CN105597786A - 一种锯齿状Cu2MoS4纳米片的制备方法及在电、光催化中的应用 - Google Patents
一种锯齿状Cu2MoS4纳米片的制备方法及在电、光催化中的应用 Download PDFInfo
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Abstract
本发明公开了一种锯齿状Cu2MoS4纳米片电、光催化剂的制备方法,其特征在于,所述制备方法包括:合成Cu2O前躯体以及合成锯齿状Cu2MoS4纳米片。本发明有益效果在于:所需原料来源丰富、路线绿色、方法重复性好、可大规模合成;本发明制备的材料可用于电催化产氢、光催化降解污染物。反应高效,操作简单,制备的材料稳定性好,具有很好的实用价值和应用前景。
Description
技术领域
本发明涉及一种高效的锯齿状Cu2MoS4纳米片电、光催化剂的制备方法,属于无机纳米材料领域。
背景技术
随着社会与经济的发展,环境问题变得日趋严重。为了从根本上解决环境问题,可以从以下两个方面入手。第一,寻找可替代的绿色能源降低人类对不可再生化石燃料的依赖程度。氢气便是一种理想的清洁能源。水裂解是一种理想的制备氢气路线。因此,开发高效的裂解水产氢电催化剂具有重要意义。另一方面,在各类污染当中,水体污染尤其严重,亟待解决。
光催化技术可以利用“绿色”的太阳光,催化降解水体中的有机污染物,从而有效净化环境。如何发展廉价、高效的光催化剂也是当前研究的重要课题。
目前,效率最高的电催化裂解水产氢催化剂是铂、钯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电催化分解水方面的实际应用。发展非贵金属电催化剂用于电催化分解水是其下一步大规模应用的必然。另一方面,现在商品化的光催化剂主要是TiO2(P25)。但该光催化剂只能吸收紫外光,而太阳光谱中紫外光<5%。因此,开发高效的可见光响应的光催化剂是实现光催化技术应用的前提。Cu2MoS2是一类具有层状结构的窄带隙半导体。文献报道该材料可以电解水产氢,也可以用于降解有机污染物。然而,未经改性的Cu2MoS2,其电、光催化活性比较低,不足实际应用。纳米片具有大的比表面积,通过刻蚀获得锯齿状结构,可暴露更多的活性位点。基于以上两点,申请人研发了由高丰度且廉价元素Cu、Mo、S组成的Cu2MoS2锯齿状纳米片。该材料具有高效的电、光催化活性,可应用于电催化分解水制氢及环境净化。
发明内容
鉴于上述目前,本发明旨在于提供一种高效的锯齿状Cu2MoS4纳米片电、光催化剂的制备方法,该材料具有比表面积大,活性位点多,吸光能力强,电催化分解水及光催化降解污染物活性高等优点,且产品制备路线绿色,重复性好,可规模化。
为了实现上述目的,本发明采用的技术方案如下:
一种锯齿状Cu2MoS4纳米片电、光催化剂的制备方法,所述制备方法包括以下步骤:
S1合成Cu2O前躯体:
S1.16.66gPVP在40℃水浴条件下溶解于100mL去离子水中,待完全溶解后用100mL去离子水冷却溶液;
S1.2向所述溶液中加入2mmol的氯化铜,搅拌溶解后再逐滴加入20mL2MNaOH溶液,搅拌老化30min,待溶液颜色由浅蓝色变成深褐色后再逐滴加入20mL0.6M抗坏血酸溶液;
S1.3上述混合溶液在室温条件下搅拌3h后待溶液颜色变成棕黄色后停止搅拌,将获得的产物Cu2O用去离子水、乙醇各离心3次并在真空干燥箱中60℃下烘干待用即可;
S2合成锯齿状Cu2MoS4纳米片:
S2.1155mg二水合钼酸钠在超声条件下溶解于100mL乙二醇溶液中,加入350mg硫代乙酰胺继续超声溶解待变成澄清溶液后加入150mg上述所述Cu2O继续超声溶解至溶液变成深褐色溶液后转移至反应釜中210℃反应24h;
S2.2反应结束后将获得产物Cu2MoS4纳米片用去离子水、乙醇各离心4次并真空干燥箱中60℃下烘干待用;
S3取50mg所述Cu2MoS4纳米片的粉体于50mL烧杯中,加入20mL4MHNO3溶液后在室温条件下搅拌2-10h,反应结束后用去离子水、乙醇各离心3次并真空干燥箱中60℃下烘干即可获得锯齿状Cu2MoS4纳米片。
需要说明的是,所述PVP即聚乙烯吡咯烷酮,M=58000。
需要说明的是,所述锯齿状Cu2MoS4纳米片为高丰度非贵金属元素构成的三元复合半导体材料。
需要说明的是,所述锯齿状Cu2MoS4纳米片为边缘锯齿状的纳米片,其颗粒大小为4~5微米。
作为本发明的应用如下:
一种使用锯齿状Cu2MoS4纳米片在光催化中的应用,所述锯齿状Cu2MoS4纳米片可作为催化剂。
一种使用锯齿状Cu2MoS4纳米片在电催化中的应用,所述锯齿状Cu2MoS4纳米片作为催化剂。
本发明有益效果在于:
1、本发明所需原料来源丰富、路线绿色、方法重复性好、可大规模合成;
2、本发明制备的材料可用于电催化产氢、光催化降解污染物。反应高效,操作简单,制备的材料稳定性好,具有很好的实用价值和应用前景。
附图说明
图1为Cu2MoS4纳米片的扫描电镜像。
图2为本发明制备的锯齿状Cu2MoS4纳米片的透射电镜像。
图3为本发明制备的锯齿状Cu2MoS4纳米片的粉末X射线衍射花样。
图4为本发明制备的锯齿状Cu2MoS4纳米片的X射线光电子能谱。
图5为本发明制备的锯齿状Cu2MoS4纳米片的紫外漫反射谱。
图6为本发明制备的锯齿状Cu2MoS4纳米片的氮气吸附-脱附等温线。
图7为本发明制备的刻锯齿状Cu2MoS4纳米片与未经刻的Cu2MoS4纳米片的接触角照片。
图8为本发明制备的刻锯齿状Cu2MoS4纳米片与未经刻的Cu2MoS4纳米片的电催化极化曲线。
图9为本发明制备的刻锯齿状Cu2MoS4纳米片与未经刻的Cu2MoS4纳米片的光催化降解罗丹明B的活性。
图10为合成的锯齿状Cu2MoS4纳米片在1000圈循环伏安前后的电化学极化曲线。
具体实施方式
以下实例进一步阐述本发明的技术方案,但不代表或限制本发明的权利保护范围,本发明的保护范围以权利要求为准。
实施例1
一种锯齿状Cu2MoS4纳米片电、光催化剂的制备方法,所述制备方法包括以下步骤:
S1合成Cu2O前躯体:
S1.16.66gPVP在40℃水浴条件下溶解于100mL去离子水中,待完全溶解后用100mL去离子水冷却溶液;
S1.2向所述溶液中加入2mmol的氯化铜,搅拌溶解后再逐滴加入20mL2MNaOH溶液,搅拌老化30min,待溶液颜色由浅蓝色变成深褐色后再逐滴加入20mL0.6M抗坏血酸溶液;
S1.3上述混合溶液在室温条件下搅拌3h后待溶液颜色变成棕黄色后停止搅拌,将获得的产物Cu2O用去离子水、乙醇各离心3次并在真空干燥箱中60℃下烘干待用即可;
S2合成锯齿状Cu2MoS4纳米片:
S2.1155mg二水合钼酸钠在超声条件下溶解于100mL乙二醇溶液中,加入350mg硫代乙酰胺继续超声溶解待变成澄清溶液后加入150mg上述所述Cu2O继续超声溶解至溶液变成深褐色溶液后转移至反应釜中210℃反应24h;
S2.2反应结束后将获得产物Cu2MoS4纳米片用去离子水、乙醇各离心4次并真空干燥箱中60℃下烘干待用;
S3取50mg所述Cu2MoS4纳米片的粉体于50mL烧杯中,加入20mL4MHNO3溶液后在室温条件下搅拌2-10h,反应结束后用去离子水、乙醇各离心3次并真空干燥箱中60℃下烘干即可获得锯齿状Cu2MoS4纳米片。
需要说明的是,所述PVP即聚乙烯吡咯烷酮,M=58000。
需要说明的是,所述锯齿状Cu2MoS4纳米片为高丰度非贵金属元素构成的三元复合半导体材料。
需要说明的是,所述锯齿状Cu2MoS4纳米片为边缘锯齿状的纳米片,其颗粒大小为4~5微米。
进一步的,步骤2.2所获得Cu2MoS4纳米片扫描电镜像显示如图1所示;
进一步的,步骤3所获得锯齿状Cu2MoS4纳米片透射电镜像如图2所示。
如图3所示,锯齿状Cu2MoS4纳米片X射线衍射花样研究表明其是纯相的Cu2MoS4。
如图4的本发明锯齿状Cu2MoS4纳米片样品的紫外漫反射谱,测试显示锯齿状Cu2MoS4纳米片对波长700nm以下的紫外与可见光均具有良好的光吸收能力。
如图5所示,X射线光电子谱表面锯齿状Cu2MoS4纳米片样品中所含的Cu、Mo与S元素分别为+1,+6与-2价。刻蚀过程对材料的结构与成键能无明显影响。
实例2
如图6所述,显示了刻蚀对锯齿状Cu2MoS4纳米片粉体亲水性程度的影响。其结果表明,经过刻蚀后,锯齿状Cu2MoS4纳米片具有更好的亲水性。
实例3
如图7所示,显示了刻蚀对锯齿状Cu2MoS4纳米片比表面积的影响。经过刻蚀获得的锯齿状Cu2MoS4纳米片具有更大的比表面积。
实例4
通过下述实验了解刻蚀对锯齿状Cu2MoS4纳米片在0.5MH2SO4体系中的电催化活性影响,具体的说:
取5mg锯齿状Cu2MoS4纳米片样品分散于1mL异丙醇/水(体积比2:1)混合溶液中,超声10min后加入40μL5wt%Nafion继续超声30min待用。取上述溶液4μL滴在打磨过的玻碳电极表面上,室温下放置过夜后用作工作电极,参比电极为饱和甘汞电极,对电极为铂丝电极。采用线性伏安扫描法,扫描范围-0.8-0.2V,扫描速度5mV/s。通过上述实验方法,其产氢性能如图8所示,结果表明,刻蚀后的锯齿状Cu2MoS4纳米片显示更高的电催化活性。
实例5
通过下述实验了解刻蚀对锯齿状Cu2MoS4纳米片纳米片的光催化活性的影响性,具体的说:
分别取本发明制备的锯齿状Cu2MoS4纳米片和未经刻蚀的Cu2MoS4纳米片100mg样品加入100mL10-5M罗丹明B溶液中,在500W氙灯下(滤去400nm以下的波长)可见光辐照下,催化降解有机物罗丹明B。降解效果如图9所示,锯齿状Cu2MoS4纳米片明显展示出更好的光催化活性,在90min内几乎完全降解罗丹明B。而同样条件下,未经刻蚀的Cu2MoS4纳米片仅降解68%的罗丹明B。
电化学测试条件与实施例4的实验方法基本一致。如图10所示,经过1000圈循环,本发明所制备的锯齿状Cu2MoS4纳米片的电催化活性几乎不变,表明该材料具有很好的稳定性。
对于本领域的技术人员来说,可根据以上描述的技术方案以及构思,做出其它各种相应的改变以及变形,而所有的这些改变以及变形都应该属于本发明权利要求的保护范围之内。
Claims (5)
1.一种锯齿状Cu2MoS4纳米片电、光催化剂的制备方法,其特征在于,所述制备方法包括以下步骤:
S1合成Cu2O前躯体:
S1.16.66gPVP在40℃水浴条件下溶解于100mL去离子水中,待完全溶解后用100mL去离子水冷却溶液;
S1.2向所述溶液中加入2mmol的氯化铜,搅拌溶解后再逐滴加入20mL2MNaOH溶液,搅拌老化30min,待溶液颜色由浅蓝色变成深褐色后再逐滴加入20mL0.6M抗坏血酸溶液;
S1.3上述混合溶液在室温条件下搅拌3h后待溶液颜色变成棕黄色后停止搅拌,将获得的产物Cu2O用去离子水、乙醇各离心3次并在真空干燥箱中60℃下烘干待用即可;
S2合成锯齿状Cu2MoS4纳米片:
S2.1155mg二水合钼酸钠在超声条件下溶解于100mL乙二醇溶液中,加入350mg硫代乙酰胺继续超声溶解待变成澄清溶液后加入150mg上述所述Cu2O继续超声溶解至溶液变成深褐色溶液后转移至反应釜中210℃反应24h;
S2.2反应结束后将获得产物Cu2MoS4纳米片用去离子水、乙醇各离心4次并真空干燥箱中60℃下烘干待用;
S3取50mg所述Cu2MoS4纳米片的粉体于50mL烧杯中,加入20mL4MHNO3溶液后在室温条件下搅拌2-10h,反应结束后用去离子水、乙醇各离心3次并真空干燥箱中60℃下烘干即可获得锯齿状Cu2MoS4纳米片。
2.根据权利要求1所述的锯齿状Cu2MoS4纳米片电、光催化剂的制备方法,其特征在于,所述锯齿状Cu2MoS4纳米片为高丰度非贵金属元素构成的三元复合半导体材料。
3.根据权利要求1所述的锯齿状Cu2MoS4纳米片电、光催化剂的制备方法,其特征在于,所述锯齿状Cu2MoS4纳米片为边缘锯齿状的纳米片,其颗粒大小为4~5微米。
4.一种使用权利要求1所述的锯齿状Cu2MoS4纳米片在光催化中的应用,其特征在于,所述锯齿状Cu2MoS4纳米片作为催化剂。
5.一种使用权利要求1所述的锯齿状Cu2MoS4纳米片在电催化中的应用,其特征在于,所述锯齿状Cu2MoS4纳米片作为催化剂。
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106830080A (zh) * | 2016-12-13 | 2017-06-13 | 中国科学技术大学 | Cu2MoS4纳米材料及其制备方法 |
CN106882855A (zh) * | 2017-03-17 | 2017-06-23 | 中国科学技术大学 | Cu2MoS4纳米管在光催化中的应用 |
CN107200354A (zh) * | 2017-05-31 | 2017-09-26 | 张泰泓 | 一种简易Cu2MoS4量子点材料合成方法 |
CN110327943A (zh) * | 2019-07-16 | 2019-10-15 | 安徽师范大学 | 一种Cu-Mo-S复合材料及其制备方法和应用 |
CN112838201A (zh) * | 2021-04-06 | 2021-05-25 | 湖南镕锂新材料科技有限公司 | 一种Cu2MoS4复合负极材料及其制备方法和钠离子电池 |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105098576A (zh) * | 2015-08-27 | 2015-11-25 | 浙江大学 | Cu2MoS4二维晶体的用途及其构成的饱和吸收体器件 |
CN105126867A (zh) * | 2015-08-03 | 2015-12-09 | 浙江大学 | 一种碳负载Pt-Ru-Ni催化剂及其制备方法和应用 |
-
2016
- 2016-01-25 CN CN201610048952.XA patent/CN105597786A/zh active Pending
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105126867A (zh) * | 2015-08-03 | 2015-12-09 | 浙江大学 | 一种碳负载Pt-Ru-Ni催化剂及其制备方法和应用 |
CN105098576A (zh) * | 2015-08-27 | 2015-11-25 | 浙江大学 | Cu2MoS4二维晶体的用途及其构成的饱和吸收体器件 |
Non-Patent Citations (3)
Title |
---|
CARLOS G.MORALES-GUIO ET AL.: ""Nanostructured hydrotreating catalysts for electrochemical hydrogen evolution"", 《CHEMICAL SOCIETY REVIEWS》 * |
HAILONG YU ET AL.: ""A strategy to synergistically increase the number of active edge sites and the conductivity of MoS2 nanosheets for hydrogen evolution"", 《NANOSCALE》 * |
WENXING CHEN ET AL.: ""Solvothermal Synthesis of Ternary Cu2MoS4 Nanosheets: Structural Characterization at the Atomaic Level"", 《SMALL》 * |
Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106830080A (zh) * | 2016-12-13 | 2017-06-13 | 中国科学技术大学 | Cu2MoS4纳米材料及其制备方法 |
CN106830080B (zh) * | 2016-12-13 | 2018-08-24 | 中国科学技术大学 | Cu2MoS4纳米材料及其制备方法 |
CN106882855A (zh) * | 2017-03-17 | 2017-06-23 | 中国科学技术大学 | Cu2MoS4纳米管在光催化中的应用 |
CN106882855B (zh) * | 2017-03-17 | 2020-05-05 | 中国科学技术大学 | Cu2MoS4纳米管在光催化中的应用 |
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