CN110201674B - 一种镍掺杂四氧化三锡纳米花光催化材料及制备方法 - Google Patents
一种镍掺杂四氧化三锡纳米花光催化材料及制备方法 Download PDFInfo
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- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims description 3
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Abstract
本发明公开了一种镍掺杂的四氧化三锡纳米花光催化材料，所述光催化材料是通过水热法合成由大小100~400nm，厚度为10~20nm的纳米片组装而成的镍掺杂的四氧化三锡纳米花。通过镍的掺杂能够形成活性中心，有效的促进光生载流子的分离和传输，并且增强催化反应动力学。本发明公开的光催化剂在可见光下表现出优异的分解水产氢以及有机污染物降解性能，且其制备成本低，方法简单，效率可观，工业化应用前景广阔。
Description
技术领域
本发明涉及一种光催化剂及其改性方法，尤其涉及一种镍掺杂四氧化三锡纳米花光催化材料及其制备方法与应用，属于纳米材料光催化技术领域。
背景技术
氢气是一种具有高能量密度的绿色可再生燃料，被称为化石燃料的潜在替代品。目前，作为解决能源短缺和环境污染问题的有效的途径，利用半导体光催化技术分解水产氢引起了广泛的研究。众所周知，优良的光催化剂必须满足三个基本条件：1)实现全光谱吸收，提高太阳能利用率；2)光生载流子有效分离并能够快速传输到表面参与氧化还原反应；3)高效的光催化反应动力学。
四氧化三锡是一种层状金属氧化物，带隙能为2.7eV，能够被可见光激发，表现出光催化分解水产氢以及氧化降解有机污染物的巨大潜力。然而其自身仍然存在载流子复合率高，高催化活性面暴露少，光催化反应动力学差等问题。通过简单地方法在四氧化三锡上掺杂镍，能够形成高活性中心，有效的促进光生载流子的分离并使其快速传输到催化剂表面参与反应，提高催化反应动力学；同时还使催化剂的光吸收范围进一步红移，提高光能利用率。然而迄今为止，对于镍掺杂四氧化三锡纳米花光催化剂，以及利用该光催化剂进行光催化产氢及污染物降解的应用还未见报道。
发明内容
针对现有技术的不足，本发明所要解决的技术问题是提供一种镍掺杂四氧化三锡纳米花光催化材料及其制备方法。
本发明所述的镍掺杂四氧化三锡纳米花光催化材料，其特征在于：所述光催化材料是以由大量纳米片组装而成的纳米花状四氧化三锡为基础，通过掺杂镍进行改性。其中所述纳米片的大小为100～400nm，厚度为10～20nm，其中所述光催化剂中镍与锡元素摩尔比为1：1～10。
上述镍掺杂四氧化三锡纳米花光催化材料优选的实施方式是：所述光催化材料是以由大量大小为200nm±50nm，厚度为18nm±2nm的纳米片组装而成的纳米花状四氧化三锡为基础，通过掺杂镍进行改性，其中所述光催化剂中镍与锡元素摩尔比为1：5～10，最优选为1：7。
本发明所述镍掺杂四氧化三锡纳米花光催化材料的制备方法，步骤是：
①以物质的量比计，将氯化亚锡、柠檬酸钠、氢氧化钠按0.2～2：0.5～5：8～80的比例混合，超声30min，搅拌30min，得到锡前驱体溶液；
②按镍与锡元素摩尔比1：1～10将氯化镍加入上述前驱体溶液中，搅拌1～2h，得到复合溶液；
③将复合溶液转移至50ml反应釜内，在180±10℃下反应12h±2h；
④反应结束后使反应釜自然冷却至室温，所得产物用去离子水和无水乙醇分别洗涤3～5次，再于80±10℃下干燥12±2h，得到的固体粉末即为镍掺杂四氧化三锡光催化材料。
上述镍掺杂四氧化三锡纳米花光催化材料的制备方法中，步骤①所述锡前驱体溶液中优选将氯化亚锡、柠檬酸钠、氢氧化钠按2：5：20～80的比例混合。
上述镍掺杂四氧化三锡纳米花光催化材料的制备方法中，步骤②所述复合溶液中镍与锡元素摩尔比优选为1：5～10，最优选为1：7。
本发明所述的镍掺杂四氧化三锡纳米花光催化材料在光催化产氢和催化降解污染物中的应用。
本发明采用水热法合成了由大量纳米片组装而成的四氧化三锡纳米花，并通过镍掺杂进行改性，获得了镍掺杂四氧化三锡纳米花光催化材料，具有原料丰富，制备成本低，方法简单的特点，其突出效果体现在：本发明公开的方法通过在四氧化三锡中掺杂镍，能够形成高活性中心，有效的促进光生载流子的分离和传输；降低光催化氧化还原反应的势垒，提高催化反应动力学；同时还使催化剂的光吸收范围进一步红移，有效提高了光能利用率。
本发明方法得到的光催化材料为新型可见光催化剂，实验证明该催化剂在可见光下能够高效催化水分解产氢以及氧化降解有机污染物，其环境友好，原料丰富，成本低，适合规模化生产，在分解水产氢以及甲基橙等难降解有机污染物的催化降解中具有广泛的应用前景。
附图说明
图1为本发明实施例1、2和3制备的镍掺杂四氧化三锡纳米花光催化材料以及四氧化三锡的X-射线衍射(XRD)图谱。
图2为本发明实施例2制备的镍掺杂四氧化三锡纳米花光催化材料不同放大倍数下的扫描电镜图(SEM)。
图3为本发明实施例2制备的镍掺杂四氧化三锡纳米花光催化材料的透射电镜图(TEM)以及高分辨透射电镜图(HRTEM)。
图4为本发明实施例1、2和3制备的镍掺杂四氧化三锡纳米花光催化材料以及四氧化三锡在可见光下光催化降解甲基橙(a)以及光催化分解水产氢(b)的性能对比。
具体实施方式
下面结合实施例及说明书附图对本发明的技术方案做进一步说明，但本发明所保护范围不仅限于此。
实施例1：
①称取5mM二水氯化亚锡(SnCl2·2H2O)，12.5mM二水柠檬酸钠(Na3C6H5O7·2H2O)溶解于12.5ml去离子水中，然后加入12.5ml含有0.2M氢氧化钠(NaOH)的水溶液，超声30min，搅拌30min，使其完全分散溶解，得到锡前驱体溶液；
②按镍与锡元素摩尔比1:10称取一定质量的六水氯化镍(NiCl2·6H2O)加入上述前驱体溶液中，搅拌2h，得到复合溶液；
③将复合溶液转移至50ml反应釜内，在180下反应12h；
④反应结束后使反应釜自然冷却至室温，所得产物用去离子水和无水乙醇分别洗涤3次，再于80℃下干燥12h，得到的固体粉末即为镍掺杂四氧化三锡光催化材料。
实施例2：
①称取5mM二水氯化亚锡(SnCl2·2H2O)，12.5mM二水柠檬酸钠(Na3C6H5O7·2H2O)溶解于12.5ml去离子水中，然后加入12.5ml含有0.2M氢氧化钠(NaOH)的水溶液，超声30min，搅拌30min，使其完全分散溶解，得到锡前驱体溶液；
②按镍与锡元素摩尔比1:7称取一定质量的六水氯化镍(NiCl2·6H2O)加入上述前驱体溶液中，搅拌2h，得到复合溶液；
③将复合溶液转移至50ml反应釜内，在180下反应12h；
④反应结束后使反应釜自然冷却至室温，所得产物用去离子水和无水乙醇分别洗涤3次，再于80℃下干燥12h，得到的固体粉末即为镍掺杂四氧化三锡光催化材料。
将所得的镍掺杂四氧化三锡纳米花光催化材料用德国布鲁克D8X射线衍射仪分析(图1)。
将所得的镍掺杂四氧化三锡纳米花光催化材料用HITACHI S-4800场发射扫描电子显微镜(图2)和JOEL JEM 2100透射电镜(图3)进行观察。
将所得的镍掺杂四氧化三锡纳米花光催化材料在可见光下进行降解甲基橙测试(图4a)，相比于纯四氧化三锡，镍掺杂四氧化三锡光催化材料的降解效率显著提高；同时，可见光照射下的光催化分解水产氢测试(图4b)表明，镍掺杂四氧化三锡光催化材料的产氢速率比纯四氧化三锡提高了约3.4倍。
实施例3：
①称取5mM二水氯化亚锡(SnCl2·2H2O)，12.5mM二水柠檬酸钠(Na3C6H5O7·2H2O)溶解于12.5ml去离子水中，然后加入12.5ml含有0.2M氢氧化钠(NaOH)的水溶液，超声30min，搅拌30min，使其完全分散溶解，得到锡前驱体溶液；
②按镍与锡元素摩尔比1:5称取一定质量的六水氯化镍(NiCl2·6H2O)加入上述前驱体溶液中，搅拌2h，得到复合溶液；
③将复合溶液转移至50ml反应釜内，在180下反应12h；
④反应结束后使反应釜自然冷却至室温，所得产物用去离子水和无水乙醇分别洗涤3次，再于80℃下干燥12h，得到的固体粉末即为镍掺杂四氧化三锡光催化材料。
Claims (2)
1.一种镍掺杂四氧化三锡纳米花光催化材料的制备方法，步骤是：
①以物质的量比计，将氯化亚锡、柠檬酸钠、氢氧化钠按0.2～2：0.5～5：8～80的比例混合，超声30min，搅拌30min，得到锡前驱体溶液；
②按镍与锡元素摩尔比1：1～10将氯化镍加入上述前驱体溶液中，搅拌1～2h，得到复合溶液；
③将复合溶液转移至50ml反应釜内，在180±10℃下反应12h±2h；
④反应结束后使反应釜自然冷却至室温，所得产物用去离子水和无水乙醇分别洗涤3～5次，再于80±10℃下干燥12±2h，得到的固体粉末即为镍掺杂四氧化三锡光催化材料。
2.根据权利要求1所述镍掺杂四氧化三锡纳米花光催化材料的制备方法，其特征在于：步骤②所述复合溶液中镍与锡元素最优摩尔比为1:7。
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