CN106964369B - 一种异质结光催化剂的制备方法和应用 - Google Patents
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Abstract
本发明公开了一种制备异质结光催化剂的方法,该方法包括以下步骤:(1)将二乙基二硫代氨基甲酸镉,2‑硫醇基苯并咪唑锌,二甲基二硫代氨基甲酸钼加入到溶剂中,搅拌,超声;(2)将步骤(1)中的反应液进行微波加热反应;(3)将步骤(2)中的反应液冷却至室温,离心,烘干,即得Cd0.8Zn0.2S‑MoS2异质结。本发明制备方法简单,成本低廉,反应时间较短,能够有效光催化水产生氢,对缓解能源危机和环境问题有重要的意义。
Description
技术领域
本发明涉及一种光催化剂及其制备方法和应用,尤其涉及异质结催化剂Cd0.8Zn0.2S-MoS2及其制备方法和应用。
背景技术
光催化分解水产氢为解决日益严重的能源危机和环境问题提供了一种很有前景的方法。自从20世纪70年代日本学者Fujishima和Honda发现TiO2电极存在光催化分解水的现象以来,一系列的化合物半导体和金属半导体作为光催化剂被运用于光催化分解水产氢中。在这些半导体催化剂中,CdS因具有2.4eV的带隙以及合适的导带电势而被作为一种重要的光催化剂得到了研究。
但是,CdS半导体光催化剂在没有进行表面修饰和改性时存在两个严重的问题:第一,因光生电子-空穴对的复合导致CdS的活性太低;第二,CdS在长时间的光照下会发生光腐蚀现象,从而导致其稳定性下降。为了解决以上两个问题,许多学者研究了不同的制备方法、材料改性手段等对CdS的影响。到目前为止,CdS材料的主要改性方法有:形貌调控,沉积、负载助催化剂(沉积贵金属、负载碳材料、金属硫化物或金属复合氧化物)、复合半导体形成固溶体,构造异质结等。
为了结合各种改性方法的优点,CdS材料复合半导体形成固溶体,同时负载助催化剂形成异质结形貌应该是一条解决CdS问题的可行方法。通过相关的研究证明,ZnS能和CdS能很好的形成固溶体CdxZn1-xS,改变Zn/Cd的比例,可以有效的改善CdS的导带和价带的位置,使其更好地符合产氢的电势,提高CdS的活性。同时,负载金属硫化物助催化剂提高CdS的稳定性。
合成异质结CdxZn1-xS基复合光催化材料方法有多种。例如,通过水热法再沉积石墨烯可以得到Cd0.4Zn0.6S/graphene纳米粒子;利用化学溶液法共沉积得到三元Cd0.5Zn0.5S/NiS/Reduced Graphene Oxide纳米材料;通过水热-化学气相沉积法合成Cd0.4Zn0.6S/WS2纳米球。但以上合成方法还存在诸多缺陷。例如:水热法反应合成时间久,不便于大量生产,而且反应在反应釜中进行无法原位观察晶体生长过程不便于研究晶体生长机理。而化学气相沉积法合成条件要求苛刻,一般需要高温加热,冲入惰性气体,控制基底温度等,操作复杂。因此,为解决上述问题,设计出一种操作简便,方法简单,快速及经济环保的合成方法具有重要的实用意义。
发明内容
为了克服现有技术的不足,本发明的目的在于提供一种异质结光催化剂的制备方法和应用。
本发明的目的采用以下技术方案实现:
一种制备异质结光催化剂的方法,该方法包括以下步骤:
(1)将二乙基二硫代氨基甲酸镉,2-硫醇基苯并咪唑锌,二甲基二硫代氨基甲酸钼依次加入到溶剂中,搅拌,超声;
(2)将步骤(1)中的反应液进行微波加热反应;
(3)将步骤(2)中的反应液冷却至室温,离心,烘干,即得Cd0.8Zn0.2S-MoS2异质结。
优选地,二乙基二硫代氨基甲酸镉,2-硫醇基苯并咪唑锌,二甲基二硫代氨基甲酸钼的质量比为(4~6):1:(3~5)。
优选地,上述步骤(1)中搅拌时间为5~15min。
优选的,上述步骤(1)中超声时间为20~35min。
优选的,上述步骤(2)中微波加热温度分两个阶段,第一阶段为85~100℃,加热时间5~15min,第二阶段为145~165℃,加热时间为5~15min。
优选的,第一阶段的升温速率为15~20℃/min,第二阶段的升温速率为10~15℃/min。
优选的,步骤(3)中离心转速为15000r/min~20000r/min。
优选的,所述烘干温度为85~100℃,烘干时间为10~15h。
上述方法制备的Cd0.8Zn0.2S-MoS2异质结光催化剂用于光催化水产生氢的应用。
相比现有技术,本发明的有益效果在于:利用本发明所制备的Cd0.8Zn0.2S-MoS2异质结光催化剂具有优异的光催化活性,制备方法简单,成本低廉,反应时间较短,能够有效光催化水产生氢,对缓解能源危机和环境问题有重要的意义。
附图说明
图1为本发明实施例1所制得的样品的低倍扫描电镜图(SEM)和透射电镜图(TEM)图;
图2为本发明实施例1所制得样品的能谱图(EDX);
图3为本发明实施例1所制得样品的X射线光电子能谱图(XPS);
图4为本发明实施例1和对比例1-3所制得样品的漫反射图;
图5为本发明实施例1和对比例1-3所制得样品的光催化产氢图;
图6为本发明实施例1和对比例1-3所制得样品的光催化稳定性图,图6表明实施例1的样品的光催化稳定性最好。
具体实施方式
下面,结合附图以及具体实施方式,对本发明做进一步描述:
实施例1
二乙基二硫代氨基甲酸镉(CED)(0.5000g)、2-硫醇基苯并咪唑锌(MBZ)(0.1000g)、二甲基二硫代氨基甲酸钼(0.4000g)混合于500ml乙二醇溶液中,搅拌十分钟,超声30min,在微波中反应,5min加热到90℃,此温度下保持10min,再耗时5min从90℃加热到160℃,并保温10min。反应完全后,冷却到室温,在18000r/min转速下,用水和酒精离心三次,在90℃条件下烘12h,得到0.4g的Cd0.8Zn0.2S-MoS2样品。
对比例1
二乙基二硫代氨基甲酸镉(CED)(0.5000g)加入到500ml乙二醇溶液中,搅拌十分钟,超声30min,在微波中反应,5min加热到90℃,此温度下保持10min,再耗时5min从90℃加热到160℃,并保温10min。反应完全后,冷却到室温,在18000r/min转速下,用水和酒精离心三次,在90℃条件下烘12h,分别得到0.15mg的CdS样品。
对比例2
二乙基二硫代氨基甲酸镉(CED)(0.5000g)和2-硫醇基苯并咪唑锌(MBZ)(0.1000g)加入到500ml乙二醇溶液中,搅拌十分钟,超声30min,在微波中反应,5min加热到90℃,此温度下保持10min,再耗时5min从90℃加热到160℃,并保温10min。反应完全后,冷却到室温,在18000r/min转速下,用水和酒精离心三次,在90℃条件下烘12h,得到0.2mg的Cd0.8Zn0.2S样品。
对比例3
二乙基二硫代氨基甲酸镉(CED)(0.5000g)和二甲基二硫代氨基甲酸钼(0.4000g)原料加入到500ml乙二醇溶液中,搅拌十分钟,超声30min,在微波中反应,5min加热到90℃,此温度下保持10min,再耗时5min从90℃加热到160℃,并保温10min。反应完全后,冷却到室温,在18000r/min转速下,用水和酒精离心三次,在90℃条件下烘12h,得到0.3mg的CdS-MoS2样品。
光解水制氢步骤:
将实施例1所得的异质结光催化剂Cd0.8Zn0.2S-MoS2复合材料用于光解水制氢,具体处理方法为:将50mg样品加入到8ml乳酸和72ml水组成的混合物中,用太阳光模拟器照射,使用420nm以下的滤光片过滤,并用气相色谱检测产出的H2。
对比例1-3采用上述制氢步骤,并用气相色谱检测产出的H2。结果如图5所示,Cd0.8Zn0.2S-MoS2光催化产氢性能得到了明显的提高。
对本领域的技术人员来说,可根据以上描述的技术方案以及构思,做出其它各种相应的改变以及形变,而所有的这些改变以及形变都应该属于本发明权利要求的保护范围之内。
Claims (5)
1.一种制备异质结光催化剂的方法,其特征在于,该方法包括以下步骤:
(1)将二乙基二硫代氨基甲酸镉,2-硫醇基苯并咪唑锌,二甲基二硫代氨基甲酸钼加入到溶剂中,搅拌,超声;
(2)将步骤(1)中的反应液进行微波加热反应;
(3)将步骤(2)中的反应液冷却至室温,离心,烘干,即得Cd0.8Zn0.2S-MoS2异质结;
二乙基二硫代氨基甲酸镉,2-硫醇基苯并咪唑锌,二甲基二硫代氨基甲酸钼的质量比为(4~6):1:(3~5);
步骤(2)中微波加热温度分两个阶段,第一阶段为85~100℃,加热时间5~15min,第二阶段为145~165℃,加热时间为5~15min,第一阶段的升温速率为15~20℃/min,第二阶段的升温速率为10~15℃/min。
2.根据权利要求1所述的制备方法,其特征在于,上述步骤(1)中搅拌时间为5~15min。
3.根据权利要求1所述的制备方法,其特征在于,上述步骤(1)中超声时间为20~35min。
4.根据权利要求1所述的制备方法,其特征在于,步骤(3)中离心转速为15000r/min~20000r/min。
5.根据权利要求1所述的制备方法,其特征在于,所述烘干温度为85~100℃,烘干时间为10~15h。
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