CN112169785A - 暴露高能晶面二氧化铈光催化剂的制备 - Google Patents
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Abstract
本发明涉及一种暴露高能晶面二氧化铈光催化剂的制备方法。本发明通过简单的水热合成方法，通过控制反应条件制备了纳米球形、纳米立方和纳米棒状等不同形貌和晶面暴露的CeO2纳米材料。二氧化铈的制备过程包括如下步骤：分别将适量的铈盐和不同浓度的强碱溶于蒸馏水中配成溶液，在体系中加入适量的表面活性剂，常温搅拌后，将混合液转移到水热釜中反应，通过控制反应温度，获得不同形貌的产物。本发明操作简单、通过改变近似制备条件可以很好调控CeO2纳米粒子的形貌及其高能晶面组成，对相关催化材料的应用具有重要意义。
Description
技术领域
本发明涉及一种制备暴露高能晶面二氧化铈光催化剂的方法，并通过控制反应条件制备了不同形貌具有高能晶面的二氧化铈；本发明还研究了不同形貌和晶面暴露二氧化铈纳米材料的光催化降解有机污染物的性能。
背景技术
CeO2作为一种常见的光催化半导体材料，近年来在环境催化领域受到了广泛关注。二氧化铈的化学性质非常特别，其外层电子充填方式为4f1,5d1,6s2。因此，铈除了像其它稀土元素以三价状态存在外，它还可以以正四价稳定存在。由于Ce3+/Ce4+之间的低氧化还原电位的特性，使其具有丰富的氧空位，被认为是一种很有前途的光催化剂。但由于光诱导的电子空穴对的快速重组和宽带隙(2.7-3.4eV)阻碍了其在光催化领域的应用。近期根据董江课题组对不同晶面的结构研究发现，在CeO2暴露出的{100}和{110}的高能晶面上，Ce3+密度和表面的晶格氧缺陷要远高于普通的{111}晶面，高能晶面的催化速率为普通晶面的3～5倍，可以显著改善催化材料的氧化还原反应能力和催化性能，从而提高光催化剂的活性。
发明内容
本发明的目的是针对二氧化铈表面光催化活性较低的问题，提供一种暴露高能晶面二氧化铈光催化剂的制备方法，以增强二氧化铈的光催化活性，进而使其具有更强的氧化还原性和更高的催化效率。
一、暴露高能晶面二氧化铈光催化剂的制备
本发明水热法制备暴露高能晶面二氧化铈光催化剂的方法，是先将铈盐和强碱性溶液溶解在去离子水中搅拌0.5h；然后将两透明溶液混合后在室温下再搅拌0.5h；在混合液中加入重量百分比为0.1～1％的表面活性剂；然后将乳状混合液置于水热合成反应釜中，于不同温度下进行水热反应，抽滤，洗涤，干燥，得到不同形貌的CeO2。
水热反应的温度为160～200℃、强碱溶液浓度为3～10mol/L、反应时间为12～24h，得到的产物为立方型CeO2，记为C-C，其暴露的择优晶面为{100}。
水热反应的温度为100～120℃、强碱溶液浓度为0.1～0.5mol/L、反应时间为12～24h；得到的产物为纳米球型CeO2，记为C-S，其暴露的择优晶面为{111}。
水热反应的温度为100～120℃、强碱溶液浓度为3～10mol/L、反应时间为12～24h；得到的产物为纳米棒型CeO2，记为C-R，其暴露的择优晶面为{110}和{100}。
图1、2分别为不同形貌CeO2的TEM图和XRD图。通过结合图1和图2的表征结果，可以很清楚的观察到不同形貌具有高能晶面的二氧化铈，图1A中，可以明显看到二氧化铈的立方体结构，其六个晶面都是{100}晶面；图1B中，可以很清楚的看到二氧化铈球，其择优晶面为{111}晶面；图1C中可以观察到二氧化铈的棒状结构，其晶面为{100}和{110}。通过图2中的XRD可知，与二氧化铈的标准图谱对比，说明C-C、C-P和C-S被成功制备出来。
二、不同形貌二氧化铈的光催化性能
1、光催化活性测试
催化剂的光催化反应是在光反应器上进行的，光源为500W氙灯。以罗丹明B(RhB)实验来评价样品光催化活性。实验用RhB浓度是10ppm，体积是100mL，催化剂用量是50mg。准确称取50mg催化剂加入到150mL的烧杯中，然后加入100mL的RhB溶液，超声处理10min。然后再暗搅拌吸附0.5h，达到吸附平衡。然后开启灯电源，冷凝泵等进行光反应。每间隔15min吸取5mL溶液，反应2.5h后停止光照。将取出的悬浮液高速离心10min，取上清液测量其溶液吸光度。通过测量得出的数据，作出二氧化铈的光降解曲线图。图3为不同形貌二氧化铈降解RhB的曲线图。图3的图示结果表明，三种形貌二氧化铈的光催化活性强度依次为：C-C>C-R>C-S>商业化。三种形貌的二氧化铈中，立方体二氧化铈{100}具有最强的光催化活性，是商品化CeO2的10多倍。
附图说明
图1为不同形貌CeO2的高倍透射电镜。
图2为不同形貌CeO2的XRD。
图3为不同形貌二氧化铈降解RhB的降解曲线。
具体实施方式
下面通过具体实例对本发明暴露高能晶面二氧化铈光催化剂的制备、结构性能作进一步说明。
实施例1、立方体状CeO2的制备
将10mmol Ce(NO3)3·6H2O溶解到25ml去离子水中，搅拌10min，记为A溶液。同时量取9mol/L NaOH溶液50ml，搅拌0.5h，记为B溶液。然后将B溶液逐滴滴加到A溶液中。常温下搅拌0.5h，将上述悬浮液转移到150ml聚四氟乙烯反应釜中，在180℃下加热12h。然后将混合液冷却至室温，抽滤得到固体颗粒，用去离子水和无水乙醇洗涤三次，80℃下干燥6h，研磨后得到立方体状的CeO2，其结构如图1A。
实施例2、纳米球型CeO2的制备
将10mmol Ce(NO3)3·6H2O溶解到25ml去离子水中，搅拌0.5h，记为A溶液。同时量取0.2mol/L NaOH溶液50ml，搅拌0.5h，记为B溶液。然后将B溶液逐滴滴加到A溶液中。常温下搅拌0.5h，将上述悬浮液转移到150ml聚四氟乙烯反应釜中，在100℃下加热12h。然后将混合液冷却至室温，抽滤得到固体颗粒，用去离子水和无水乙醇洗涤三次，80℃下干燥6h，研磨后得到CeO2的纳米球，其结构如图1B。
实施例3、棒状CeO2的制备
将10mmol Ce(NO3)3·6H2O溶解到25ml去离子水中，搅拌0.5h，记为A溶液。同时量取6mol/L NaOH溶液50ml，搅拌0.5h，记为B溶液。然后将B溶液逐滴滴加到A溶液中。常温下搅拌0.5h，将上述悬浮液转移到150ml聚四氟乙烯反应釜中，在110℃下加热12h。然后将混合液冷却至室温，抽滤得到固体颗粒，用去离子水和无水乙醇洗涤三次，80℃下干燥6h，研磨后得到棒状的CeO2，其结构如图1C。
Claims (9)
1.水热法制备暴露高能晶面二氧化铈光催化剂的方法，是先将铈盐和强碱性溶液分别制备成溶液；然后将溶液混合搅拌；在混合液中加入表面活性剂；然后将混合液置于水热合成反应釜中，于不同温度下进行水热反应，抽滤，洗涤，干燥，得到不同形貌的二氧化铈。
2.如权利要求1所述水热法制备暴露高能晶面二氧化铈光催化剂的方法，其特征在于：水热反应的温度为140～200℃、强碱的浓度为3～10mol/L、反应时间为12～24h，得到的产物为立方型CeO2，其暴露的择优晶面为{100}。
3.如权利要求1所述水热法制备暴露高能晶面二氧化铈光催化剂的方法，其特征在于：水热反应的温度为100～120℃、强碱的浓度为0.1～0.5mol/L、反应时间为12～24h，得到的产物为纳米球型CeO2，其暴露的择优晶面为{111}。
4.如权利要求1所述水热法制备暴露高能晶面二氧化铈光催化剂的方法，其特征在于：水热反应的温度为100～120℃、强碱的浓度为3～10mol/L、反应时间为12～24h，得到的产物为纳米棒型CeO2，其暴露的择优晶面为{110}和{100}。
5.如权利要求1所述水热法制备暴露高能晶面二氧化铈光催化剂的方法，其特征在于：铈盐一般用硝酸铈或者氯化铈等铈盐，强碱溶液一般用氢氧化钠或者氢氧化钾等强碱溶液。
6.如权利要求2、3或4所述任意一种水热法制备具有高能晶面二氧化铈光催化剂的方法,其特征在于：表面活性剂加入的重量比为0.1～1％。
7.如权利要求2、3或4所述任意一种水热法制备具有高能晶面二氧化铈光催化剂的方法,其特征在于：表面活性剂可以选取聚乙烯吡咯烷酮、十六烷基三甲基溴化铵、十二烷基硫酸钠和十二烷基苯磺酸钠等常见的表面活性剂。
8.如权利要求2、3或4所述水热法制备暴露高能晶面二氧化铈光催化剂的方法，其特征在于：将三价铈盐和强碱溶液分别在室温下搅拌0.5h，然后再混合搅拌0.5h。
9.如权利要求2、3或4所述水热法制备暴露高能晶面二氧化铈光催化剂的方法，其特征在于：所述干燥是在80℃的烘箱中烘干6h。
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