CN109160494B - 一种毛球状CdSe纳米材料的制备方法 - Google Patents
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Abstract
本发明涉及一种毛球状CdSe纳米材料的制备方法，包括：将含有镉源和硒源的混合溶液置于高压反应釜中在120℃下反应，冷却，分离所得沉淀，洗涤，干燥，得到毛球状CdSe纳米材料。本发明选用Na2SeSO3作为硒源是合成毛球状CdSe的关键，同时研究了合成过程的最优条件，合成的CdSe纳米材料具备优良的光催化性能，能作为光催化剂，作用于污水处理，分解有色染料等，具有良好的应用前景。
Description
技术领域
本发明属于纳米材料领域，特别涉及一种毛球状CdSe纳米材料的制备方法。
背景技术
光催化过程就是光生电子-空穴对的产生、输运以及利用。主要是把半导体作为催化剂，进而吸收并利用太阳能。光催化技术是一个比较复杂的过程，涉及了化学、物理和材料等多个学科。带隙能，又称为禁带宽度Eg，位于价带与导带之间，数值等于价带和导带的能级差，是由于半导体化合物电子的费米能级的不连续性，使其电子轨道中具有空的能量区域。光生电子-空穴对的产生是由于在太阳光的照射下，半导体化合物价带上的电子吸收光量子跃迁到导带，在导带上形成光生电子，与之相对应，价带上产生空穴。光生电子-空穴对有两种去向，一是光生电子与空穴复合，即电子从导带跃迁回价带，能量由热能或其他形式消散；但当催化剂表面存在缺陷或者捕获剂时，光生电子和空穴就有可能被捕获，抑制了光生电子-空穴对的复合，从而使其在半导体表面发生氧化还原反应。价带空穴本身具有一定的氧化性，可以直接氧化有机物，也可以与溶液中的氢氧根离子反应产生羟基自由基具有很强的氧化性，可以将半导体表面吸附的有机物氧化，从而达到降解污染物的效果；导带中的电子具有还原性，一般与溶液中的吸附氧反应生成超氧自由基等活性基团。以二氧化钛为半导体导带与价带的位置以及半导体表面吸附物质的氧化还原电位的大小决定了光生电子-空穴对的迁移速率和复合率。如果价带的位置低于吸附物质的氧化电势，那么吸附物质就有可能被氧化。
CdSe，一种直接带隙的Ⅱ-Ⅵ族化合物半导体。因为硒及其硒化物作为主要的半导体材料,具有非常好的光电特性。到目前为止，Ⅱ～Ⅵ族的元素及其化合物是人们研究的主要的半导体材料，由于其合成相对其他材料更为简单、材料毒性较小、荧光特性更为良好等优点，同时，硒作为生命活动的必备元素之一，因此Ⅱ-Ⅵ族元素及其化合物被大量运用于生命科学、生物医药及荧光器件等各个领域。而具有独特性质的纳米硒及硒化物在材料学和生物学上具有更重要的意义。硒化镉主要采用水热法对于进行合成制备,并通过改变反应条件研究不同反应体系对最终产物形貌的影响，从而得到了多种不同形态的硒化镉,可以作为光催化剂应用于污水治理、分解有色染料等方面。
发明内容
本发明所要解决的技术问题是提供一种毛球状CdSe纳米材料的制备方法，该方法选用Na2SeSO3作为硒源是合成毛球状CdSe的关键，同时研究了合成过程的最优条件，合成的CdSe纳米材料具备优良的光催化性能，能作为光催化剂，作用于污水处理，分解有色染料等，具有良好的应用前景。
本发明提供了一种毛球状CdSe纳米材料的制备方法，包括：
将含有镉源和硒源的混合溶液置于高压反应釜中在120℃下反应，冷却，分离所得沉淀，洗涤，干燥，得到毛球状CdSe纳米材料；其中，所述硒源为Na2SeSO3，镉源和硒源的质量比为1:0.1-0.3。优选的，镉源和硒源的质量比为1:0.19。
所述镉源为Cd(NO3)2·4H2O。
所述含有镉源和硒源的混合溶液的制备方法包括：称量Cd(NO3)2·4H2O，用去离子水溶解，加入相同物质的量的乙二胺四乙酸二钠，滴加氨水调节溶液pH值至9-11；然后加入硒代硫酸钠溶液，再加入十六烷基三甲基溴化铵，搅拌，得到含有镉源与硒源的混合溶液。
优选的，所述硒代硫酸钠溶液的制备方法包括：称量亚硫酸钠，用去离子水溶解，加热至溶液沸腾后加入硒粉，常温搅拌8-10小时，得到硒代硫酸钠溶液；其中，亚硫酸钠与硒粉的质量比为1:0.1-0.3。更有选的，亚硫酸钠与硒粉的质量比为1:0.3。
优选的，所述十六烷基三甲基溴化铵与硒代硫酸钠的质量比为1:1-3。更有选的，所述十六烷基三甲基溴化铵与硒代硫酸钠的质量比为1:1.57。
所述反应时间为12h。
所述毛球状CdSe纳米材料用于污水处理、分解有色染料。
本发明中首次证明，当温度高于120℃反应产物的形状不规则，很少存在球形产物，产物尺寸比较大，生成产物表面比较粗糙，且具有明显的团聚现象。当温度为120℃生成物的形貌相对规则了许多，球形产物更加多，产物的平均直径大小在2μm左右，产物表面不是十分光滑，团聚现象也比较明显，产品的结构为毛球状。
有益效果
本发明选用Na2SeSO3作为硒源是合成毛球状CdSe的关键，同时研究了合成过程的最优条件，合成的CdSe纳米材料具备优良的光催化性能，能作为光催化剂，作用于污水处理，分解有色染料等，具有良好的应用前景。
附图说明
图1为实施例1得到的CdSe纳米材料的SEM图片。
图2为CdSe纳米材料的光致发光光谱。
图3为CdSe作为催化剂，Rh B随降解时间的吸收光谱。
图4为对比例1得到的CdSe纳米材料的SEM图片。
图5为对比例2得到的CdSe纳米材料的SEM图片。
具体实施方式
下面结合具体实施例，进一步阐述本发明。应理解，这些实施例仅用于说明本发明而不用于限制本发明的范围。此外应理解，在阅读了本发明讲授的内容之后，本领域技术人员可以对本发明作各种改动或修改，这些等价形式同样落于本申请所附权利要求书所限定的范围。
实施例1
(1)制备Na2SeSO3水溶液：用电子天平准确称量6.3g的亚硫酸钠，倒入烧杯中用去离子水溶解，使用酒精灯加热至100℃，并不断搅拌，在溶液沸腾后加入1.925g的硒粉，利用恒温磁力搅拌器常温搅拌8小时，等硒粉完全反应，得到硒代硫酸钠溶液。
(2)使用电子天平称量1.542g Cd(NO3)2·4H2O，将去离子水加入烧杯中，用玻璃棒搅拌至完全溶解，加入相同物质的量的乙二胺四乙酸二钠，溶液将出现浑浊，通过滴加氨水来使浑浊变澄清并且调节溶液的酸碱度，呈现偏碱性(pH值在9-11之间)。向其中加入10mL硒代硫酸钠溶液。利用磁力搅拌机搅拌半个小时至均匀，得到含有镉源与硒源的混合溶液。
(3)将含有镉源和硒源的混合溶液倒入高压反应釜，之后将其转入电热恒温鼓风干燥箱中，反应温度为120℃，反应时间为12个小时。当反应结束后，冷却至常温，从反应釜取出反应溶液，使用电动离心机进行离心操作，用去离子水和无水乙醇交替清洗所合成的样品，最后将其放入干燥箱干燥5-6小时，得到毛球状的CdSe纳米材料，如图1所示。
图2是CdSe纳米材料的光致发光光谱(简称PL谱)。图3为在可见光照射下10mg/LRh B水溶液的光催化降解的紫外-可见光谱，该光催化剂是毛球状的CdSe纳米材料。光催化结果表明，Rh B的特征吸收带在554nm附近，峰值在240min内迅速下降，说明本发明毛球状的CdSe纳米材料具有优越的光催化性能。
对比例1
将实施例1中的含有镉源和硒源的混合溶液倒入高压反应釜，之后将其转入电热恒温鼓风干燥箱中，反应温度为180℃，反应时间为12个小时。当反应结束后，冷却至常温，从反应釜取出反应溶液，使用电动离心机进行离心操作，用去离子水和无水乙醇交替清洗所合成的样品，最后将其放入干燥箱干燥5-6小时，得到CdSe纳米材料。
所得的CdSe纳米材料的SEM图片如图4所示。由图4可知，反应温度过高，反应产物的形状不规则，很少存在球形产物，表面粗糙，且具有明显团聚现象。
对比例2
类似于实验例1，区别在于，反应过程中添加CTAB。所得的CdSe纳米颗粒的SEM图片如图5所示，结果表明反应过程中添加CTAB反应生成的产物的形状相对更加规则，呈现较为均匀规则的球形，生成产物表面相对会光滑许多。
Claims (4)
1.一种毛球状CdSe纳米材料的应用，其特征在于：所述毛球状CdSe纳米材料用于污水处理、分解有色染料；所述毛球状CdSe纳米材料制备方法包括：
将含有镉源和硒源的混合溶液置于高压反应釜中在120℃下反应，冷却，分离所得沉淀，洗涤，干燥，得到毛球状CdSe纳米材料；其中，所述硒源为Na2SeSO3，镉源和硒源的质量比为1:0.1-0.3；所述含有镉源和硒源的混合溶液的制备方法包括：称量Cd(NO3)2·4H2O，用去离子水溶解，加入相同物质的量的乙二胺四乙酸二钠，滴加氨水调节溶液pH值至9-11；然后加入硒代硫酸钠溶液，再加入十六烷基三甲基溴化铵，搅拌，得到含有镉源与硒源的混合溶液。
2.根据权利要求1所述的应用，其特征在于：所述硒代硫酸钠溶液的制备方法包括：称量亚硫酸钠，用去离子水溶解，加热至溶液沸腾后加入硒粉，常温搅拌8-10小时，得到硒代硫酸钠溶液；其中，亚硫酸钠与硒粉的质量比为1:0.1-0.3。
3.根据权利要求1所述的应用，其特征在于：所述十六烷基三甲基溴化铵与硒代硫酸钠的质量比为1:1-3。
4.根据权利要求1所述的应用，其特征在于：所述反应时间为12h。
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