CN111068657B - 一种Mo掺杂诱导水热制备BiVO4空心立方体的方法 - Google Patents
一种Mo掺杂诱导水热制备BiVO4空心立方体的方法 Download PDFInfo
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Abstract
本发明涉及一种Mo掺杂诱导水热制备BiVO4空心立方体的方法，属于半导体光催化材料制备技术领域，其特征在于包括以下步骤：以五水合硝酸铋和偏钒酸铵为金属源，四水合钼酸铵作为Mo掺杂剂，加入量为7%‑9%，用NaOH调节混合溶液pH值为5；在180℃下水热反应24h；然后经抽滤、洗涤和烘干，最后于400℃下保温5h，即得到Mo掺杂的BiVO4空心立方体。本发明制备得到的Mo掺杂BiVO4空心立方体形貌结构可控，具有工艺过程简单、可重复性高等特点。
Description
技术领域
本发明属于半导体光催化材料制备技术领域，具体涉及一种Mo掺杂诱导水热制备BiVO4空心立方体的方法。
背景技术
近年来，从纺织、造纸、印刷、染色和农业工业排出的废水中包含大量的有机和无机污染物，如染料和重金属离子等，是污染水源的罪魁祸首，对人体健康和生态系统具有严重的危害。因此，迫切需要寻找一种有效方法解决废水处理问题。半导体光催化技术作为一种绿色技术，以其室温深度反应和可直接利用太阳光作为光源来驱动反应等独特性能而成为一种理想的环境污染治理技术，可以将水中难降解的有毒污染物分解为小分子无毒物质，对解决环境污染问题具有十分大的潜在应用价值。
在众多可见光响应型半导体材料中，BiVO4由于具有合适的带隙结构、良好的水相稳定性、无毒等优点而引起人们的广泛关注。然而，纯相BiVO4存在光生电子空穴对复合快等缺点而限制其实际应用。因此，常需对其进行改性，如掺杂、形貌调控、半导体复合、贵金属沉积等。其中，掺杂被认为是一种简单有效的改性手段。Tian等采用水热法，通过掺杂不同量的Mo，合成出饼状BiVO4样品，相比于纯BiVO4样品，Mo掺杂BiVO4样品表现出更好的光催化性能（X Tian, et al. J. Mater. Sci.: Mater. El., 2019, 30: 19335-19342）。
此外，研究报道发现，催化剂的形貌结构与催化性能密切相关。其中，空心结构由于具有较大比表面积，不仅可以增加催化剂与底物之间的接触面积，而且具有较多的催化活性位点。此外，空心结构可以缩短光生载流子的迁移距离，从而降低复合几率，增强光催化性能。专利CN 101746824A以聚乙烯吡咯烷酮为表面活性剂，采用水热法合成了空心球状多孔BiVO4，表现出较好的光催化性能。Chen等以赖氨酸为表面活性剂，Ag为复合剂，当Ag复合量为6.5wt%时可诱导合成空心球状结构Ag/BiVO4复合物，相比于纯BiVO4和Ag掺杂BiVO4样品，该复合物样品表现出更好的光催化活性（L Chen, et al. RSC Adv., 2013, 3:24354-24361）。
迄今为止，尚无文献和专利报道过以Mo掺杂诱导水热制备BiVO4空心立方体的方法。
发明内容
本发明的目的在于提供一种Mo掺杂诱导水热制备BiVO4空心立方体的方法，本发明制备的Mo掺杂BiVO4样品为四方白钨矿结构，形貌为规整的空心立方体结构，直径约0.6-0.7μm，吸收边界为510nm。
本发明采用的技术方案如下：
步骤1. 在搅拌条件下，将摩尔比为1-x：x（x为7-9%，总物质的量为8mmol）的偏钒酸铵和钼酸铵溶解于30mL热水（80℃）中，标记为A液；
步骤2. 在超声条件下，将8mmol硝酸铋溶解于30mL乙二醇中，标记为B液；
步骤3. 在室温搅拌条件下，将步骤1得到的A液逐滴加入步骤2得到的B液中，继续搅拌30min；
步骤4. 用2mol/L的NaOH溶液调节步骤3所得混合溶液的pH值为5，继续搅拌30min；
步骤5. 将步骤4得到的溶液转移至100mL反应釜内衬中，将密封好的反应釜置于恒温烘箱中于180℃下水热反应24h；
步骤6. 待自然冷却至室温后，取出样品对其进行抽滤，用去离子水和乙醇洗涤3次，将所得固体产物于60℃烘干12h，然后以5℃/min的升温速率升温到400℃，保温5h，即得到Mo掺杂的BiVO4空心立方体。
本发明以硝酸铋和偏钒酸铵为金属源，钼酸铵为钼源，作为掺杂剂，采用水热法制备BiVO4空心立方体。Mo掺杂量对BiVO4空心立方体的形成起到重要作用。
本发明的有益效果在于：
（1）本发明以Mo作为掺杂剂，通过调控钼酸铵的加入量，诱导水热制备BiVO4空心立方体；
（2）本发明制备的Mo掺杂BiVO4空心立方体具有原料廉价易得、制备工艺简单、形貌和结构可控、可重复性高等优点；
（3）本发明制备的Mo掺杂BiVO4空心立方体，增大了催化剂与污染物之间的接触面积，缩短了光生电子和空穴的迁移距离，降低了光生载流子的复合几率，可以有效降解水中污染物，在污水处理方面具有优良的应用前景。
附图说明
为了进一步了解本发明，下面以实施例作详细说明，并给出附图描述本发明得到的Mo掺杂BiVO4空心立方体，其中：
图1为制得的Mo掺杂BiVO4空心立方体的X射线衍射（XRD）谱图，其中曲线（A）和（B）分别为实施例1和实施例3样品的XRD谱图，曲线（C）为四方白钨矿相BiVO4（JCPDS No. 78-1534）标准卡片。
图2为制得的Mo掺杂BiVO4空心立方体的扫描电子显微镜（SEM）照片，其中图2（A）和2（B）分别为实施例1和实施例3样品的SEM照片。
图3为制得的Mo掺杂BiVO4空心立方体的紫外-可见漫反射（UV-vis DRS）谱图，其中曲线（A）和（B）分别为实施例1和实施例3样品的UV-vis DRS谱图。
具体实施方式
实施例1：
步骤1. 在搅拌条件下，将摩尔比为0.93：0.07（总物质的量为8mmol）的偏钒酸铵和钼酸铵溶解于30mL热水（80℃）中，标记为A液；
步骤2. 在超声条件下，将8mmol硝酸铋溶解于30mL乙二醇中，标记为B液；
步骤3. 在室温搅拌条件下，将步骤1得到的A液逐滴加入步骤2得到的B液中，继续搅拌30min；
步骤4. 用2mol/L的NaOH溶液调节步骤3所得混合溶液的pH值为5，继续搅拌30min；
步骤5. 将步骤4得到的溶液转移至100mL反应釜内衬中，将密封好的反应釜置于恒温烘箱中于180℃下水热反应24h；
步骤6. 待自然冷却至室温后，取出样品对其进行抽滤，用去离子水和乙醇洗涤3次，将所得固体产物于60℃烘干12h，然后以5℃/min的升温速率升温到400℃，保温5h，即得到Mo掺杂的BiVO4空心立方体。
经实施例1制得的Mo掺杂BiVO4空心立方体的X射线衍射（XRD）谱图见图1中曲线（A），扫描电子显微镜（SEM）照片见图2（A），以及紫外-可见漫反射（UV-vis DRS）谱图见图3中曲线（A）。结果表明，制得的BiVO4样品为四方白钨矿结构，相比于标准卡片JCPDS No.78-1534，X射线衍射峰向小角度方向偏移，原因是Mo6+离子半径稍大于V5+离子半径，意味着Mo成功掺杂进入BiVO4晶格，样品形貌为规整的空心立方体，直径约0.7μm，吸收边界为510nm。
实施例2：
步骤1. 在搅拌条件下，将摩尔比为0.92：0.08（总物质的量为8mmol）的偏钒酸铵和钼酸铵溶解于30mL热水（80℃）中，标记为A液；
步骤2. 在超声条件下，将8mmol硝酸铋溶解于30mL乙二醇中，标记为B液；
步骤3. 在室温搅拌条件下，将步骤1得到的A液逐滴加入步骤2得到的B液中，继续搅拌30min；
步骤4. 用2mol/L的NaOH溶液调节步骤3所得混合溶液的pH值为5，继续搅拌30min；
步骤5. 将步骤4得到的溶液转移至100mL反应釜内衬中，将密封好的反应釜置于恒温烘箱中于180℃下水热反应24h；
步骤6. 待自然冷却至室温后，取出样品对其进行抽滤，用去离子水和乙醇洗涤3次，将所得固体产物于60℃烘干12h，然后以5℃/min的升温速率升温到400℃，保温5h，即得到Mo掺杂的BiVO4空心立方体。
实施例3：
步骤1. 在搅拌条件下，将摩尔比为0.91：0.09（总物质的量为8mmol）的偏钒酸铵和钼酸铵溶解于30mL热水（80℃）中，标记为A液；
步骤2. 在超声条件下，将8mmol硝酸铋溶解于30mL乙二醇中，标记为B液；
步骤3. 在室温搅拌条件下，将步骤1得到的A液逐滴加入步骤2得到的B液中，继续搅拌30min；
步骤4. 用2mol/L的NaOH溶液调节步骤3所得混合溶液的pH值为5，继续搅拌30min；
步骤5. 将步骤4得到的溶液转移至100mL反应釜内衬中，将密封好的反应釜置于恒温烘箱中于180℃下水热反应24h；
步骤6. 待自然冷却至室温后，取出样品对其进行抽滤，用去离子水和乙醇洗涤3次，将所得固体产物于60℃烘干12h，然后以5℃/min的升温速率升温到400℃，保温5h，即得到Mo掺杂的BiVO4空心立方体。
经实施例3制得的Mo掺杂BiVO4空心立方体的X射线衍射（XRD）谱图见图1中曲线（B），扫描电子显微镜（SEM）照片见图2（B），以及紫外-可见漫反射（UV-vis DRS）谱图见图3中曲线（B）。结果表明，制得的BiVO4样品为四方白钨矿结构，相比于标准卡片JCPDS No.78-1534，X射线衍射峰向小角度方向偏移，原因是Mo6+离子半径稍大于V5+离子半径，意味着Mo成功掺杂进入BiVO4晶格，样品形貌为规整的空心立方体，直径约0.6μm，吸收边界为510nm。
Claims (1)
1.一种Mo掺杂诱导水热制备BiVO4空心立方体的方法，其特征在于，所述方法为：
步骤1. 在搅拌条件下，将摩尔比为1-x：x的偏钒酸铵和钼酸铵溶解于30mL热水中，标记为A液；
步骤2. 在超声条件下，将8mmol硝酸铋溶解于30mL乙二醇中，标记为B液；
步骤3. 在室温搅拌条件下，将步骤1得到的A液逐滴加入步骤2得到的B液中，继续搅拌30min；
步骤4. 用2mol/L的NaOH溶液调节步骤3所得混合溶液的pH值为5，继续搅拌30min；
步骤5. 将步骤4得到的溶液转移至100mL反应釜内衬中，将密封好的反应釜置于恒温烘箱中于180℃下水热反应24h；
步骤6. 待自然冷却至室温后，取出样品对其进行抽滤，用去离子水和乙醇洗涤3次，将所得固体产物于60℃烘干12h，然后以5℃/min的升温速率升温到400℃，保温5h，即得到Mo掺杂的BiVO4空心立方体；
所述x为7-9%，所述偏钒酸铵和钼酸铵总物质的量为8mmol，所述热水的温度是80℃。
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101746824A (zh) * | 2009-12-18 | 2010-06-23 | 北京工业大学 | 一种表面活性剂辅助的制备空心球状多孔BiVO4的方法 |
| CN102626616A (zh) * | 2012-03-26 | 2012-08-08 | 哈尔滨工业大学 | 一种钒酸盐光催化材料的制备方法 |
| CN104138755A (zh) * | 2014-07-09 | 2014-11-12 | 盐城工学院 | 具有纳米空心结构的BiVO4光催化材料的制备方法 |
| CN108585041A (zh) * | 2018-04-17 | 2018-09-28 | 河钢股份有限公司承德分公司 | 一种掺杂钼元素的钒酸铋颜料的制备方法 |
-
2019
- 2019-12-25 CN CN201911360662.9A patent/CN111068657B/zh active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101746824A (zh) * | 2009-12-18 | 2010-06-23 | 北京工业大学 | 一种表面活性剂辅助的制备空心球状多孔BiVO4的方法 |
| CN102626616A (zh) * | 2012-03-26 | 2012-08-08 | 哈尔滨工业大学 | 一种钒酸盐光催化材料的制备方法 |
| CN104138755A (zh) * | 2014-07-09 | 2014-11-12 | 盐城工学院 | 具有纳米空心结构的BiVO4光催化材料的制备方法 |
| CN108585041A (zh) * | 2018-04-17 | 2018-09-28 | 河钢股份有限公司承德分公司 | 一种掺杂钼元素的钒酸铋颜料的制备方法 |
Non-Patent Citations (3)
| Title |
|---|
| Irreversible phase transition in BiVO4 nanostructures synthesized by a polyol method and enhancement in photo degradation of methylene blue;Swati Nikam et al.;《RSC Advances》;20161110;第6卷;摘要、第2.1节、流程图1、第3.1节和第3.3节 * |
| Preparation and photocatalytic properties of Mo-doped BiVO4;Xin Tian et al.;《Journal of Materials Science: Materials in Electronics》;20191005;第30卷(第21期);摘要、第2.2节、第3.1节和图4 * |
| 新型光催化剂BiVO4的制备及光催化性能;耿晓菊等;《信阳师范学院学报(自然科学版)》;20130110;第26卷(第01期);摘要和试验部分 * |
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