CN115555020A - 一种银/钒酸银纳米棒复合材料的微波水热制备及其应用 - Google Patents
一种银/钒酸银纳米棒复合材料的微波水热制备及其应用 Download PDFInfo
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Abstract
本发明公开了一种银/钒酸银纳米棒复合材料的微波‑水热制备方法，该微波‑水热合成系统具有时间和温度编程的能力，能够快速地优化实验因素，对创建大量的合成配方，制备高质量的纳米材料，和大规模的工业生产大有裨益；该催化剂促进了AgVO3和Ag纳米颗粒之间的电荷转移，减小了钒酸银的带隙，扩展了其光学吸收，有效提高了二氧化钛的光催化性能。其次，该材料的一维纳米棒结构表面上的更大的纵横比和更有效的电荷分离将促进的光催化活性，在光催化降解罗丹明B(RhB)方面表现出较高的活性，在污水处理领域具有潜在的应用前景。
Description
技术领域
本发明属于半导体光催化材料技术领域，具体地说，涉及一种可以提高可见光光催化降解污染物活性的银/钒酸银纳米棒复合材料的微波-水热制备及其应用。
背景技术
近年来，如何处理随着社会经济的快速发展而带来的环境污染问题成为热点。半导体光催化技术作为一门新兴技术，不仅能够光催化分解水产氢作为清洁能源，而且还可以光催化降解污染物，越来越受到人们的普遍关注。光催化材料的合成方法是对于光催化材料的性能和应用价值至关重要，经过不同途径合成出来的光催化材料在结构，形貌，尺寸等方面都会有一定程度的影响，而这些也会进一步使得光催化性能产生差异。
因为二氧化钛相对较宽的带隙(3.2eV)使它对紫外线照射的响应仅为太阳能的4％，限制了其光催化应用。因此，人们近年来致力于开发新的可见光驱动催化剂来有效利用可见光。在银钒氧化物(SVOs)中，AgVO3材料因带隙宽度较小(2.3eV)，而具有良好的可见光响应。但由于AgVO3分离电子空穴对的能力较低，因此其光催化活性仍然不显著，限制了其实际的广泛应用。因此，需要进一步研究其光催化性能以供实际应用。专利CN106140159B将硝酸银加入到葡萄糖和五氧化二钒混合溶液中，用氨水调节pH值，采用沉淀辅助微波水热法合成制备棒状AgVO3纳米光催化剂，得到的偏钒酸银粉末为单晶结构，具有较大的比表面积，提高了材料的光催化性能；Zhao等人在Facile in-suit synthesis of Ag/AgVO3one-dimensional hybrid nanoribbons with enhanced performance of plasmonicvisible-light photocatalysis中，通过硼氢化钠在室温下原位还原AgVO3，合成了新型一维Ag/AgVO3等离子体光催化剂，结果表明，Ag/AgVO3的光催化效率优于AgVO3。
针对上述问题，在本发明中，我们首次提出了以NH4VO3和AgNO3为原材料，采用简单的微波-水热法制备了银/钒酸银纳米棒复合材料，并通过光催化降解罗丹明B(RhB)测试了其光催化活性。据我们所知，这种Ag/AgVO3纳米棒光催化剂的新型合成尚未见报道。
发明内容
本发明的目的是在于提供了一种以银为掺杂元素的钒酸银纳米棒复合材料的制备方法，该制备方法采用微波水热法实现，具有工艺简单，操作方便，适合大规模生产等优点。该催化剂有效提高了钒酸银的光催化性能，在光催化降解罗丹明B(RhB)方面表现出较高的活性。
为了实现上述目的，本发明采取了如下技术方案：
一种以银为掺杂元素的钒酸银纳米棒复合光催化材料，首先以简单的水热法制备了钒酸银纳米棒，然后以微波水热180℃制备了银/钒酸银纳米棒复合材料。
具体步骤如下：
1.NH4VO3(2mmol,0.24g)溶100ml,85℃水中，再加入不同含量AgNO3(2-4mmol,0.34-0.68g)搅拌5min，得到黄色絮状物，浸泡水洗8-10次，再经水离心洗涤3次,得到样品钒酸银纳米棒C-2(2mmol),C-4(4mmol)。
2.NH4VO3(2mmol,0.24g)溶于100ml,85℃水中，再加入不同含量AgNO3(2-4mmol,0.34-0.68g)搅拌5min，得到黄色絮状物,再将絮状物微波水热180℃，30min,将得到的沉淀经过滤洗涤得到样品银/钒酸银纳米棒MW-2(2mmol),MW-4(4mmol)。
本发明与现有技术相比，本发明的有益效果为：
(1)本发明制备银/钒酸银纳米棒复合材料的微波水热制备法，微波-水热合成系统(MDS-6,Sineo,Shanghai,China)具有时间和温度编程的能力，能够快速地优化实验因素。这对创建大量的合成配方，制备高质量的纳米材料，和大规模的工业生产大有裨益。
(2)本发明制备的银/钒酸银纳米棒复合光催化剂提高了光催化降解污染物活性。针对目前应用光催化方法解决环境污染效率较低的问题，通常有两种方法来提高其可见的光催化活性。一是设计具有不同形态的特定结构，从而获得更好的性能。其中，一维(1D)结构具有较高的活性，因为它们具有较大的长径比，表面存在广泛的电荷分离。另一种方法是与由贵金属(如Au和Ag)制成的等离子体纳米粒子(NPs)结合，由于其较强的表面等离子体共振(SPR)，在较宽的可见光谱范围内具有较高的吸收系数。在我们合成的材料中，掺杂的银纳米颗粒具有较高的导电率和电子存储能力，因此在AgVO3导带中产生的电子会迅速转移到Ag纳米颗粒上，促进了AgVO3和Ag纳米颗粒之间的电荷转移，银纳米颗粒中的光生电子和从AgVO3转移的光生电子可以被O2-捕获，形成O2-活性氧显著提高了光催化活性；其次，独特的一维纳米棒结构表面上的更大的纵横比和更有效的电荷分离将促进的光催化活性。
(3)本发明制备/钒酸银纳米棒复合材料的制备方法，具备工艺条件温和、操作简便、适合大规模生产等特点。
附图说明
图1为实施例1，本发明所制备的光催化剂的X射线衍射(XRD)图谱；
图2为实施例1，本发明所制备的光催化剂的扫描电镜(SEM)形貌图；
图3为实施例1，本发明所制备样品的紫外-可见吸收光谱(UV-Vis)图；
图4为实施例1，本发明所制备的光催化剂在可见光辐射下罗明丹的降解效果图；
具体实施方式：
下面将结合具体的实施例对本发明的技术方案做进一步的详细说明。应理解，所举实施例的目的在于进一步阐述本发明的内容，而不能在任何意义上解释为对本发明保护范围的限制。
实施例1：
银/钒酸银纳米棒复合光催化材料的制备方法，步骤如下：
步骤1、钒酸银纳米棒的制备：
1.1将NH4VO3(2mmol,0.24g)溶于100ml,85℃水中，再加入不同含量AgNO3(2-4mmol,0.34-0.68g)搅拌5min，得到黄色絮状物；
1.2再将絮状物浸泡水洗8-10次，再经水离心洗涤3次,得到样品C-2(2mmol),C-4(4mmol)；
步骤2、银/钒酸银纳米棒的制备：
2.1将NH4VO3(2mmol,0.24g)溶于100ml,85℃水中，再加入不同含量AgNO3(2-4mmol,0.34-0.68g)搅拌5min，得到黄色絮状物；
2.2再将絮状物微波水热180℃，30min,将得到的沉淀经过滤洗涤得到样品MW-2(2mmol),MW-4(4mmol)；
为了验证银/钒酸银纳米棒复合材料相对钒酸银的性能提升，对上述实施例1中所得材料进行光催化降解罗丹明B(RhB)水溶液活性实验，具体步骤如下：
(1)将0.1g的样品分散在浓度为1×10-5M的20mL RhB水溶液中，置于9.0cm培养皿中；
(2)在可见光照射前，让混合溶液在光催化剂、RhB和水之间达到吸附-解吸平衡，然后在距离反应溶液25cm处放置350W氙灯作为可见光源，触发光催化反应；
(3)用紫外滤光片将波长小于400nm的紫外光全部滤光。在可见光照射之前，让溶液在光催化剂、RhB和水之间达到吸附-解吸平衡30分钟。用紫外-可见分光光度计(UV-2550，日本岛津)测定RhB的浓度；
(4)在可见光照射一段时间后(每15min)，过滤反应溶液，测量RhB的浓度变化。为了进一步确定材料提升的性能，我们同时测定了C-2和MW-2样品的RhB降解活性作为参考。
由图1可见实施例1所制备样品的XRD对比图，均显示钒酸银AgVO3的晶体结构，说明Ag/AgVO3不会改变材料的晶体结构。
图2为实施例1，图2a和图2b为步骤一所合成的钒酸银AgVO3纳米棒(C-4)的扫描电镜(SEM)图，图2c和图2d为步骤二所合成的Ag/AgVO3纳米棒(MW-4)的扫描电镜(SEM)图，可以看出，所合成样品具有纳米棒结构且钒酸银纳米棒上吸附了银纳米颗粒，成功制备了银/钒酸银纳米棒复合光催化材料。
图3为实施例1，所制备光催化剂体系的紫外-可见吸收光谱；可以看出，吸收带边发生了红移,提升了材料的光吸收性能。
图4为实施例1，制备的光催化剂在可见光辐射下罗明丹的降解效果图，可以看出，所合成的C-4和MW-4复合材料降解效率相对C-2和MW-2都有了很大提升，其中MW-4表现出最高的降解活性，体现了本发明所制备材料的优越性。
应当指出，以上所述具体实施方式可以使本领域的技术人员更全面地理解本发明，但不以任何方式限制本发明。因此，本领域技术人员应当理解，仍然可以对本发明进行修改或者等同替换；而一切不脱离本发明的精神和技术实质的技术方案及其改进，其均应涵盖在本发明专利的保护范围当中。
Claims (5)
1.一种银/钒酸银纳米棒复合材料的微波-水热制备法，其特征在于，材料由微波-水热制备而成，其合成过程中未加入任何有机或无机溶剂，材料具有纳米棒结构。
2.根据权利要求1所述复合材料的制备方法，其特征在于，步骤如下：
将NH4VO3 (2 mmol, 0.24 g)溶100 ml, 85℃水中，再加入不同含量AgNO3 (2-4mmol,0.34-0.68 g)搅拌5 min，得到黄色絮状物，浸泡水洗8-10次，再经水离心洗涤3次,得到样品钒酸银纳米棒C-2 (2 mmol), C-4 (4 mmol)。
3.根据权利要求2所述的制备方法，其特征在于，步骤如下，将NH4VO3 (2 mmol, 0.24g)溶于100 ml, 85℃水中，再加入不同含量AgNO3 (2-4mmol, 0.34-0.68 g)搅拌5 min，得到黄色絮状物,再将絮状物微波水热180 ℃，30 min,将得到的沉淀经过滤洗涤得到样品银/钒酸银纳米棒MW-2 (2 mmol), MW-4 (4 mmol)。
4.根据权利要求2-3项中所述方法制备得到的银/钒酸银纳米棒复合材料。
5.一种权利要求4所述复合光催化材料的应用，其特征在于，所述材料作为光催化剂在光降解罗丹明B (RhB)中的应用。
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