CN108273527A - FeSe/CdS纳米复合光催化剂及制备方法 - Google Patents
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Abstract
本发明涉及光催化分解水制氢技术，尤其涉及FeSe/CdS纳米复合光催化剂及制备方法，该催化剂将FeSe纳米棒沉积在CdS纳米颗粒表面，该制备方法为：水热合成法制备CdS纳米颗粒；CdS纳米颗粒和FeSe纳米棒混合后分散在乙醇中；上述悬浊液蒸发得到FeSe/CdS复合光催化剂。本发明将CdS纳米颗粒与FeSe纳米棒复合，FeSe作为光生电子的搜集体和载体，能够有效分离光生电子空穴对，光生电子与氢离子发生反应生成氢气。当FeSe的浓度为2wt%，其光催化产氢性能最佳，是纯CdS纳米颗粒产氢性能的7倍。在420nm单波长光激发下，测得其量子效率为6.71%。
Description
技术领域
本发明涉及光催化技术领域，尤其涉及一种用于光催化分解水制氢的FeSe/CdS纳米复合光催化剂及制备方法。
背景技术
随着现代工业的发展，能源越来越短缺。光催化分解水制氢，是一种利用太阳能制氢的绿色技术。ZnO和TiO2等半导体光催化剂由于带隙较宽，不能充分利用太阳光。因此，科学家们研发了多种可见光响应的半导体光催化剂，其中，CdS具有较好的可见光响应，主要是由于CdS具有合适的导带边位置、好的可见光吸收范围、优异的电子迁移性。但是，高的电子-空穴复合率限制了其产氢速率。因此，迫切需要寻找降低电子-空穴复合的方法。
目前一些研究者利用金、银、铂等贵金属与半导体复合，能够有效降低电子-空穴复合率，但贵金属价格昂贵不利于大面积推广，而且贵金属等助催化剂在半导体光催化剂表面分布不够均匀。FeSe是一种优异的导体，强的电子吸引力，与半导体复合后，能够将半导体表面的电子转移到FeSe表面。
发明内容
针对上述问题，本发明提供一种成本较低、效率高的FeSe/CdS纳米复合光催化剂及制备方法。
为达上述发明目的，本发明采用的技术方案为：一种FeSe/CdS纳米复合光催化剂，包括有FeSe纳米棒、CdS纳米颗粒，FeSe纳米棒沉积在CdS纳米颗粒表面。
较佳地，所述的CdS纳米颗粒尺寸为25 nm。
较佳地，所述的FeSe纳米棒长度为0.3~ 1.2 µm、直径为30 nm。
一种FeSe/CdS纳米复合光催化剂制备方法，其特征在于：包括以下步骤：
S1，利用水热合成法制备CdS纳米颗粒；
S2，采用固相烧结法和超声剥离法制备FeSe纳米棒；
S3，将步骤S1制备的CdS纳米颗粒和S2制备的FeSe纳米棒按98:2混合后超声分散在无水乙醇中；
S4，将步骤S3分散好的悬浊液蒸发，得到FeSe/CdS纳米复合光催化剂。
S5，将步骤S4得到的粉体于200℃退火处理2小时。
较佳地，所述步骤S4具体为：将S3中分散好的悬浊液在油浴磁力搅拌器中于80℃搅拌加热8小时，随后在氩气管式炉中200℃退火处理2小时，得到FeSe/CdS纳米复合光催化剂。
本发明将CdS纳米颗粒与FeSe纳米棒复合，FeSe作为光生电子的搜集体和载体，能够有效分离光生电子空穴对，光生电子与氢离子发生反应生成氢气。将奈酚分散在FeSe和CdS纳米颗粒的悬浊液中，能够将FeSe均匀分散在CdS纳米颗粒表面，利于光生电子从CdS转移到FeSe表面。当FeSe的浓度为2wt%，其光催化产氢性能最佳，是纯CdS纳米颗粒产氢性能的7倍。在420nm单波长光激发下，测得其量子效率为6.71%。
附图说明
图1为本发明实施例制备FeSe/CdS纳米复合光催化剂的场发射扫描电子显微镜图；
图2为本发明实施例的光催化制氢机理图；
图3为本发明实施例制备FeSe/CdS纳米复合光催化剂用于分解水制氢的效率图。
图4为本发明实施例制备FeSe/CdS纳米复合光催化剂用于分解水制氢的4次循环图。
具体实施方式
为更好地理解本发明，下面将结合附图和具体实施方式对本发明的技术方案做进一步说明，参见图1至图4：
按本发明实施的FeSe/CdS纳米复合光催化剂，进一步提高CdS纳米的光催化效率，其材料由CdS纳米颗粒表面沉积FeSe纳米棒制得。CdS纳米颗粒大小为25 nm，FeSe纳米棒长度为0.3~ 1.2 µm、直径为30 nm。图1为本发明实施例制备FeSe/CdS纳米复合光催化剂的场发射扫描电子显微镜图，从图1可看出，FeSe纳米棒不均匀地分布在CdS纳米颗粒表面。
按本发明实施的FeSe/CdS纳米复合光催化剂制备方法，包括以下步骤：
S1，利用水热合成法制备CdS纳米颗粒：首先将5.244 g Na2S 和 19.362 g Cd(OAc)2分别溶解在 480 ml 和 600 ml 去离子水中。然后将两种溶液混合在一起搅拌24小时，接着放置24小时。随后将混合溶液离心得到的黄色浆料放入72 mL 去离子水中，并放入100mL水热反应釜中，于473 K 反应 72 小时。将过滤得到的黄色浆料用去离子水和乙醇清洗，烘干后在真空条件下于368 K退火处理 24 小时。
S2，采用固相烧结法和超声剥离法制备FeSe纳米棒；
S3，将步骤S1制备的CdS纳米颗粒和S2制备的FeSe纳米棒按98:2混合后超声分散在无水乙醇中；
S4，将S3中分散好的悬浊液在油浴磁力搅拌器中于80℃搅拌加热8小时，随后在氩气管式炉中200℃退火处理2小时，得到FeSe/CdS纳米复合光催化剂。
如图2，本发明工作机理图为：CdS纳米颗粒与FeSe纳米棒复合后，FeSe作为光生电子的搜集体和载体，能够有效分离光生电子空穴对，光生电子与氢离子发生反应生成氢气。因此，FeSe与CdS纳米颗粒复合后能够有效提高其光催化制氢性能。
通过分解水制氢来表征FeSe/CdS纳米复合物的光催化性能。将50mg的FeSe/CdS纳米复合物放入含有0.1 M Na2S·9H2O 和 0.1 M Na2SO3的100mL去离子水中。在300W氙灯激发下（过滤掉420 nm以下的光），每隔1小时取一次样。其结果如图3所示。从图3中可以得出，当FeSe的浓度为2wt%，其光催化产氢性能最佳，是纯CdS纳米颗粒产氢性能的7倍。而且，2wt% FeSe/CdS纳米复合物的光催化性能高于2wt% Pt与CdS纳米颗粒的复合物。在420nm单波长光激发下，测得其量子效率为6.71%。图4为2wt% FeSe/CdS纳米复合物经过4次循环后的光催化性能，从图中可以看出，经过4次循环后，其性能没有降低，表明所制备的FeSe/CdS纳米复合物具有优异的稳定性。
Claims (6)
1.一种FeSe/CdS纳米复合光催化剂，其特征在于：包括有FeSe纳米棒、CdS纳米颗粒，FeSe纳米棒均匀沉积在CdS纳米颗粒表面。
2.根据权利要求1所述的FeSe/CdS纳米复合光催化剂，其特征在于：所述的CdS纳米颗粒尺寸大约为25nm。
3.根据权利要求1所述的FeSe/CdS纳米复合光催化剂制备方法，其特征在于：包括以下步骤：
S1，利用水热合成法制备CdS纳米颗粒；
S2，采用固相烧结法和超声剥离法制备FeSe纳米棒；
S3，将步骤S1制备的0.4 g CdS纳米颗粒和S2制备的0.08 g FeSe纳米棒混合，接着放入50 mL无水乙醇中形成悬浊液，将0.1 g奈酚放入上述悬浊液中，随后磁力搅拌1个小时；
S4，将步骤S3分散好的悬浊液蒸发，得到FeSe/CdS纳米复合光催化剂；
S5，将步骤S4得到的粉体于200℃退火处理2小时。
4.根据权利要求3所述的FeSe/CdS纳米复合光催化剂制备方法，其特征在于：所述步骤S4的化学沉积法为：将长度为0.3~ 1.2 µm、直径为30 nm FeSe纳米棒均匀分散在25 nmCdS纳米颗粒表面。
5.根据权利要求3所述的FeSe/CdS纳米复合光催化剂制备方法，其特征在于：所述步骤S4具体为：将S3中分散好的溶液在油浴磁力搅拌器中于80℃搅拌加热8小时。
6.根据权利要求3所述的FeSe/CdS纳米复合光催化剂制备方法，其特征在于：所述步骤S5具体为：在氩气管式炉中200℃退火处理2小时，得到FeSe/CdS纳米复合光催化剂。
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104941665A (zh) * | 2015-05-29 | 2015-09-30 | 江苏大学 | 具有高效光催化性能的GO-CdS复合材料的水热合成制备法 |
| CN105797752A (zh) * | 2016-04-01 | 2016-07-27 | 上海师范大学 | 富勒烯修饰的石墨烯/硫化镉催化剂及其制备方法与应用 |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104941665A (zh) * | 2015-05-29 | 2015-09-30 | 江苏大学 | 具有高效光催化性能的GO-CdS复合材料的水热合成制备法 |
| CN105797752A (zh) * | 2016-04-01 | 2016-07-27 | 上海师范大学 | 富勒烯修饰的石墨烯/硫化镉催化剂及其制备方法与应用 |
Non-Patent Citations (1)
| Title |
|---|
| WENWU ZHONG等: "Conductive FeSe nanorods：A novel and efficientco-catalyst deposited on BiVO4 for enhanced photocatalytic activity under visible light", 《JOURNAL OF ENVIRONMENTAL CHEMICAL ENGINEERING》 * |
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