CN114400263B - 一种基板负载卤化氧铋/硫化铋纳米片异质结器件的制备方法及应用 - Google Patents
一种基板负载卤化氧铋/硫化铋纳米片异质结器件的制备方法及应用 Download PDFInfo
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Abstract
本发明公开了一种基板负载BiOX/Bi2S3(X＝I、Br、Cl)纳米片异质结器件的制备方法及应用，属于光电材料技术领域。包括以下步骤：将负载氧化物层的基板放入含有卤化铋、硫源和N,N‑二甲基甲酰胺溶剂的混合体系中，进行沉积反应，得所述基板负载BiOX/Bi2S3纳米片异质结器件。所得BiOX/Bi2S3纳米片异质结能够吸收整个可见光，提升材料的可见光捕集能力，通过后续简易的电池组件空穴层组装，在太阳能电池器件中具有良好的应用前景。
Description
技术领域
本发明属于光电材料技术领域，具体涉及一种基板负载BiOX/Bi2S3(X＝I、Br、Cl)纳米片异质结器件的制备方法及应用。
背景技术
目前，面对能源危机及环境污染，太阳能作为一种可再生能源是满足全球范围内日益增长的能源需求的重要方法之一。太阳能电池是基于材料的光生伏特效应将太阳能转换为电能从而有效利用太阳能的一种有效技术。
太阳能电池依据发展历程主要可以分为晶硅太阳电池，薄膜太阳电池和新型太阳电池三类。其中，晶硅太阳电池可分为单晶硅和多晶硅太阳电池，薄膜太阳电池主要为碲化镉和铜铟镓硒太阳电池等；新型太阳能电池主要有染料敏化和钙钛矿太阳电池。值得关注的是，新型电池中的钙钛矿太阳电池(Perovskite Solar Cells，简写为PSCs)以其低成本、高效率、可液相制备、原料来源丰富等优点从众多的光伏器件中脱颖而出，已经超过了很多经过多年发展的其他类型太阳能电池，但因钙钛矿结构对湿度及温度的敏感性，并且使用大量的有毒Pb源使是制约其进一步发展的最大原因。因此，研发高效、低成本、无毒的新型太阳电池是实现太阳能光伏发电广泛应用的必要技术基础。
卤化铋(BiOX，X＝Cl\Br\I)材料具有无毒、成本低、水介质中耐腐蚀、化学稳定性好、地球丰度高等特点，被广泛用于水净化领域和光催化领域。且BiOX属于四方晶系，为典型多组分V–VI–VII分层结构半导体，具有独特的层状晶体结构，具有良好的载流子传输特性。其中，带隙为1.9eV的BiOI，因其合适的带隙，独特的层状结构，在可见光照射下表现出明显的可见光响应，有望做太阳能电池中的光吸收材料。但在太阳能领域，BIOI的带隙对可见光的响应仍然较弱，且BiOI具有一定的光分解性，限制了其在太阳能电池的应用。而构建异质结亦是一种行之有效的改性方法。通过在Bi基材料中负载S元素，可形成一定的Bi2S3，使其形成的BiOI/Bi2S3异质结材料既能保持原有各个单体材料的特性，提升BiOI材料对可见光的吸收范围，增强BiOI材料的稳定性，亦能促进异质结材料中的光生载流子的分离和传输。
中国专利申请CN201410022942.X公开了一种BiOI/Bi2S3异质结薄膜及柔性光电化学太阳能电池器件。所述的BiOI/Bi2S3异质结薄膜呈膜状，由生长在ITO/PET柔性基底上的相互交错的纳米片状结构的BiOI和分散在纳米片状BiOI表面和边缘上的纳米球状Bi2S3组成，所述BiOI纳米片的厚度为10-40nm，所述Bi2S3的粒度为10-200nm。该专利先制备BiOI层、待烘干后再制备Bi2S3层，耗时长、制备相对麻烦。
有鉴于此，本发明基于负载一层氧化物的导电玻璃为基板，利用低温水热方法，通过成本经济的卤化铋、硫源和N,N-二甲基甲酰胺溶剂直接反应一步得到BiOX/Bi2S3纳米片异质结器件。所得BiOX/Bi2S3纳米片异质结能够吸收整个可见光，提升材料的可见光捕集能力，通过后续简易的电池组件空穴层组装，可作为太阳能电池器件应用。
发明内容
本发明的目的是提供一种基板负载BiOX/Bi2S3纳米片异质结器件的制备方法及应用，此制备方法可一步得到BiOX/Bi2S3纳米片异质结器件，可重复性高，应用在太阳能电池器件中具有良好的性能。
为实现上述发明目的，本发明技术方案如下：
一方面，本发明提供一种基板负载BiOX/Bi2S3纳米片异质结器件的制备方法，包括以下步骤：
将负载氧化物层的基板放入含有卤化铋、硫源和溶剂的混合体系中，进行沉积反应，得所述基板负载BiOX/Bi2S3纳米片异质结器件。
其中，X＝I、Br、Cl。
优选地，所述氧化物层选自ZnO2、TiO2、SnO2中的至少一种。
优选地，所述基板为FTO导电玻璃、ITO导电玻璃、白玻璃中的任一种，本发明中优选为FTO导电玻璃。
术语“FTO导电玻璃”是指：掺杂氟的SnO2导电玻璃。
优选地，所述负载氧化物层的基板可按照以下方式制备：
通过旋涂法把氧化物凝胶颗粒旋涂在基板上，煅烧得负载氧化物层的基板。
优选地，所述沉积反应在反应釜中进行。
优选地，所述负载氧化物层的基板放反应釜中时，负载氧化物面的基板朝下或者垂直于反应釜壁。
优选地，所述卤化铋选自碘化铋、氯化铋、溴化铋中的至少一种，进一步优选为碘化铋。
优选地，所述硫源选自硫代乙酰胺、硫脲、单质硫中的至少一种，进一步优选为硫代乙酰胺。
所述溶剂选自N,N-二甲基甲酰胺、二甲基亚砜、吡啶、中的至少一种，本发明中优选N,N-二甲基甲酰胺。
优选地，卤化铋在溶剂中的浓度为0.1-100mg/mL，硫源中S元素含量为卤化铋中Bi元素的0.1-1.5倍。
优选地，所述沉积反应的反应温度为120-200℃，反应时间为0.5-12h。
优选地，所述混合体系中还包括添加剂，所述添加剂为聚乙烯吡咯烷酮(PVP)。
优选地，所述添加剂的添加量为0-1mol/ml。
优选地，上述负载氧化物面的基板在没有硫源情况下，只在卤化铋和N,N-二甲基甲酰胺溶剂两种物质中，通过上述反应温度为120-200℃，反应时间为0.5-12h条件下，可以一步反应得到BiOX纳米片结构。
另一方面，本发明提供上述基板负载BiOX/Bi2S3纳米片异质结器件在太阳能电池、含发光器件产品、催化领域、医学领域中的应用，但不局限于此领域应用。
最后，本发明提供一种太阳能电池，包括上述BiOX/Bi2S3纳米片异质结器件。
作为本申请的一个具体实施例，所述太阳能电池器件按照以下方法制备：
将所述BiOI/Bi2S3纳米片异质结器件用乙醇冲洗，120-200℃干燥处理，后续旋涂空穴传输材料形成空穴层，随后蒸镀Au电极进行完整器件组装，得太阳能电池。
本发明的有益效果为：
(1)BiOX/Bi2S3纳米片异质结材料的合成，拓宽了相应BiOX的可见光的吸收范围，增强了BiOX单体的稳定性。
(2)BiOX/Bi2S3纳米片异质结材料的合成具有工艺简单，耗能低，原料成本经济等特点，通过相应卤化铋、硫源、和N,N-二甲基甲酰胺溶剂，利用一步低温水热就可以合成。
(3)BiOX/Bi2S3纳米片异质结材料的方法具有普适性。由于各BiOX(X＝Cl\Br\I)间均具有相似的层状晶体结构，因此很容易通过改变卤素原X-的种类及含量对其能带结构进行精准调控。
(4)FTO导电玻璃负载BiOX/Bi2S3纳米片异质结材料器件应用方式多样且简单，通过后续简单的电池空穴层的旋涂和电极蒸镀，就可作为太阳能电池器件应用在能源领域。
附图说明
图1为实施例1所制备的BiOI纳米片的SEM图片；
图2是实施例2所制备的BiOI纳米片的SEM图片；
图3是实施例1和2所制备的BiOI/TiO2/FTO和BiOI/ZnO2/FTO结构器件的吸收图谱；
图4是实施例3所制备的BiOI//Bi2S3器件上表面的SEM图片和元素Mapping图片；
图5是实施例3所制备的BiOI//Bi2S3器件的吸收图谱；
图6是对比例1所制备的样品的SEM图片；
图7是实施例3所制备的BiOI//Bi2S3太阳能电池器件在反扫模式下的电流电压曲线图。
具体实施方式
以下非限制性实施例可以使本领域的普通技术人员更全面的理解本发明，但不以任何方式限制本发明。下述内容仅仅是对本申请要求保护的范围的示例性说明，本领域技术人员可以根据所公开的内容对本申请的发明作出多种改变和修饰，而其也应当属于本申请要求保护的范围之中。
本文所公开的“范围”以下限和上限的形式。可以分别为一个或多个下限，和一个或多个上限。给定范围是通过选定一个下限和一个上限进行限定的。选定
的下限和上限限定了特别范围的边界。所有可以这种方式进行限定的范围是包含和可组合的，即任何下限可以与任何上限组合形成一个范围。例如，针对特定参数列出了60-120和80-110的范围，理解为60-110和80-120的范围也是预料到的。此外，如果列出的最小范围值1和2，和如果列出了最大范围3，4和5，则下面的范围可全部预料到：1-2、1-4、1-5、2-3、2-4和2-5。
本发明中，除非有其他说明，数值范围“a-b”表示a到b之间的任意实数组合的缩略表示，其中a和b都是实数。例如数值范围“0-5”表示本文中已经全部列出了“0-5”之间的全部实数，“0-5”只是这些数值组合的缩略表示。
在本发明中，如果没有特别的说明，本文所提到的所有实施方式以及优选实施方式可以互相组合形成新的技术方案。
下面以具体实施例的方式对本发明作进一步的说明。本发明实施例中所使用的各种化学试剂如无特殊说明均通过常规商业途径获得。
实施例1
以TiO2/FTO基板为衬底，BiOI/TiO2/FTO纳米片器件的制备：
步骤一、利用钛酸异丙酯乙醇溶液旋涂在FTO上，马弗炉煅烧450℃、60min形成TiO2/FTO基板。
步骤二、称量235.75mg的BiI3溶解在20mL的N,N-二甲基甲酰胺(DMF)溶剂中，形成BiI3溶液，上述制备的TiO2/FTO基板放入含有BiI3溶液的反应釜中，160℃下反应2h，得到BiOI/TiO2/FTO纳米片器件。
图1为所制备的BiOI/TiO2/FTO器件上表面的SEM图片。可以看出，BiOI在TiO2/FTO基板上，呈现规则的纳米片结构。
实施例2
以ZnO2/FTO基板为衬底，BiOI/ZnO2/FTO纳米片器件的制备：
步骤一、ZnO2/FTO基板的制备
首先制备ZnO种子溶液：称量2.95g的无水醋酸锌，溶解在125mL无水乙醇中，65℃加热搅拌溶解，然后滴加KOH的乙醇溶液，搅拌20min，得到透明的种子溶液；
随后利用旋涂工艺，把ZnO溶液旋涂在清洗好的FTO玻璃上(2000的转速，20s)，125℃加热5min，重复三次。然后把有ZnO的FTO基板放入含有硝酸锌和六亚甲基四胺的水溶剂反应釜中(60mL的水溶液中含有535.48mg的硝酸锌及252.34mg的六亚甲基四胺)，90℃反应3h，得到ZnO2纳米棒的FTO基板，简称ZnO2/FTO基板。
步骤二、以ZnO2/FTO基板为衬底，BiOI/ZnO2/FTO纳米片器件的制备
称量235.75mg的BiI3溶解在20mL的N,N-二甲基甲酰胺(DMF)溶剂中，形成BiI3溶液，上述制备的ZnO2/FTO基板放入含有BiI3溶液的反应釜中，160℃下反应2h，得到BiOI/ZnO2/FTO器件。
图2为所制备的BiOI/ZnO2/FTO器件上表面的SEM图片。可以看出，BiOI在ZnO2/FTO基板上，呈现规则的纳米片结构。
图3是以ZnO2/FTO和TiO2/FTO基板为衬底，对应制备的BiOI/ZnO2/FTO和BiOI/TiO2/FTO器件的吸收图谱。可以看出，BiOI/ZnO2/FTO结构器件的在可见光的吸收范围高于BiOI/TiO2/FTO结构。
实施例3
步骤一、按照实施例2方法制备ZnO2/FTO基板。
步骤二、ZnO2/FTO基板为衬底，BiOI//Bi2S3纳米片器件的制备
称量30.05mg的硫代乙酰胺，235.75mg的BiI3溶解在20mL的N,N-二甲基甲酰胺(DMF)溶剂中，形成含有硫源的BiI3溶液，上述制备的ZnO2/FTO基板放入含有硫源的BiI3溶液反应釜中，160℃下反应2h，得到BiOI//Bi2S3异质结器件。
图4是以ZnO2/FTO基板为衬底，所制备的BiOI//Bi2S3器件上表面的SEM图片和元素Mapping图片。可以看出，BiOI//Bi2S3呈现规则的纳米片结构，硫源均匀分布在纳米片上，且硫源的添加并没有改变原始BiOI纳米片的结构形貌。
图5是以ZnO2/FTO基板为衬底，所制备的BiOI//Bi2S3器件的吸收图谱。可以看出，异质结的形成，使其BiOI//Bi2S3材料的吸收覆盖整个可见光。
对比例1
FTO玻璃为衬底，BiOI//Bi2S3纳米片器件的制备：
称量30.05mg的硫代乙酰胺，235.75mg的BiI3溶解在20mL的N,N-二甲基甲酰胺(DMF)溶剂中，形成含有硫源的BiI3溶液，上述FTO玻璃放入含有硫源的BiI3溶液反应釜中，160℃下反应2h，得到BiOI//Bi2S3异质结器件。
图6是以FTO基板为衬底，所制备的BiOI//Bi2S3器件上表面的SEM图片。可以看出，基板表面形貌没有呈现纳米片结构，说明BiOI//Bi2S3材料没有成功负载在基板上。
应用例
太阳能电池的制备：
上述合成的BiOI//Bi2S3纳米片器件，经过旋涂有机空穴材料(2,2',7,7'-四[N,N-二(4-甲氧基苯基)氨基]-9,9'-螺二芴简称Spiro-OMeTAD，或3-己基取代聚噻吩简称P3HT)，形成空穴层，随后蒸镀金电极(80nm厚度)，装配成太阳能电池。通过太阳光模拟器，在100mW cm-2标准光的照射下，反扫模式下测试光电转化效率，结果见图7和表1。电池的有效面积为0.0625cm2。
表1.
可以看出，相应的FTO/ZnO2/BiOI/Bi2S3/P3HT/Au纳米器件相对FTO/ZnO2/BiOI/P3HT/Au提高了太阳能电池的性能；通过改变相应的P3HT空穴传输层，FTO/FTO/ZnO2/BiOI/Bi2S3/Spiro-OMeTAD/Au结构的电池性能的效率进一步提升。
以上所述仅为本发明的较佳或者具体的应用实施例而已，并不用以限制本发明的实际应用领域，凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。
Claims (10)
1.一种基板负载BiOI/Bi2S3纳米片异质结器件的制备方法，其特征在于，包括以下步骤：
将负载氧化物层的基板放入含有BiI3、硫源和N,N-二甲基甲酰胺溶剂的混合体系中，进行沉积反应，得所述基板负载BiOI/Bi2S3纳米片异质结器件；
其中，所述BiI3在所述溶剂中的浓度为0.1-100mg/mL，所述硫源中S元素的含量为所述BiI3中Bi元素的0.1-1.5倍；所述沉积反应的反应温度为120-200℃，反应时间为0.5-12h。
2.根据权利要求1所述的制备方法，其特征在于，所述氧化物层选自ZnO2、TiO2、SnO2中的至少一种；所述基板为FTO导电玻璃、ITO导电玻璃、白玻璃中的任一种。
3.根据权利要求1所述的制备方法，其特征在于，所述负载氧化物层的基板按照以下方式制备：通过旋涂法把氧化物凝胶颗粒旋涂在基板上，煅烧得负载氧化物层的基板。
4.根据权利要求1所述的制备方法，其特征在于，所述沉积反应在反应釜中进行。
5.根据权利要求4所述的制备方法，其特征在于，所述沉积反应在反应釜中进行具体为：负载氧化物层的基板放反应釜中时，负载氧化物面的基板垂直于反应釜壁。
6.根据权利要求1所述的制备方法，其特征在于，所述硫源选自硫代乙酰胺、硫脲、单质硫中的至少一种。
7.根据权利要求1所述的制备方法，其特征在于，所述混合体系中还包括添加剂，所述添加剂为聚乙烯吡咯烷酮。
8.权利要求1-7任一项所述制备方法制备的基板负载BiOI/Bi2S3纳米片异质结器件，在太阳能电池、含发光器件产品、催化领域、医学领域中的应用。
9.一种太阳能电池，其特征在于，包括权利要求1-7任一项所述制备方法制备的基板负载BiOI/Bi2S3纳米片异质结器件。
10.根据权利要求9所述的一种太阳能电池，其特征在于，所述太阳能电池按照以下方法制备：
将所述BiOI/Bi2S3纳米片异质结器件用乙醇冲洗，120-200℃干燥处理，后续旋涂空穴传输材料形成空穴层，随后蒸镀Au电极进行完整器件组装，得太阳能电池。
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