CN107815701B - 一种纳米片状氟化铋薄膜的电化学制备方法及其应用 - Google Patents
一种纳米片状氟化铋薄膜的电化学制备方法及其应用 Download PDFInfo
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Abstract
一种纳米片状氟化铋薄膜的电化学制备方法及其应用，属于Bi基薄膜光催化材料研发、太阳能光催化剂固定化技术、有机污染物处理技术领域，可解决现有薄膜固定化技术复杂或能耗较高的问题，以Bi板作为阳极，石墨作阴极，氟化铵浓度为0.5%～1.5%的不同体积比乙二醇和蒸馏水的混合溶液作电解质，常温常压下在Bi板原位生长纳米片状BiF3薄膜，是一种简单经济可行的纳米片状Bi基催化剂薄膜固定化技术。本发明应用于罗丹明B的光催化降解，过程环保、工艺简单、易于操作、重复性强和周期短。
Description
技术领域
本发明属于Bi基薄膜光催化材料研发、太阳能光催化剂固定化技术、有机污染物处理技术领域，具体涉及一种纳米片状氟化铋薄膜的电化学制备方法及其应用。
背景技术
随着人类社会生活的快速进步与现代化工业的迅速发展，生活环境逐步面临着气液固污染物的危害，有效控制环境污染和资源环保利用已成为人类社会面临和亟待解决的重大问题之一。然而，太阳能光催化氧化技术利用可再生清洁资源太阳能处理有机污染物，因其具有能源便利、反应简单、深度矿化和无二次污染等优点而备受广泛关注。
新型高效光催化材料的研发与固定化是实现太阳能光催化氧化技术工业化的关键问题之一。研究发现，氟化铋（BiF3）具有较高的价带位置，易形成较多的强氧化性羟基自由基，且F元素具有较高的电负性，可产生电子诱导效应，进而有利于光生电子-空穴对的有效分离，加之简单水浴沉淀法即可得到具有优异紫外光光催化性能的纳米BiF3粉体催化剂，成为Bi基光催化材料的新星(J. Mol. Catal.: Chem. 401 (2015) 35-40）。为了进一步提高其光吸收能力和光催化性能，2017年，Yang等人采用水热法制备了BiOCl/BiF3粉体复合光催化剂，其光催化降解2-硝基苯酚速率是纯BiOCl和BiF3的5.3和5.8倍（Appl.Cataly.: Environ. 205 (2017) 412-420）。但是，粉体光催化剂普遍存在易团聚、分散性差、固液分离难且不易回收循环利用等缺陷，进而研究者普遍采用负载技术和薄膜固定化解决上述问题。但现有薄膜固定化技术复杂或能耗较高而且针对BiOF的薄膜固定化制备技术却至今未曾报道。
发明内容
本发明为了解决现有薄膜固定化技术复杂或能耗较高的问题，提供一种纳米片状氟化铋薄膜的电化学制备方法及其应用。
本发明采用如下技术方案：
一种纳米片状氟化铋薄膜的电化学制备方法，包括如下步骤：
第一步，配制电解质溶液，按体积比为1:20-20:1的比例分别量取乙二醇和蒸馏水，配置为100-300mL的混合溶液A，称取1-4.57g NH4F加入到上述混合溶液A中，充分搅拌使其完全溶解，配置成氟化铵浓度为0.5%～1.5%的溶液B；
第二步，打磨Bi板，采用磨砂纸打磨Bi板至光滑，并分别用乙醇和水将打磨后的Bi板冲洗干净，待用；
第三步，制备BiF3薄膜，将第二步的Bi板作阳极，石墨作阴极，阴阳电极距离为2～8 cm，溶液B作为电解质，在30～60 V电压下沉积0.5～3 h后，将Bi板取出自然晾干，即得纳米片状BiF3薄膜。
所述Bi板的尺寸为4 cm×1.5 cm×0.5 cm。
所述磨砂纸为400目的磨砂纸。
一种氟化铋薄膜应用于罗丹明B的光催化降解。
本发明以Bi板作为阳极，石墨作阴极，氟化铵浓度为0.5%～1.5%的不同体积比乙二醇和蒸馏水的混合溶液作电解质，常温常压下在Bi板原位生长纳米片状BiF3薄膜，是一种简单经济可行的纳米片状Bi基催化剂薄膜固定化技术。
常温常压下，所制备纳米片状BiF3薄膜在不同光源照射下可有效矿化罗丹明B、双酚A、苯酚任一种有机污染物。不同光源，为紫外光、可见光、模拟太阳光的任一种光源。
本发明的有益效果如下：
1. 本发明制备的薄膜为片状结构；
2. 电化学方法过程环保、工艺简单、易于操作、重复性强和周期短；
3. Bi板原位生长制备纳米片状BiF3薄膜，从物质基础属性出发制备薄膜样品，其与基体为化学结合，所以其与基体结合了强、分散均匀、不易脱落，用拉伸法测得的本发明制得的BiOF薄膜与基底结合力为25～40 MPa，比常规方法制得的薄膜与基体的结合力提高了50%～70%；
4. Bi板既为原料又作电极，避免了其他固定化催化剂多带来的繁琐工序；
5. 该电化学制备技术可推广至其他Bi基薄膜材料的应用。
附图说明
图1为本发明实施例1制备的纳米片状BiF3薄膜光催化材料的XRD图谱；
图2为本发明实施例1制备的纳米片状BiF3薄膜光催化材料的SEM图谱，放大倍数为100nm；
图3为本发明实施例1制备的纳米片状BiF3薄膜光催化材料的SEM图谱，放大倍数为200nm。
具体实施方式
实施例1，
第一步，配置300 mL体积比为20:1乙二醇和蒸馏水的混合溶液A，称取4.57g分析纯NH4F放置于溶液A中，充分搅拌使其完全溶解，作为溶液B；
第二步，采用400 目大小的磨砂纸将4 cm×1.5 cm×0.5 cm的Bi板打磨光滑，用无水乙醇和蒸馏水将打磨后的Bi板冲洗干净，待用；
第三步，将第二步的Bi板作阳极，石墨作阴极，阴阳电极距离为5 cm，溶液B作为电解质，在60 V电压下沉积0.5 h后，将Bi板取出自然晾干，即得纳米片状BiF3薄膜，记为BiF3-1。
通过扫描电镜显示，本实施例制备的BiF3薄膜为片状形貌。
实施例2，
第一步，配置200 mL容量比为15:1乙二醇和蒸馏水的混合溶液A，称取1.1 g分析纯NH4F放置于溶液A中，充分搅拌使其完全溶解，作为溶液B；
第二步，采用400 目大小的磨砂纸将4 cm×1.5 cm×0.5 cm的Bi板打磨光滑，用无水乙醇和蒸馏水将打磨后的Bi板冲洗干净，待用；
3）将第二步的Bi板作阳极，石墨作阴极，阴阳电极距离为2 cm，溶液B作为电解质，在40 V电压下沉积2 h后，将Bi板取出自然晾干，即得纳米片状BiF3薄膜，记为BiF3-2。
实施例3，
第一步，配置100 mL容量比为1:20乙二醇和蒸馏水的混合溶液A，称取1 g分析纯NH4F放置于溶液A中，充分搅拌使其完全溶解，作为溶液B；
第二步，采用400目大小的磨砂纸将4 cm×1.5 cm×0.5 cm的Bi板打磨光滑，用第一步中溶液A将打磨后的Bi板冲洗干净，待用；
第三步，将第二步的Bi板作阳极，石墨作阴极，阴阳电极距离为8 cm，溶液B作为电解质，在30 V电压下沉积3 h后，将Bi板取出自然晾干，即得纳米片状BiF3薄膜，记为BiF3-3。
BiF3薄膜应用于罗丹明B的光催化降解。
准确称取10 mg的罗丹明B，将其放入盛有900 mL蒸馏水的1000 mL定量瓶中使其充分溶解，加蒸馏水至1000 mL，制得10 mg/L的待降解液，放置24 h待用；用移液管准确移取100 mL 10 mg/L的待降解液放入分别固定好BiF3-1、BiF3-2、BiF3-3薄膜样品的光催化反应装置，室温下在避光条件下吸附1 h，以期达到吸附平衡，然后打开模拟太阳光灯，进行光催化降解实验，每隔1 h取样一次，利用紫外-可见分光光度法对溶液中的染料浓度进行分析并计算其降解率，见表1所示。
表1 罗丹明B的降解速率
从表1中看出，随着时间的延长，BiF3薄膜对罗丹明B的降解率高达98.9%。
Claims (5)
1.一种纳米片状氟化铋薄膜的电化学制备方法，其特征在于：包括如下步骤：
第一步，配制电解质溶液，按体积比为20:1 的比例分别量取乙二醇和蒸馏水，配置为300mL的混合溶液A，称取4.57g NH4F 加入到上述混合溶液A 中，充分搅拌使其完全溶解，配置成氟化铵浓度为1.5%的溶液B；
第二步，打磨Bi 板，采用磨砂纸打磨Bi 板至光滑，并分别用乙醇和水将打磨后的Bi板冲洗干净，待用；
第三步，制备BiF3 薄膜，将第二步的Bi 板作阳极，石墨作阴极，阴阳电极距离为5cm，溶液B 作为电解质，在60 V 电压下沉积0.5h 后，将Bi 板取出自然晾干，即得纳米片状BiF3 薄膜。
2.根据权利要求1 所述的一种纳米片状氟化铋薄膜的电化学制备方法，其特征在于：所述Bi 板的尺寸为4 cm×1.5 cm×0.5 cm。
3.根据权利要求1 所述的一种纳米片状氟化铋薄膜的电化学制备方法，其特征在于：所述磨砂纸为400 目的磨砂纸。
4.根据权利要求1-3任一项所述的纳米片状氟化铋薄膜的电化学制备方法得到氟化铋薄膜。
5.根据权利要求1-3任一项所述的纳米片状氟化铋薄膜的电化学制备方法得到氟化铋薄膜在罗丹明B光催化降解中的应用。
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