CN107188235B - 一种Bi2WO6纳米球的制备方法 - Google Patents
一种Bi2WO6纳米球的制备方法 Download PDFInfo
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- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G41/00—Compounds of tungsten
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- B01J23/24—Chromium, molybdenum or tungsten
- B01J23/31—Chromium, molybdenum or tungsten combined with bismuth
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Abstract
本发明涉及一种Bi2WO6纳米球的制备方法，包括以下步骤：1)将硝酸铋溶液滴加到钨酸钠溶液中；所述硝酸铋溶液的摩尔浓度0.20～0.60mol/L，所述钨酸钠溶液的摩尔浓度0.10～0.30mol/L；2)继续滴加四甲基氢氧化铵溶液，混合后进行水热反应，过滤，清洗，得到Bi2WO6纳米球；所述四甲基氢氧化铵溶液的摩尔浓度0.01～0.05mol/L。该方法制备过程简单，自组装型结构的形貌易于调控，尺寸均一。
Description
技术领域
本发明涉及Bi2WO6的合成领域，具体涉及一种Bi2WO6纳米球的制备方法。
背景技术
近年来的研究发现，纳米材料的性能不仅受其尺寸影响，也受其形貌巨大地影响。因此纳米结构的制备引起了人们极大的关注，不仅有零维纳米颗粒、一维纳米棒、纳米纤维、三维枝杈晶等形貌的大量报道，也制备出了许多自组装介孔球、纳米管等。
Bi2WO6是由(Bi2O2)2+层和WO6层互相交替排列的钙钛矿片层组成的层状结构。Bi2WO6中W原子的5d轨道形成导带，Bi原子的6s和原子的2p杂化轨道形成价带，二者组成Bi2WO6的能带结构，由于Bi 6s轨道和O 2p轨道杂化，导致其价带电位升高，禁带宽度变窄。
因此，Bi2WO6可吸收利用近紫外光(300～400nm)甚至是部分可见光。这也使得Bi2WO6光催化剂具有如下特点：(1)良好的紫外和可见光响应；(2) 热稳定；(3)光催化稳定；(4)成本相对较低；(5)环境友好。因此，研究开发Bi2WO6光催化材料，将会增加太阳能的利用率，在环境污染问题的治理和新能源的开发应用方面有着重大的意义。由于Bi2WO6具有特殊的层状结构，使得其与其它光催化剂相比在表面催化上的应用具有明显的优势地位。通过对Bi2WO6晶体的合成和表征进行研究分析，改变合成的反应条件来获取复杂的多级结构，可以改善其光催化活性，并且将对这一系列氧化物纳米晶体的生长机理具有指导作用。
当今中国正处于工业化和城镇化高速发展的阶段，对高效利用太阳能的技术研发尤为紧迫。而随着Bi2WO6光催化剂研究的不断深入，利用光催化氧化分解有机污染物和光解水制氢的新途径将会被逐步开辟出来，这在治理环境问题和解决能源短缺方面具有巨大的经济效益和重要的实用价值。
发明内容
本发明的目的在于针对现有技术的不足，提供一种Bi2WO6纳米球的制备方法，该方法制备过程简单，自组装型结构的形貌易于调控，尺寸均一。
本发明所提供的技术方案为：
一种Bi2WO6纳米球的制备方法，包括以下步骤：
1)将硝酸铋溶液滴加到钨酸钠溶液中；所述硝酸铋溶液的摩尔浓度 0.20～0.60mol/L，所述钨酸钠溶液的摩尔浓度0.10～0.30mol/L；
2)继续滴加四甲基氢氧化铵溶液，混合后进行水热反应，过滤，清洗，得到Bi2WO6纳米球；所述四甲基氢氧化铵溶液的摩尔浓度0.01～0.05mol/L。
上述技术方案中，以钨酸钠和硝酸铋为反应物料，以四甲基氢氧化铵为表面活性剂，最终实现了Bi2WO6纳米球的制备。钨酸钠为强碱弱酸盐，硝酸铋为强酸弱碱盐，其混合溶液显示一定的弱酸性，并且四甲基氢氧化铵显碱性，OH-离子较多。在较多的OH-离子作用下，形核点数量增加，有利于形核并且得到尺寸较小的纳米片。为减小系统表面能，纳米片进行自组装，最终形成Bi2WO6纳米球。
优选的，所述硝酸铋溶液、钨酸钠溶液与四甲基氢氧化铵溶液的体积比为13～17:13～17:10。
优选的，所述硝酸铋溶液的摩尔浓度0.30～0.40mol/L。
优选的，所述钨酸钠溶液的摩尔浓度0.15～0.20mol/L。
优选的，所述四甲基氢氧化铵溶液的摩尔浓度0.02～0.03mol/L。
优选的，所述水热反应的反应温度为180～250℃，反应时间为12～32h。
优选的，所述水热反应的反应温度为190～200℃，反应时间为20～24h。
优选的，所述清洗为：将过滤得到的产物依次用稀醋酸、去离子水和乙醇反复清洗。进一步优选为三次。用稀醋酸对水热合成产物的清洗是为了将前驱体中混入二氧化碳所形成的CO3 2-、HCO3 -去除，用去离子水清洗是为了将反应物料引入的钠离子、硝酸根离子、铵根离子及有机成分与合成的Bi2WO6纳米粉体充分分离，得到纯相的Bi2WO6自组装纳米球。
优选的，所述步骤1)和步骤2)中的滴加速度1～2滴/秒。
作为优选，所述钨酸钠溶液的摩尔浓度0.19～0.20mol/L，硝酸铋溶液的摩尔浓度0.39～0.40mol/L，四甲基氢氧化铵溶液的摩尔浓度0.02～0.03mol/L；所述硝酸铋溶液、钨酸钠溶液与四甲基氢氧化铵溶液的体积比为 14～16:14～16:10；所述水热反应的反应温度为195～200℃，反应时间为19～21h。在上述的条件下，所得Bi2WO6纳米球的形貌最好，质量稳定，粉体颗粒分散性好。
同现有技术相比，本发明的有益效果体现在：
(1)本发明中的制备工艺过程简单，易于控制，无环境污染，成本低，易于规模化生产。
(2)本发明制备得到的Bi2WO6纳米球的尺寸为2～4μm，纳米片厚度为 10～20nm，产物质量稳定，粉体颗粒分散性好，且具有优异的光催化性能。
附图说明
图1为实施例2合成的Bi2WO6纳米球的X射线衍射图；
图2为实施例2合成的Bi2WO6纳米球的扫描电子显微镜图；
图3为对比例1合成的片状Bi2WO6的X射线衍射图；
图4为对比例1合成的片状Bi2WO6的扫描电子显微镜图；
图5为实施例2合成的Bi2WO6纳米球降解罗丹明B的降解图；
图6为罗丹明B的自降解图。
具体实施方式
以下结合具体的实施例对本发明作进一步说明。
实施例1
1)将1.5mmol二水钨酸钠溶解于15ml去离子水中，使得二水钨酸钠溶液的摩尔浓度0.10mol/L；
2)将3mmol五水硝酸铋溶解于15ml去离子水中，使得五水硝酸铋溶液的摩尔浓度0.20mol/L，将0.10mmol四甲基氢氧化铵溶于10ml去离子水中；
再将五水硝酸铋溶液以1～2滴/秒的速度滴加到钨酸钠溶液中，并将四甲基氢氧化铵溶液以相同的滴加速率滴加到上述混合溶液中，搅拌30min后，在180℃下保温12小时进行热处理。然后，降至室温，取出反应产物，过滤，依次用稀醋酸、去离子水和乙醇清洗，60℃温度下烘干，得到Bi2WO6纳米球。
实施例2
1)将3mmol二水钨酸钠溶解于15ml去离子水中，使得二水钨酸钠溶液的摩尔浓度0.20mol/L；
2)将6mmol五水硝酸铋溶解于15ml去离子水中，使得五水硝酸铋溶液的摩尔浓度0.40mol/L，将0.25mmol四甲基氢氧化铵溶于10ml去离子水中；
再将五水硝酸铋溶液以1～2滴/秒的速度滴加到钨酸钠溶液中，并将四甲基氢氧化铵溶液以相同的滴加速率滴加到上述混合溶液中，搅拌30min后，在200℃下保温20小时进行热处理。然后，降至室温，取出反应产物，过滤，依次用稀醋酸、去离子水和乙醇清洗，60℃温度下烘干，得到Bi2WO6纳米球。
所合成的Bi2WO6纳米球的X射线衍射图，如图1所示，产物为Bi2WO6纳米球，没有其他杂质峰，说明产物为纯相的Bi2WO6；扫描电子显微镜SEM 照片如图2所示，制得的Bi2WO6纳米球的尺寸为2～4μm，纳米片厚度为 10～20nm，形貌为球状。
实施例3
1)将4.5mmol二水钨酸钠溶解于15ml去离子水中，使得二水钨酸钠溶液的摩尔浓度0.30mol/L；
2)将9mmol五水硝酸铋溶解于15ml去离子水中，使得五水硝酸铋溶液的摩尔浓度0.60mol/L，再将0.5mmol四甲基氢氧化铵溶于10ml去离子水中；
将五水硝酸铋溶液以1～2滴/秒的速度滴加到钨酸钠溶液中，并将四甲基氢氧化铵溶液以相同的滴加速率滴加到上述混合溶液中，搅拌30min后，在 250℃下保温32小时进行热处理。然后，降至室温，取出反应产物，过滤，依次用稀醋酸、去离子水和乙醇清洗，60℃温度下烘干，得到Bi2WO6纳米球。
对比例1
1)将3mmol二水钨酸钠溶解于15ml去离子水中，使得二水钨酸钠溶液的摩尔浓度0.20mol/L；
2)将6mmol五水硝酸铋溶解于15ml去离子水中，使得五水硝酸铋溶液的摩尔浓度0.40mol/L，将一定量的KOH片剂溶于10ml去离子水中，使得氢氧化钾溶液摩尔浓度为0.8mol/L；
将五水硝酸铋溶液以1～2滴/秒的速度滴加到钨酸钠溶液中，并将氢氧化钾溶液以相同的滴加速率滴加到上述混合溶液中，搅拌30min后，在200℃下保温20小时进行热处理。然后，降至室温，取出反应产物，过滤，依次用稀醋酸、去离子水和乙醇清洗三次，60℃温度下烘干，得到片状Bi2WO6。
所合成的片状Bi2WO6的X射线衍射图，如图3所示；扫描电子显微镜 SEM照片如图4所示，制得的片状Bi2WO6厚度约为20nm。
降解罗丹明B性能实验：
在10-5mol/L的60mL的罗丹明B溶液中加入0.2g实施例2所制备的 Bi2WO6纳米球，暗搅拌60min后在可见光下照射，每隔一定时间取一次样，所得紫外-可见吸收光谱如图5所示。
另一组作为空白组，不添加任何催化剂，进行罗丹明B可见光自降解，所得紫外-可见吸收光谱如图6所示。
通过对比可知，本方法所制备的Bi2WO6纳米球具有优异的可见光光催化性能。
Claims (3)
1.一种Bi2WO6纳米球的制备方法，其特征在于，包括以下步骤：
1)将硝酸铋溶液滴加到钨酸钠溶液中；所述硝酸铋溶液的摩尔浓度0.39～0.40mol/L，所述钨酸钠溶液的摩尔浓度0.19～0.20mol/L；
2)继续滴加四甲基氢氧化铵溶液，混合后进行水热反应，过滤，清洗，得到Bi2WO6纳米球；所述四甲基氢氧化铵溶液的摩尔浓度0.02～0.03mol/L；所述水热反应的反应温度为195～200℃，反应时间为20～21h；
所述硝酸铋溶液、钨酸钠溶液与四甲基氢氧化铵溶液的体积比为14～16:14～16:10。
2.根据权利要求1所述的Bi2WO6纳米球的制备方法，其特征在于，所述清洗为：将过滤得到的产物依次用稀醋酸、去离子水和乙醇反复清洗。
3.根据权利要求1所述的Bi2WO6纳米球的制备方法，其特征在于，所述步骤1)和步骤2)中的滴加速度1～2滴/秒。
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| CN104226212A (zh) * | 2014-09-30 | 2014-12-24 | 天津大学 | 暴露{010}晶面族的Bi2WO6球形团簇的制备 |
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| CN104226212A (zh) * | 2014-09-30 | 2014-12-24 | 天津大学 | 暴露{010}晶面族的Bi2WO6球形团簇的制备 |
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