CN113289610A - 一种Bi2WO6/Si复合光电催化阳极材料及其制备方法 - Google Patents
一种Bi2WO6/Si复合光电催化阳极材料及其制备方法 Download PDFInfo
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Abstract
本发明涉及一种Bi2WO6/Si复合纳米阵列光电催化阳极材料，由Bi2WO6纳米花球和硅纳米线阵列组成，其制备方法采用金属辅助化学刻蚀的方法制得硅纳米线阵列，通过水热法制备Bi2WO6纳米花球，经过旋涂法将Bi2WO6纳米花球负载在硅纳米线阵列表面。本发明中采用硅纳米线阵列结构增强入射光的散射几率，提高光吸收效率；负载的Bi2WO6纳米花球可以与之形成异质结，促进光生电子空穴对的分离，从而提高光电催化降解抗生素等污染物的效率。
Description
技术领域
本发明属于光电催化降解相关技术领域，具体地涉及一种 Bi2WO6/Si复合光电催化阳极材料及其制备方法。
背景技术
近年来，随着鱼类养殖，家禽畜牧业以及医疗技术领域的不断发展，越来越多的抗生素被用于养殖与各种疾病的治疗，但随之而来的抗生素污染等问题也日趋严重，特别是含抗生素废液排放处理不当的问题，对人体健康造成很大的威胁。全球各类抗生素药物的需求量呈指数增长，抗生素废液处理不彻底的问题引起水体污染，影响人们的生活与健康。关于含抗生素废水的处理，传统的解决手段主要是通过吸附、过滤等物理方法来解决，但这些方法操作流程复杂，且难以彻底处理降解抗生素，还可能因处理不当造成环境的二次污染。光催化降解抗生素技术，因其环境友好等优点已引起广泛的关注。但目前，大多数光催化剂为粉末状，在降解过程中难以回收利用，这不仅不利于催化剂的循环使用，而且还会造成水体环境的二次污染。同时，单一光催化效率仍然偏低，因此，研发一种易于回收利用并能高效实现抗生素降解的材料及制备方法十分迫切。
发明内容
针对水体中存在的抗生素污染降解问题，本发明的目的是：提供一种易于回收利用、降解性能良好的Bi2WO6/Si复合光电催化阳极材料的制备方法，并获得高效降解抗生素的Bi2WO6/Si复合光电催化阳极材料，该材料能综合利用光能与电能，实现抗生素的高效降解，同时其片层结构易于重复使用，避免对环境造成二次污染。
为实现上述目的，本发明提供如下技术：
一种Bi2WO6/Si复合光电催化阳极材料，以硅为基底材料，制备均匀的一维硅纳米阵列，通过与Bi2WO6复合，得到Bi2WO6/Si复合光电催化阳极材料。
一种Bi2WO6/Si复合光电催化阳极材料的制备方法，采用金属辅助化学刻蚀方法制得硅纳米线阵列，通过水热法制备Bi2WO6纳米花球，经过旋涂和后处理将Bi2WO6纳米花球负载在硅纳米线阵列表面。
优选地，所述的Bi2WO6/Si复合光电催化阳极材料的制备方法，其特征在于：具体包含以下步骤：
(1)依次用丙酮、无水乙醇、去离子水清洗硅片，然后用硫酸与过氧化氢混合液彻底清洗硅片，接着将硅片放入氢氟酸中浸泡去除表面氧化层；
(2)将氢氟酸和硝酸银配制成银沉积溶液，将氢氟酸和过氧化氢配置成酸性刻蚀液，将硝酸和去离子水配成除银液；
(3)将硅片依次放入步骤(2)中的银沉积溶液、酸性刻蚀液、除银液中分别进行反应，制备得到硅纳米线阵列；
(4)将钨酸钠、硝酸铋和去离子水配置成水热反应的前驱体溶液，将前驱体溶液放入高温反应釜中进行水热反应，将水热反应后冷却得到的钨酸铋悬浊液进行离心、清洗及干燥制得花球状的钨酸铋粉末；
(5)向钨酸铋粉末中加入N-甲基吡咯烷酮配置成钨酸铋溶液，并取钨酸铋溶液均匀旋涂于硅纳米线阵列上，制备得Bi2WO6/Si复合光电催化阳极材料。
优选地，清洗硅片的硫酸与过氧化氢的体积比为3:1，氢氟酸浓度为5wt％。
优选地，银沉积溶液成分为4.8M氢氟酸和0.02M硝酸银；酸性刻蚀液成分为4.8M氢氟酸和0.3M过氧化氢；除银液由体积比为 1:1的硝酸与去离子水配置。
优选地，水热前驱体溶液成分为2.5mmol钨酸钠、5mmol硝酸铋和50mL去离子水，水热温度为135-145℃，水热时间为11-13h。
优选地，步骤(4)中离心清洗是采用去离子水和无水乙醇分别离心清洗2-4次，干燥温度为75-85℃，干燥时间为11-13h。
优选地，配置的钨酸铋溶液浓度为1mg/mL，旋涂体积为18-22 μL。
与现有技术相比，本发明的有益效果体现在：
1、相对于传统的粉末状纳米颗粒催化剂，本发明制备的 Bi2WO6/Si复合光电催化阳极材料易于重复使用，避免水体二次污染，而且因其独特的复合结构，不仅具备良好的光吸收效率，还能充分利用外加电场，实现抗生素的高效降解。
2、本发明的制备方法中对硅片进行化学刻蚀与水热生长两步即可得到Bi2WO6/Si复合光电催化阳极材料，制备简单、成本低廉。
3、本发明的Bi2WO6/Si复合光电催化阳极材料在光照条件下将水体中的OH-氧化成·OH，而·OH具有强氧化性，能够有效的降解抗生素，而Si与Bi2WO6界面的异质结构能够有效的抑制光生载流子的复合，提升降解效率，在外加电场的作用下，降解效率可以进一步提升。
附图说明
图1为Bi2WO6/Si复合光电催化阳极材料的制备流程图；
图2为Bi2WO6/Si复合光电催化阳极材料的降解机理图。
具体实施方式
以下结合实施例对本发明作进一步的说明，需要说明的是，仅仅是对本发明构思所作的举例和说明，所属本技术领域的技术人员对所描述的具体实施例做各种各样的修改或补充或采用类似的方式替代，只要不偏离发明的构思或者超越本权利要求书所定义的范围，均应视为落入本发明的保护范围。
下面将结合具体的实施例来说明本发明的内容。
实施例1：
(1)硅纳米线阵列的制备：
将硅片依次于丙酮、无水乙醇、去离子水中超声清洗15min，然后在硫酸与过氧化氢体积比为3:1的混合溶液中进行彻底清洗，接着在5wt％氢氟酸溶液中进行表面氧化成的去除，将处理后的硅片在4.8 M氢氟酸与0.02M硝酸银的混合溶液中进行银的沉积，接着在4.8M 氢氟酸与0.3M过氧化氢的酸性刻蚀液中进行刻蚀，最后在硝酸与去离子水体积比为1:1的混合溶液中将银去除，制备得硅纳米线阵列。
其中，硅片长、宽均为10mm，厚度为500μm，电阻率为1-10Ω/cm，单晶硅晶向为〈100〉。
(2)一步水热法制备Bi2WO6助催化剂：
采用2.5mmol钨酸钠、5mmol硝酸铋、50mL去离子水的混合溶液作为水热前驱体溶液，将前驱体溶液放入高压反应釜中进行水热反应，反应温度为140℃，反应时间为12h，将制得的钨酸铋悬浊液进行离心清洗并干燥，制得花球状钨酸铋粉末。
其中，离心清洗是采用去离子水和无水乙醇分别离心清洗3次，干燥温度为80℃，干燥时间为12h。
(3)Bi2WO6/Si复合光电催化阳极材料的制备
将钨酸铋粉末配置成浓度为1mg/mL的溶液，并取20μL溶液均匀旋涂于硅纳米线阵列上，制备得Bi2WO6/Si二元光电催化剂。
(4)以环丙沙星为目标降解物考察其光电催化降解性能
在CHI660D电化学工作站中，将100ml含10mg/L环丙沙星与 0.1M Na2SO4的电解质加入到一个三电极密封的电解池中进行光电化学催化降解环丙沙星性能的测量。采用Bi2WO6/Si复合光电催化阳极材料作为工作电极，铂片作为对电极，Ag/AgCl电极作为参比电极。使用装有截止波长420nm滤波片，功率为300W的氙灯光源作为模拟阳光的光源。在10mV/s的条件下，LSV电压测量范围从0V到3 V。瞬态光电流测试在2V电压下进行。在0.1Hz～1MHz频率范围内，交流振幅为10mV，进行了电化学阻抗谱(EIS)测量。光电流稳定性在不同电压下进行，同时每隔30min取5ml电解质液并用紫外可见光光度计测量在276nm波长下的吸光度，以此计算电解质液中环丙沙星的浓度。此外，试验中所有的电位都转化为可逆氢电极(RHE)，其中:ERHE＝EAg/AgCl+0.197V+0.059*PH。
在可见光照射2h、电流密度为1mA/cm2条件下，硅纳米线阵列电极对10mg/L的环丙沙星光电催化降解率为9％，而Bi2WO6/Si电极光电催化降解率提升了10％；在可见光照射2h、电流密度为10 mA/cm2条件下，硅纳米线阵列电极对10mg/L的环丙沙星光电催化降解率为16％，而Bi2WO6/Si电极光电催化降解率提升了10-15％。
Claims (8)
1.一种Bi2WO6/Si复合光电催化阳极材料，其特征在于：以硅为基底材料，制备均匀的一维硅纳米阵列，通过与Bi2WO6复合，得到Bi2WO6/Si复合光电催化阳极材料。
2.一种如权利要求1所述的Bi2WO6/Si复合光电催化阳极材料的制备方法，其特征在于：采用金属辅助化学刻蚀方法制得硅纳米线阵列，通过水热法制备Bi2WO6纳米花球，经过旋涂和后处理Bi2WO6纳米花球负载在硅纳米线阵列表面。
3.根据权利要求2所述的Bi2WO6/Si复合光电催化阳极材料的制备方法，其特征在于：具体包含以下步骤：
(1)依次用丙酮、无水乙醇、去离子水清洗硅片，然后用硫酸与过氧化氢混合液彻底清洗硅片，接着将硅片放入氢氟酸中浸泡去除表面氧化层；
(2)将氢氟酸和硝酸银配制成银沉积溶液，将氢氟酸和过氧化氢配置成酸性刻蚀液，将硝酸和去离子水配成除银液；
(3)将硅片依次放入步骤(2)中的银沉积溶液、酸性刻蚀液、除银液中分别进行反应，制备得到硅纳米线阵列；
(4)将钨酸钠、硝酸铋和去离子水配置成水热反应的前驱体溶液，将前驱体溶液放入高温反应釜中进行水热反应，将水热反应后冷却得到的钨酸铋悬浊液进行离心、清洗及干燥制得花球状的钨酸铋粉末；
(5)向钨酸铋粉末中加入去离子水配置成钨酸铋溶液，并取钨酸铋溶液均匀旋涂于硅纳米线阵列上，制备得Bi2WO6/Si复合光电催化阳极材料。
4.根据权利要求3所述的Bi2WO6/Si复合光电催化阳极材料的制备方法，其特征在于：清洗硅片的硫酸与过氧化氢的体积比为3:1，氢氟酸浓度为5wt％。
5.根据权利要求3所述的Bi2WO6/Si复合光电催化阳极材料的制备方法，其特征在于：银沉积溶液成分为4.8M氢氟酸和0.02M硝酸银；酸性刻蚀液成分为4.8M氢氟酸和0.3M过氧化氢；除银液由体积比为1:1的硝酸与去离子水配置。
6.根据权利要求3所述的Bi2WO6/Si复合光电催化阳极材料的制备方法，其特征在于：水热前驱体溶液成分为2.5mmol钨酸钠、5mmol硝酸铋和50mL去离子水，水热温度为135-145℃，水热时间为11-13h。
7.根据权利要求3所述的Bi2WO6/Si复合光电催化阳极材料的制备方法，其特征在于：步骤(4)中离心清洗是采用去离子水和无水乙醇分别离心清洗2-4次，干燥温度为75-85℃，干燥时间为11-13h。
8.根据权利要求3所述的Bi2WO6/Si复合光电催化阳极材料的制备方法，其特征在于：配置的钨酸铋溶液浓度为1mg/mL，旋涂体积为18-22μL。
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