CN106835183A - 一种WSe2基复合纳米片光电极的制备方法 - Google Patents
一种WSe2基复合纳米片光电极的制备方法 Download PDFInfo
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Abstract
本发明公开了一种WSe2基复合纳米片光电极的制备方法,包括:合成WSe2纳米片光电极、构筑CdS‑WSe2异质结光电极和Pt‑In2S3‑CdS‑WSe2复合纳米片光电极。本发明有益效果在于:所需原料来源丰富、合成方法简单、重复性好,材料稳定性好;本发明制备的材料可用于光电催化分解水产氢,具有很好的实用价值和应用前景。
Description
技术领域
本发明涉及无机纳米材料技术领域,具体涉及一种WSe2基复合纳米片光电极的制备方法。
背景技术
随着人们对能源需求的不断增加以及环境污染问题的日益严重,探索新型能源取代化石燃料已经成为全人类的重大课题,而氢气作为最有前景的清洁能源,如何高效并且持续的生产已经成为科研界研究的热点。太阳能是最理想的可再生资源,利用太阳光驱动反应的光电化学技术,已成为清洁能源生产的重要手段。因此,制备出成本低、稳定性好的光电催化剂迫在眉睫。
1972年,Fujishima首次报道由TiO2半导体组成的光电化学池可将水分解成氢气和氧气,拉开了光电化学分解水研究的序幕,但TiO2只能吸收5%的太阳光,因此,开发高效的可见光响应的光催化剂变得至关重要。二硒化钨(1.2eV)作为一种半导体材料,由于其高光吸收系数、层状结构的各向异性和能量转换效率高达17%,在20世纪80年代得到了广泛研究。而p型WSe2作为光电极产氢的理想材料具有如下优势:1、带隙窄,易于光电化学产氢2、高的载流子迁移率3、光电转换效率仅次于硅,但光稳定性高于硅。
目前,文献报道的p型WSe2作为光电极产氢的文献并不是很多,而且大多提高WSe2光电催化活性的方法主要是负载是铂、钌一类贵金属及其相应复合物,由于其价格昂贵且地球含量低,极大地限制该类材料在光电催化分解水方面的实际应用。利用非贵金属组成的半导体与WSe2复合构筑p-n异质结是提高WSe2光电催化分解水的主要手段之一,在此基础上为了进一步提高材料的光电活性,可通过负载贵金属。
发明内容
针对现有技术的不足,本发明旨在提供一种WSe2基复合纳米片光电极的制备方法,研发了由高丰度且廉价元素W、Se组成的WSe2纳米片光电极,然后通过水浴沉积的方法构筑了CdS-WSe2异质结,为了避免CdS光腐蚀、便于Pt沉积,在异质结的外面通过水浴沉积的方法沉积一层In2S3,最后通过光还原的方法得到Pt-In2S3-CdS-WSe2复合纳米片光电极。该材料在近中性条件下具有较好的光电催化活性,可应用于光电催化分解水制氢。
为了实现上述目的,本发明采用如下技术方案:
一种WSe2基复合纳米片光电极的制备方法,包括如下步骤:
S1合成WO3纳米片光电极;
S2合成WSe2纳米片光电极:
2.1)称取四氯化硒,平铺于瓷舟内,瓷舟上方放置WO3纳米片光电极,然后置于石英管内,石英管的两端用由锡纸包裹的石英塞子塞住,然后通氩气,之后关闭气体,煅烧;
2.2)待冷却至室温,从石英管中取出步骤2.1)中最终得到的产物,用蒸馏水和无水乙醇交替清洗,然后置于真空干燥箱中烘干,即可制得WSe2纳米片光电极;
S3合成CdS-WSe2异质结光电极:
3.1)将步骤S2制得的WSe2纳米片光电极置于浓氨水中,加入然后置于水浴锅中,在水浴条件下进行吸附,吸附完毕后,加入硫脲,水浴条件下沉积;
3.2)反应结束后,用镊子将步骤3.1)得到的产物取出,用蒸馏水冲洗,然后置于真空干燥箱中干燥,即可获得CdS-WSe2异质结光电极;
S4合成In2S3-CdS-WSe2光电极
4.1)将CdS-WSe2异质结光电极置于19mL水中,依次加入冰醋酸和In2(SO4)3,然后置于水浴锅中,在水浴条件下进行吸附,吸附完毕之后,加入硫代乙酰胺,水浴条件下沉积;
4.2)反应结束后,用镊子将步骤4.1)最终得到的产物取出,用蒸馏水冲洗然后置于真空干燥箱中烘干,即可获得In2S3-CdS-WSe2光电极;
S5合成Pt-In2S3-CdS-WSe2复合纳米片光电极
5.1)将Na2SO4溶于水,然后加入H2PtCl6.6H2O,不断搅拌下稀释,即可获得含有H2PtCl6.6H2O的硫酸钠溶液;
5.2)取步骤5.1)得到的H2PtCl6.6H2O的硫酸钠溶液置于光电化学池中,采用三电极系统,以Pt为对电极,饱和甘汞为参比电极,以In2S3-CdS-WSe2光电极为工作电极,使用时间电流曲线法,设定电压-0.1V,时间为600s,然后打开氙灯,点击运行系统;
5.3)反应结束后,用镊子将步骤5.2)最终得到的产物取出,用蒸馏水冲洗,然后置于干燥箱中烘干,即可得到Pt-In2S3-CdS-WSe2复合纳米片光电极。
需要说明的是,步骤S1具体为:
1.1)将W网依次置于氢氧化钠溶液、丙酮溶液中超声;
1.2)将浓硝酸和浓盐酸加入到反应釜中;然后往反应釜放入经过步骤1.1)处理的W网,80℃下溶剂热反应3h;
1.3)将步骤1.2)制得的产物依次用蒸馏水、无水乙醇冲洗,并用超声清洗仪超声1min,制得WO3.xH2O,烘干,500℃煅烧1h即可得WO3纳米片光电极。
上述制备方法制备得到的Pt-In2S3-CdS-WSe2复合纳米片光电极在光电催化分解水中的应用,具体在光电催化分解水中作为光电极。
本发明的有益效果在于:
1、研发了由高丰度且廉价元素W、Se组成的WSe2纳米片光电极,然后通过水浴沉积的方法构筑了CdS-WSe2异质结,为了避免CdS光腐蚀、便于Pt沉积,在异质结的外面通过水浴沉积的方法沉积一层In2S3,最后通过光还原的方法得到Pt-In2S3-CdS-WSe2复合纳米片光电极。该材料在近中性条件下具有较好的光电催化活性,可应用于光电催化分解水制氢。
2、本发明所需原料来源丰富、路线简单、重复性好、材料稳定性高。
附图说明
图1为WSe2纳米片光电极的扫描电镜像。
图2为本发明制备的WSe2纳米片光电极的透射电镜像。
图3为本发明制备的WSe2纳米片光电极的EDX能谱
图4为本发明制备的WSe2纳米片光电极的X射线衍射花样。
图5为本发明制备的WSe2纳米片光电极的X射线光电子能谱。
图6为本发明制备的CdS-WSe2纳米片光电极的SEM图片。
图7为本发明制备的Pt-In2S3-CdS-WSe2纳米片光电极的SEM图片。
图8为本发明制备的WSe2、CdS-WSe2和Pt-In2S3-CdS-WSe2纳米片光电极的光电催化性能。
图9为本发明制备的WSe2和Pt-In2S3-CdS-WSe2纳米片光电极的交流阻抗谱。
具体实施方式
以下将结合附图对本发明作进一步的描述,需要说明的是,本实施例以本技术方案为前提,给出了详细的实施方式和具体的操作过程,但本发明的保护范围并不限于本实施例。
一种WSe2基复合纳米片光电极的制备方法,包括以下步骤:
S1合成WO3纳米片光电极:
1.1)将1.5*4cm的W网依次置于10%的氢氧化钠溶液、丙酮中超声30min;
1.2)将5mL浓硝酸,15mL浓盐酸加入到40mL反应釜中;然后放入洗干净的W网,80℃下溶剂热反应3h;
1.3)将制得的产物依次用蒸馏水、无水乙醇冲洗,并用超声清洗仪超声1min,可制得WO3.xH2O,60℃条件下烘干,500℃煅烧1h即可得WO3纳米片光电极;
S2合成WSe2纳米片光电极:
2.1)准确称取220mg的四氯化硒,平铺于瓷舟内,瓷舟上方放置WO3纳米片光电极,然后置于内径为22mm,长度为80mm的石英管内,石英管的两端用由锡纸包裹的直径为20mm的石英塞子塞住,然后通氩气25min,氩气的流速为600mL/min,之后关闭气体,750℃条件下煅烧1h;
2.2)待冷却至室温,从石英管中取出,用蒸馏水和无水乙醇清洗3次,然后置于60℃真空干燥箱中,即可制得WSe2纳米片光电极;
S3合成CdS-WSe2异质结光电极:
3.1)将WSe2纳米片光电极置于23mL浓氨水中,加入80mg的然后置于65℃水浴锅中,吸附10min,吸附完毕后,加入420mg的硫脲,65℃水浴条件下沉积7min;
3.2)反应结束后,用镊子将光电极取出,用蒸馏水冲洗3次,然后置于60℃真空干燥箱中,即可获得CdS-WSe2异质结光电极;
S4合成In2S3-CdS-WSe2光电极
4.1)将CdS-WSe2异质结光电极置于19mL水中,依次加入120μL冰醋酸,258mg In2(SO4)3,然后置于80℃水浴锅中,吸附10min,吸附完毕之后,加入300mg硫代乙酰胺,80℃水浴条件下沉积13min;
4.2)反应结束后,用镊子将光电极取出,用蒸馏水冲洗3次,然后置于60℃真空干燥箱中,即可获得In2S3-CdS-WSe2光电极;
S5合成Pt-In2S3-CdS-WSe2复合纳米片光电极
5.1)将1.42g Na2SO4溶于50mL水,然后加入52mg H2PtCl6.6H2O,不断搅拌下,稀释到100mL,即可获得含有0.1mM H2PtCl6.6H2O的硫酸钠溶液;
5.2)取100mL上述电解质溶液置于光电化学池中,采用三电极系统,以Pt为对电极,饱和甘汞为参比电极,以In2S3-CdS-WSe2光电极为工作电极,确保插入电解质溶液的电极面积为3cm2,使用时间电流曲线法,设定电压-0.1V,时间为600s,然后打开300W氙灯,用直尺测量工作电极距离氙灯灯头的距离为10cm,点击运行;
5.3)反应结束后,用镊子将光电极取出,用蒸馏水冲洗3次,然后置于60℃的干燥箱中烘干,即可得到Pt-In2S3-CdS-WSe2复合纳米片光电极。
上述制备方法制备得到的Pt-In2S3-CdS-WSe2复合纳米片光电极在光电催化分解水中的应用,具体在光电催化分解水中作为光阴极。
步骤S2所获得WSe2纳米片光电极扫描电镜图像如图1所示,二维的纳米片均匀生长在一维的W线上,从而构筑了三维结构的光电极,其中纳米片的厚度为77nm。
步骤S2所获得WSe2纳米片光电极的透射电镜图像如图2所示。
步骤S2所获得WSe2纳米片光电极EDX图像如图3所示,其中W和Se的原子的比值为1:1.83,基本接近理论比值1:2。
步骤S2所获得WSe2纳米片光电极的X射线衍射花样如图4所示,结果表明其是纯相的WSe2。
步骤S2所获得WSe2纳米片光电极的X射线光电子能谱如图5所示,在W的X射线光电子光谱中,在37.5eV附近的小峰归属于WO3的W4f5/2,主要原因是样品制备和转移期间发生了氧化。
步骤S3所获得的CdS-WSe2异质结光电极的SEM图,如图6所示,颗粒状的CdS生长在WSe2纳米片上,其中CdS纳米颗粒的尺寸为57nm。
步骤S4所获得的Pt-In2S3-CdS-WSe2复合纳米片光电极的SEM图,如图7所示,纳米片的厚度变大,材料表面不能观察到Pt纳米颗粒的存在。
步骤S2、S3和S4所获得的WSe2、CdS-WSe2和Pt-In2S3-CdS-WSe2纳米片光电极的光电催化性能如图8所示,修饰了CdS之后,形成了p-n异质结,同时增加了WSe2的亲水性,光电催化性能有所增加,而继续修饰了In2S3和Pt之后,减少了CdS的光腐蚀,光电催化性能进一步提升。
进一步的,步骤S2、S3和S4所获得的WSe2、CdS-WSe2和Pt-In2S3-CdS-WSe2纳米片光电极的交流阻抗谱,如图9所示,电阻的大小顺序为WSe2>Pt-In2S3-CdS-WSe2。
下面通过实验说明WSe2、CdS-WSe2和Pt-In2S3-CdS-WSe2复合纳米片光电极的光电性能:
取100mL 0.5M Na2SO4溶液置于光电化学池中,采用三电极系统,以Pt为对电极,饱和甘汞为参比电极,分别以WSe2、CdS-WSe2和Pt-In2S3-CdS-WSe2复合纳米片光电极为工作电极,确保插入电解质溶液的电极面积为3cm2,使用线性循环伏安法,设定电压范围为-0.6V-0V,然后打开300W氙灯,用直尺测量工作电极距离氙灯灯头的距离为10cm,点击运行。通过上述实验方法,其光电催化性能如图8所示,结果表明,Pt-In2S3-CdS-WSe2复合纳米片光电极与裸的WSe2和CdS-WSe2异质结光电极相比具有更好的光电催化性能。
对于本领域的技术人员来说,可以根据以上的技术方案和构思,作出各种相应的改变和变形,而所有的这些改变和变形都应该包括在本发明权利要求的保护范围之内。
Claims (3)
1.一种WSe2基复合纳米片光电极的制备方法,其特征在于,包括如下步骤:
S1合成WO3纳米片光电极;
S2合成WSe2纳米片光电极:
2.1)称取四氯化硒,平铺于瓷舟内,瓷舟上方放置WO3纳米片光电极,然后置于石英管内,石英管的两端用由锡纸包裹的石英塞子塞住,然后通氩气,之后关闭气体,煅烧;
2.2)待冷却至室温,从石英管中取出步骤2.1)中最终得到的产物,用蒸馏水和无水乙醇交替清洗,然后置于真空干燥箱中烘干,即可制得WSe2纳米片光电极;
S3合成CdS-WSe2异质结光电极:
3.1)将步骤S2制得的WSe2纳米片光电极置于浓氨水中,加入然后置于水浴锅中,在水浴条件下进行吸附,吸附完毕后,加入硫脲,水浴条件下沉积;
3.2)反应结束后,用镊子将步骤3.1)最终得到的产物取出,用蒸馏水冲洗,然后置于真空干燥箱中干燥,即可获得CdS-WSe2异质结光电极;
S4合成In2S3-CdS-WSe2光电极
4.1)将CdS-WSe2异质结光电极置于19mL水中,依次加入冰醋酸和In2(SO4)3,然后置于水浴锅中,在水浴条件下进行吸附,吸附完毕之后,加入硫代乙酰胺,水浴条件下沉积;
4.2)反应结束后,用镊子将步骤4.1)最终得到的产物取出,用蒸馏水冲洗然后置于真空干燥箱中烘干,即可获得In2S3-CdS-WSe2光电极;
S5合成Pt-In2S3-CdS-WSe2复合纳米片光电极
5.1)将Na2SO4溶于水,然后加入H2PtCl6.6H2O,不断搅拌下稀释,即可获得含有H2PtCl6.6H2O的硫酸钠溶液;
5.2)取步骤5.1)得到的H2PtCl6.6H2O的硫酸钠溶液置于光电化学池中,采用三电极系统,以Pt为对电极,饱和甘汞为参比电极,以In2S3-CdS-WSe2光电极为工作电极,使用时间电流曲线法,设定电压-0.1V,时间为600s,然后打开氙灯,点击运行系统;
5.3)反应结束后,用镊子将步骤5.2)最终得到的产物取出,用蒸馏水冲洗,然后置于干燥箱中烘干,即可得到Pt-In2S3-CdS-WSe2复合纳米片光电极。
2.根据权利要求1所述的一种WSe2基复合纳米片光电极的制备方法,其特征在于,步骤S1具体为:
1.1)将W网依次置于氢氧化钠溶液、丙酮溶液中超声;
1.2)将浓硝酸和浓盐酸加入到反应釜中;然后往反应釜放入经过步骤1.1)处理的W网,80℃下溶剂热反应3h;
1.3)将步骤1.2)制得的产物依次用蒸馏水、无水乙醇冲洗,并用超声清洗仪超声1min,制得WO3.xH2O,烘干,500℃煅烧1h即可得WO3纳米片光电极。
3.一种如权利要求1-2任一所述的制备方法制备得到的Pt-In2S3-CdS-WSe2复合纳米片光电极在光电催化分解水中的应用。
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