CN115490260A - 富含S空位的CuInS2超薄纳米片的制备方法及应用 - Google Patents
富含S空位的CuInS2超薄纳米片的制备方法及应用 Download PDFInfo
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Abstract
本发明公开了一种富含S空位的CuInS2超薄纳米片的制备方法,将Cu(NO3)2·3H2O溶解在乙醇溶液中,搅拌,记为溶液A;将In(NO3)3·xH2O溶解在溶液A中,搅拌,记为溶液B;将硫脲溶解在溶液B中,记为溶液C;将溶液C搅拌超声后,放入聚四氟乙烯内衬的高压反应釜中反应,将反应后的产物洗涤,在烘箱中干燥,得到富含S空位的CuInS2超薄纳米片。制备的材料可作为光催化产氢、CO2还原等材料,而且的富含S空位的CuInS2超薄纳米片制备过程简单高效、成本低廉、重复性高、活性位点多、比表面积大。
Description
技术领域
本发明属于纳米材料技术领域,涉及一种富含S空位的CuInS2超薄纳米片的制备方法。
背景技术
化石燃料燃烧导致的二氧化碳排放迅速增加,给我们的社会带来了全球变暖的问题;将二氧化碳转化为增值燃料,同时使用半导体介导的阳光驱动的光催化策略减少温室气体二氧化碳的数量,被认为是帮助解决这些问题的理想方法;CuInS2作为一种ABX2族半导体,近年来成为人们关注的热点由于其诱人的优势,作为一种可见光响应型光催化剂,在能源-环境相关领域引起了广泛的跨学科兴趣。具体而言,其约2.06eV的禁带宽度,使其在可见光区具有较强的响应此外,与众所周知的硫化镉(CdS)相比,它表现出较高的物理化学稳定性,因而在光催化反应中具有相当的耐久性。与传统的金属硫化物(CdS、NiS、Sb2S3)相比,其毒性较小,在环境修复领域具有更大的应用潜力;另外,由于其原料广泛,化学成分简单,生产相对容易。然而,其光催化效率仍不理想,主要是由于载流子分离和迁移动力学迟缓。鉴于此,在过去的几年里,鼓励实验以提高其光催化性能,为高效CuInS2基光催化剂的合理设计和合成提供指导;探索一种简单高效、成本低廉、重复性高、活性位点多、比表面积大的纳米CuInS2具有重要意义。
发明内容
本发明的目的是提供一种富含S空位的CuInS2超薄纳米片的制备方法,解决了现有光催化材料光催化中存在的效率低的问题。
本发明所采用的技术方案是,一种富含S空位的CuInS2超薄纳米片的制备方法,具体按以下步骤实施:
步骤1,将Cu(NO3)2·3H2O溶解在乙醇溶液中,搅拌,记为溶液A;
步骤2;将In(NO3)3·xH2O溶解在溶液A中,搅拌,记为溶液B;
步骤3,将硫脲溶解在溶液B中,记为溶液C;
步骤4,将溶液C搅拌超声后,放入聚四氟乙烯内衬的高压反应釜中反应,将反应后的产物洗涤,在烘箱中干燥,得到富含S空位的CuInS2超薄纳米片。
本发明的特点还在于:
其中Cu(NO3)2·3H2O、In(NO3)3·xH2O和硫脲的质量比为1:1:8;
其中步骤1中,Cu(NO3)2·3H2O与乙醇的比例是5mmol:30ml,乙醇的浓度为≥99.7%,搅拌时间为10~15min;
其中步骤2中搅拌时间为55-65min;
其中步骤4中搅拌时间为10~15min,超声时间为10~15min;
其中步骤4中将溶液C搅拌超声后,放入聚四氟乙烯内衬的高压反应釜中在150~170℃保持10~14h,自然冷却至室温;
其中步骤4中洗涤过程为用无水乙醇和去离子水交替洗涤,最后在65℃的真空烘箱中干燥24h。
一种富含S空位的CuInS2超薄纳米片的制备方法制备的富含S空位的CuInS2超薄纳米片在光催化产气中的应用
本发明的有益效果是
本发明的一种富含S空位的CuInS2超薄纳米片的制备方法采用简单的水热法合成了富含S空位的CuInS2超薄纳米片,其制备过程简单高效、成本低廉、重复性高、活性位点多、比表面积大,同时提高了光催化剂的活性;
所采用的富含S空位的CuInS2超薄纳米片制备方法,产量大,对环境友好,适合批量生产;
本发明采用简单的水热法合成的富含S空位的CuInS2超薄纳米片性能稳定,对光催化CO2还原、产氢、Cr6+还原等效果明显。
附图说明
图1是本发明的一种富含S空位的CuInS2超薄纳米片的制备方法制备的富含S空位的CuInS2超薄纳米片材料X射线衍射能谱图;
图2是本发明的一种富含S空位的CuInS2超薄纳米片的制备方法制备的富含S空位的CuInS2超薄纳米片材料扫描电子图。
具体实施方式
下面结合附图和具体实施方式对本发明进行详细说明。
本发明提供了一种富含S空位的CuInS2超薄纳米片的制备方法,具体的将0.1208gCu(NO3)2·3H2O溶解在30ml乙醇溶液中,搅拌10~15min,记为溶液A;将0.1504gIn(NO3)3·xH2O溶解在溶液A中,用手慢慢晃动烧杯使In(NO3)3·xH2O完全溶解直到没有固体小颗粒,然后搅拌55~65min,记为溶液B;再将0.3045g硫脲溶解在溶液B中,记为溶液C,搅拌10~15min,再超声10~15min后,然后将溶液C放入聚四氟乙烯内衬的高压反应釜中,在150~170℃保持10~14h,自然冷却至室温;将反应后的产物用无水乙醇和去离子水交替洗涤,在65℃的真空烘箱中干燥24h,得到富含S空位的CuInS2超薄纳米片,如图1和图2所示;前驱体物质的量之比为:Cu(NO3)2·3H2O:In(NO3)3·xH2O:硫脲=1:1:8;
实施例1
分别将0.1208g Cu(NO3)2·3H2O溶解在30ml乙醇溶液中,搅拌10min,记为溶液A;将0.1504g In(NO3)3·xH2O溶解在溶液A中,用手慢慢晃动烧杯使In(NO3)3·xH2O完全溶解直到没有固体小颗粒,然后搅拌65min,记为溶液B;再将0.3045g硫脲溶解在溶液B中,记为溶液C;搅拌15min,再超声15min后,然后将溶液C放入聚四氟乙烯内衬的高压反应釜中,在170℃保持14h,自然冷却至室温;将反应后的产物用无水乙醇和去离子水交替洗涤,在65℃的真空烘箱中干燥24h,得到富含S空位的CuInS2超薄纳米片;
然后称取30mg所制备的富含S空位的CuInS2超薄纳米片,放入体积为500ml含有100ml去离子水的密闭夹套反应器中,以CO2为反应器填充气,暗反应1h,光照三小时,每间隔一小时取一次样;CH4产率为0.81μmol·g-1·h-1、CO产率为2.31μmol·g-1·h-1;
实施例2
分别将0.1208g Cu(NO3)2·3H2O溶解在30ml乙醇溶液中,搅拌15min,记为溶液A;将0.1504g In(NO3)3·xH2O溶解在溶液A中,用手慢慢晃动烧杯使In(NO3)3·xH2O完全溶解直到没有固体小颗粒,然后搅拌55min,记为溶液B;再将0.3045g硫脲溶解在溶液B中,记为溶液C。搅拌10min,再超声10min后,然后将溶液C放入聚四氟乙烯内衬的高压反应釜中,在150℃保持10h,自然冷却至室温。将反应后的产物用无水乙醇和去离子水交替洗涤,在65℃的真空烘箱中干燥24h,得到富含S空位的CuInS2超薄纳米片;
称取10mg所制备的富含S空位的CuInS2超薄纳米片,放入体积为500ml含有100ml去离子水的密闭夹套反应器中,以CO2为反应器填充气,暗反应1h,光照三小时,每间隔一小时取一次样。H2产率为9.47μmol·g-1·h-1。
实施例3
分别将0.1208g Cu(NO3)2·3H2O溶解在30ml乙醇溶液中,搅拌15min,记为溶液A;将0.1504g In(NO3)3·xH2O溶解在溶液A中,用手慢慢晃动烧杯使In(NO3)3·xH2O完全溶解直到没有固体小颗粒,然后搅拌55min,记为溶液B;再将0.3045g硫脲溶解在溶液B中,记为溶液C。搅拌10min,再超声10min后,然后将溶液C放入聚四氟乙烯内衬的高压反应釜中,在160℃保持12h,自然冷却至室温。将反应后的产物用无水乙醇和去离子水交替洗涤,在65℃的真空烘箱中干燥24h,得到富含S空位的CuInS2超薄纳米片;
称取10mg所制备的富含S空位的CuInS2超薄纳米片,放入体积为500ml含有100ml去离子水的密闭夹套反应器中,以CO2为反应器填充气,暗反应1h,光照三小时,每间隔一小时取一次样。H2产率为35.31μmol·g-1·h-1,产率提高3.73倍。
Claims (8)
1.一种富含S空位的CuInS2超薄纳米片的制备方法,其特征在于,具体按以下步骤实施:
步骤1,将Cu(NO3)2·3H2O溶解在乙醇溶液中,搅拌,记为溶液A;
步骤2;将In(NO3)3·xH2O溶解在溶液A中,搅拌,记为溶液B;
步骤3,将硫脲溶解在溶液B中,记为溶液C;
步骤4,将溶液C搅拌超声后,放入聚四氟乙烯内衬的高压反应釜中反应,将反应后的产物洗涤,在烘箱中干燥,得到富含S空位的CuInS2超薄纳米片。
2.根据权利要求1所述的一种富含S空位的CuInS2超薄纳米片的制备方法,其特征在于,所述Cu(NO3)2·3H2O、In(NO3)3·xH2O和硫脲的质量比为1:1:8。
3.根据权利要求1所述的一种富含S空位的CuInS2超薄纳米片的制备方法,其特征在于,所述步骤1中,乙醇的浓度≥99.7%,搅拌时间为10~15min。
4.根据权利要求1所述的一种富含S空位的CuInS2超薄纳米片的制备方法,其特征在于,所述步骤2中搅拌时间为55-65min。
5.根据权利要求1所述的一种富含S空位的CuInS2超薄纳米片的制备方法,其特征在于,所述步骤4中搅拌时间为10~15min,超声时间为10~15min。
6.根据权利要求1所述的一种富含S空位的CuInS2超薄纳米片的制备方法,其特征在于,所述步骤4中将溶液C搅拌超声后,放入聚四氟乙烯内衬的高压反应釜中在150~170℃保持10~14h,自然冷却至室温。
7.根据权利要求1所述的一种富含S空位的CuInS2超薄纳米片的制备方法,其特征在于,所述步骤4中洗涤过程为用无水乙醇和去离子水交替洗涤,最后在65℃的真空烘箱中干燥24h。
8.一种富含S空位的CuInS2超薄纳米片的制备方法制备的富含S空位的CuInS2超薄纳米片在光催化产气中的应用。
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