CN106268900B - 一种g-C3N4量子点敏化AgVO3纳米线的制备方法 - Google Patents
一种g-C3N4量子点敏化AgVO3纳米线的制备方法 Download PDFInfo
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Abstract
本发明属于一种g‑C3N4量子点敏化AgVO3纳米线的制备方法。制备方法包括以下步骤:1)g‑C3N4量子点的制备,2)AgVO3纳米线的制备,3)g‑C3N4敏化AgVO3纳米线量子点的制备。本申请所述方法简单易行、操作方便、成本较低、可重复性高、产物的可见光催化活性高,在复合纳米材料的制备和应用领域有着广阔的发展前景。
Description
技术领域
本发明属于纳米材料制备的技术领域,特别涉及了一种g-C3N4量子点敏化AgVO3纳米线的制备方法。
背景技术
含有不同比例的银、钒、氧等复合氧化物统称为钒酸银,根据银、钒、氧比例不同,钒酸银具有多种不同的组成与结构。钒酸银材料是一类广泛应用于光学、电学和催化等方面的功能材料,近年来,对于纳米尺寸的钒酸银的制备工艺、微观结构、物理和化学性能的研究也逐渐成为研究人员的热点问题,多种不同组成、结构及形貌的钒酸银纳米材料被研究报道,并在电化学、磁学、催化、抗菌等领域显示出优异的性能。
金属钒酸盐是一类优良的光催化材料,例如钒酸铋、钒酸铟、钒酸铁等钒酸盐材料在光催化领域均展现出巨大的应用潜力,其中 AgVO3具有良好的光催化性能。g-C3N4以其光催化性能高、稳定性好、原料价格便宜、尤其是不含金属这一突出优点,使它成为一种新型的光催化剂。在改良研究方面,大多数的无机化合物和无机金属离子能够结合或者插入到g-C3N4基质中,能够有效地微调g-C3N4的结构进而提高反应活性。研究还发现,通过对g-C3N4的改进,可拓展其可见光的响应范围,抑制g-C3N4的光生电子和空穴的复合,提高 g-C3N4的光催化活性,这对工业化应用有着重要意义。g-C3N4常见的耦合体有很多,但未见g-C3N4量子点敏化AgVO3纳米线复合催化剂的相关报道。
发明内容
本发明的目的是要提供一种g-C3N4量子点敏化AgVO3纳米线的制备方法,此方法简单易行,成本较低,可重复性高,产物的可见光催化活性高。
本发明的技术方案是:
g-C3N4量子点敏化AgVO3纳米线的制备方法包括以下步骤:
1)g-C3N4量子点的制备:采用三聚氰胺为原料,先将三聚氰胺加热到500℃,于500℃保温4h。在室温下,获得的块状g-C3N4于室温下在浓硫酸和浓硝酸混合液回流2h,再用去离子水稀释混合物,并用去离子水洗数次,然后将固体分散在浓氨水中,把混合悬浮物装入内衬聚四氟乙烯不锈钢反应釜中进行水热反应,冷却至室温,用去离子水洗涤数次沉淀物,将合成的固体分散在水中,超声分散6 h,以7000rpm离心分离,得到沉淀;
2)AgVO3纳米线的制备:将质量比为2.8432:1.0192的硝酸银和偏钒酸钠于搅拌下分别溶于去离子水中,搅拌均匀后向偏钒酸钠溶液中加入1mL 65%的硝酸,然后将硝酸银溶液逐滴加到偏钒酸钠溶液中,继续磁力搅拌30min,在磁力搅拌下用4mol·L-1的氢氧化钠将溶液pH调节为3,将其混合超声分散30min,装入内衬聚四氟乙烯不锈钢反应釜中进行水热反应,反应后的悬浊液经超声分散30min 后,离心分离,得到沉淀,将沉淀分别用去离子水和无水乙醇洗涤2 次后,于真空干燥箱内60℃烘干,即可获得AgVO3纳米线;
3)g-C3N4敏化AgVO3纳米线量子点的制备:将g-C3N4量子点于磁力搅拌下逐滴加入到偏钒酸银溶液中,于70℃下搅拌30min,反应后得到的悬浊液经超声分散30min后,离心分离,得到沉淀,将沉淀分别用去离子水和无水乙醇洗涤2次后,于真空干燥箱内70℃烘干,即得g-C3N4量子点敏化AgVO3纳米线复合光催化剂。
本发明的有益效果是:
1、本申请所述方法简单易行、操作方便、成本较低、可重复性高、产物的可见光催化活性高,在复合纳米材料的制备和应用领域有着广阔的发展前景。
2、本申请在g-C3N4量子点敏化AgVO3纳米线的制备中,所用的原料只是三聚氰胺、硝酸银和偏钒酸钠,不需要任何助剂及模版剂。
附图说明
图1为g-C3N4量子点敏化AgVO3纳米线的制备流程示意图;
图2为所制备的g-C3N4量子点、AgVO3纳米线以及复合催化剂的XRD图
图3所制备的g-C3N4量子点、AgVO3纳米线以及g-C3N4/AgVO3复合催化剂的FTIR图
图4为所制备样品的SEM、TEM及HRTEM照片
图4a为所制备的AgVO3样品SEM照片
图4b为所制备的CNQDs/AgVO3样品SEM照片
图4c为所制备的AgVO3样品TEM照片
图4d为所制备的CNQDs/AgVO3样品TEM照片
图4e为所制备的CNQDs/AgVO3样品HRTEM照片
图4f为所制备的CNQDs/AgVO3样品另一角度HRTEM照片
具体实施方式
本申请是一种g-C3N4量子点敏化AgVO3纳米线复合可见光催化材料的制备方法。采用X-射线衍射仪、红外光谱仪、扫描电子显微镜及透射电子显微镜等测试手段对所制备的材料进行表征。该方法过程包括:通过简单的水热法,以AgNO3和NaVO3为反应物制备AgVO3纳米线材料;通过三聚氰胺的缩聚反应制备g-C3N4,进而再通过水热法,得到g-C3N4量子点。最后采用共沉淀法制备g-C3N4量子点敏化 AgVO3纳米线复合可见光催化材料。该方法制备过程简单易控、操作方便、成本低、产物的可见光催化活性高。
具体步制备过程如下:
1.g-C3N4量子点的制备:采用三聚氰胺为原料,先将三聚氰胺以升温速率2.3℃/min加热到500℃,于500℃保温4h。获得的块状 g-C3N4于室温下在浓硫酸和浓硝酸混合液回流2h,再用去离子水稀释混合物,并用去离子水洗数次,然后将固体分散在浓氨水中,把混合悬浮物装入内衬聚四氟乙烯不锈钢反应釜中,充填度为70%,于 200℃加热12h,冷却至室温。用去离子水洗涤数次沉淀物,将合成的固体分散在水中,超声分散6h,以7000rpm离心分离,得到沉淀。
2.AgVO3纳米线的制备:将2.8432g硝酸银和1.0192g偏钒酸钠于搅拌下分别溶于30mL和60mL的去离子水中,搅拌均匀后向偏钒酸钠溶液中加入1mL 65%的硝酸,然后将硝酸银溶液逐滴加到偏钒酸钠溶液中,继续磁力搅拌30min。在磁力搅拌下用4mol·L-1的氢氧化钠将溶液pH调节为3,将其混合超声分散30min,装入内衬聚四氟乙烯不锈钢反应釜中,充填度为70%,于干燥箱内160℃加热6h。反应后的悬浊液经超声分散30min后,离心分离,得到沉淀,将沉淀分别用去离子水和无水乙醇洗涤2次后,于真空干燥箱内60℃烘干,即可获得AgVO3纳米线。
3.g-C3N4敏化AgVO3纳米线量子点的制备:取22.2222mg AgVO3于40mL蒸馏水中配成溶液,将1mg/mL g-C3N4量子点(2mL) 于磁力搅拌下逐滴加入到偏钒酸银溶液中,于70℃下搅拌30min。反应后得到的悬浊液经超声分散30min后,离心分离,得到沉淀。将沉淀分别用去离子水和无水乙醇洗涤2次后,于真空干燥箱内70℃烘干,即得g-C3N4量子点敏化AgVO3纳米线复合光催化剂。
图2为所制备样品的XRD图。从图1可知所制备的g-C3N4量子点(CNQDs)/AgVO3样品为单斜结构(JCPDS:29-1154),从图中没有观察到g-C3N4的衍射峰,这是由于g-C3N4量子点的尺寸较小。
图3为所制备样品的FT-IR图。所有g-C3N4的特征峰(1636cm-1、 1575cm-1、1462cm-1、1405cm-1、1322cm-1、1235cm-1、813cm-1) 都可以从CNQDs/AgVO3图谱中可以观察到,说明g-C3N4的成功负载。
图4为所制备样品的SEM、TEM及HRTEM照片。其中图4a为所制备的AgVO3样品SEM照片,其形貌为一维纳米线。从图4c可以观察到所制备的纯相AgVO3表面光滑。图4b为所制备的CNQDs/AgVO3样品SEM照片,可以看出低浓度g-C3N4量子点没有引起AgVO3纳米线的形貌变化。图4d中可以观察到g-C3N4量子点负载在AgVO3纳米线的表面上。从图4e和4f中可以测量出晶格条纹距离分别为0.35和0.336nm,分别对应AgVO3(110)和CNQD (002)的晶面间距。
Claims (5)
1.一种g-C3N4量子点敏化AgVO3纳米线的制备方法,其特征在于:该方法包括以下步骤:
1)g-C3N4量子点的制备:采用三聚氰胺为原料,先将三聚氰胺加热到500℃,于500℃保温4h;在室温下,获得的块状g-C3N4于室温下在浓硫酸和浓硝酸混合液回流2h,再用去离子水稀释混合物,并用去离子水洗数次,然后将固体分散在浓氨水中,把混合悬浮物装入内衬聚四氟乙烯不锈钢反应釜中进行水热反应,冷却至室温,用去离子水洗涤数次沉淀物,将合成的固体分散在水中,超声分散6h,以7000rpm离心分离,得到沉淀;
2)AgVO3纳米线的制备:将质量比为2.8432:1.0192的硝酸银和偏钒酸钠于搅拌下分别溶于去离子水中,搅拌均匀后向偏钒酸钠溶液中加入1mL65%的硝酸,然后将硝酸银溶液逐滴加到偏钒酸钠溶液中,继续磁力搅拌30min,在磁力搅拌下用4mol·L-1的氢氧化钠将溶液pH调节为3,将其混合超声分散30min,装入内衬聚四氟乙烯不锈钢反应釜中进行水热反应,反应后的悬浊液经超声分散30min后,离心分离,得到沉淀,将沉淀分别用去离子水和无水乙醇洗涤2次后,于真空干燥箱内60℃烘干,即可获得AgVO3纳米线,所述水热反应条件为充填度为70%,于干燥箱内160℃加热6h;
3)g-C3N4敏化AgVO3纳米线量子点的制备:将g-C3N4量子点于磁力搅拌下逐滴加入到AgVO3纳米线溶液中,于70℃下搅拌30min,反应后得到的悬浊液经超声分散30min后,离心分离,得到沉淀,将沉淀分别用去离子水和无水乙醇洗涤2次后,于真空干燥箱内70℃烘干,即得g-C3N4量子点敏化AgVO3纳米线复合光催化剂。
2.根据权利要求1所述的一种g-C3N4量子点敏化AgVO3纳米线的制备方法,其特征在于:所述步骤1)中三聚氰胺加热升温速率2.3℃/min。
3.根据权利要求1所述的一种g-C3N4量子点敏化AgVO3纳米线的制备方法,其特征在于:所述步骤1)水热反应条件为充填度为70%,于200℃加热12h。
4.根据权利要求1所述的一种g-C3N4量子点敏化AgVO3纳米线的制备方法,其特征在于:所述步骤2)将2.8432克硝酸银和1.0192克的偏钒酸钠于搅拌下分别溶于30mL和60mL的去离子水。
5.根据权利要求1所述的一种g-C3N4量子点敏化AgVO3纳米线的制备方法,其特征在于:所述步骤3)取22.2222mg AgVO3纳米线于40mL蒸馏水中配成溶液,将1mg/mL g-C3N4量子点2mL于磁力搅拌下逐滴加入到AgVO3纳米线溶液中。
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