CN113083267B - 一种用于光电催化降解罗丹明B的TiO2/Ce-BaTiO3复合薄膜材料的制备方法 - Google Patents
一种用于光电催化降解罗丹明B的TiO2/Ce-BaTiO3复合薄膜材料的制备方法 Download PDFInfo
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Abstract
本发明公开一种用于光电催化降解罗丹明B的TiO2/Ce‑BaTiO3复合薄膜材料的制备方法。该方法首先采用水热法制备TiO2薄膜,然后将TiO2薄膜作为反应基底,采用水热法进行原位转化将掺Ce的BaTiO3纳米晶粒负载到TiO2薄膜上,最终得到Ce掺杂的TiO2/Ce‑BaTiO3复合薄膜材料。所制备的复合薄膜材料提升了TiO2的可见光吸收及载流子分离效率,促进了光电催化性能的提高,制备方法简单易操作,整体成本低廉。
Description
技术领域
本发明属于光电催化薄膜材料制备技术领域,具体为一种用于光电催化降解罗丹明B的TiO2/Ce-BaTiO3复合薄膜材料的制备方法。
背景技术
当今社会,环境和能源问题已经引起越来越多人的关注。随着工业的不断发展,工业废水的随意排放,导致水污染和空气污染日益严重,给人类的健康带来巨大的威胁。因此,亟需寻找一种高效的降解污染物的催化剂用于环境的治理。自二氧化钛(TiO2)电极上的光电催化分解水以来,由于在太阳能的能量转换和催化降解方面的独特性能,同时TiO2廉价、无毒无害、化学性质稳定,使其成为当之无愧的最传统的光电催化半导体材料。但是,TiO2的带隙(~3.2eV)较宽,不能够有效地利用太阳光,这将极大地限制其应用;与此同时,TiO2激发产生的电子和空穴很容易复合,使得光生载流子的量子效率降低,从而降低了光电催化效率。因此,为了提高光电催化效率,多相光电催化的发展进入了新时代。
钛酸钡(BaTiO3)是一种典型的铁电材料,具有热释电性、压电性、线性电光效应和非线性光学等效应,广泛用于光电子技术领域。然而在光电催化降解污染物方面的研究不是很多。在此,通过20~50℃的冷热交替来激发BaTiO3的热电效应,进而产生极化电场驱动TiO2载流子的分离和转移,提升TiO2的催化效率。但是BaTiO3对可见光的利用效率仍不能令人满意,而Ce的掺入可以有效调节BaTiO3的费米能级,降低导带的位置,拓宽光吸收范围,提升TiO2复合薄膜的催化效率。
发明内容
为了解决TiO2纳米棒在光电催化降解方面的上述问题,本发明的目的在于提供一种光电催化复合薄膜材料的制备方法,能够提升TiO2的光电催化降解性能。
为了达到上述目的,本发明提供光电催化降解罗丹明B的TiO2/Ce-BaTiO3复合薄膜材料的制备方法包括按顺序进行的下列步骤:
(1)将稀盐酸与去离子水按1∶1的比例混合均匀后,将钛酸四丁酯溶液滴入混合液中搅拌均匀,制备TiO2前驱体反应液。将FTO导电玻璃以导电面朝下的方式放入到已加入反应液的反应釜内胆中,在一定温度下水热反应一定时间后,将反应后的样品进行干燥处理。再将样品放到坩埚中,转移到马弗炉中处理,制得附在FTO 导电玻璃上的棒状结构的TiO2薄膜。
(2)将二乙二醇、异丙醇、四丁基氢氧化铵溶液加入到去离子水中配制混合溶剂,将八水合氢氧化钡和氢氧化铈按比例溶于配制好的溶液中,采用水热法进行原位转化将掺Ce的BaTiO3纳米晶粒负载到TiO2薄膜上,再经过马沸炉退火处理,制得 Ce掺杂BaTiO3纳米晶粒包裹的TiO2/Ce-BaTiO3复合薄膜材料。
在步骤(1)中,所述的钛酸四丁酯的体积为0.500~1.000mL,水热反应的温度和时间分别为160~180℃和18~24h,干燥箱中干燥2~4h,再将FTO放到坩埚中热处理2h,温度为500~600℃。
在步骤(2)中,所述的八水合氢氧化钡溶度为0.500~1.000mM,氢氧化铈的掺入比例2~10%,水热反应的温度和时间分别为180~200℃和6~10h,干燥箱中干燥 1h,再将FTO放入到坩埚中热处理2h,温度为450~550℃。
本发明提供的一种用于光电催化降解罗丹明B的TiO2/Ce-BaTiO3复合薄膜材料的制备方法具有如下有益效果:
(1)本发明能够有效拓宽可见光吸收范围。
(2)热电效应产生的极化场可以驱动光生电子-空穴对的分离。
(3)本发明的制备方法简单易操作,整体成本低廉。
(4)本发明所制得的TiO2/Ce-BaTiO3复合薄膜材料可见光吸收优异,光电催化性能较高。
附图说明
图1为实施例中所得TiO2/Ce-BaTiO3薄膜复合材料对罗丹明B的降解率。
具体实施方式
下面的实施例可以使本专业技术人员更全面的理解本发明,但不以任何方式限制本发明。
实施例1
一种用于光电催化降解罗丹明B的TiO2/Ce-BaTiO3复合薄膜材料的制备方法,包括如下步骤:
(1)将10mL稀盐酸与去离子水按1∶1的比例混合均匀后,将0.5mL钛酸四丁酯溶液滴入混合液中搅拌均匀,将FTO导电玻璃以导电面朝下的方式放入到已加入反应液的反应釜内胆中,在160℃下水热反应18h后,将反应后的样品进行干燥处理。再将样品放到坩埚中,转移到马弗炉中500℃退火处理2h,制得附在FTO导电玻璃上的棒状结构的TiO2薄膜。
(2)将5mL二乙二醇、5mL异丙醇、3mL四丁基氢氧化铵溶液加入到5mL去离子水中配制混合溶剂,将0.5mM八水合氢氧化钡和0.05mM氢氧化铈按比例溶于配制好的溶液中,磁力搅拌溶液0.5h,将FTO导电玻璃以导电面朝下的方式放入到已加入反应液的反应釜内胆中,在180℃下水热反应10h后,干燥箱中干燥1h,再将FTO置入到方舟中550℃热处理2h,制得含10%的Ce掺杂BaTiO3纳米晶粒包裹的 TiO2/Ce-BaTiO3复合薄膜材料。
实施例2
一种用于光电催化降解罗丹明B的TiO2/Ce-BaTiO3复合薄膜材料的制备方法,包括如下步骤:
(1)将10mL稀盐酸与去离子水按1∶1的比例混合均匀后,将0.8mL钛酸四丁酯溶液滴入混合液中搅拌均匀,将FTO导电玻璃以导电面朝下的方式放入到已加入反应液的反应釜内胆中,在180℃下水热反应16h后,将反应后的样品进行干燥处理。再将样品放到坩埚中,转移到马弗炉中550℃退火处理2h,制得附在FTO导电玻璃上的棒状结构的TiO2薄膜。
(2)将5mL二乙二醇、5mL异丙醇、3mL四丁基氢氧化铵溶液加入到5mL去离子水中配制混合溶剂,将0.5mM八水合氢氧化钡和0.025mM氢氧化铈按比例溶于配制好的溶液中,磁力搅拌溶液0.5h,将FTO导电玻璃以导电面朝下的方式放入到已加入反应液的反应釜内胆中,在200℃下水热反应8h后,干燥箱中干燥1h,再将FTO置入到坩埚中500℃热处理2h,制得含5%的Ce掺杂BaTiO3纳米晶粒包裹的 TiO2/Ce-BaTiO3复合薄膜材料。
实施例3
一种用于光电催化降解罗丹明B的TiO2/Ce-BaTiO3复合薄膜材料的制备方法,包括如下步骤:
(1)将10mL稀盐酸与去离子水按1∶1的比例混合均匀后,将1.0mL钛酸四丁酯溶液滴入混合液中搅拌均匀,将FTO导电玻璃以导电面朝下的方式放入到已加入反应液的反应釜内胆中,在180℃下水热反应20h后,将反应后的样品进行干燥处理。再将样品放到坩埚中,转移到马弗炉中600℃退火处理2h,制得附在FTO导电玻璃上的棒状结构的TiO2薄膜。
(2)将5mL二乙二醇、5mL异丙醇、3mL四丁基氢氧化铵溶液加入到5mL去离子水中配制混合溶剂,将0.5mM八水合氢氧化钡和0.01mM氢氧化铈按比例溶于配制好的溶液中,磁力搅拌溶液0.5h,将FTO导电玻璃以导电面朝下的方式放入到已加入反应液的反应釜内胆中,在200℃下水热反应10h后,干燥箱中干燥1h,再将FTO置入到坩埚中450℃热处理2h,制得含2%的Ce掺杂BaTiO3纳米晶粒包裹的 TiO2/Ce-BaTiO3复合薄膜材料。
以上通过实施例对本发明进行了详细说明,但所述内容仅为本发明的示例性实施例,不能被认为用于限定本发明的实施范围。本发明的保护范围由权利要求书限定。凡利用本发明所述的技术方案,或本领域的技术人员在本发明技术方案的启发下,在本发明的实质和保护范围内,设计出类似的技术方案而达到上述技术效果的,或者对申请范围所作的均等变化与改进等,均应仍归属于本发明的专利涵盖保护范围之内。应当注意,为了清楚的进行表述,本发明的说明中省略了部分与本发明的保护范围无直接明显的关联但本领域技术人员已知的部件和处理的表述。
Claims (3)
1.一种用于光电催化降解罗丹明B的TiO2/Ce-BaTiO3复合薄膜材料的制备方法, 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)将稀盐酸与去离子水按1∶1的比例混合均匀后,将钛酸四丁酯溶液滴入混合液中搅拌均匀,制备TiO2前驱体反应液; 将FTO导电玻璃以导电面朝下的方式放入到已加入反应液的反应釜内胆中,在一定温度下水热反应一定时间后,将反应后的样品进行干燥处理;再将样品放到坩埚中,转移到马弗炉中处理,制得附在FTO导电玻璃上的棒状结构的TiO2薄膜;
(2)将二乙二醇、异丙醇、四丁基氢氧化铵溶液加入到去离子水中配制混合溶剂,将八水合氢氧化钡和氢氧化铈按比例溶于配制好的溶液中,采用水热法进行原位转化将掺Ce的BaTiO3纳米晶粒负载到TiO2薄膜上,再经过马弗 炉退火处理,制得Ce掺杂BaTiO3纳米晶粒包裹的TiO2/Ce-BaTiO3复合薄膜材料。
2.根据权利要求1所述的用于光电催化降解罗丹明B的TiO2/Ce-BaTiO3复合薄膜材料的制备方法,其特征在于:在步骤(1)中,所述的钛酸四丁酯的体积为0.500~1.000mL,水热反应的温度和时间分别为160~180℃和18~24h,干燥箱中干燥2~4h,再将FTO放入到坩埚中热处理2h,温度为500~600℃。
3.根据权利要求1所述的用于光电催化降解罗丹明B的TiO2/Ce-BaTiO3复合薄膜材料的制备方法,其特征在于:在步骤(2)中,所述的八水合氢氧化钡溶度为0.500~1.000mM,氢氧化铈的掺入比例2~10%,通过水热法将TiO2原位转化为BaTiO3纳米晶粒,制备掺入一定量Ce的TiO2/Ce-BaTiO3复合薄膜材料。
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