CN110904474A - 一种金属铟修饰的硅光电阴极薄膜制备方法和应用 - Google Patents
一种金属铟修饰的硅光电阴极薄膜制备方法和应用 Download PDFInfo
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- PSCMQHVBLHHWTO-UHFFFAOYSA-K Indium trichloride Inorganic materials Cl[In](Cl)Cl PSCMQHVBLHHWTO-UHFFFAOYSA-K 0.000 claims abstract description 9
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Abstract
本发明公开了一种金属铟修饰的硅光电阴极薄膜制备方法，将硅片依次置于有机溶剂清洗剂和去离子水中超声清洗30±10分钟，其后将硅片放入10±5％氢氟酸水溶液中刻蚀20‑100秒备用；2)将金属铟盐In(NO3)3·4H2O或InCl3溶解于1±0.3M NaNO3溶液中，制得0.02M的In(NO3)3·4H2O或InCl3溶液，用于光辅助硅光电极的电沉积；将清洗好的硅片与电化学工作站连接，在‑1.0V(vs.SCE)电位下，通过紫外可见光照30±10秒，得到金属铟修饰的硅光电阴极薄膜。该法制备得到的金属铟修饰的硅光电阴极薄膜在光电催化水分解、二氧化碳还原等领域具有较大应用潜力。
Description
技术领域
本发明属于半导体材料技术领域，具体涉及一种金属铟修饰的硅光电阴极薄膜及其制备方法
背景技术
二十一世纪以来化石燃料燃烧引发的环境污染、温室效应和能源短缺等问题已成为人类社会向前发展的严峻阻力。因此，开发环境友好和可持续的新型能源替代传统的化石燃料已成为人类社会急需解决的重大挑战。取之不尽用之不竭的太阳能被认为是最有可能取代化石燃料的清洁能源。利用太阳能光电催化进行水分解和二氧化碳，将可再生的太阳能转化为化学能的同时减缓温室效应并能够有效解决环境污染问题。
硅在地壳中含量丰富，极具低成本优势。其带隙为1.12ev，完全满足可见光吸收对带隙的要求，其导带位置也满足光解水制氢和二氧化碳还原及多种污染物降解的需求。此外，目前硅的提纯和制备技术已相对成熟，现已被广泛应用于太阳能光伏产业中。硅的优质特性迎合了光电催化对半导体材料的需要，这也使得硅成为光电化学体系中一种非常有前景的半导体材料。
虽然硅光电阴极具有低成本和带隙合适等优势，但利用硅光电阴极进行水分解、二氧化碳还原和污染物降解存在低的反应活性、选择性和法拉第效率等问题。为了解决硅光电阴极半导体的此类问题。本发明提出了一种对金属铟溶液具有普适性的光辅助电沉积(光电沉积)的方法，通过此法能够得到金属铟修饰的硅光电阴极薄膜。光电沉积金属的反应原料采用少量或微量的金属溶液即可，在不同偏压的条件下，可以稳定的生成从纳米至微米等不同大小的金属颗粒。光电沉积相对于原子层沉积和真空离子溅射或者化学气相沉积具有低成本，反应条件温和，可调控等诸多优势。此外硅光电阴极和金属颗粒优异的界面性能将有助于快速输导电子，使得光生电子和空穴能够有效的分离和转移，进而能够显著提高硅光电阴极的光电性能。此发明制备得到的金属铟修饰的硅光电阴极薄膜在光电催化分解水产氢、二氧化碳还原等领域具有较大应用潜力。
发明内容
本发明的目的是，提出了一种对各种金属铟溶液具有普适性的光辅助电沉积于硅光电阴极薄膜上的方法，通过此法能够在温和条件下，低成本的得到金属铟修饰的硅光电阴极薄膜。硅光电阴极和金属颗粒优异的界面性能将有助于快速输导电子，使得光生电子和空穴能够有效的分离和转移，进而能够显著提高硅光电阴极的光电性能。此发明制备得到的金属铟修饰的硅光电阴极薄膜在光电催化分解水产氢、二氧化碳还原和污染物降解等领域具有较大应用潜力。
本发明目的的技术解决方案是：一种金属铟修饰硅光电阴极薄膜的方法，步骤为：
1)将硅片依次置于有机溶剂清洗剂和去离子水中超声清洗30±10分钟，其后将硅片放入10±5％氢氟酸水溶液中刻蚀20-100秒备用；
2)将金属铟盐In(NO3)3·4H2O或InCl3溶解于1±0.3M NaNO3溶液中，制得0.02M的In(NO3)3·4H2O或InCl3溶液，用于光辅助硅光电极的电沉积；
3)将清洗好的硅片与电化学工作站连接，在-1.0V(vs.SCE)电位下，通过紫外可见光照30±10秒，得到金属铟修饰的硅光电阴极薄膜。
所述步骤(1)中的有机溶剂清洗剂包括但不限于丙酮、乙醇以及甲醇等。
用于沉积的金属铟盐溶液包括但不限于In(NO3)3·5H2O，InCl3等。
光辅助电沉积过程应处于室温和光强稳定的条件下进行。
制备得到的金属铟修饰的硅光电阴极薄膜在光电催化水分解、二氧化碳还原反应中的应用。
有益效果：此发明制备得到的金属铟修饰的硅光电阴极薄膜在光电催化分解水产氢、二氧化碳还原和污染物降解等领域具有较大应用潜力。如图6所示，不含金属铟的硅光电阴极薄膜的二氧化碳还原光电流和斩波电流均明显低于含金属铟修饰的硅光电阴极薄膜的二氧化碳还原光电流和斩波电流。如图7所示，通过此法担载的金属铟修饰的硅光电阴极薄膜，相对于于在氩气环境下，在二氧化碳环境中具有高的光电流和斩波电流，表明，该材料具有高的二氧化碳还原性能。同时，该金属铟修饰的硅光电阴极薄膜在氩气中的光电流来自于水分解制氢表明该材料就有高的水分解制氢性能。如图8所示，在紫外可见光照射下，将此金属铟修饰的硅光电阴极薄膜在不同偏压下进行两小时的二氧化碳还原反应。二氧化碳还原电流随偏压的增加而增大。在-1VRHE偏压下，具有超过16mA cm-2的光电流。如图9，10,11所示，将此金属铟修饰的硅光电阴极薄膜在不同偏压下进行两小时的二氧化碳还原反应。在-1VRHE偏压下，两小时的反应产生了超过180μmol cm-2的甲酸，300μmol cm-2的氢气，6μmol cm-2的一氧化碳，能明显超过无金属铟的硅光电阴极。
附图说明
图1为金属铟修饰的硅光电阴极薄膜结构示意图；
图2为金属铟修饰的硅光电阴极薄膜扫描电镜图；
图3为金属铟修饰的硅光电阴极薄膜的XRD特征峰；
图4为金属铟修饰的硅光电阴极薄膜的硅的XPS特征峰；
图5为金属铟修饰的硅光电阴极薄膜的铟的XPS特征峰；
图6为不含金属铟和含金属铟修饰的硅光电阴极薄膜的二氧化碳还原光电流对比图
图7为金属铟修饰的硅光电阴极薄膜的二氧化碳还原光电流对比图；
图8为金属铟修饰的硅光电阴极薄膜在不同电位下二氧化碳还原电流值；
图9为金属铟修饰的硅光电阴极薄膜在不同电位下将二氧化碳还原为甲酸的产物时间图；
图10为金属铟修饰的硅光电阴极薄膜在不同电位下将水分解分氢气的产物时间图；
图11为金属铟修饰的硅光电阴极薄膜在不同电位下将二氧化碳还原为一氧化碳的产物时间图。
具体实施方式
以下结合附图本对发明做进一步详细描述。通过下面的实施例可以使本专业技术人员更全面地理解本发明。以下以金属铟修饰的硅光电阴极薄膜的制备和应用为例，将有助于相关领域的技术工作人员进一步理解本发明，但不以任何形式限制本发明。同时，这里指出对本领域的普通技术人员来说，本发明中的数据只针对本发明，在不脱离本发明构思的前提下，合理地若干调整和改进，都属于本发明的保护范围。
基本制备参数:
1)将硅片依次置于有机溶剂清洗剂和去离子水中超声清洗30分钟，其后将硅片放入10％氢氟酸水溶液中刻蚀1分钟备用；
2)将包括但不限于种类的金属铟盐In(NO3)3·4H2O，InCl3溶解于1M NaNO3溶液中，制得0.02M的目标金属盐溶液用于光辅助电沉积；
3)将清洗好的硅片与电化学工作站连接，在-1.0V(vs.SCE)电位下，通过紫外可见光照30秒，得到金属铟修饰的硅光电阴极薄膜。
有机溶剂清洗剂包括但不限于丙酮、乙醇以及甲醇等。
光辅助电沉积过程应处于室温和光强稳定的条件下进行。
制备得到的金属铟修饰的硅光电阴极薄膜在光电催化水分解、二氧化碳还原反应中的应用。
实施例1
用玻璃刀将硅片切割为面积大小1*1.5cm的样品，用硅胶将硅片背面导电银胶进行封装，再将封装好的硅片样品依次置于丙酮、乙醇溶液和去离子水中超声清洗30分钟，其后将硅片放入10％氢氟酸水溶液中刻蚀1分钟，将刻蚀完成后的硅片置于氮气保护气氛下备用。
实施例2
根据薄膜的应用目的选择某种金属盐溶液溶解于1M NaNO3溶液中，制得0.02M的目标金属盐溶液用于光辅助电沉积。以金属铟溶液为例，称量8.4995g NaNO3溶解于100ml去离子水中，待固体完全溶解后加入0.7817g In(NO3)3·5H2O充分混合。将制备得到的100ml沉积溶液密封备用。
实施例3
将实施例2中的金属铟溶液倒入标准光电化学池中。将实施例1中得到的硅片连接到电化学工作站阴极，对电极阳极采用面积大小为2*3cm的铂片电极，参比电极选用饱和甘汞电极。将硅片需要沉积金属铟的部分置于溶液中，并使其正面对准打开的氙灯光源。在电化学工作站it模式，-1.0V电位下开始沉积30秒后停止沉积。得到如图2所示的金属铟修饰的硅光电阴极薄膜。底层是硅光电阴极薄膜，薄膜表面的白色颗粒即为金属铟，金属铟的分布粒径从纳米至微米级。如图3所示，即为金属铟修饰的硅光电阴极薄膜的XRD图，圆形标识为硅的特征峰，菱形标志为铟的特征峰。如图4所示，即为金属铟修饰的硅光电阴极薄膜的硅的特征峰。图5为金属铟修饰的硅光电阴极薄膜的铟的特征峰。
Claims (5)
1.一种金属铟修饰硅光电阴极薄膜的方法，其特征在于：
1)将硅片依次置于有机溶剂清洗剂和去离子水中超声清洗30±10分钟，其后将硅片放入10±5％氢氟酸水溶液中刻蚀20-100秒备用；
2)将金属铟盐In(NO3)3·4H2O或InCl3溶解于1±0.3M NaNO3溶液中，制得0.02M的In(NO3)3·4H2O或InCl3溶液，用于光辅助硅光电极的电沉积；
3)将清洗好的硅片与电化学工作站连接，在-1.0V(vs.SCE)电位下，通过紫外可见光照30±10秒，得到金属铟修饰的硅光电阴极薄膜。
2.如权利要求1所述的方法，其特征在于，所述步骤(1)中的有机溶剂清洗剂包括但不限于丙酮、乙醇以及甲醇等。
3.如权利要求1所述的方法，其特征在于，用于沉积的金属铟盐溶液包括但不限于In(NO3)3·5H2O，InCl3等。
4.如权利要求1所述的方法，其特征在于，光辅助电沉积过程应处于室温和光强稳定的条件下进行。
5.一种根据权利要求1-4之一制备得到的金属铟修饰的硅光电阴极薄膜在光电催化水分解、二氧化碳还原反应中的应用。
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