CN115007174A - 一种二维CdIn2S4纳米片及其制备方法、用途 - Google Patents
一种二维CdIn2S4纳米片及其制备方法、用途 Download PDFInfo
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Abstract
本发明公开了一种具有可见光催化活性的二维超薄CdIn2S4纳米片的制备方法,解决当前光催化领域中光催化材料光吸收性能差,电荷分离效率低,载流子复合率高,光催化性能不高的问题,二维超薄CdIn2S4纳米片独特的结构和优良的光催化活性,具有更多暴露的活性面,更高的导带和通过飞秒时间分辨瞬态吸收测量获得更长的平均电子衰变寿命。
Description
技术领域
本本发明涉及光催化剂技术领域,特别是一种二维超薄CdIn2S4纳米片的制备方法及应用。
背景技术
工业化革命以来,世界经济和人口得到了快速的增长。但随之而来的资源短缺、空气污染和温室效应等问题严重制约了人类的生存与发展。因此,大力探索绿色清洁的可再生能源来代替化石能源,成为了人类目前的首要问题。其中太阳能作为一种储量丰富的可再生清洁能源,是建立文明社会实现可持续发展的必有之路。而光催化技术就是利用太阳能将水转化为氢能的技术。氢能具有高燃烧热值,清洁、无污染等优点,是一种极具发展潜力的清洁能源。传统的半导体光催化剂,如:TiO2、WO3等,只能利用紫外光,无法吸收可见光严重制约了其发展。金属硫化物普遍具有较窄的带隙宽度,可以很好的吸收可见光。CdS是当前研究最多的S化物材料之一,不过CdS稳定性较差,容易发生光腐蚀。
三元金属硫化物CdIn2S4作为AB2X4族半导体中的成员,具有较高的化学稳定性、合适的带隙以及较好的可见光响应能力。单纯的CdIn2S4光催化性能仍比较弱,大多数改性CdIn2S4的方法是通过负载其他光催化剂,提高光的吸收和光生电荷的分离效率。其改性方法复杂,没有从CdIn2S4自身结构出发,光催化性能提高有限。
发明内容
本发明的目的是要提供一种具有可见光催化活性的二维超薄CdIn2S4纳米片的制备方法,解决当前光催化领域中光催化材料光吸收性能差,电荷分离效率低,载流子复合率高,光催化性能不高的问题,二维超薄CdIn2S4纳米片独特的结构和优良的光催化活性,具有更多暴露的活性面,更高的导带和通过飞秒时间分辨瞬态吸收测量获得更长的平均电子衰变寿命。
一种二维CdIn2S4纳米片的制备方法,包括:
步骤(1),将铟源、镉源和表面活性剂量溶解于极性溶液中,取一定量去离子水/乙二醇混合溶液,放入到清洗干净的烧杯中,加入表面活性剂,搅拌时间为20-40分钟;
步骤(2),向步骤(1)中加入硫源继续搅拌20-40分钟,得到混合溶液;
步骤(3),将混合溶液倒入聚四氟乙烯反应釜中,于100-200℃下反应8-48h,得到二维超薄CdIn2S4纳米片。
进一步,步骤(1)中所述镉源为硝酸镉、醋酸锌、氯化镉、硫酸镉中任意一种。
进一步,步骤(1)中所述铟盐为三氯化铟、四水合三氯化铟、硝酸铟、中任意一种;
进一步,步骤(2)中所述硫源为硫化钠、硫代乙酰胺、L-半胱氨酸、硫脲中任意一种。
进一步,所述镉源、铟源、硫源的摩尔比为:1:2:4~8。
进一步,所述表面活性剂柠檬酸钠和所述硫源的摩尔比为:1:0.3~1.5。根据权利要求6所述的一种二维CdIn2S4纳米片的制备方法,其特征在于,所述表面活性剂为十二烷基苯磺酸钠(SDBS)、柠檬酸钠中(SC)、十六烷基三甲基溴化铵(CTAB)和硬脂酸钠(SS)的一种。
一种二维CdIn2S4纳米片,其特征在于,如权利要求1-7任意一项所述方法制备得到。
一种二维CdIn2S4纳米片用于可见光催化剂。
一种二维CdIn2S4纳米片用于可见光催化分解水制氢。
本发明的有益效果:
1.通过控制表面活性剂的加入量,制备出了一种二维超薄CdIn2S4纳米片,纳米片的厚度约为2.6~5nm,尺寸约为100nm。
2.由于二维超薄CdIn2S4纳米片制备工艺简单,化学性质稳定,循环产氢后,仍能维持均匀的形貌和优良的光催化制氢能力,因此具备可回收性,可以循环利用。
3.由于其独特的二维超薄形态,电荷可以迅速传输到催化剂表面进行分解水反应,不易发生复合,有效分离了电子-空穴对。
4.本发明复合光催化剂具有较为合适的带隙,因此可见光响应范围相对较宽,适用于太阳能转化利用和光催化产氢领域。
附图说明
图1为本发明实施例3中二维超薄CdIn2S4纳米片的XRD图谱。
图2为本发明实施例3中三维CdIn2S4纳米花的SEM图谱。
图3为本发明实施例3中二维超薄CdIn2S4纳米片的SEM图谱。
图4为本发明实施例3中三维CdIn2S4纳米花的TEM图谱。
图5为本发明实施例3中二维CdIn2S4纳米花的TEM图谱。
图6为本发明实例1和实施例3中二维超薄CdIn2S4纳米片的PL图谱对比。
图7为本发明实例1和实施例3中二维超薄CdIn2S4纳米片的产氢性能图。
图8为本发明实例1和实施例3中二维超薄CdIn2S4纳米片的孔隙率测试曲线。
图9为本发明实例1和实施例3中二维超薄CdIn2S4纳米片的电流时间曲线。
具体实施方式
下面将对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
一种二维CdIn2S4纳米片的制备方法,包括:
步骤(1),将铟源、镉源和表面活性剂量溶解于极性溶液中,取一定量去离子水/乙二醇混合溶液,放入到清洗干净的烧杯中,加入表面活性剂,搅拌时间为20-40分钟;
步骤(2),向步骤(1)中加入硫源继续搅拌20-40分钟,得到混合溶液;
步骤(3),将混合溶液倒入聚四氟乙烯反应釜中,于100-200℃下反应8-48h,得到二维超薄CdIn2S4纳米片。由于二维超薄CdIn2S4纳米片制备工艺简单,化学性质稳定,循环产氢后,仍能维持均匀的形貌和优良的光催化制氢能力,具备可回收性,可以循环利用。由于其独特的二维超薄形态,电荷可以迅速传输到催化剂表面进行分解水反应,不易发生复合,有效分离了电子-空穴对。
在具体实施例中,镉源为硝酸镉、醋酸锌、氯化镉、硫酸镉中任意一种。
在具体实施例中,铟盐为三氯化铟、四水合三氯化铟、硝酸铟、中任意一种;
在具体实施例中,硫源为硫化钠、硫代乙酰胺、L-半胱氨酸、硫脲中任意一种。
在具体实施例中,镉源、铟源、硫源的摩尔比为:1:2:4~8。
在具体实施例中,表面活性剂和所述硫源的摩尔比为:1:0.3~1.5。通过控制表面活性剂的加入量,制备出了一种二维超薄CdIn2S4纳米片,纳米片的厚度约为2.6~5nm,尺寸约为100nm。
在具体实施例中,表面活性剂为十二烷基苯磺酸钠(SDBS)、柠檬酸钠(SC)中的一种。
实施例1:
量取50ml去离子水和10ml乙二醇,放入到清洗干净的烧杯中,加入2mmol InCl3·4H2O和1mmol CdCl2,搅拌时间为30min。随后加入硫代乙酰胺(TAA)继续搅拌30分钟,得到混合溶液;将混合溶液倒入聚四氟乙烯反应釜中,于120℃下反应12h,得到花球形CdIn2S4。
实施例2:
量取50ml去离子水和10ml乙二醇,放入到清洗干净的烧杯中,加入2mmol InCl3、1mmol CdCl2和200mg柠檬酸钠(SC),搅拌时间为30min。随后加入硫脲继续搅拌30分钟,得到混合溶液;将混合溶液倒入聚四氟乙烯反应釜中,于150℃下反应12h,得到二维超薄CdIn2S4纳米片。
实施例3:
量取50ml去离子水和10ml乙二醇,放入到清洗干净的烧杯中,加入2mmol InCl3·4H2O、1mmol CdCl2和300mg柠檬酸钠(SC),搅拌时间为30min。随后加入硫代乙酰胺(TAA)继续搅拌30分钟,得到混合溶液;将混合溶液倒入聚四氟乙烯反应釜中,于120℃下反应12h,得到二维超薄CdIn2S4纳米片。
实施例4:量取30ml去离子水和30ml乙二醇,放入到清洗干净的烧杯中,加入2mmolInCl3、1mmol CdCl2和800mg十二烷基苯磺酸钠(SDBS),搅拌时间为30min。随后加入硫代乙酰胺(TAA)继续搅拌30分钟,得到混合溶液;将混合溶液倒入聚四氟乙烯反应釜中,于150℃下反应12h,得到二维超薄CdIn2S4纳米片。。
本实施例通过一步水热法的方式,得到了一种二维CdIn2S4纳米片,用于可见光催化剂。
量取超纯水置于光反应容器中,然后加入实施例3中制得的CdIn2S4纳米片,搅拌混合均匀,然后采用硅橡胶将反应容器密封,进行可见光照射,其中,所述超纯水和CdIn2S4纳米片的用量比为100mL:0.05g。图7为本发明实施例3中二维超薄CdIn2S4纳米片的产氢性能图,结果表明,在无助催化剂的情况下,进行可见光照射时,超薄CdIn2S4膜的产氢活性从0.21mmol g-1h-1增加到2.58mmol g-1h-1,达到10.1%,是纯CdIn2S4的12.3倍。
以上所述的实施例仅是对本发明的优选方式之一进行描述,并非对本发明的范围进行限定,在不脱离本发明设计精神的前提下,本领域普通技术人员对本发明的技术方案做出的各种变形和改进,均应落入本发明权利要求书确定的保护范围内。
Claims (10)
1.一种二维CdIn2S4纳米片的制备方法,其特征在于,所述方法包括:
步骤(1),将铟源、镉源和表面活性剂量溶解于极性溶液中,取一定量去离子水/乙二醇混合溶液,放入到清洗干净的烧杯中,加入表面活性剂,搅拌时间为20-40分钟;
步骤(2),向步骤(1)中加入硫源继续搅拌20-40分钟,得到混合溶液;
步骤(3),将混合溶液倒入聚四氟乙烯反应釜中,于100-200℃下反应8-48h,用水和乙醇反复清洗数次后,于烘箱中40-80℃干燥0.5-6h,得到二维超薄CdIn2S4纳米片。
2.根据权利要求1所述的一种二维CdIn2S4纳米片的制备方法,其特征在于,步骤(1)中所述镉源为硝酸镉、醋酸锌、氯化镉、硫酸镉中任意一种。
3.根据权利要求1所述的一种二维CdIn2S4纳米片的制备方法,其特征在于,步骤(1)中所述铟盐为三氯化铟、四水合三氯化铟、硝酸铟、中任意一种。
4.根据权利要求1所述的一种二维CdIn2S4纳米片的制备方法,其特征在于,步骤(2)中所述硫源为硫化钠、硫代乙酰胺、L-半胱氨酸、硫脲中任意一种。
5.根据权利要求1所述的一种二维CdIn2S4纳米片的制备方法,其特征在于,所述镉源、铟源、硫源的摩尔比为:1:2:4~8。
6.根据权利要求1所述的一种二维CdIn2S4纳米片的制备方法,其特征在于,所述表面活性剂柠檬酸钠(SC)和所述硫源的摩尔比为:1:0.3~1.5。
7.根据权利要求6所述的一种二维CdIn2S4纳米片的制备方法,其特征在于,所述表面活性剂为十二烷基苯磺酸钠(SDBS)、柠檬酸钠中(SC)、十六烷基三甲基溴化铵(CTAB)和硬脂酸钠(SS)的一种。
8.一种二维CdIn2S4纳米片,其特征在于,如权利要求1-7任意一项所述方法制备得到。
9.一种如权利要求8所述的二维CdIn2S4纳米片用于可见光催化剂。
10.一种如权利要求8所述的二维CdIn2S4纳米片用于可见光催化分解水制氢。
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