CN109126829B - 一种三维异质结构CdS-MoS2复合粉体的制备方法 - Google Patents
一种三维异质结构CdS-MoS2复合粉体的制备方法 Download PDFInfo
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Abstract
一种三维异质结构CdS‑MoS2复合粉体的制备方法,涉及适用于新能源和环境污水修复方面复合材料的制备技术领域。将钼酸铵、硫脲和甘氨酸或L‑天冬氨酸加入离子水进行混合溶解,超声处理后放到恒温鼓风烘箱中进行反应,反应后经后处理得到黑色MoS2粉体;将二硫化钼、乙酸镉和硫脲加入离子水进行混合溶解,超声处理后放到恒温鼓风烘箱中进行反应,反应后经后处理得到黄褐色或黑色CdS‑MoS2粉体。本发明通过两步水热法成功的获得一种形貌可控三维异质结构CdS‑MoS2复合粉体。通过系列实验结果表明通过改变负载的CdS的量可以获得不同形貌的CdS‑MoS2复合粉体,其具有粒度分布较窄、形貌分布均一和粒径可控等特点。
Description
技术领域
本发明涉及适用于新能源和环境污水修复方面复合材料的制备技术领域,具体是涉及一种三维异质结构CdS-MoS2复合粉体的制备方法。
背景技术
研究发现,对于MoS2负载型催化剂,载体主要起到修饰、增强基体的作用。使催化剂具有特定的外观形貌,提高其吸附性和催化活性等。目前,已合成出的各种复合型光催化剂中,如载体为γ-Al2O3时,其会与MoS2之间存在相互作用而限制了催化剂的加氢脱硫活性;而当TiO2和ZrO2作为载体材料时,降低了催化剂的比表面积并且容易受热分解;介孔分子筛和活性炭负载型催化剂,由于其特定的结构,能够催化降解的物质很有限。综上所述,一般的载体材料对MoS2的催化性能有一定的增强作用,但也带来一些弊端。因此,需要寻找其它更为理想的载体来进一步提升MoS2负载型催化剂的性能。
CdS半导体由于其禁带宽度较窄,能够在可见光照射下激发产生光生电子-空穴对,可以对有机污染物发生氧化还原反应,并进行催化降解。研究发现,纳米状的CdS材料具有量子尺寸效应,使其禁带宽度更宽,光生电子和空穴的氧化还原能力增强;而且其比表面积增大,可以吸附更多的有机污染物质;同时,光生电子-空穴对的复合几率降低,其催化能力增强。但如果使纳米CdS直接作用于光催化降解水中有机物,容易导致部分CdS颗粒在水中形成残留,难以与水进行彻底分离,从而引发二次污染。
本发明采用微纳米结构的二硫化钼为载体,通过水热法合成了CdS/MoS2复合粉体光催化剂,并研究其光催化降解罗丹明B的性能。所得到的一系列三维异质结构CdS-MoS2复合粉体具有优异的吸附和催化性能,有望用于污水处理领域。
发明内容
本发明要解决的技术问题为提供一种工艺简单、成本低、适合工业化规模生产的三维异质结构CdS-MoS2复合粉体的制备方法。
为了实现上述目的,本发明所采用的技术方案为:一种三维异质结构CdS-MoS2复合粉体的制备方法,骤如下:
1)、MoS2粉体的制备
按照质量比为1:1.5~6.5:0.65~5.7称取钼酸铵、硫脲和甘氨酸或L-天冬氨酸于烧杯中,加入离子水进行混合溶解,并放入超声清洗器中超声处理,然后将混合溶液转移到聚四氟乙烯内衬的反应釜中;将反应釜盖好放到恒温鼓风烘箱中进行反应,反应后经后处理得到黑色MoS2粉体;
2)、CdS-MoS2复合粉体的制备
按照质量比为6:1~9:0~3称取二硫化钼、乙酸镉和硫脲于烧杯中,加入去离子水进行混合分散,并放入超声清洗器中超声处理,再将混合溶液倒入聚四氟乙烯内衬反应釜中,将反应釜盖好放到恒温鼓风烘箱中进行反应,反应后经后处理得到黄褐色或黑色CdS-MoS2粉体。
作为本发明的三维异质结构CdS-MoS2复合粉体制备方法的优选技术方案,步骤1)中水热反应温度为160~180℃,反应时间为10~36h,步骤2)中水热反应温度为140~160℃,反应时间为8~36h,步骤1)和2)中于超声清洗器中超声处理时间为0.5~2h。后处理是将反应产物固液分离后分别使用无水乙醇及去离子水交替洗涤,然后置于恒温干燥箱中进行干燥,恒温干燥箱中干燥温度为40~80℃,干燥时间为6~18h。
本发明通过两步水热法成功的获得一种形貌可控三维异质结构CdS-MoS2复合粉体。通过系列实验结果表明通过改变负载的CdS的量可以获得不同形貌的CdS-MoS2复合粉体,其具有粒度分布较窄、形貌分布均一和粒径可控等特点。
与现有技术相比,本发明还具有以下优点:
1).本发明实现了两步水热法得到形貌可控三维异质结构CdS-MoS2复合粉体,为二硫化钼基复合纳米材料的合成提供了一种新的途径。
2).本发明工艺简单,整个制备体系容易构建、操作简便、条件易控、成本低廉、产物组成易控、产物分布均匀、不易团聚、适合于大规模工业生产。
3).本发明是采用常规可溶性钼酸铵和可溶性镉盐作为反应物,在制备过程中不添加其它的辅助物质,产生的副产物少,对环境污染较小,是一种环保型合成工艺。
4).本发明制备的产物具有良好的吸附性能和催化活性,能用在环境污染修复和新能源 (光解水产氢)等方面。
附图说明
以下结合实施例和附图对本发明的三维异质结构CdS-MoS2复合粉体的制备方法作出进一步的详述。
图1a-b是实施例1制备的CdS-MoS2复合粉体的场发射扫描电镜(FE-SEM)图(图a、b分别对应低、高倍率图像);图1c是实施例1制备的三维异质结构CdS-MoS2复合粉体的元素分析图(EDS);图1d是实施例1制备的三维异质结构CdS-MoS2复合粉体的XRD图。
图2a是实施例1制备的三维异质结构CdS-MoS2复合粉体的XPS图;图2b是实施例1制备的三维异质结构CdS-MoS2复合粉体的BET图;图2c是实施例1制备的三维异质结构CdS-MoS2复合粉体作为催化剂时,可见光下罗丹明B的降解图。
图3a-b是实施例2制备的CdS-MoS2复合粉体的场发射扫描电镜(FE-SEM)图(图a、b分别对应低、高倍率图像);图3c是实施例2制备的三维异质结构CdS-MoS2复合粉体的 XRD图;图3d是实施例2制备的三维异质结构CdS-MoS2复合粉体作为催化剂时,可见光下罗丹明B的降解图。
图4a-b是实施例3制备的CdS-MoS2复合粉体的场发射扫描电镜(FE-SEM)图(图a、b分别对应低、高倍率图像);图4c是实施例3制备的三维异质结构CdS-MoS2复合粉体作为催化剂时,可见光下罗丹明B的降解图。
具体实施方式
实施例1
CdS(20wt%)-MoS2复合粉体的制备
1)、MoS2粉体的制备
称取0.298g钼酸铵、0.609g硫脲和0.5g甘氨酸于烧杯中,加入15mL去离子水进行混合溶解,并放入超声清洗器中超声30min。将混合溶液倒入25mL聚四氟乙烯反应釜内衬中,另外再量取5mL去离子水冲洗烧杯,并将冲洗液倒入反应釜中。将反应釜放入烘箱中,加热到180℃,保温24h。将反应后的产物移出到离心试管内,用无水乙醇和去离子水交替清洗各3次。将洗涤后的产物放入烘箱,设置温度60℃,保温12h,干燥得到MoS2黑色粉末。
2)、CdS-MoS2复合粉体的制备
称取0.270g二硫化钼和0.111g乙酸镉于烧杯中,加入15mL去离子水进行混合溶解,并放入超声清洗器中超声30min。将混合溶液倒入25mL聚四氟乙烯反应釜内衬中,另外再量取5mL去离子水冲洗烧杯,并将冲洗液倒入反应釜中。将反应釜放入烘箱中,加热到160℃,保温12h。将反应后的产物移出到离心试管内,用无水乙醇和去离子水交替清洗各3次。将洗涤后的产物放入烘箱,设置温度60℃,保温12h,烘干得到干燥黑色粉末。
图1a-b是实施例1制备的CdS(20wt%)-MoS2复合粉体的场发射扫描电镜(FE-SEM)图 (图a、b分别对应低、高倍率图像),由图可知,基体MoS2表面为片层状,片层厚度均一,整体呈近球状,粒径大约为2μm。其上均匀附着的小颗粒即为纳米CdS,粒径约为0.3μm。载体CdS均匀分散生长在基体MoS2上,达到预期复合效果。对图1b进行局部EDS分析,如图1c所示可知该复合粉体中含有较多的S元素和Mo元素,以及有少量的Cd元素。图 1d是实施例1制备的三维异质结构CdS-MoS2复合粉体的XRD图谱,其中衍射角2θ在 25.034°、26.539°、28.031°、36.733°、43.830°、47.950°和51.93°出现衍射峰,其晶面为(100)、 (002)、(101)、(102)、(110)、(103)、(112),与CdS的标准卡片JCPDS(77-2306)相比较,三强峰均可对上,表明该复合粉体中含有CdS,并且为六方晶型。在2θ为29.323°时,出现一个较明显衍射峰,推测应属于MoS2。
另外,图2a为实施例1所得到复合粉体的XPS谱图。如图所示,可以得出其主要峰所对应的元素分别为Mo、S和Cd。图2b为实施例1所得到复合粉体的N2吸附/脱附等温曲线谱图。图中曲线为IV型等温线。依据BET方程计算样品的比表面积为5.496m2/g,孔体积为0.018cc/g,平均孔径为3.857nm。图2c为实施例1所得到复合粉体的可见光催化降解罗丹明B的效果图,由图可知在10min时,罗丹明B的吸收峰强度出现大幅度降低,到20min 时,吸收峰强度接近0,罗丹明B几乎完全被降解。
实施例2
CdS(10wt%)-MoS2复合粉体的制备
步骤同实施例1,制备CdS-MoS2复合粉体时所采用原料为0.240g二硫化钼、0.056g乙酸镉和0.016g硫脲。
图3a-b是实施例2制备的CdS(10wt%)-MoS2的场发射扫描电镜(FE-SEM)图(图a、b分别对应低、高倍率图像),由图可知基体MoS2部分表面为片层结构,部分表面较为致密,整体呈近球状,粒径约为1μm。关于MoS2表面出现致密化现象,可能是由于CdS直接取代了部分表层的MoS2,形成一种新型结构。图3c为实施例2制备的CdS(10wt%)-MoS2复合粉体的XRD图,在衍射角2θ分别为13.973°、32.549°和35.882°时出现较强衍射峰,其晶面为(002)、(100)、和(102),与MoS2的标准卡片JCPDS(75-1539)相比较,三强峰均可对上。而且可以得出MoS2的晶体结构为2H型。由于负载的CdS较少,所以其衍射峰不明显,在图谱中并未完全检测到。图3d为实施例2所得到复合粉体的可见光催化降解罗丹明 B的效果图。在20min、40min、60min和80min时的罗丹明B最强吸收峰强度均有不同程度的降低,到80min时,吸收峰几乎消失,催化较为彻底。
实施例3
CdS(30wt%)-MoS2复合粉体的制备
步骤同实施例1,制备CdS-MoS2复合粉体时所采用原料为0.210g二硫化钼、0.166g乙酸镉和0.100g硫脲。
图4a-b是实施例3制备的CdS(30wt%)-MoS2复合粉体的场发射扫描电镜(FE-SEM)图 (图a、b分别对应低、高倍率图像),由图可知基体MoS2呈近球状,表面为片层结构,且粒径大小不一,在1~2μm之间。载体CdS形貌亦存在不均匀生长,部分呈团簇状,部分呈棒状。关于图中出现的薄膜状物质,猜测为CdS。基体和载体分别独立生长,未能良好复合在一起。图4c为实施例3所得到复合粉体的可见光催化降解罗丹明B的效果图。由图可知随着时间的推移,罗丹明B的吸收峰强度出现小幅度降低。在80min时,罗丹明B仍存在较强吸收峰强度,降解不彻底。
实施例4
CdS-MoS2复合粉体的制备
1)、MoS2粉体的制备
称取0.298g钼酸铵、1.2g硫脲和1.7g L-天冬氨酸于烧杯中,加入15mL去离子水进行混合溶解,并放入超声清洗器中超声110min。将混合溶液倒入25mL聚四氟乙烯反应釜内衬中,另外再量取5mL去离子水冲洗烧杯,并将冲洗液倒入反应釜中。将反应釜放入烘箱中,加热到180℃,保温10h。将反应后的产物移出到离心试管内,用无水乙醇和去离子水交替清洗各3次。将洗涤后的产物放入烘箱,设置温度50℃,保温6h,干燥得到MoS2黑色粉末。
2)、CdS-MoS2复合粉体的制备
称取0.240g二硫化钼、0.056g乙酸镉和0.016g硫脲于烧杯中,加入15mL去离子水进行混合溶解,并放入超声清洗器中超声90min。将混合溶液倒入25mL聚四氟乙烯反应釜内衬中,另外再量取5mL去离子水冲洗烧杯,并将冲洗液倒入反应釜中。将反应釜放入烘箱中,加热到160℃,保温12h。将反应后的产物移出到离心试管内,用无水乙醇和去离子水交替清洗各3次。将洗涤后的产物放入烘箱,设置温度60℃,保温18h,烘干得到干燥黑色粉末。
实施例5
CdS-MoS2复合粉体的制备
1)、MoS2粉体的制备
称取0.298g钼酸铵、0.45g硫脲和0.95g甘氨酸于烧杯中,加入15mL去离子水进行混合溶解,并放入超声清洗器中超声40min。将混合溶液倒入25mL聚四氟乙烯反应釜内衬中,另外再量取5mL去离子水冲洗烧杯,并将冲洗液倒入反应釜中。将反应釜放入烘箱中,加热到160℃,保温36h。将反应后的产物移出到离心试管内,用无水乙醇和去离子水交替清洗各3次。将洗涤后的产物放入烘箱,设置温度40℃,保温10h,干燥得到MoS2黑色粉末。
2)、CdS-MoS2复合粉体的制备
称取0.240g二硫化钼、0.056g乙酸镉和0.016g硫脲于烧杯中,加入15mL去离子水进行混合溶解,并放入超声清洗器中超声80min。将混合溶液倒入25mL聚四氟乙烯反应釜内衬中,另外再量取5mL去离子水冲洗烧杯,并将冲洗液倒入反应釜中。将反应釜放入烘箱中,加热到140℃,保温36h。将反应后的产物移出到离心试管内,用无水乙醇和去离子水交替清洗各3次。将洗涤后的产物放入烘箱,设置温度50℃,保温12h,烘干得到干燥黑色粉末。
实施例6
CdS-MoS2复合粉体的制备
1)、MoS2粉体的制备
称取0.298g钼酸铵、1.85g硫脲和0.2g L-天冬氨酸于烧杯中,加入15mL去离子水进行混合溶解,并放入超声清洗器中超声60min。将混合溶液倒入25mL聚四氟乙烯反应釜内衬中,另外再量取5mL去离子水冲洗烧杯,并将冲洗液倒入反应釜中。将反应釜放入烘箱中,加热到170℃,保温20h。将反应后的产物移出到离心试管内,用无水乙醇和去离子水交替清洗各3次。将洗涤后的产物放入烘箱,设置温度60℃,保温8h,干燥得到MoS2黑色粉末。
2)、CdS-MoS2复合粉体的制备
称取0.270g二硫化钼和0.111g乙酸镉于烧杯中,加入15mL去离子水进行混合溶解,并放入超声清洗器中超声50min。将混合溶液倒入25mL聚四氟乙烯反应釜内衬中,另外再量取5mL去离子水冲洗烧杯,并将冲洗液倒入反应釜中。将反应釜放入烘箱中,加热到150℃,保温8h。将反应后的产物移出到离心试管内,用无水乙醇和去离子水交替清洗各3次。将洗涤后的产物放入烘箱,设置温度40℃,保温15h,烘干得到干燥黑色粉末。
以上内容仅仅是对本发明的构思所作的举例和说明,所属本技术领域的技术人员对所描述的具体实施例做各种各样的修改或补充或采用类似的方式替代,只要不偏离发明的构思或者超越本权利要求书所定义的范围,均应属于本发明的保护范围。
Claims (1)
1.一种三维异质结构CdS-MoS2复合粉体的制备方法,其特征在于,步骤如下:
1)、MoS2粉体的制备
称取0.298 g钼酸铵、0.609 g硫脲和0.5 g甘氨酸于烧杯中,加入15 mL去离子水进行混合溶解,并放入超声清洗器中超声30min;将混合溶液倒入25 mL聚四氟乙烯反应釜内衬中,另外再量取5 mL去离子水冲洗烧杯,并将冲洗液倒入反应釜中;将反应釜放入烘箱中,加热到180℃,保温24 h;将反应后的产物移出到离心试管内,用无水乙醇和去离子水交替清洗各3次;将洗涤后的产物放入烘箱,设置温度60℃,保温12 h,干燥得到MoS2黑色粉末;
2)、CdS-MoS2复合粉体的制备
称取0.270 g二硫化钼和0.111 g乙酸镉于烧杯中,加入15 mL去离子水进行混合溶解,并放入超声清洗器中超声30min;将混合溶液倒入25 mL聚四氟乙烯反应釜内衬中,另外再量取5 mL去离子水冲洗烧杯,并将冲洗液倒入反应釜中;将反应釜放入烘箱中,加热到160℃,保温12 h;将反应后的产物移出到离心试管内,用无水乙醇和去离子水交替清洗各3次;将洗涤后的产物放入烘箱,设置温度60℃,保温12 h,烘干得到干燥黑色粉末。
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