CN110935440A - 一种自减薄多孔三氧化钨纳米薄片材料的制备方法及其应用 - Google Patents
一种自减薄多孔三氧化钨纳米薄片材料的制备方法及其应用 Download PDFInfo
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- 239000008367 deionised water Substances 0.000 claims abstract description 11
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Abstract
本发明公开了一种自减薄多孔三氧化钨纳米薄片材料的制备方法及其应用，所述方法包括以下步骤，步骤一、材料制备：将钨网进行剪裁，分别用丙酮，乙醇，去离子水超声洗涤15min；在50mL的烧杯中加入50mL的去离子水和2.66mL的浓硫酸，搅拌，25V电压下，阳极氧化4h，钨网由黑色变为淡黄色；马弗炉500℃，升温速率为2℃/min，煅烧4h，自然冷却到室温得WO3；步骤二、第一次还原：在3V的电压下，以0.5mol/L的硫酸钠溶液为电解质，阴极还原进行9h，洗涤，烘干得1R‑WO3；步骤三、第二次还原：在3V的电压下，以0.5mol/L的硫酸钠溶液为电解质，阴极还原进行9h，洗涤，烘干得2R‑WO3；本发明工艺简单，绿色环保，操作快捷。
Description
技术领域
本发明涉及光电催化材料制备技术领域，具体涉及一种自减薄多孔三氧化钨纳米薄片材料的制备方法及其应用。
背景技术
在众多的光阳极中,三氧化钨由于其带隙窄和价带位置高而成为理想的光阳极材料之一。尽管如此,三氧化钨阳极的实际应用受到光生电子和空穴的严重复合以及电极表面缓慢反应动力学的限制。
三氧化钨已经成为一种很有前途的光电阳极材料由于它体现内在的优秀特质包括12％的太阳光谱吸收(Eg＝2.5-2.8eV),快速地电子传递速率(≈12cm2V-1S-1)相比二氧化钛(0.5cm2V-1S-1)以及有吸引力的耐光性。然而，原生WO3光阳极的光生孔在整个光阳极氧演化反应过程中，包括生成、迁移、反应等过程中，往往会遇到一系列不可避免的阻碍，光催化效率不理想。因此，为了进一步突破高电位WO3光阳极的能量转换性能，拆除综合上述制约因素势在必行。
受原子薄石墨烯类薄片的启发，超薄薄片结构为实现几乎完全暴露的高活性晶格平面提供了理想的构建块/架构，不仅如此，超薄片状结构还具有界面电荷快速传递、二维传导通道、增加载流子输运等优良特性，有利于光电催化性能的提高。遗憾的是，在暴露于WO3纳米薄片的{001}面中，沿着W-O-W链沿x方向长时间迁移的空穴，不可避免地会发生大量的电子空穴重组，严重影响了光电催化性质。为了解决这一矛盾，在超薄纳米板表面人工制造孔结构可以有效缩短光子产生孔的扩散途径。此外，孔周围丰富的未满足化学键为促进反应分子的化学反应提供了良好的化学环境，进而促进催化反应动力学。
发明内容
本发明所要解决的问题是：提供一种自减薄多孔三氧化钨纳米薄片材料的制备方法，工艺简单，绿色环保，操作快捷。
本发明为解决上述问题所提供的技术方案为：一种自减薄多孔三氧化钨纳米薄片材料的制备方法，所述方法包括以下步骤，
步骤一、材料制备：将钨网进行剪裁，分别用丙酮，乙醇，去离子水超声洗涤15min；在50mL的烧杯中加入50mL的去离子水和2.66mL的浓硫酸，搅拌，25V电压下，阳极氧化4h，钨网由黑色变为淡黄色；马弗炉500℃，升温速率为2℃/min，煅烧4h，自然冷却到室温得WO3；
步骤二、第一次还原：在3V的电压下，以0.5mol/L的硫酸钠溶液为电解质，阴极还原进行9h，洗涤，烘干得1R-WO3；
步骤三、第二次还原：在3V的电压下，以0.5mol/L的硫酸钠溶液为电解质，阴极还原进行9h，洗涤，烘干得2R-WO3；
优选的，所述步骤一中钨网的规格为1.5×4.0cm。
一种自减薄多孔三氧化钨纳米薄片材料的应用，包括以下步骤，
步骤一、制备电解液：在100mL的石英烧杯中分别加入20mL，10mg/L的氟苯尼考溶液，20mL，0.1mol/L的硫酸钠溶液，60mL的去离子水；
步骤二、氟苯尼考降解：分别用所述权利要求1中的步骤一制得三种WO3、1R-WO3、2R-WO3作为工作电极，以Pt电极作为对电极，以饱和甘汞电极作为参比电极组成三电极系统，将步骤二制备的混合液作为电解液，打开磁力搅拌器开始搅拌，在1.2V的电压，模拟太阳光下，降解氟苯尼考溶液。
与现有技术相比，本发明的优点是：本发明的制备方法具有工艺简单，绿色环保，操作快捷的优点；制备的自减薄多孔三氧化钨纳米薄片材料有效地减少了光生电子和空穴的严重复合现象。本方法制得的自减薄多孔三氧化钨纳米薄片材料可以广泛用于光电催化氧化领域。本发明制备的WO3、1R-WO3、2R-WO3三氧化钨中的纳米薄片的厚度分别为18nm、5nm、5nm，形成多孔三氧化钨纳米薄片，制备的孔洞将提供更多的活性位点。
附图说明
此处所说明的附图用来提供对本发明的进一步理解，构成本发明的一部分，本发明的示意性实施例及其说明用于解释本发明，并不构成对本发明的不当限定。
图1是本发明制备三种纳米片状(WO3、1R-WO3、2R-WO3)的材料SEM图；
图2是本发明制备三种纳米片状(WO3、1R-WO3、2R-WO3)的材料TEM图；
图3是本发明制备三种纳米片状(WO3、1R-WO3、2R-WO3)的材料AFM图；
图4是本发明制备三种纳米片状(WO3、1R-WO3、2R-WO3)的材料光电流图；
图5是本发明制备三种纳米片状(WO3、1R-WO3、2R-WO3)的材料对氟苯尼考的降解性能图；
具体实施方式
以下将配合附图及实施例来详细说明本发明的实施方式，藉此对本发明如何应用技术手段来解决技术问题并达成技术功效的实现过程能充分理解并据以实施。
一种自减薄多孔三氧化钨纳米薄片材料的制备方法，所述方法包括以下步骤，
步骤一、材料制备：将钨网剪裁成1.5×4.0cm的规格大小，分别用丙酮，乙醇，去离子水超声洗涤15min；在50mL的烧杯中加入50mL的去离子水和2.66mL的浓硫酸，搅拌，25V电压下，阳极氧化4h，钨网由黑色变为淡黄色；马弗炉500℃，升温速率为2℃/min，煅烧4h，自然冷却到室温得WO3；
步骤二、第一次还原：在3V的电压下，以0.5mol/L的硫酸钠溶液为电解质，阴极还原进行9h，洗涤，烘干得1R-WO3；
步骤三、第二次还原：在3V的电压下，以0.5mol/L的硫酸钠溶液为电解质，阴极还原进行9h，洗涤，烘干得2R-WO3；
一种自减薄多孔三氧化钨纳米薄片材料的应用，包括以下步骤，
步骤一、制备电解液：在100mL的石英烧杯中分别加入20mL，10mg/L的氟苯尼考溶液，20mL，0.1mol/L的硫酸钠溶液，60mL的去离子水；
步骤二、氟苯尼考降解：分别用所述权利要求1中的步骤一制得三种WO3、1R-WO3、2R-WO3作为工作电极，以Pt电极作为对电极，以饱和甘汞电极作为参比电极组成三电极系统，将步骤二制备的混合液作为电解液，打开磁力搅拌器开始搅拌，在1.2V的电压，模拟太阳光下，降解氟苯尼考溶液。
图1是试验一制备三种纳米片状(WO3、1R-WO3、2R-WO3)材料SEM图，从图中可以看出原始三氧化钨材料为花状纳米片，一次还原后，三氧化钨片的还原后依旧保持花状结构。
图2是试验一制备三种纳米片状(WO3、1R-WO3、2R-WO3)材料TEM图；从图中可以看2R-WO3纳米片上的孔径大于1R-WO3纳米片上的孔径
图3试验一制备三种纳米片状(WO3、1R-WO3、2R-WO3)材料AFM图；从图中可以看出，还原后的三氧化钨材料片的厚度从WO3的18nm纳米片厚度减少到1R-WO3、2R-WO3的5nm纳米片厚度，有一个剧减变薄的现象。
图4试验一制备三种纳米片状(WO3、1R-WO3、2R-WO3)材料光电流图；从图中可以看出，还原后的三氧化钨材料片的光电流效果更好。
图5试验一制备三种纳米片状(WO3、1R-WO3、2R-WO3)的WO3材料对氟苯尼考的降解性能；从图中可以看出，改性后的材料对氟苯尼考的降解高达90％，说明改性后的材料光生电子与空穴的符合率降低，活性位点增多，加大了对污染物氟苯尼考的降解。
以上仅就本发明的最佳实施例作了说明，但不能理解为是对权利要求的限制。本发明不仅局限于以上实施例，其具体结构允许有变化。凡在本发明独立权利要求的保护范围内所作的各种变化均在本发明保护范围内。
Claims (3)
1.一种自减薄多孔三氧化钨纳米薄片材料的制备方法，其特征在于：所述方法包括以下步骤，
步骤一、材料制备：将钨网进行剪裁，分别用丙酮，乙醇，去离子水超声洗涤15min；在50mL的烧杯中加入50mL的去离子水和2.66mL的浓硫酸，搅拌，25V电压下，阳极氧化4h，钨网由黑色变为淡黄色；马弗炉500℃，升温速率为2℃/min，煅烧4h，自然冷却到室温得WO3；
步骤二、第一次还原：在3V的电压下，以0.5mol/L的硫酸钠溶液为电解质，阴极还原进行9h，洗涤，烘干得1R-WO3；
步骤三、第二次还原：在3V的电压下，以0.5mol/L的硫酸钠溶液为电解质，阴极还原进行9h，洗涤，烘干得2R-WO3。
2.根据权利要求1所述的一种自减薄多孔三氧化钨纳米薄片材料的制备方法，其特征在于：所述步骤一中钨网的规格为1.5×4.0cm。
3.一种如权利要求1或2所述的自减薄多孔三氧化钨纳米薄片材料的制备方法制得的自减薄多孔三氧化钨纳米薄片材料的应用，其特征在于：包括以下步骤，
步骤一、制备电解液：在100mL的石英烧杯中分别加入20mL，10mg/L的氟苯尼考溶液，20mL，0.1mol/L的硫酸钠溶液，60mL的去离子水；
步骤二、氟苯尼考降解：分别用所述权利要求1中的步骤一制得三种WO3、1R-WO3、2R-WO3作为工作电极，以Pt电极作为对电极，以饱和甘汞电极作为参比电极组成三电极系统，将步骤二制备的混合液作为电解液，打开磁力搅拌器开始搅拌，在1.2V的电压，模拟太阳光下，降解氟苯尼考溶液。
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