明本发明,列举下列实施实例,但它并不限制各附加权利要求所定义的发明范围。
具体实施例1:
将该钙钛矿光阳极作为工作电极,与参比电极和对电极组成三电极系统。以1M氢氧化钾溶液为电解质,测试了光阳极得光电性能,并对比了导电银浆对其性能的影响(见附图5)。在偏压为1.23V时拍摄了光阳极表面析出氧气的照片(见附图5d)
具体实施例2:
为测试该钙钛矿光阳极得稳定性,我们分别将光阳极置于酸性、碱性、中性电解质溶液中进行长时间的光电流测试,偏压设为1.23V。测试结果见附图6,结果表明在不同电解质溶液中,该光阳极均有较好的工作稳定性。
Claims (2)
1.一种有机金属卤化物钙钛矿光阳极,其特征在于:具有光电催化氧化性能和良好的稳定性;
所述有机金属卤化物钙钛矿化学式为(5-AVA)x(MA)1-xPbI3,5-AVA为5-氨基戊酸,化学式为:NH2(CH2)4CO2H;MA为甲胺阳离子,化学式为:CH3NH3 +;
所述光阳极的构成材料为FTO导电玻璃,TiO2,有机金属卤化物钙钛矿,ZrO2,导电碳浆,导电银胶;
所述有机金属卤化物钙钛矿光阳极的制备方法如下:
(一)介孔骨架的合成:
以FTO导电玻璃作为电极基底,首先用去离子水、丙酮、乙醇分别对FTO进行超声清洗,后在FTO上旋涂浓度为0.3mol/L的钛酸四异丙酯的乙醇溶液,转速为2500rpm,时间为60s,后放入马弗炉450℃烧结30分钟形成TiO2致密层;在TiO2致密层上丝网印刷一层TiO2介孔层,丝印浆料为:P25:松油醇=1:16;丝印网板孔径为300目,后在马弗炉中450℃烧结30分钟;然后在TiO2介孔层上依次丝网印刷介孔ZrO2层和介孔碳层,ZrO2浆料为:纳米ZrO2:乙基纤维素:松油醇=2:1:10;丝印ZrO2层网板孔径为300目;碳层浆料为:8000目石墨粉:纳米碳粉:乙基纤维素:松油醇=4:1:16,后在马弗炉中400℃烧结30分钟;
(二)填充钙钛矿:
首先配制钙钛矿前驱液:取0.63gPbI2、0.212gCH3NH3I、0.015g5-AVA溶于1.4mL丁内酯中,60℃搅拌20分钟即合成为钙钛矿前驱液;取4.5μL前驱液滴在介孔骨架的碳层上,静置2小时,使钙钛矿前驱液填充整个结构,后50℃烘干两小时,形成钙钛矿;
(三)钙钛矿光阳极的制备:
在上述的含有钙钛矿的介孔骨架上,直接用100目的丝印网板丝网印刷两层导电碳浆,而后80℃烘干20分钟,而后将40μL的导电银胶均匀地涂抹在之前印刷的导电碳浆上,而后50℃烘干30分钟;取用二甲酸酯稀释的导电碳浆30μL涂抹在导电银浆之上,后80℃烘干20分钟;最后用环氧树脂对电极的四周进行封边处理,随即光阳极制备完成。
2.按照权利要求1所述的有机金属卤化物钙钛矿光阳极,其特征在于:该电极与电解质水溶液直接接触,用于水溶液中的光电催化氧化反应。
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