CN106378160B - 一种制备CdS/MoS2复合空心方块光催化剂的方法 - Google Patents
一种制备CdS/MoS2复合空心方块光催化剂的方法 Download PDFInfo
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Abstract
本发明涉到复合纳米材料技术领域，特指一种以醋酸镉，碳酸氢钠，PVP，钼酸钠，硫脲为原料制备CdS/MoS2复合空心方块光催化剂的方法，尤其是一种制备工艺简单，产品具有良好可见光催化活性的复合光催化剂的制备方法。称取醋酸镉和PVP按照质量比1:10溶于去离子水中，再向其中加入碳酸氢钠，使醋酸镉和碳酸氢钠的物质的量的比为1:2，室温下搅拌反应2小时，反应结束后，将产物洗涤离心得到碳酸镉；然后再将碳酸镉，钼酸钠和硫脲按照物质的量的比为1:0.15‑1.4:4溶于去离子水中混合搅拌后，在220摄氏度条件下水热反应24小时，反应结束后经过洗涤，离心，干燥得到CdS/MoS2复合光催化剂。
Description
技术领域
本发明涉到复合纳米材料技术领域，特指一种以醋酸镉，碳酸氢钠，PVP，钼酸钠，硫脲为原料制备CdS/MoS2复合空心方块光催化剂的方法，尤其是一种制备工艺简单，产品具有良好可见光催化活性的复合光催化剂的制备方法。
技术背景
自21世纪以来，大量使用化石燃料带来的资源耗尽和环境污染等问题使环境友好的新型清洁能源的开发利用日益紧迫，其中氢能作为最具潜力的清洁能源吸引了大量研究投入。光分解水制氢是一个很有前途的技术可以实现太阳能到化学能量转换，而且氢能无污染的燃烧过程使氢在绿色能源方面有着不可比拟的优势。光分解水的性能受到吸收光谱、光生电荷转移、带隙结构和稳定性直接影响，因此设计具有良好催化活性的复合催化剂对光分解水具有至关重要的影响。
助催化剂是影响光催化性能的另一个决定性因素，近年来，以具有类石墨烯结构的MoS2为代表的二维层状金属硫化物由于具有优异的光电性质、侧边硫原子高活性析氢反应位点等优势，在光催化领域引起大量关注，与硫化物半导体 (如CdS，ZnS和ZnInS2等)复合也展示了优异的助催化性能。日本国立物质材料研究所的叶金花教授组报道了MoS2/石墨烯/CdS纳米级复合体系催化剂，其中石墨烯可增加体系的导电性，将CdS纳米晶产生的电子从MoS2的低活性平面位硫原子传递到高活性侧边硫原子。该工作中石墨烯尺寸为200-300 nm，MoS2尺寸约50-100nm，进一步减小MoS2横向尺寸至量子级别，大幅度缩短光生电子扩散至MoS2侧边活性位点的距离，能够显著提高光催化效率。最近，新加坡南洋理工大学的张华教授组报道了4-14nm的CdS和单层MS2 复合纳米晶(M＝W or Mo)，光生电子扩散到MS2侧边活性位点的距离非常小，且MS2单层的富硫面选择性生长于CdS的富Cd(001)面形成异质结，极大的提高了光生电子空穴在界面处的的分离效率，从而提高了光催化活性。然而，构筑具有均一结构的高性能的空心方块结构的CdS/MoS2异质结复合光催化剂的报道还没有。
发明内容
本发明目的是提供一种以醋酸镉，碳酸氢钠，PVP，钼酸钠，硫脲为原料，利用水热法来合成具有良好可见光催化活性的复合光催化剂的方法。
本发明通过以下步骤实现：
(1)称取醋酸镉和PVP按照质量比1:10溶于去离子水中，再向其中加入碳酸氢钠，使醋酸镉和碳酸氢钠的物质的量的比为1:2，室温下搅拌反应2小时，反应结束后，将产物洗涤离心得到碳酸镉；然后再将碳酸镉，钼酸钠和硫脲按照物质的量的比为1:0.15-1.4:4溶于去离子水中混合搅拌后，在220摄氏度条件下水热反应24小时，反应结束后经过洗涤，离心，干燥得到CdS/MoS2复合光催化剂。
(2)本发明所制备的CdS/MoS2复合光催化剂，晶化完全，分散性良好。
(3)利用X射线衍射仪(XRD)、扫描电子显微镜(SEM)、透射电子显微镜(TEM)、X光电子能谱仪等仪器对产物进行结构分析，以乳酸作为牺牲剂进行催化制氢，以评估其光催化活性。
附图说明
图1为所制备的CdS/MoS2复合光催化剂的XRD衍射谱图。
图2为所制备CdS/MoS2复合光催化剂的扫描电子显微镜图。
图3为所制备CdS/MoS2复合光催化剂的透射电镜照片。
图4为所制备CdS/MoS2复合光催化剂光催化产氢的性能图。
具体实施方式
实施例1CdS/MoS2复合光催化剂的制备
选取300mg碳酸镉，钼酸钠和500mg硫脲，钼酸钠的加入量分别按照物质的量的比为1:0:4，1:0.15:4，1:0.3:4，1:0.6:4，1:1.2:4，1:1.4:4加入，得到6组样本分别溶于35ml去离子水中，磁力搅拌，在220摄氏度条件下水热反应24小时，反应结束后，将所得产物依次用去离子水和乙醇洗净，过滤，放置于恒温干燥箱中60 摄氏度烘干。
实施例2CdS/MoS2异质结复合光催化剂的表征分析
如图1所示，从图中可以看出有CdS和MoS2衍射峰，并无其他杂相，说明我们得到的复合结构纯度高。
如图2所示，从图中可以看到均匀分布的空心方块结构。
如图3所示，从图中可以看到MoS2纳米片成功包覆在CdS空心方块表面，形成异质结构。
如图4所示，图中可以清楚看到CdS/MoS2复合光催化剂具有优异的光催化产氢性能。在碳酸镉，钼酸钠和硫脲的物质的量的比为1:1.2:4时，光催化产氢效率最高。
实施例3CdS/MoS2异质结复合光催化剂的可见光催化活性实验
(1)称取CdS/MoS2复合光催化剂100mg，置于光催化制氢反应器中，加入 100ml水，和10ml乳酸搅拌20分钟。
(2)每1小时用气相色谱对产生的氢气的量进行测定。
(3)由图4可见所制备的复合光催化剂具有优异的可见光催化活性，复合后的样品，比纯的CdS的产氢性能都要高。
Claims (2)
1.一种制备CdS/MoS2复合空心方块光催化剂的方法，其特征在于：将碳酸镉，钼酸钠和硫脲按照物质的量的比为1:0.15-1.4:4溶于去离子水中混合搅拌后，在220摄氏度条件下水热反应24小时，反应结束后经过洗涤，离心，干燥得到CdS/MoS2复合光催化剂；所述碳酸镉的制备方法如下：称取醋酸镉和PVP按照质量比1:10溶于去离子水中，再向其中加入碳酸氢钠，使醋酸镉和碳酸氢钠的物质的量的比为1:2，室温下搅拌反应2小时，反应结束后，将产物洗涤离心得到碳酸镉。
2.如权利要求1所述的一种制备CdS/MoS2复合空心方块光催化剂的方法，其特征在于，碳酸镉，钼酸钠和硫脲物质的量的比为1:1.2:4。
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| CN107460513A (zh) * | 2017-09-08 | 2017-12-12 | 华南师范大学 | MoS2/CdS薄膜电极的制备方法和应用 |
| CN108686681B (zh) * | 2018-05-14 | 2021-05-28 | 南昌航空大学 | 一种具有可见光催化活性的石墨烯/ZnS-MoS2纳米固溶体光催化剂 |
| CN109954504B (zh) * | 2019-04-02 | 2020-06-23 | 浙江大学 | 一种CdS纳米棒@少层ReS2纳米片复合光催化剂 |
| CN110368955B (zh) * | 2019-08-12 | 2022-06-07 | 陕西科技大学 | 一种VS2/CdS复合光催化剂的制备方法 |
| CN110787814B (zh) * | 2019-11-07 | 2022-11-08 | 汕头大学 | 一种分层中空ZnCdS/MoS2异质结笼及其制备与应用 |
| CN113441155A (zh) * | 2021-05-18 | 2021-09-28 | 南昌航空大学 | 一种硫化铟银/还原氧化石墨烯/1t相硫化钼三元复合材料的制备方法 |
| CN114713262B (zh) * | 2022-04-13 | 2023-01-06 | 南京工业大学 | 一种全固态异质结构催化剂材料及其制备方法与应用 |
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| CN103566953A (zh) * | 2013-11-28 | 2014-02-12 | 中国石油大学(华东) | 一维复合纳米光催化剂及其制备方法和应用 |
| CN105688945A (zh) * | 2016-03-22 | 2016-06-22 | 福州大学 | MoS2纳米片/CdS纳米线核壳结构复合光催化剂 |
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| Microwave-assisted synthesis of porous CdO–CdS core–shell nanoboxes with enhanced visible-light-driven photocatalytic reduction of Cr(VI);Wenlong Yang，et.al.;《J. Mater. Chem.》;20120611;第22卷;第13895-13898页 * |
| One-pot Synthesis of CdS Nanocrystals Hybridized with Single-Layer Transition-Metal Dichalcogenide Nanosheets for Efficient Photocatalytic Hydrogen Evolution;Junze Chen,et.al.;《Angew. Chem. Int. Ed.》;20151231;第54卷;第1210-1214页 * |
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