CN109133669A - 一种Ag/AgCl/WO3纳米薄膜材料及其制备方法 - Google Patents

一种Ag/AgCl/WO3纳米薄膜材料及其制备方法 Download PDF

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CN109133669A
CN109133669A CN201811056673.3A CN201811056673A CN109133669A CN 109133669 A CN109133669 A CN 109133669A CN 201811056673 A CN201811056673 A CN 201811056673A CN 109133669 A CN109133669 A CN 109133669A
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李贺
牟宗信
张家良
刘升光
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Dalian University of Technology
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Abstract

本发明公开了一种Ag/AgCl/WO3纳米薄膜材料及其制备方法。其制备方法为以玻璃为基底，先采用磁控溅射法在基底上制备WO3纳米薄膜，然后采用浸渍‑沉淀‑光还原法将Ag/AgCl纳米颗粒附着到WO3薄膜表面。本发明得到的纳米薄膜可用于光电催化，太阳能电池等多个领域，具有成本低，操作简单，性能稳定等特点。

Description

一种Ag/AgCl/WO3纳米薄膜材料及其制备方法
技术领域
本申请涉及纳米薄膜材料，特别是涉及到一种Ag/AgCl/WO3纳米薄膜材料，还涉及到这种复合薄膜的制备方法。
背景技术
太阳能是地球上用之不竭，取之不尽的可循环能源，具有其他能源所不可比拟的优点。制备具有高催化活性、高可见过利用率，高催化稳定性以及低成本的光催化材料一直是该领域的研究热点。传统光催化材料TiO2由于其禁带宽度较宽(3.2eV)，决定其只能利用太阳光中很少的一部分，而占据了太阳光光谱43％的可见光却不能充分利用。因此，人们不断寻找新的可见光响应的光催化材料。
WO3作为一种重要的n型半导体材料，其最热门的应用主要光(电)致变色、气敏特性，而近几年开始应用于新型的可见光驱动的光催化剂，因为其禁带宽度为2.8eV，可被480nm波长(可见光)激发，同时其价带电位为+3.2eV,使得价带空穴具有强的氧化能力。但是WO3光催化材料的在实际应用中的量子利用率还是很低，对WO3进行改性来降低电子空穴复合速率至关重要。
纳米Ag/AgCl材料由于表面存在的Ag0原子可以通过等离子体共振(SPR)效应大大加强AgCl在可见光区域的光响应，并且增强其在光照下的稳定性，AgCl与WO3异质结的合成可以有效的分离光生电子空穴，这些因素可以提高催化剂的光催化效率。此外薄膜状的光催化剂更是可以增加材料的重复利用率，降低回收难度，节约使用成本。
发明内容
本发明的目的是主要针对单一WO3薄膜对太阳光利用率低的问题，提供了一种Ag/AgCl/WO3纳米薄膜材料及其制备方法。
本发明的技术方案：
一种Ag/AgCl/WO3纳米薄膜材料，以玻璃为基底，基底上覆有一层WO3纳米薄膜，WO3纳米薄膜上负载有纳米Ag/AgCl颗粒；其中，WO3纳米薄膜的厚度为300-600nm。
所述的玻璃为医用载玻片或者氧化铟锡透明导电玻璃。
以玻璃为基底，先采用磁控溅射法在基底上制备纳米WO3薄膜，然后采用浸渍-沉淀-光还原法将纳米Ag/AgCl颗粒附着到纳米WO3薄膜表面。
一种Ag/AgCl/WO3纳米薄膜材料的制备方法，步骤如下：
(1)基底的预处理：玻璃基底经超声清洗后，待用；步骤(1)中所述的预处理是依次在丙酮，无水乙醇和去离子水中超声波清洗10-20min；
(2)WO3纳米薄膜的制备：采用磁控溅射方法，以金属钨为溅射靶材，以氩气和氧气为工作气体，制备WO3纳米薄膜，随后在马弗炉中退火处理，自然降温至室温；
步骤(2)中所述的磁控溅射法为直流反应磁控溅射法。工艺参数为工作气压为1-2Pa，溅射功率为80-100W，溅射时间为30-60min。
步骤(2)中所述的氩气流量为60-100sccm，氧气流量为20-50sccm。
步骤(2)中所述的退火处理是将磁控溅射后薄膜置于马弗炉中，以5-10℃/min的速率升温至400-500℃，保温1-2h后自然降温至室温。
(3)纳米Ag/AgCl/WO3薄膜的制备：以步骤(2)中制备的WO3纳米薄膜为基底，分别依次浸渍在AgNO3和NaCl溶液中5-10min，循环1-5次，晒干后，在紫外光下照射10-20min，得到Ag/AgCl/WO3纳米薄膜。
步骤(3)中所述的AgNO3和NaCl溶液的浓度为0.001-0.01mol/L。
步骤(3)中所述的紫外光为20-100W的365nm的紫外光。
本发明的有益效果：
(1)本发明Ag/AgCl/WO3纳米薄膜材料具有较窄的禁带宽度，可见光吸收率比单独的WO3薄膜更高，增大了光电转化效率。
(2)本发明Ag/AgCl/WO3纳米薄膜材料的制备方法采用在固体基质上沉积WO3薄膜，有利于纳米颗粒的回收循环使用。
(3)本发明制备的薄膜材料具有简单易行、安全可靠、性能稳定等优点。
附图说明
图1是本发明实例1制备的未掺杂Ag/AgCl的WO3薄膜扫描电镜图。
图2是本发明实例1制备的Ag/AgCl/WO3薄膜扫描电镜图。
图3是本发明实例2制备的Ag/AgCl/WO3薄膜扫描电镜图。
图4是本发明实例1制备的Ag/AgCl/WO3薄膜与纯WO3紫外可见吸收光谱图。
具体实施方式
下面结合实施例对本发明的突出特点和显著进步作进一步阐明，仅在于说明本发明而决不局限于以下实例。
实施例1
首先，将玻璃基底用丙酮、无水乙醇、去离子水经超声仪分别清洗10min后，待用。将清洗后的基片放入真空室，以直流反应磁控溅射方法，以金属钨为溅射靶材，以氩气和氧气为工作气体，氩气流量为80sccm，氧气为30sccm，溅射功率为100W，溅射时间为1h，制备WO3纳米薄膜，随后在马弗炉中400℃退火处理，自然降温至室温。将制备的WO3纳米薄膜为基底，分别依次浸渍在0.01mol/L的AgNO3和0.01mol/L的NaCl溶液中10min，循环3次，晒干后，在24W的365nm紫外光下照射15min，得到Ag/AgCl/WO3纳米薄膜。
实施例2
首先，将玻璃基底用丙酮、无水乙醇、去离子水经超声仪分别清洗10min后，待用。将清洗后的基片放入真空室，以直流反应磁控溅射方法，以金属钨为溅射靶材，以氩气和氧气为工作气体，氩气流量为80sccm，氧气为30sccm，溅射功率为100W，溅射时间为1h，制备WO3纳米薄膜，随后在马弗炉中400℃退火处理，自然降温至室温。将制备的WO3纳米薄膜为基底，分别依次浸渍在0.005mol/L的AgNO3和0.005mol/L的NaCl溶液中10min，循环5次，晒干后，在24W的365nm紫外光下照射15min，得到Ag/AgCl/WO3纳米薄膜。
结果对比分析
图1为制备的WO3膜扫描电镜图。从图1中可以看出，薄膜形貌均匀、致密和完整。
图2为本发明实例1制备的Ag/AgCl/WO3膜扫描电镜图。从图2中可以看出，Ag/AgCl已附着在WO3薄膜表面。
图3为本发明实例2制备的Ag/AgCl/WO3膜扫描电镜图。从图3中可以看出，Ag/AgCl已附着在WO3薄膜表面。
图4是本发明实例1制备的Ag/AgCl/WO3薄膜与纯WO3紫外可见吸收光谱图。从图4中可以看出Ag/AgCl/WO3薄膜具有更窄的禁带宽度和更强可见光吸收率，可增强光催化。
由以上技术方案可以看出，本发明的Ag/AgCl/WO3薄膜，既可以增加WO3薄膜的比表面积，从而增加与污染物接触面积，又可以增强WO3薄膜的可见光吸收率，可广泛应用于光电催化等技术领域，能够显著提高光电催化速率。
本发明制备的薄膜材料具有简单易行、安全可靠、性能稳定等优点。
对于本领域技术人员而言，显然本发明不限于上述示范性实施例的细节，而且在不背离本发明的精神或基本特征的情况下，能够以其他的具体形式实现本发明。因此，无论从哪一点来看，均应将实施例看作是示范性的，而且是非限制性的，本发明的范围由所附权利要求而不是上述说明限定，因此旨在将落在权利要求的等同要件的含义和范围内的所有变化囊括在本发明内。不应将权利要求中的任何附图标记视为限制所涉及的权利要求。

Claims (10)

1.一种Ag/AgCl/WO3纳米薄膜材料，其特征在于，以玻璃为基底，基底上覆有一层WO3纳米薄膜，WO3纳米薄膜上负载有纳米Ag/AgCl颗粒。
2.根据权利要求1所述的Ag/AgCl/WO3纳米薄膜材料，其特征在于，所述的WO3纳米薄膜的厚度为300-600nm。
3.根据权利要求1或2所述的Ag/AgCl/WO3纳米薄膜材料，其特征在于，所述的玻璃为医用载玻片或氧化铟锡透明导电玻璃。
4.一种Ag/AgCl/WO3纳米薄膜材料的制备方法，其特征在于，步骤如下：
(1)基底的预处理：玻璃基底经超声清洗后，待用；
(2)WO3纳米薄膜的制备：采用磁控溅射方法，以金属钨为溅射靶材，以氩气和氧气为工作气体，制备WO3纳米薄膜，随后在马弗炉中退火处理，自然降温至室温；
所述的磁控溅射的工艺参数为工作气压为1-2Pa，溅射功率为80-100W，溅射时间为30-60min；
所述的马弗炉中退火处理：以5-10℃/min的速率升温至400-500℃，保温1-2h后自然降温至室温；
(3)纳米Ag/AgCl/WO3薄膜的制备：以步骤(2)中制备的WO3纳米薄膜为基底，分别依次浸渍在AgNO3和NaCl溶液中各5-10min，循环1-5次，晒干后，在紫外光下照射10-20min，得到Ag/AgCl/WO3纳米薄膜。
5.根据权利要求4所述的制备方法，其特征在于，步骤(2)中所述的磁控溅射法为直流反应磁控溅射法；所述的氩气流量为60-100sccm，氧气流量为20-50sccm。
6.根据权利要求4或5所述的制备方法，其特征在于，步骤(3)中所述的AgNO3和NaCl溶液的浓度均为0.001-0.01mol/L。
7.根据权利要求4或5所述的制备方法，其特征在于，步骤(3)中所述的紫外光为20-100W的365nm的紫外光。
8.根据权利要求6所述的制备方法，其特征在于，步骤(3)中所述的紫外光为20-100W的365nm的紫外光。
9.根据权利要求4、5或8所述的制备方法，其特征在于，步骤(1)中所述的预处理是依次在丙酮，无水乙醇和去离子水中超声波清洗10-20min。
10.根据权利要求7所述的制备方法，其特征在于，步骤(1)中所述的预处理是依次在丙酮，无水乙醇和去离子水中超声波清洗10-20min。
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