CN111774099A - 一种ZnS/PCPA/CoPi光电催化材料及其制备方法 - Google Patents
一种ZnS/PCPA/CoPi光电催化材料及其制备方法 Download PDFInfo
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- LWIHDJKSTIGBAC-UHFFFAOYSA-K tripotassium phosphate Chemical compound [K+].[K+].[K+].[O-]P([O-])([O-])=O LWIHDJKSTIGBAC-UHFFFAOYSA-K 0.000 claims description 4
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Abstract
一种ZnS/PCPA/CoPi光电催化材料及其制备方法。该方法首先采用醋酸锌和硫脲混合溶液配制ZnS前驱体反应液,随后利用水热反应制得ZnS薄膜;然后将ZnS薄膜浸入三羟甲基氨基甲烷、邻苯二酚和四乙烯五二胺溶液中,室温下制得的聚(邻苯二酚/多胺)有机半导体聚合物负载到ZnS薄膜上;最后通过光辅助沉积法将CoPi助催化剂沉积到ZnS/PCPA薄膜表层,得到ZnS/PCPA/CoPi光电催化材料。所制备的ZnS/PCPA/CoPi光电催化剂制备过程简单、成本低廉、无毒无污染,在可见光照射下能产生较强的光电流,相较于单独的ZnS电极光电流密度提升了7倍。
Description
技术领域
本发明属于光电催化材料制氢领域,具体涉及一种ZnS/PCPA/CoPi光电催化材料及其制备方法。
背景技术
近几年,能源枯竭和环境污染引起了人们的广泛关注,发展清洁的新能源材料迫在眉睫。半导体光电催化技术可将低密度太阳能转换为高密度的氢能,有效的缓解环境污染问题,真正实现能源的合理化利用。经各国科研工作者多年的探索,半导体光电催化制氢技术日趋成熟,但目前太阳能光电转换效率仍然较低,且成本较高,距离用于商业化生产仍有很大差距。因此,开发新型光电极材料,并对材料进行表面修饰和改性以增加光生载流子的分离和转移效率,从而提高光电催化制氢效率。
硫化锌(ZnS)由于价格低廉、储量丰富、具有独特的光电性质且易于制备而备受人们的青睐,使得其在未来大量应用于工业生产成为可能。但ZnS仍然存在以下两方面的缺陷限制了其应用:(1)由于其本身禁带宽度较宽,导致对可见光利用受限;(2)ZnS中硫离子易于在溶液中的水和氧气作用下与光生空穴发生反应,产生光腐蚀现象。针对以上缺陷,研究人员采取对半导体进行形貌控制、元素掺杂、表面修饰及构建异质结构等修饰途径,在提高其光电催化活性的基础上也提高了其稳定性。
在光电催化分解水过程中,加入适当助催化剂,以提供更多的反应活性位点,进而促进光生载流子分离和转移,改善催化反应动力学。同时有机半导体材料由于柔性较好、价格低廉和化学性能稳定等特点成为光电催化复合材料研究热点。但多数有机半导体制备过程复杂、反应时间较长且对环境造成污染,故而探寻一种制备过程简单、价格低廉且对环境无污染的有机半导体催化材料极为重要。
发明内容
有鉴于此,本发明的目的在于提供一种高活性可见光响应的ZnS/PCPA/CoPi光电催化材料及其制备方法,制备的光电催化材料具有较高的催化活性。
为了达到上述目的,本发明提供的ZnS/PCPA/CoPi光电催化材料及其制备方法包括按顺序进行的下列步骤:
(1)将醋酸锌二水合物溶于去离子水中,制备醋酸锌溶液,将硫脲溶于去离子水中,
制备硫脲溶液,随后将硫脲溶液缓慢滴入醋酸锌溶液中,配置ZnS前驱体反应液。
(2)将洁净的FTO玻璃放入水热釜内胆中,并加入适量的ZnS前驱体反应液,在一定温度下水热反应一定时间,再将反应后的样品取出风干,制得ZnS/FTO薄膜。
(3)将一定量三羟甲基氨基甲烷、邻苯二酚和四乙烯五二胺溶于去离子水中,室温下机械搅拌,反应一段时间后得到聚(邻苯二酚/多胺)(PCPA)共聚物,将ZnS/FTO薄膜浸入上述溶液中,继续搅拌一段时间,得到由PCPA修饰的ZnS光电极。
(4)将一定量的磷酸二氢钾和磷酸氢二钾溶于去离子水中,制备PH约为7的升磷酸钾溶液,将一定量六水合硝酸钴加入上述混合溶液中,搅拌至药品完全溶解。将其转移至石英电解池中,作为电解液。采用光辅助电沉积法,以所述ZnS/PCPA为工作电极,在三电极体系中,PCPA层表面负载CoPi助催化剂,得到ZnS/PCPA/CoPi光电催化材料。
在步骤(1)中,所述的醋酸锌和硫脲的溶度分别为0.140~0.160M和0.600-1.800M。
在步骤(2)中,所述的水热反应的温度和时间分别为150~170℃和1~3h。
在步骤(3)中,所述的三羟甲基氨基甲烷、邻苯二酚和四乙烯五二胺的浓度分别为0.010~0.030M、0.022~0.026M和0.110~0.150M,浸入ZnS电极后搅拌时间为4~12h。
在步骤(4)中,所述的磷酸二氢钾、磷酸氢二钾溶液浓度为0.1M,所述的六水合硝酸钴溶液浓度为0.5mM,所述的电沉积法负载CoPi助催化剂时间为2~10min。
本发明提供的ZnS/PCPA/CoPi光电催化材料及其制备方选用PCPA作为有机半导体催化剂,其制备工艺简单、所需时间短、价格低廉且对仪器设备要求低。同时光辅助沉积法制作成本低、操作简单方便,能使CoPi助催化剂均匀分布ZnS/PCPA薄膜表层,有效提高了光电催化活性。制备的ZnS/PCPA/CoPi光电催化材料在可见光照射下能产生较强的光电流,相较于单独的ZnS电极光电流密度提升了7倍。
附图说明
图1是ZnS和ZnS/PCPA/CoPi光电流密度-时间曲线对比图。
具体实施方式
下面结合具体实施例对本发明作详细说明:
实施例一:
(1)将醋酸锌二水合物溶于去离子水中,制备0.140M醋酸锌溶液,将硫脲溶于去离子水中,制备0.600M硫脲溶液,随后将硫脲溶液缓慢滴入醋酸锌溶液中,配置ZnS前驱体反应液。
(2)将洁净的FTO玻璃放入水热釜内胆中,并加入适量的ZnS前驱体反应液,在一定150℃下水热反应1h,再将反应后的样品取出风干,制得ZnS/FTO薄膜。
(3)将三羟甲基氨基甲烷、邻苯二酚和四乙烯五二胺溶于去离子水中,制备0.010M三羟甲基氨基甲烷、0.022M邻苯二酚和0.110M四乙烯五二胺溶液,室温下机械搅拌,反应0.5h后得到聚(邻苯二酚/多胺)(PCPA)共聚物,将ZnS/FTO薄膜浸入上述溶液中,继续搅拌4h,得到由PCPA修饰的ZnS光电极。
(4)将0.5mM硝酸钴溶于0.1M磷酸二氢钾和磷酸氢二钾缓冲溶液中得到CoPi电镀液。采用光辅助电沉积法,以所述ZnS/PCPA为工作电极,在三电极体系中,PCPA层表面负载2min CoPi助催化剂,得到ZnS/PCPA/CoPi光电催化材料。
实施例二:
(1)将醋酸锌二水合物溶于去离子水中,制备0.150M醋酸锌溶液,将硫脲溶于去离子水中,制备1.200M硫脲溶液,随后将硫脲溶液缓慢滴入醋酸锌溶液中,配置ZnS前驱体反应液。
(2)将洁净的FTO玻璃放入水热釜内胆中,并加入适量的ZnS前驱体反应液,在一定160℃下水热反应2h,再将反应后的样品取出风干,制得ZnS/FTO薄膜。
(3)将三羟甲基氨基甲烷、邻苯二酚和四乙烯五二胺溶于去离子水中,制备0.020M三羟甲基氨基甲烷、0.024M邻苯二酚和0.130M四乙烯五二胺溶液,室温下机械搅拌,反应0.5h后得到聚(邻苯二酚/多胺)(PCPA)共聚物,将ZnS/FTO薄膜浸入上述溶液中,继续搅拌8h,得到由PCPA修饰的ZnS光电极。
(4)将0.5mM硝酸钴溶于0.1M磷酸二氢钾和磷酸氢二钾缓冲溶液中得到CoPi电镀液。采用光辅助电沉积法,以所述ZnS/PCPA为工作电极,在三电极体系中,PCPA层表面负载6min CoPi助催化剂,得到ZnS/PCPA/CoPi光电催化材料。
实施例三:
(1)将醋酸锌二水合物溶于去离子水中,制备0.160M醋酸锌溶液,将硫脲溶于去离子水中,制备1.800M硫脲溶液,随后将硫脲溶液缓慢滴入醋酸锌溶液中,配置ZnS前驱体反应液。
(2)将洁净的FTO玻璃放入水热釜内胆中,并加入适量的ZnS前驱体反应液,在一定170℃下水热反应3h,再将反应后的样品取出风干,制得ZnS/FTO薄膜。
(3)将三羟甲基氨基甲烷、邻苯二酚和四乙烯五二胺溶于去离子水中,制备0.030M三羟甲基氨基甲烷、0.026M邻苯二酚和0.150M四乙烯五二胺溶液,室温下机械搅拌,反应0.5h后得到聚(邻苯二酚/多胺)(PCPA)共聚物,将ZnS/FTO薄膜浸入上述溶液中,继续搅拌12h,得到由PCPA修饰的ZnS光电极。
(4)将0.5mM硝酸钴溶于0.1M磷酸二氢钾和磷酸氢二钾缓冲溶液中得到CoPi电镀液。采用光辅助电沉积法,以所述ZnS/PCPA为工作电极,在三电极体系中,PCPA层表面负载10min CoPi助催化剂,得到ZnS/PCPA/CoPi光电催化材料。
为了验证本发明的效果,本发明人给出了上述实施例1制备的ZnS和ZnS/PCPA/CoPi光电流密度-时间曲线,如图1所示。
Claims (5)
1.一种ZnS/PCPA/CoPi光电催化材料及其制备方法,其特征在于:所述的制备方法包括按顺序进行的下列步骤:
(1)将醋酸锌二水合物溶于去离子水中,制备醋酸锌溶液,将硫脲溶于去离子水中,制备硫脲溶液,随后将硫脲溶液缓慢滴入醋酸锌溶液中,配置ZnS前驱体反应液。
(2)将洁净的FTO玻璃放入水热釜内胆中,并加入适量的ZnS前驱体反应液,在一定温度下水热反应一定时间,再将反应后的样品取出风干,制得ZnS/FTO薄膜。
(3)将一定量三羟甲基氨基甲烷、邻苯二酚和四乙烯五二胺溶于去离子水中,室温下机械搅拌,反应一段时间后得到聚(邻苯二酚/多胺)(PCPA)共聚物,将ZnS/FTO薄膜浸入上述溶液中,继续搅拌一段时间,得到由PCPA修饰的ZnS光电极。
(4)将一定量的磷酸二氢钾和磷酸氢二钾溶于去离子水中,制备PH约为7的升磷酸钾溶液,将一定量六水合硝酸钴加入上述混合溶液中,搅拌至药品完全溶解。将其转移至石英电解池中,作为电解液。采用光辅助电沉积法,以所述ZnS/PCPA为工作电极,在三电极体系中,PCPA层表面负载CoPi助催化剂,得到ZnS/PCPA/CoPi光电催化材料。
2.根据权利要求1所述的ZnS/PCPA/CoPi光电催化材料及其制备方法,其特征在于:在步骤(1)中,所述的醋酸锌和硫脲的溶度分别为0.140~0.160M和0.600~1.800M。
3.根据权利要求1所述的ZnS/PCPA/CoPi光电催化材料及其制备方法,其特征在于:在步骤(2)中,所述的水热反应的温度和时间分别为150~170℃和1~3h。
4.根据权利要求1所述的ZnS/PCPA/CoPi光电催化材料及其制备方法,其特征在于:在步骤(3)中,所述的三羟甲基氨基甲烷、邻苯二酚和四乙烯五二胺溶液的浓度分别为0.010~0.030M、0.022~0.026M和0.110~0.150M,浸入ZnS电极后搅拌时间为4~12h。
5.根据权利要求1所述的ZnS/PCPA/CoPi光电催化材料及其制备方法,其特征在于:在步骤(4)中,所述的磷酸二氢钾、磷酸氢二钾溶液浓度为0.1M,所述的六水合硝酸钴溶液浓度为0.5mM,所述的电沉积法负载CoPi助催化剂时间为2~10min。
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