CN110252349A - 一种原位光沉积制备CdS@MoS2复合光催化剂的制备方法 - Google Patents
一种原位光沉积制备CdS@MoS2复合光催化剂的制备方法 Download PDFInfo
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Abstract
本发明公开了一种原位光沉积制备CdS@MoS2复合光催化剂的制备方法。以乙酰丙酮镉和硫代丙酰胺作为前驱物,以乙二胺为溶剂,通过溶剂热法合成CdS纳米棒。然后通过光沉积的方法,以MoCl5为前驱物和以氙灯为光源,在上述CdS表面原位光沉积MoS2,最终制得CdS@MoS2。该催化剂的MoS2与CdS两组分之间结合紧密,且CdS表面原来易受光腐蚀的S2‑固定在CdS的表面可减缓CdS的光腐蚀。同时,表面的MoS2能够发挥助催化剂特性促进CdS的光生载流子分离,还有着丰富的活性位点,大大地提升CdS的光催化活性。本发明提出的制备方法具有设备简单、操作方便、合成高效的特点。
Description
技术领域
本发明属于纳米材料制备技术领域,具体涉及一种原位光沉积制备CdS@MoS2复合光催化剂的制备方法。
背景技术
随着经济的快速发展,环境污染与能源紧缺问题日益凸显,成为21世纪人类社会发展道路上面临的两大挑战。半导体光催化技术是以太阳能转化与储存为核心,以光能驱动光催化反应,将太阳能转化成化学能的新兴技术,被认为是解决能源与环境这两个问题的一种理想的途径。但是,目前光催化剂技术在实际生产中的应用仍然面临着许多问题。例如,量子效率低,光催化剂光响应范围窄,稳定性差等。因此,制备高效、稳定的可见光光催化材料是实现光催化技术实际应用的先决条件,也是光催化材料研究者所需要解决的首要任务之一。
CdS作为一种重要的可见光催化剂,由于它独特的电学、光学、磁学及其发光性能,在光催化反应中得到广泛的研究。然而,CdS的光生电子和空穴快速复合以及严重的光腐蚀仍然是限制其广泛应用的主要壁垒。因此,如何促进其载流子有效分离和防止光腐蚀对于提高半导体金属硫化物光催化性能至关重要。
近年来,为了降低CdS的光腐蚀,促进CdS的光生载流子分离,提升CdS的光催化活性,研究者们展开了大量研究,其中将CdS与助催化剂复合是提升CdS光催化性能的有效途径之一。而在众多的助催化剂当中,MoS2因其导电性好,活性位点丰富而备受研究者们的关注。研究者们对于CdS/MoS2复合光催化剂也开展了许多研究,例如:专利CN 103566953A公开了一种以为复合纳米光催化剂及其制备方法和应用,该发明以四硫代钼酸铵和Cd(S2CNEt2)2分别为MoS2和CdS的前驱体,先以乙二胺为溶剂通过溶剂热反应制备了CdS,再以乙二醇为溶剂通过溶剂热反应在CdS表面附着MoS2,最后通过煅烧得到原子层厚度MoS2修饰的一维CdS纳米棒结构。所得样品有高效,稳定的光催化活性。专利CN 105664977A和专利CN106362774A分别公开了一种二硫化钼-硫化镉纳米复合材料及其制备方法和一种1D/2D垂直状CdS/MoS2产氢催化剂的制备方法,两种方法均通过二次溶剂热法先制得CdS后再制得CdS/MoS2,所得样品有很高的光催化产氢活性和光催化稳定性。CN 105688945A公开了一种MoS2纳米片/CdS纳米棒核壳结构复合光催化剂,该发明先以溶剂热制备了CdS纳米棒,再将酸化后的CdS与MoS2前驱盐一起溶剂热最后得到MoS2纳米片/CdS纳米棒核壳结构复合光催化剂。上述专利虽均制得MoS2/CdS纳米棒一维复合光催化材料,但仍然存在制备工艺繁琐,MoS2与CdS结合不紧密等问题。本发明相较于上述专利重要区别在于:(1)本发明虽也以溶剂热法制得CdS纳米棒,但是前驱物、反应条件均不同;(2)本发明通过光沉积的方式将MoS2原位生长在CdS纳米棒表面上;(3)本发明在负载 MoS2时未引入S源而是直接利用CdS纳米棒表面光腐蚀生成的S原位合成MoS2(4)本发明两组分原位生长,结合紧密,有利于使用中光生载流子的传输。
发明内容
本发明的目的在于针对CdS光生载流子易复合和光腐蚀严重的问题,提供一种原位光沉积制备CdS@MoS2复合光催化剂的制备方法,利用CdS表面因光腐蚀产生的S原位沉积了MoS2使得MoS2与CdS两组分之间结合更紧密,并且将CdS表面易受光腐蚀的S2-固定在CdS的表面减缓CdS的光腐蚀提升CdS的光催化稳定性;利用MoS2能够将CdS中光生电子导出的助催化剂特性促进CdS的光生载流子分离,提升CdS的光催化活性;利用MoS2表面丰富的活性位点进一步提升CdS@MoS2复合光催化材料的光催化性能。该方法具有制备条件要求低、操作方便、合成高效和产品性能稳定的特点。
为实现上述目的,本发明采用如下技术方案:
一种原位光沉积制备CdS@MoS2复合光催化剂的制备方法,其包括以下步骤:
(1)分别按比例5:1-1:5要求称取乙酰丙酮镉和硫代丙酰胺溶解于50~80mL的乙二胺中,搅拌0.5~3h,将所得到的混合溶液转入100mL聚四氟乙烯的反应釜中,用钢套封装后置于鼓风干燥箱内,加热至140~200℃并保温12~36h,冷却至室温后将所得黄色沉淀离心洗涤干燥后得CdS纳米棒。
(2)将所得一定量CdS纳米棒分散于50~200mL水中,并加入一定摩尔比的MoCl5超声溶解。将所得的悬浮液在真空中强力搅拌并使用氙灯光照0.5~3h。将光照后所得墨绿色沉淀离心洗涤干燥后得具有核壳结构的CdS@MoS2。
本发明的优点:
(1)利用原位光沉积所得的CdS@MoS2两组分之间有着更紧密的接触;
(2)利用原位沉积的MoS2将CdS表面易被光腐蚀的S2-固定从而减缓CdS的光腐蚀;
(3)利用MoS2能够将CdS的光生电子导出的助催化剂特性促进CdS的光生载流子分离,提升光催化性能;
(4)利用MoS2表面丰富的活性位点提升CdS@MoS2复合光催化剂的光催化性能;
(5)制备条件要求低、操作方便、合成高效。
附图说明
图1为本发明所合成的CdS@MoS2复合光催化剂的扫描电镜图;
图2为本发明的CdS@MoS2和CdS的光催化分解水产氢活性对比图。
具体实施方式
为了使本发明所述的内容更加便于理解,下面结合具体实施方式对本发明所述的技术方案做进一步的说明,但是本发明不仅限于此。
实施例1
称取5g乙酰丙酮镉和3.7g硫代丙酰胺溶解到60mL乙二胺中,搅拌1h,将所得到的混合溶液转入100mL的聚四氟乙烯的反应釜中,用钢套封装后置于鼓风干燥箱内,加热至180℃并保持24h,将所得到的黄色沉淀洗涤干燥得CdS纳米棒。取100mg CdS纳米棒分散于100mL水中,在水中加入170mg MoCl5溶解后在真空搅拌的条件下使用氙灯光照2h,将得到的墨绿色样品洗涤干燥得到CdS@MoS2。
实施例2
称取4.5g乙酰丙酮镉和3.2g硫代丙酰胺溶解到60mL乙二胺中,搅拌1h,将所得到的混合溶液转入100mL的聚四氟乙烯的反应釜中,用钢套封装后置于鼓风干燥箱内,加热至180℃并保持12h,将所得到的黄色沉淀洗涤干燥得CdS纳米棒。取100mg CdS纳米棒分散于100mL水中,在水中加入180mg MoCl5溶解后在真空搅拌的条件下使用氙灯光照2h,将得到的墨绿色样品洗涤干燥得到CdS@MoS2。
实施例3
称取3g乙酰丙酮镉和2g硫代丙酰胺溶解到70mL乙二胺中,搅拌1h,将所得到的混合溶液转入100mL的聚四氟乙烯的反应釜中,用钢套封装后置于鼓风干燥箱内,加热至180℃并保持24h,将所得到的黄色沉淀洗涤干燥得CdS纳米棒。取100mg CdS纳米棒分散于100mL水中,在水中加入150mg MoCl5溶解后在真空搅拌的条件下使用氙灯光照1h,将得到的墨绿色样品洗涤干燥得到CdS@MoS2。
实施例4
称取3.5g乙酰丙酮镉和4.5g硫代丙酰胺溶解到60mL乙二胺中,搅拌1h,将所得到的混合溶液转入100mL的聚四氟乙烯的反应釜中,用钢套封装后置于鼓风干燥箱内,加热至170℃并保持30h,将所得到的黄色沉淀洗涤干燥得CdS纳米棒。取100mg CdS纳米棒分散于80mL水中,在水中加入170mg MoCl5溶解后在真空搅拌的条件下使用氙灯光照1.5h,将得到的墨绿色样品洗涤干燥得到CdS@MoS2。
实施例5
按实施例1合成的催化剂,经扫描电镜观察,MoS2成功生长在CdS纳米棒表面,参见附图1。
实施例6
按实施例1合成的催化剂,具有核壳结构的CdS@MoS2光催化分解水产氢活性相对于CdS有着明显的提升,参见附图2。
以上所述仅为本发明的较佳实施例,凡依本发明申请专利范围所做的均等变化与修饰,皆应属本发明的涵盖范围。
Claims (6)
1.一种原位光沉积制备CdS@MoS2复合光催化剂的制备方法,其特征在于:包括以下步骤:
(1)在乙二胺中加入乙酰丙酮镉和硫代丙酰胺,搅拌溶解后,经溶剂热反应得到CdS纳米棒;
(2)将步骤(1)得到的CdS纳米棒分散于水中,加入MoCl5,在真空搅拌条件下经光沉积反应得到核壳结构的CdS@MoS2。
2.根据权利要求1所述的制备方法,其特征在于:步骤(1)中加入的乙酰丙酮镉和硫代丙酰胺的摩尔比为5:1~1:5,乙二胺的体积为50~80mL。
3.根据权利要求1所述的制备方法,其特征在于:步骤(1)中搅拌溶解时间为0.5~3h。
4.根据权利要求1所述的制备方法,其特征在于:步骤(1)中溶剂热反应的温度为140~200℃,时间为12~36h。
5.根据权利要求1所述的制备方法,其特征在于:步骤(2)中水的体积为50~200mL,加入的MoCl5与CdS的摩尔比为1:20~2:1。
6.根据权利要求1所述的制备方法,其特征在于:步骤(2)中光照时间为0.5~3h。
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