CN107224986B - 一种二硫化钼/铌酸锡复合纳米材料及用途 - Google Patents
一种二硫化钼/铌酸锡复合纳米材料及用途 Download PDFInfo
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- 229910052982 molybdenum disulfide Inorganic materials 0.000 title claims abstract description 66
- 239000002131 composite material Substances 0.000 title claims abstract description 47
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract description 47
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 14
- 238000006243 chemical reaction Methods 0.000 claims abstract description 44
- 229910052961 molybdenite Inorganic materials 0.000 claims abstract description 35
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 31
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 26
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims abstract description 22
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- RWVGQQGBQSJDQV-UHFFFAOYSA-M sodium;3-[[4-[(e)-[4-(4-ethoxyanilino)phenyl]-[4-[ethyl-[(3-sulfonatophenyl)methyl]azaniumylidene]-2-methylcyclohexa-2,5-dien-1-ylidene]methyl]-n-ethyl-3-methylanilino]methyl]benzenesulfonate Chemical compound [Na+].C1=CC(OCC)=CC=C1NC1=CC=C(C(=C2C(=CC(C=C2)=[N+](CC)CC=2C=C(C=CC=2)S([O-])(=O)=O)C)C=2C(=CC(=CC=2)N(CC)CC=2C=C(C=CC=2)S([O-])(=O)=O)C)C=C1 RWVGQQGBQSJDQV-UHFFFAOYSA-M 0.000 claims abstract description 11
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- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 6
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 6
- 239000011941 photocatalyst Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 230000006798 recombination Effects 0.000 description 5
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- 229910052718 tin Inorganic materials 0.000 description 5
- 239000002245 particle Substances 0.000 description 4
- FWPIDFUJEMBDLS-UHFFFAOYSA-L tin(II) chloride dihydrate Chemical compound O.O.Cl[Sn]Cl FWPIDFUJEMBDLS-UHFFFAOYSA-L 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
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- 230000009286 beneficial effect Effects 0.000 description 2
- 230000004298 light response Effects 0.000 description 2
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 description 2
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 description 2
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- RZVAJINKPMORJF-UHFFFAOYSA-N Acetaminophen Chemical compound CC(=O)NC1=CC=C(O)C=C1 RZVAJINKPMORJF-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
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- 229910052750 molybdenum Inorganic materials 0.000 description 1
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- 231100000252 nontoxic Toxicity 0.000 description 1
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- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
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- 229910052723 transition metal Inorganic materials 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明针对单一二维层状二硫化钼可见光催化效率低的问题,提供了一种简单的二硫化钼/铌酸锡复合纳米材料的制备方法,主要用于光催化分解水产氢的技术中,属于复合材料技术领域和清洁能源领域。称取SnNb2O6溶于去离子水中,第一次磁力搅拌,超声分散,再称取二水合钼酸钠、硫脲溶于上述溶液,第二次磁力搅拌,待反应物混合均匀后将反应液将溶液转移至内衬为聚四氟乙烯的反应釜中,放入烘箱中,水热反应,待自然冷却至室温后,离心,水洗和醇洗数次,烘干得到所述MoS2/SnNb2O6复合材料;片状的MoS2分散在SNO纳米片上。
Description
技术领域
本发明针对单一二维层状二硫化钼可见光催化效率低的问题,提供了一种简单的二硫化钼/铌酸锡复合纳米材料,主要用于光催化分解水产氢的技术中,属于复合材料技术领域和清洁能源领域。
技术背景
随着经济的增长,日益恶化的环境问题变的尤为突出;以半导体及其衍生材料为媒介的光催化技术可以利用清洁、可持续的太阳能处理环境中有机污染物及分解水制氢,已经受到社会上愈来愈多的关注;近年来以二维层状二硫化钼(MoS2)为代表的二维过渡金属硫化物等新兴材料引起了研究工作者的极大兴趣,因其具备天然可调控的带隙结构(1.20~1.92eV)、良好的电子迁移率、化学稳定性;然而单纯的MoS2的光生电子空穴对的复合率高,导致单一的二硫化钼材料仍然无法达到所期望的光催化效果。因此,人们试图通过半导体复合构建异质结来提高电荷分离效率和增强光催化活性。
铌酸锡(SnNb2O6)作为典型的层状铌酸盐半导体材料,由于其独特的晶体结构和合适的能带结构和可见光响应等性能受到了很多研究者的关注;通过与二硫化钼复合形成异质结结构可以有效地弥补二硫化钼本身存在的缺点,不仅能进一步扩大了MoS2材料的光响应范围,同时抑制载流子的复合,从而提高量子效率,提高光催化剂的光催化分解水制氢活性。
迄今为止,尚未有人报道采用水热法制备MoS2/SnNb2O6复合材料,所用的SNO化学和物理性质稳定,原材料廉价易得,无毒,且以其为载体制备MoS2/SnNb2O6复合材料的反应工艺简单,所得产品光催化制氢活性好,稳定性高,在环境、能源等领域有良好应用前景。
发明内容
本发明目的是提供一种新的在室温条件下,以简单易行的水热法合成的MoS2/SnNb2O6复合材料。
本发明通过以下步骤实现:
(1)制备铌酸锡(SnNb2O6)纳米片:称取五氧化二铌,氢氧化钾于内衬为聚四氟乙烯的反应釜中,向其中加入去离子水,然后将反应釜放入烘箱中,第一次水热反应;待自然冷却至室温后,得到澄清前驱体溶液,用稀盐酸调节溶液pH值,再加入二水合氯化亚锡,再次用稀盐酸调节pH值,将溶液转移至内衬为聚四氟乙烯的反应釜中,将反应釜放入烘箱中,第二次水热反应,待自然冷却至室温后,离心出黄色颗粒,水洗和醇洗数次,离心,烘干;具体可参考Z.Y.Zhang,D.L.Jiang,D.Li,M.He,M.Chen,Appl.Catal.B:Environ.183(2016)113-123。
所述第一次水热反应的温度为160~200℃,反应时间为45~50h。
所述稀盐酸溶液的浓度为2mol·L-1。
所述第一次稀盐酸调节溶液pH值为7~9。
所述第二次稀盐酸调节溶液pH值为1~3。
所述第二次水热反应的温度为180~220℃,反应时间为45~50h。
(2)制备二硫化钼(MoS2)纳米片:称取二水合钼酸钠、硫脲于烧杯中,加入去离子水,磁力搅拌,将所得澄清溶液转移至内衬为聚四氟乙烯的反应釜中,将反应釜放入烘箱中,水热反应,待自然冷却至室温后,离心出黑色颗粒,水洗和醇洗后离心,烘干;具体可参考W.C.Peng,X.Wang,X.Y.Li,Nanoscale,6(2014)8311-8317。
所述磁力搅拌的时间为20~40min。
所述水热反应的温度为200~220℃,反应时间为20~28h。
(3)制备MoS2/SnNb2O6复合材料:称取SnNb2O6纳米片溶于去离子水中,第一次磁力搅拌,超声分散,再称取二水合钼酸钠、硫脲溶于上述溶液,第二次磁力搅拌,待反应物混合均匀后将反应溶液转移至内衬为聚四氟乙烯的反应釜中,放入烘箱中,水热反应,待自然冷却至室温后,离心,水洗和醇洗数次,烘干得到所述MoS2/SnNb2O6复合材料;片状的MoS2分散在SNO纳米片上。
所述第一次磁力搅拌的时间为10-20min。
所述超声分散指在功率为250W的超声机中超声40-80min。
所述第二次磁力搅拌的时间为20-40min。
所述水热反应的温度为200~220℃,反应时间为20~28h。
所述MoS2/SnNb2O6复合材料中MoS2与SnNb2O6的质量比为0.05-0.3:1;优选0.1:1。
本发明的有益效果为:
1、本发明首次制备可见光响应MoS2/SnNb2O6异质结材料,采用水热法,其操作简单、生产成本低廉、合成的产率较高,适合扩大化生产的要求。
2、MoS2/SnNb2O6异质结材料可作为性能优良的可见光光催化剂。通过对制备的样品进行了XRD、TEM、XPS等一系列表征,结果表明MoS2与SnNb2O6复合后形成的异质结结构不但有利于提高了光生电子和空穴的寿命,促进光生电荷的传输,而且有效地提升了复合后催化剂的稳定性。
3、本发明所得到的材料具有较好的光催化分解水制氢效果。在光催化实际应用领域具有广阔的前景。
附图说明
图1为所制备单纯MoS2、SnNb2O6、MoS2/SnNb2O6复合材料的XRD衍射谱图。
图2为所制备单纯SnNb2O6、MoS2/SnNb2O6复合光催化剂样品的透射电镜照片;图2a为单纯SnNb2O6透射电镜图,以薄片状形式存在;图2b为单纯MoS2透射电镜图,以薄片形式存在;图2c为MoS2/SnNb2O6复合材料透射电镜图从图中可以看出MoS2负载在SnNb2O6薄片表面,结果表明形成异质结。
图3为单纯SnNb2O6、MoS2、10%-MoS2/SnNb2O6复合光催化剂的XPS图,图中可以看出Sn、Nb、O、Mo、S元素的存在。
图4为单纯的MoS2、SnNb2O6以及不同质量比的MoS2/SnNb2O6复合材料在可见光下光催化分解水制氢产量图,从图中可以看出10%-MoS2/SnNb2O6复合材料具有最高的光催化制氢活性。
具体实施方式
实施例1SnNb2O6纳米片的制备
SnNb2O6的制备采用的是水热反应的方法:称取0.5g五氧化二铌、2.2443g氢氧化钾于50mL内衬为聚四氟乙烯的反应釜中,向其中加入35mL去离子水,将反应釜放入烘箱,180℃水热反应48h,待自然冷却至室温后,得到澄清前驱体溶液,将溶液转移至50mL烧杯中,用浓度为2mol/L稀盐酸调节溶液pH至8,再加入0.4245g二水合氯化亚锡,再次用浓度为2mol/L稀盐酸调节溶液pH至2,将溶液转移至100mL内衬为聚四氟乙烯的反应釜中,放入烘箱,200℃水热反应48h,冷却至室温,离心得到黄色颗粒,水洗和醇洗各三次,离心,于烘箱中60℃干燥12h。
实施例2MoS2纳米片的制备
MoS2的制备采用的是水热反应的方法:称取0.242g二水合钼酸钠、0.38g硫脲溶于60ml去离子水,磁力搅拌30min,形成澄清溶液,将溶液转移至100mL内衬为聚四氟乙烯的反应釜中,放入烘箱,210℃水热反应24h,冷却至室温,离心得到黑色颗粒,水洗和醇洗三次,离心,于烘箱中60℃干燥12h。
实施例3 5%-MoS2/SnNb2O6复合材料的制备
MoS2/SnNb2O6复合材料的制备采用的是水热法:称取80mg SnNb2O6溶于60ml去离子水中,磁力搅拌15min,然后在功率为250W的超声机中超声60min,得到均一的黄色溶液,称取6.35mg二水合钼酸钠、10mg硫脲溶于上述溶液,磁力搅拌30min,将溶液转移至100mL内衬为聚四氟乙烯的反应釜中,放入烘箱中,210℃水热反应24h,待自然冷却至室温后,离心,水洗和醇洗各三次,于烘箱中60℃干燥12h得到所述5%-MoS2/SnNb2O6复合材料。
实施例4 10%-MoS2/SnNb2O6复合材料的制备
MoS2/SnNb2O6复合材料的制备采用的是水热法:称取80mg SnNb2O6溶于60ml去离子水中,磁力搅拌15min,然后在功率为250W的超声机中超声60min,得到均一的黄色溶液,称取13.31mg二水合钼酸钠、21.03mg硫脲溶于上述溶液,磁力搅拌30min,将溶液转移至100mL内衬为聚四氟乙烯的反应釜中,放入烘箱中,210℃水热反应24h,待自然冷却至室温后,离心,水洗和醇洗各三次,于烘箱中60℃干燥12h得到所述10%-MoS2/SnNb2O6复合材料。
实施例5 20%-MoS2/SnNb2O6复合材料的制备
MoS2/SnNb2O6复合材料的制备采用的是水热法:称取80mg SnNb2O6溶于60ml去离子水中,磁力搅拌15min,然后在功率为250W的超声机中超声60min,得到均一的黄色溶液,称取30.25mg二水合钼酸钠、47.58mg硫脲溶于上述溶液,磁力搅拌30min,将溶液转移至100mL内衬为聚四氟乙烯的反应釜中,放入烘箱中,210℃水热反应24h,待自然冷却至室温后,离心,水洗和醇洗各三次,于烘箱中60℃干燥12h得到所述20%-MoS2/SnNb2O6复合材料。
实施例6 30%-MoS2/SnNb2O6复合材料的制备
MoS2/SnNb2O6复合材料的制备采用的是水热法:称取80mg SnNb2O6溶于60ml去离子水中,磁力搅拌15min,然后在功率为250W的超声机中超声60min,得到均一的黄色溶液,称取51.89mg二水合钼酸钠、81.65mg硫脲溶于上述溶液,磁力搅拌30min,将溶液转移至100mL内衬为聚四氟乙烯的反应釜中,放入烘箱中,210℃水热反应24h,待自然冷却至室温后,离心,水洗和醇洗各三次,于烘箱中60℃干燥12h得到所述30%-MoS2/SnNb2O6复合材料。
实施例7不同比例MoS2/SnNb2O6复合光催化剂的光催化制氢实验
以300W的氙灯为光源,整个系统的温度通过冷凝水保持在室温。准确称量所制备的催化剂50mg与氯铂酸(质量百分数约为1%),溶解于含40mL去离子水和10mL甲醇的派热克斯玻璃反应器中,并磁力搅拌使催化剂均匀悬浮,把反应器与系统连接起来。采用原位光还原进行Pt的负载。光照前,将光催化剂悬浮液超声分散5min,然后通入N2 20min,以去除系统中的溶解氧及其它气体,再置于光源下开始光催化反应。在磁力搅拌条件下连续光照反应3h,每隔一段时间从光催化反应器的气体取样口中采集气体样品,利用气相色谱(GC-14C,日本岛津公司,TCD,载气N2,5A分子筛填充柱)进行H2含量的定量分析。
Claims (9)
1.一种二硫化钼/铌酸锡复合纳米材料,其特征在于,按照如下方法制备:称取SnNb2O6纳米片溶于去离子水中,第一次磁力搅拌,超声分散,再称取二水合钼酸钠、硫脲溶于上述溶液,第二次磁力搅拌,待反应物混合均匀后将反应溶液转移至内衬为聚四氟乙烯的反应釜中,放入烘箱中,水热反应,待自然冷却至室温后,离心,水洗和醇洗数次,烘干得到所述二硫化钼/铌酸锡复合材料。
2.如权利要求1所述的一种二硫化钼/铌酸锡复合纳米材料,其特征在于,所述的二硫化钼/铌酸锡复合纳米材料,片状的MoS2分散在SnNb2O6纳米片上。
3.如权利要求1所述的一种二硫化钼/铌酸锡复合纳米材料,其特征在于,所述第一次磁力搅拌的时间为10-20min。
4.如权利要求1所述的一种二硫化钼/铌酸锡复合纳米材料,其特征在于,所述超声分散指在功率为250W的超声机中超声40-80min。
5.如权利要求1所述的一种二硫化钼/铌酸锡复合纳米材料,其特征在于,所述第二次磁力搅拌的时间为20-40min。
6.如权利要求1所述的一种二硫化钼/铌酸锡复合纳米材料,其特征在于,所述水热反应的温度为200~220℃,反应时间为20~28h。
7.如权利要求1所述的一种二硫化钼/铌酸锡复合纳米材料,其特征在于,所述二硫化钼/铌酸锡复合材料中,MoS2与SnNb2O6的质量比为0.05-0.3:1。
8.如权利要求7所述的一种二硫化钼/铌酸锡复合纳米材料,其特征在于,所述二硫化钼/铌酸锡复合材料中,MoS2与SnNb2O6的质量比为0.1:1。
9.如权利要求1-8任一所述的二硫化钼/铌酸锡复合纳米材料在光催化分解水制氢领域的用途。
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