CN106521546A - 一种光解水制氢用多层BiVO4/CuWO4复合膜及其制备方法 - Google Patents
一种光解水制氢用多层BiVO4/CuWO4复合膜及其制备方法 Download PDFInfo
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Abstract
本发明涉及一种用于光解水制氢的多层复合膜电极材料及其制备方法。本发明根据BiVO4和CuWO4的紫外‑可见光谱特性及界面效应,设置多层复合结构,采用溶胶‑凝胶法、提拉工艺制备出了多层薄膜,所制备的多层复合膜对可见光的响应范围明显扩宽,且可调。本发明所述制备方法操作简单,易于实施。
Description
技术领域
本发明属于无机功能薄膜材料制备领域,特别涉及一种用于光解水制氢的、基于复合氧化物半导体的多层复合薄膜及其制备方法。
背景技术
新能源之一的氢能在使用过程中不产生污染,为人类应对环境污染和能源短缺的挑战带来了无限的希望。但目前氢能主要来源于化石燃料的提炼(约96%),其生产过程造成环境污染,还不能说是百分之百的清洁能源。1972年A.Fujishims等报道了发生在TiO2单晶电极表面的光致分解水生成H2和O2的现象,说明可以利用太阳能这种用之不竭的绿色能源获取氢能,有望使其成为真正意义上的清洁能源,因此引起了世人的关注和重视。
光解水制氢过程是一光催化作用下的氧化还原过程,半导体光电极吸收光子能量,使价带电子跃迁至导带,产生光生电子-空穴,电子与空穴分离并分别迁移到催化剂表面,与吸附于表面的H+发生还原反应形成H2,与OH-发生氧化反应形成O2。因此,实现光解水制氢的前提条件是光电极能吸收光能。最早报道的简单氧化物TiO2能隙为3.1~3.2eV,可以实现紫外光响应分解水制氢,但只能吸收太阳能中5~6%的紫外光,能量利用效率很低。光电极材料的能隙既要大于1.23eV,但不能过宽,一般小于3.0eV时,才能吸收415nm以上的光线,具有可见光催化特性。
通式为ABO3、ABO4、A2B2O7、AB2O4等类型的复合氧化物具有可见光响应的特点。例如,BiVO4能隙为2.4eV,理论上应具有吸收可见光的能力,但实际上的光吸收能力受材料的表面质量、内部缺陷等诸多因素的影响,吸收效率不高,往往达不到这种理论效果。
发明内容
本发明的目的在于提供一种用于光解水制氢的多层复合氧化物薄膜电极材料及其制备方法。
为提高光电极对光的整体吸收效果,薄膜材料的尺寸不宜过小;为确保光生电子、空穴能顺利分离并迁移到催化剂表面,减小在迁移过程中的复合,尺寸不宜大,这是相互矛盾的。本发明的基本思路是:设置由一种或两种的复合氧化物组成的多层膜结构,利用光子在界面的反复折射提高对光的吸收率,以克服上述的矛盾。通过溶胶-凝胶法,提拉工艺制备多层复合薄膜,通过优化工艺确保实现上述目的。
本发明所提供的多层复合氧化物薄膜具有如下特点。一是由BiVO4和CuWO4两种材料中的一种或两种组成,复合薄膜至少为五层结构。二是可以通过改变组合方式,得到不同吸收光谱的光催化电极材料。例如,相对于单层CuWO4而言,由至少五层CuWO4组成时,可见光响应范围明显拓宽;由至少五层BiVO4组成时,可见光响应范围进一步拓宽;当由不同层数的BiVO4膜和CuWO4膜组合而成,总层数不少于五层,两种材料可以交替组合,但不仅限于这种组合方式时,除可见光响应范围拓宽外,吸收系数明显提高。
本发明提供一种用于光解水制氢的多层复合氧化物薄膜的制备方法,其制备步骤如下:
1)采用溶胶-凝胶法制备CuWO4和BiVO4湿溶胶;
2)在清洗干净的FTO基体上,采用提拉法制备BiVO4、CuWO4凝胶薄膜;
3)将步骤2)的凝胶薄膜置于40~80℃温度下干燥1~3小时;
4)用无水乙醇和去离子水依次清洗步骤3)的干凝胶薄膜,并放置至自然干燥;
5)对步骤4)所得薄膜进行退火,退火温度为500~600℃,保温时间为80~280min,可以直接从室温升至退火温度,也可分两段升温,中间保温温度为80~200℃,保温时间为50~180min;
6)退火工序完成后,用无水乙醇和去离子水依次清洗薄膜,待自然干燥后,再重复步骤2~5,制备出所需结构的多层复合薄膜。
本发明所提供的多层膜及其制备方法具有如下显著效果:一是可见光响应范围显著拓宽,二是制备方法简单、易于实施。
附图说明
图1为实施例1的多层复合薄膜及其对比样的紫外-可见光谱。
图2为实施例2的多层复合薄膜及其对比样的紫外-可见光谱。
图3为实施例3的多层复合薄膜及其对比样的紫外-可见光谱。
图4为对比例的双层复合薄膜及其对比样的紫外-可见光谱。
具体实施方式
下面通过实施例,进一步阐明本发明的特点和进步,仅在于说明本发明而不限于本发明。
实施例1
1)采用溶胶-凝胶法制备CuWO4湿溶胶;
2)在清洗干净的FTO基体上,采用提拉法制备CuWO4凝胶薄膜;
3)将步骤2)的凝胶薄膜置于60℃温度下干燥2小时;
4)用无水乙醇和去离子水依次清洗步骤3)的干凝胶薄膜,并放置至自然干燥;
5)对步骤4)所得薄膜进行退火,退火温度为550℃,保温时间为180min,分两段升温,中间保温温度为100℃,保温时间为100min;
6)退火工序完成后,用无水乙醇和去离子水依次清洗薄膜,待自然干燥后,再重复步骤2~5,制备出5层结构的CuWO4薄膜。
图1说明5层结构的CuWO4薄膜的吸收边红移,吸收率有所提高。
实施例2
1)采用溶胶-凝胶法制备BiVO4湿溶胶;
2)在清洗干净的FTO基体上,采用提拉法制备BiVO4凝胶薄膜;
3)将步骤2)的凝胶薄膜置于65℃温度下干燥2.1小时;
4)用无水乙醇和去离子水依次清洗步骤3)的干凝胶薄膜,并放置至自然干燥;
5)对步骤4)所得薄膜进行退火,退火温度为570℃,保温时间为160min,分两段升温,中间保温温度为100℃,保温时间为100min;
6)退火工序完成后,用无水乙醇和去离子水依次清洗薄膜,待自然干燥后,再重复步骤2~5,制备出5层结构的BiVO4薄膜。
图2说明5层结构的BiVO4薄膜的吸收边大幅度红移,在430nm以下的吸收率大幅度提高。
实施例3
1)分别采用溶胶-凝胶法制备CuWO4和BiVO4湿溶胶;
2)在清洗干净的FTO基体上,采用提拉法制备CuWO4凝胶薄膜;
3)将步骤2)的凝胶薄膜置于60℃温度下干燥2小时;
4)用无水乙醇和去离子水依次清洗步骤3)的干凝胶薄膜,并放置至自然干燥;
5)对步骤4)所得薄膜进行退火,退火温度为550℃,保温时间为180min,分两段升温,中间保温温度为100℃,保温时间为100min;
6)退火工序完成后,用无水乙醇和去离子水依次清洗薄膜,自然干燥。
7)在步骤6)所得薄膜上,采用提拉法制备BiVO4凝胶薄膜;
8)将步骤7)的凝胶薄膜置于65℃温度下干燥2.1小时;
9)用无水乙醇和去离子水依次清洗步骤8)的干凝胶薄膜,并放置至自然干燥;
10)对步骤9)所得薄膜进行退火,退火温度为570℃,保温时间为160min,分两段升温,中间保温温度为100℃,保温时间为100min;
6)退火工序完成后,用无水乙醇和去离子水依次清洗薄膜,待自然干燥后,再重复步骤7~10,制备出结构为四层BiVO4+一层CuWO4的多层复合薄膜。
图3说明四层BiVO4+一层CuWO4的多层复合薄膜的吸收边红移,在可见光范围内的吸收率有所提高。
对比例
1)分别采用溶胶-凝胶法制备CuWO4和BiVO4湿溶胶;
2)在清洗干净的FTO基体上,采用提拉法制备CuWO4凝胶薄膜;
3)将步骤2)的凝胶薄膜置于60℃温度下干燥2小时;
4)用无水乙醇和去离子水依次清洗步骤3)的干凝胶薄膜,并放置至自然干燥;
5)对步骤4)所得薄膜进行退火,退火温度为550℃,保温时间为180min,分两段升温,中间保温温度为100℃,保温时间为100min;
6)退火工序完成后,用无水乙醇和去离子水依次清洗薄膜,自然干燥。
7)在步骤6)所得薄膜上,采用提拉法制备BiVO4凝胶薄膜;
8)将步骤7)的凝胶薄膜置于65℃温度下干燥2.1小时;
9)用无水乙醇和去离子水依次清洗步骤8)的干凝胶薄膜,并放置至自然干燥;
10)对步骤9)所得薄膜进行退火,退火温度为570℃,保温时间为160min,分两段升温,中间保温温度为100℃,保温时间为100min;
6)退火工序完成后,用无水乙醇和去离子水依次清洗薄膜,自然干燥后,即可制备出结构为一层BiVO4+一层CuWO4的双层复合薄膜。
图4说明一层BiVO4+一层CuWO4的双层复合薄膜的吸收边红移,但在450nm可见光范围内的吸收率明显下降。
综合而言,五层复合薄膜在可见光范围内的吸收率较高。
Claims (5)
1.一种用于光解水制氢的多层复合薄膜,其特征在于,由BiVO4和CuWO4两种材料中的一种或两种组成,复合薄膜至少为五层结构。
2.根据权利要求1所述的用于光解水制氢的多层复合薄膜,其特征在于,由至少五层CuWO4组成,相对于单层CuWO4而言,可见光响应范围拓宽。
3.根据权利要求1所述的用于光解水制氢的多层复合薄膜,其特征在于,由至少五层BiVO4组成,相对于五层CuWO4而言,可见光响应范围进一步拓宽。
4.根据权利要求1所述的用于光解水制氢的多层复合薄膜,其特征在于,由不同层数的BiVO4膜和CuWO4膜组合而成,总层数不少于五层,两种材料可以交替组合,除可见光响应范围拓宽外,吸收系数明显提高。
5.根据权利要求1所述的用于光解水制氢的多层复合薄膜,其特征在于,其制备步骤如下:
1)采用溶胶-凝胶法制备CuWO4和/或BiVO4湿溶胶;
2)在清洗干净的FTO基体上,采用提拉法制备BiVO4、CuWO4凝胶薄膜;
3)将步骤2)的凝胶薄膜置于40~80℃温度下干燥1~3小时;
4)用无水乙醇和去离子水依次清洗步骤3)的干凝胶薄膜,并放置至自然干燥;
5)对步骤4)所得薄膜进行退火,退火温度为500~600℃,保温时间为80~280min,可以直接从室温升至退火温度,也可分两段升温,中间保温温度为80~200℃,保温时间为50~180min;
6)退火工序完成后,用无水乙醇和去离子水依次清洗薄膜,待自然干燥后,再重复步骤2~5,制备出所需结构的多层复合薄膜。
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