CN113209990A - 一种柳絮状铜掺杂的硫铟锌光催化剂的制备方法和应用 - Google Patents
一种柳絮状铜掺杂的硫铟锌光催化剂的制备方法和应用 Download PDFInfo
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Abstract
本发明公开了一种柳絮状铜掺杂的硫铟锌光催化剂的制备方法和应用,首先将醋酸锌加入二甲基甲酰胺与乙二醇的混合溶剂(体积比1:1)中室温搅拌形成均一的透明溶液,再依次加入硝酸铜、四水合三氯化铟、硫代乙酰胺搅拌,最后将溶液倒入内衬为聚四氟乙烯的不锈钢反应釜进行水热反应。在180℃加热24h后,将所得溶液用去离子水洗涤数次,冷冻干燥12h后,得到铜掺杂硫铟锌的样品粉末。本发明具有操作简单,成本较低,稳定性好,绿色环保等优点,所得铜掺杂硫铟锌相对于硫铟锌亲水性增强,分散性提高,具有更大的比表面面积,表现出优异的光催化产氢性能。
Description
技术领域
本发明涉及光催化材料制备方法技术领域,尤其涉及一种柳絮状铜掺杂的硫铟锌光催化剂的制备方法和应用。
背景技术
在全球氢能产业快速发展的推动下,氢气作为一种高能量密度的清洁燃料受到越来越多的关注。光催化产氢可持续发展的社会中发挥关键作用,它是直接利用太阳光生产出清洁能源氢气,这不仅可以解决全球能源紧迫的问题,还能维持全球人口和经济增长。但在实际应用中,由于不可避免的光生电子-空穴复合,光催化转化效率较低。
近年来,表面修饰和内部改性被认为是提高光催化转化效率的两种有效途径。但与表面修饰相比,内部改性能在原子水平上有效地调节电荷流,为光催化反应注入了新的活力,表现了更好的光催化性能。掺杂工程和缺陷工程是实现内部改性的一种可行途径,掺杂的金属原子可以捕获空穴,有效地分离光生载流子。此外,通过缺陷工程产生电子陷阱也可以完成电荷分离的目的。过去,许多研究都集中在单个策略(掺杂工程或缺陷工程)来单独调制光生空穴或电子。但如果能将各自策略结合起来,可以对电荷分离产生很大的协同效应。对于掺杂工程,当杂原子取代主原子后,由于原子半径和配位数的不同,姜-泰勒扭曲就会存在,这使得空位产生。这种现象类似于含羞草一旦受到短暂的外部刺激就会发生卷曲的现象。因此通过杂原子掺杂来构建空位以有效分离载流子是一种可行的途径。
发明内容
本发明的目的在于解决现有技术中存在的技术问题,提供一种柳絮状铜掺杂的硫铟锌光催化剂的制备方法和应用。
为实现上述目的,本发明提供的技术方案是:一种柳絮状铜掺杂的硫铟锌光催化剂的制备方法和应用,包括以下步骤:a.将15ml二甲基甲酰胺和15ml乙二醇进行充分混合10min;
b.将0.95mmol醋酸锌加入步骤a所得溶液,搅拌混合10min;
c.将0.05mmol硝酸铜加入步骤b所得溶液,搅拌混合10min后得到均一透明的蓝色溶液;
d.将2mmol四水合三氯化铟加入步骤c所得溶液,超声1min后,继续搅拌混合10min;
e.将4mmol硫代乙酰胺加入步骤d所得溶液,搅拌混合4h后得到均一透明的橙色溶液,并将其倒入50ml的不锈钢反应釜进行水热反应,反应釜的内衬为聚四氟乙烯;
f.在180℃加热24h后,冷却至室温,将所得溶液用去离子水洗涤数次,冷冻干燥过夜,得到铜掺杂硫铟锌样品粉末。
一种如权利要求1所述的柳絮状铜掺杂的硫铟锌光催化剂在降解水中有机污染物和利用太阳光进行氢能源的制备的应用。
本发明有益效果:本发明具有操作简单,成本较低,稳定性好,绿色环保等优点,所得铜掺杂硫铟锌相对于硫铟锌亲水性增强,分散性提高,具有更大的比表面面积,表现出优异的光催化产氢性能。
附图说明
此处所说明的附图用来提供对本发明的进一步理解,构成本发明的一部分,本发明的示意性实施例及其说明用于解释本发明,并不构成对本发明的不当限定。
图1是本发明优选实施例合成的柳絮状5%铜掺杂硫铟锌和硫铟锌的扫描电子显微镜(SEM)表征图;
图2是本发明优选实施例合成的柳絮状5%铜掺杂硫铟锌和硫铟锌的粉末样品图;
图3是本发明优选实施例合成的柳絮状5%铜掺杂硫铟锌和硫铟锌的分散性测试图(浓度为0.25mg mL-1);
图4是本发明优选实施例合成的柳絮状5%铜掺杂硫铟锌和硫铟锌的接触角测试图;
图5是本发明优选实施例合成的柳絮状5%铜掺杂硫铟锌和硫铟锌的N2吸附-脱吸附等温曲线图;
图6是本发明优选实施例合成的柳絮状5%铜掺杂硫铟锌和硫铟锌产氢性能图。
具体实施方式
本部分将详细描述本发明的具体实施例,本发明之较佳实施例在附图中示出,附图的作用在于用图形补充说明书文字部分的描述,使人能够直观地、形象地理解本发明的每个技术特征和整体技术方案,但其不能理解为对本发明保护范围的限制。
参照图1-图6,本发明的优选实施例1,一种柳絮状铜掺杂的硫铟锌光催化剂的制备方法和应用,包括以下步骤:a.将15ml二甲基甲酰胺和15ml乙二醇进行充分混合10min;
b.将0.95mmol醋酸锌加入步骤a所得溶液,搅拌混合10min;
c.将0.05mmol硝酸铜加入步骤b所得溶液,搅拌混合10min后得到均一透明的蓝色溶液;
d.将2mmol四水合三氯化铟加入步骤c所得溶液,超声1min后,继续搅拌混合10min;
e.将4mmol硫代乙酰胺加入步骤d所得溶液,搅拌混合4h后得到均一透明的橙色溶液,并将其倒入50ml的不锈钢反应釜进行水热反应,反应釜的内衬为聚四氟乙烯;
f.在180℃加热24h后,冷却至室温,将所得溶液用去离子水洗涤数次,冷冻干燥过夜,得到铜掺杂硫铟锌样品粉末。
作为本发明的优选实施例,其还可具有以下附加技术特征:
一种如权利要求1所述的柳絮状铜掺杂的硫铟锌光催化剂在降解水中有机污染物和利用太阳光进行氢能源的制备的应用。
实施例2,一种无铜掺杂的硫铟锌光催化剂的制备方法包括以下步骤:
A.将15ml二甲基甲酰胺和15ml乙二醇进行充分混合10min;
B.将1mmol醋酸锌加入步骤B所得溶液,搅拌混合10min;
C.将2mmol四水合三氯化铟加入步骤B所得溶液,超声1min后,继续搅拌混合10min;
D.将4mmol硫代乙酰胺加入步骤C所得溶液,搅拌混合4h后得到均一透明的黄色溶液,并将其倒入50ml内衬为聚四氟乙烯的不锈钢反应釜进行水热反应;
E.在180℃加热24h后,冷却至室温,将所得溶液用去离子水洗涤数次,冷冻干燥过夜,得到硫铟锌样品粉末。
实施例1和实施例2进行对比:参照图1,铜掺杂硫铟锌后,催化剂的宏观形貌发生变化,原本的硫铟锌的形貌是一个由若干纳米片组成的花球,在铜掺杂后,催化剂的形貌变为分散性更好的柳絮状纳米片,这能够提高对光的吸收效果;参照图2,催化剂原本为亮黄色粉末,在掺杂铜之后,铜掺杂硫铟催化剂的颜色变为棕色粉末;参照图3和图4,将相同质量的催化剂分散在相同体积的去离子水充分混合,在静置5分钟后,原本的硫铟锌样品管中先出现黄色沉淀,而掺杂样品仍在样品管中呈现均一、分散良好的状态,与此同时,铜掺杂硫铟催化剂在水中的接触角为31.2°,小于原本硫铟锌催化剂(35.7°),说明铜掺杂硫铟催化剂能和水充分接触反应,有利于光催化产氢反应的进行;参照图5,采用N2吸附-解吸等温线测量两种催化剂的比表面积,原本硫铟锌的比面积为90.4580m2/g,而铜掺杂硫铟催化剂的比面积为131.5020m2/g,掺杂的催化剂更大的比表面积有利于暴露反应的活性位,加速光催化产氢反应;参照图6,光催化产氢效果的对比,原本硫铟锌的产氢速率为0.6640mmolg-1h-1,相同条件下,铜掺杂硫铟锌掺氢速率为9.8647mmol g-1h-1,是原本硫铟锌催化剂的14.8倍。
通过实施例1和实施例2的对比,铜掺杂硫铟锌相对于无铜掺杂的硫铟锌具有操作简单,成本较低,稳定性好,绿色环保等优点,所得铜掺杂硫铟锌相对于硫铟锌亲水性增强,分散性提高,具有更大的比表面面积,表现出优异的光催化产氢性能。
以上所述仅为本发明的优先实施方式,只要以基本相同手段实现本发明目的的技术方案都属于本发明的保护范围之内。
Claims (2)
1.一种柳絮状铜掺杂的硫铟锌光催化剂的制备方法和应用,其特征在于:包括以下步骤:a.将15ml二甲基甲酰胺和15ml乙二醇进行充分混合10min;
b.将0.95mmol醋酸锌加入步骤a所得溶液,搅拌混合10min;
c.将0.05mmol硝酸铜加入步骤b所得溶液,搅拌混合10min后得到均一透明的蓝色溶液;
d.将2mmol四水合三氯化铟加入步骤c所得溶液,超声1min后,继续搅拌混合10min;
e.将4mmol硫代乙酰胺加入步骤d所得溶液,搅拌混合4h后得到均一透明的橙色溶液,并将其倒入50ml的不锈钢反应釜进行水热反应,反应釜的内衬为聚四氟乙烯;
f.在180℃加热24h后,冷却至室温,将所得溶液用去离子水洗涤数次,冷冻干燥过夜,得到铜掺杂硫铟锌样品粉末。
2.一种如权利要求1所述的柳絮状铜掺杂的硫铟锌光催化剂在降解水中有机污染物和利用太阳光进行氢能源的制备的应用。
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