CN113399680B - 一种Ag-AgX纳米线及其制备方法 - Google Patents
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- JRMUNVKIHCOMHV-UHFFFAOYSA-M tetrabutylammonium bromide Chemical compound [Br-].CCCC[N+](CCCC)(CCCC)CCCC JRMUNVKIHCOMHV-UHFFFAOYSA-M 0.000 claims description 4
- NHGXDBSUJJNIRV-UHFFFAOYSA-M tetrabutylammonium chloride Chemical compound [Cl-].CCCC[N+](CCCC)(CCCC)CCCC NHGXDBSUJJNIRV-UHFFFAOYSA-M 0.000 claims description 4
- SZEMGTQCPRNXEG-UHFFFAOYSA-M trimethyl(octadecyl)azanium;bromide Chemical group [Br-].CCCCCCCCCCCCCCCCCC[N+](C)(C)C SZEMGTQCPRNXEG-UHFFFAOYSA-M 0.000 claims description 4
- AISMNBXOJRHCIA-UHFFFAOYSA-N trimethylazanium;bromide Chemical compound Br.CN(C)C AISMNBXOJRHCIA-UHFFFAOYSA-N 0.000 claims description 4
- CURCMGVZNYCRNY-UHFFFAOYSA-N trimethylazanium;iodide Chemical compound I.CN(C)C CURCMGVZNYCRNY-UHFFFAOYSA-N 0.000 claims description 4
- MPNXSZJPSVBLHP-UHFFFAOYSA-N 2-chloro-n-phenylpyridine-3-carboxamide Chemical compound ClC1=NC=CC=C1C(=O)NC1=CC=CC=C1 MPNXSZJPSVBLHP-UHFFFAOYSA-N 0.000 claims description 3
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- VBIIFPGSPJYLRR-UHFFFAOYSA-M Stearyltrimethylammonium chloride Chemical group [Cl-].CCCCCCCCCCCCCCCCCC[N+](C)(C)C VBIIFPGSPJYLRR-UHFFFAOYSA-M 0.000 claims description 3
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- WOWHHFRSBJGXCM-UHFFFAOYSA-M cetyltrimethylammonium chloride Chemical group [Cl-].CCCCCCCCCCCCCCCC[N+](C)(C)C WOWHHFRSBJGXCM-UHFFFAOYSA-M 0.000 claims description 3
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- DPKBAXPHAYBPRL-UHFFFAOYSA-M tetrabutylazanium;iodide Chemical compound [I-].CCCC[N+](CCCC)(CCCC)CCCC DPKBAXPHAYBPRL-UHFFFAOYSA-M 0.000 claims description 2
- HIACZXUUKNSHAN-UHFFFAOYSA-M trimethyl(octadecyl)azanium;iodide Chemical group [I-].CCCCCCCCCCCCCCCCCC[N+](C)(C)C HIACZXUUKNSHAN-UHFFFAOYSA-M 0.000 claims description 2
- CEYYIKYYFSTQRU-UHFFFAOYSA-M trimethyl(tetradecyl)azanium;chloride Chemical group [Cl-].CCCCCCCCCCCCCC[N+](C)(C)C CEYYIKYYFSTQRU-UHFFFAOYSA-M 0.000 claims description 2
- AXRFZYRPSHSKBF-UHFFFAOYSA-M trimethyl(tetradecyl)azanium;iodide Chemical group [I-].CCCCCCCCCCCCCC[N+](C)(C)C AXRFZYRPSHSKBF-UHFFFAOYSA-M 0.000 claims description 2
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Abstract
本发明属于贵金属与半导体异质材料制备技术领域,具体涉及一种Ag‑AgX纳米线及其制备方法,包括以下步骤:(1)将一定摩尔比的可溶性银源与表面活性剂A和表面活性剂B(或卤化盐)混合溶解于水中,搅拌均匀,然后加热反应一定时间;(2)将反应得到的反应液进行离心洗涤,获得产物。本发明通过一步水热法制备阴离子简便可调的Ag‑AgX均匀尺寸纳米线,方法操作过程简便,成本低,重复性好,且实用性强;还提供了采用该制备方法合成得到的均匀尺寸的一维Ag‑AgX纳米线或纳米棒,该复合异质材料在催化、光催化、生物传感检测、以及电子器件领域具有潜在的应用价值。
Description
技术领域
本发明属于贵金属与半导体异质材料制备技术领域,具体涉及一种Ag-AgX纳米线及其制备方法。
背景技术
银-卤化银复合材料属于贵金属与半导体异质材料,其既具有Ag的优异物理化学性质,如导电性、表面等离子体共振效应、表面增强拉曼效应等,又具备半导体材料的特殊功能。Ag粒子相比半导体材料具有较高的功函数,易于储存电子,因此重金属与半导体材料的复合利于光生载流子的高效分离与转移,改善材料的光催化活性,有利于材料在污染物水处理、杀菌消毒环境净化、以及能源分子转换等方面的应用研究。许多研究者对于Ag-AgX材料的研究开发具有较高的兴趣。近些年,Ag-AgX材料的合成主要有两种方式,一种是在Ag粒子合成的基础上,采用离子交换的方式,实现Ag单质向AgX半导体的转换,从而实现Ag-AgX异质材料的制备(C.C.Jia,P.Yang,et al.,ChemCatChem,2014,6,611–617;P.Yang,C.C.Jia,et al.,RSCAdv.,2015,5,17210–17215;X.Y.Li,X.Zhang,C.C.Jia,P.Yang,etal.,ChemPlusChem,2015,80,865);另一种,是首先制备AgX半导体,然后在半导体材料表面采用光-/化学还原、溶剂热等方式,实现贵金属Ag在AgX表面的沉积(P.Wang,B.B.Huang,etal,Angew.Chem.Int.Ed.,2008,47,7931–7933;Y.X.Tang,Z.L.Jiang,T.C.Sum,S.Z.Li,Z.L.Dong,Z.Chen,et al.,Adv.Funct.Mater.,2013,23,2932–2940)。以上两种方式均采用两步法制备,操作复杂,工艺较为繁琐,为此科学工作者不断探索新的合成方法。目前,探索合成成本低且工艺简单的方法制备尺寸均匀的Ag-AgX异质材料仍具有较大的挑战,因而具有较高的研究价值。
发明内容
本发明的目的在于解决现有技术中存在的一维Ag-AgX纳米线制备工艺复杂、成本高的问题,提出了一种Ag-AgX纳米线的制备方法,通过一步水热法制备阴离子简便可调的Ag-AgX均匀尺寸纳米线,方法操作过程简便,成本低,重复性好,且实用性强;本发明还提供了采用该制备方法合成得到的均匀尺寸的一维Ag-AgX纳米线或纳米棒,该复合异质材料在催化、光催化、生物传感检测、以及电子器件领域具有潜在的应用价值。
本发明的技术方案是:
一种Ag-AgX纳米线的制备方法,包括以下步骤:
(1)将一定摩尔比的可溶性银源与表面活性剂A和表面活性剂B混合溶解于水中,搅拌均匀,然后加热反应一定时间;
(2)将反应得到的反应液进行离心洗涤,获得产物;
其中,所述可溶性银源包括硝酸银、醋酸银。
该制备方法以水作为溶剂,采用可溶性银源、非极性表面活性剂与含有卤素离子的阳离子表面活性剂或卤化盐,采用一次水热法制备Ag-AgX复合异质材料,得到均匀尺寸的Ag-AgX(X=Cl,Br,I)纳米线或纳米棒。
进一步的,所述步骤(1)中可溶性银源与表面活性剂A和表面活性剂B的摩尔比为1:2~10:0.05~0.6;优选的,摩尔比为1:3~5:0.12~0.28。
进一步的,所述步骤(1)中AgNO3与表面活性剂A和表面活性剂B的摩尔比为1:3~5:0.12~0.28;同样的,CH3COOAg与表面活性剂A和表面活性剂B的摩尔比为1:3~5:0.12~0.28。
进一步的,所述步骤(1)中反应温度为180~220℃,所述反应时间为5~20h。
进一步的,可溶性银源与表面活性剂A以及表面活性剂B溶解于溶液后的总摩尔浓度为0.03~0.12mol/L。
进一步的,所述表面活性剂A为非极性表面活性剂,所述表面活性剂B为含有卤素离子的阳离子表面活性剂;优选的,所述表面活性剂A为聚乙烯吡咯烷酮、N-甲基吡咯烷酮、乙烯基吡咯烷酮或2-吡咯烷酮中的任一种;优选的,所述表面活性剂B为十八烷基三甲基溴化铵、十八烷基三甲基氯化铵、十八烷基三甲基碘化铵、十六烷基三甲基溴化铵、十六烷基三甲基氯化铵、十六烷基三甲基碘化铵、十四烷基三甲基溴化铵、十四烷基三甲基氯化铵、十四烷基三甲基碘化铵、十二烷基三甲基溴化铵、十二烷基三甲基氯化铵、十二烷基三甲基碘化铵、十烷基三甲基溴化铵、十烷基三甲基氯化铵、十烷基三甲基碘化铵、八烷基三甲基溴化铵、八烷基三甲基氯化铵、八烷基三甲基碘化铵、六烷基三甲基溴化铵、六烷基三甲基氯化铵、六烷基三甲基碘化铵、四丁基溴化铵、四丁基氯化铵、四丁基碘化铵。
进一步的,所述表面活性剂B替换为卤化盐,即所述步骤(1)为,将一定摩尔比的可溶性银源与表面活性剂A和卤化盐溶解于水中,搅拌均匀,然后加热反应一定时间。
进一步的,所述卤化盐包括溴化钠、氯化钠、碘化钾。
采用所述的制备方法制备得到的Ag-AgX纳米线,所述纳米线的形貌为一维结构,直径为25~120nm,长度为几百纳米至几十微米。
进一步的,采用该制备方法所获得的产品形貌还可以为一维纳米棒,所述一维纳米棒的直径为25~120nm,长径比为2~20。
本发明的有益效果:
(1)本发明提供了一种尺寸均匀的Ag-AgX(X=Cl、Br、I)纳米线及其制备方法,以硝酸银作为银源,水作为溶剂,与表面活性剂混合均匀后,采用一步水热法制备得到;该方法操作过程简便,制备成本低廉,可控性及重复性好,所得产品实用性强,且克服了现有工艺制备过程复杂、成本高等缺点;制备过程仅使用一步以水作为溶剂的水热法合成,且通过调控反应初始原料引入的卤素离子可以简便调节所得异质材料的成分组成,既降低了生产成本,又做到绿色环保。
(2)采用本发明所提供制备方法制得的Ag-AgX纳米线产品尺寸均匀、直径较细、长度至微米级,同时由于Ag的表面等离子共振效应、表面增强拉曼效应、优良的导电导热性,以及AgX材料的光敏、光催化特性,因此该异质材料在催化、光催化、生物传感检测以及电子器件等研究领域均具有潜在的应用价值。
附图说明
图1为本发明实施例1合成的Ag-AgBr纳米线的扫描电镜图,其中a为低放大倍数的SEM图,b为高放大倍数的SEM图;
图2为本发明实施例1合成的Ag-AgBr纳米线的X射线衍射图谱;
图3为本发明实施例2合成的Ag-AgBr纳米线的扫描电镜图,其中a为低放大倍数的SEM图,b为高放大倍数的SEM图;
图4为本发明实施例3合成的Ag-AgBr纳米线的扫描电镜图,其中a为低放大倍数的SEM图,b为高放大倍数的SEM图;
图5为本发明实施例4合成的Ag-AgBr纳米线的扫描电镜图,其中a为低放大倍数的SEM图,b为高放大倍数的SEM图;
图6为本发明实施例5合成的Ag-AgCl纳米线的扫描电镜图,其中a为低放大倍数的SEM图,b为高放大倍数的SEM图;
图7为本发明实施例6合成的Ag-AgCl纳米线的扫描电镜图;
图8为本发明实施例7合成的Ag-AgI纳米线的扫描电镜图;
图9为本发明对比例1合成的Ag-AgBr纳米颗粒的扫描电镜图,其中a为低放大倍数的SEM图,b为高放大倍数的SEM图。
具体实施方式
下面将结合本发明实施例中的附图,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。
为了进一步理解本发明,将结合附图和实施例对本发明作进一步的说明。
本发明提供了一种均匀尺寸的Ag/AgX纳米线的制备方法,以水作为溶剂,可溶性银源作为银源,与表面活性剂混合均匀后,采用一次水热法,制备得到一维结构的Ag/AgX(X=Cl,Br,I)尺寸均匀纳米线或纳米棒。制备方法包括以下步骤:
(1)将摩尔比为1:2~10:0.05~0.6(优选1:3~5:0.12~0.28)的可溶性银源(硝酸银或醋酸银)与表面活性剂A和表面活性剂B(或卤化盐)溶解于水中,搅拌均匀,混合均匀后的三种原料与混合溶液的总摩尔浓度控制在0.03~0.12mol/L范围内,随后在反应温度为180~220℃的条件下加热,反应5~20h;(2)反应得到的料液经离心洗涤,获得尺寸均匀的Ag/AgX纳米线或纳米棒。
其中,表面活性剂A选自聚乙烯吡咯烷酮、N-甲基吡咯烷酮、乙烯基吡咯烷酮或2-吡咯烷酮中的任一种;表面活性剂B选自十八烷基三甲基溴(氯、碘)化铵、十六烷基三甲基溴(氯、碘)化铵、十四烷基三甲基溴(氯、碘)化铵、十二烷基三甲基溴(氯、碘)化铵、十烷基三甲基溴(氯、碘)化铵、八烷基三甲基溴(氯、碘)化铵、六烷基三甲基溴(氯、碘)化铵、四丁基溴(氯、碘)化铵中的任一种;表面活性剂B可替换为卤化盐,卤化盐为溴化钠、氯化钠、碘化钾中的任一种。
实施例1
称取0.034g AgNO3、0.1g PVP与0.02g CTAB,溶解于20mL水中,将溶液搅拌均匀;将所得溶液转移至50mL反应釜中,在烘箱中加热200℃,反应10h,得到反应产物;
将制备的反应产物进行离心洗涤,得到Ag-AgBr样品(如图1所示,图1a是该样品低放大倍数的SED图,图1b是该样品高放大倍数的SEM图),为直径约30nm,长度大于40μm的均匀尺寸一维纳米线,其结构成分如图2所示。
实施例2
称取0.034gAgNO3、0.1g PVP与0.02g CTAB,溶解于20mL水中,将溶液搅拌均匀;将所得溶液转移至50mL反应釜中,在烘箱中加热200℃,反应5h,得到反应产物;
将制备的反应产物进行离心洗涤,得到Ag-AgBr样品(如图3所示),为直径约30nm,长度为数十微米的均匀尺寸一维纳米线。
实施例3
称取0.034gAgNO3、0.1g PVP与0.02g TBAB,溶解于20mL水中,将溶液搅拌均匀;将所得溶液转移至50mL反应釜中,在烘箱中加热200℃,反应10h,得到反应产物;
将制备的反应产物进行离心洗涤,得到Ag-AgBr样品(如图4所示),为直径约27~100nm,长度为几百纳米或者几微米的一维纳米棒或纳米线。
实施例4
称取0.034gAgNO3、0.1g PVP与0.0056g NaBr,溶解于20mL水中,将溶液搅拌均匀;将所得溶液转移至50mL反应釜中,在烘箱中加热200℃,反应10h,得到反应产物;
将制备的反应产物进行离心洗涤,得到Ag-AgBr样品(如图5所示),为直径25~70nm,长度为几百纳米或者几微米的一维纳米棒或纳米线。
实施例5
称取0.034gAgNO3、0.1g PVP与0.02g CTAC,溶解于20mL水中,将溶液搅拌均匀;将所得溶液转移至50mL反应釜中,在烘箱中加热200℃,反应10h,得到反应产物;
将制备的反应产物进行离心洗涤,得到Ag-AgCl样品(如图6所示),为直径约70nm,长度为数十微米的一维纳米线。
实施例6
称取0.034gAgNO3、0.1g PVP与0.0032g NaCl,溶解于20mL水中,将溶液搅拌均匀;将所得溶液转移至50mL反应釜中,在烘箱中加热200℃,反应10h,得到反应产物;
将制备的反应产物进行离心洗涤,得到Ag-AgCl样品(如图7所示),为直径约60nm,长度为数微米的均匀尺寸一维纳米线。
实施例7
称取0.034gAgNO3、0.1g PVP与0.0091g KI,溶解于20mL水中,将溶液搅拌均匀;将所得溶液转移至50mL反应釜中,在烘箱中加热200℃,反应10h,得到反应产物;
将制备的反应产物进行离心洗涤,得到Ag-AgI样品(如图8所示),为直径80~120nm,长度为几百纳米或者几微米的一维纳米棒或纳米线。
实施例8
称取0.034gAgNO3、0.22g PVP与0.01g十二烷基三甲基溴化铵,溶解于20mL水中,将溶液搅拌均匀;将所得溶液转移至50mL反应釜中,在烘箱中加热180℃,反应20h,得到反应产物;将制备的反应产物进行离心洗涤,得到Ag-AgBr样品,为直径约40nm,长度为数十微米的均匀尺寸一维纳米线。
实施例9
称取0.034gAgNO3、0.44g PVP与0.01g六烷基三甲基氯化铵,溶解于20mL水中,将溶液搅拌均匀;将所得溶液转移至50mL反应釜中,在烘箱中加热220℃,反应10h,得到反应产物;将制备的反应产物进行离心洗涤,得到Ag-AgCl样品,为直径约30nm,长度为数十微米的均匀尺寸一维纳米线。
实施例10
称取0.034gAgNO3、0.1g 2-吡咯烷酮与0.0082gNaI,溶解于20mL水中,将溶液搅拌均匀;将所得溶液转移至50mL反应釜中,在烘箱中加热210℃,反应15h,得到反应产物;将制备的反应产物进行离心洗涤,得到Ag-AgI样品,为直径约60nm,长度为数微米的一维纳米线。
实施例11
称取0.034gAgNO3、0.1gN-甲基吡咯烷酮与0.02g八烷基三甲基溴化铵,溶解于20mL水中,将溶液搅拌均匀;将所得溶液转移至50mL反应釜中,在烘箱中加热190℃,反应10h,得到反应产物;将制备的反应产物进行离心洗涤,得到Ag-AgBr样品,为直径约50nm,长度为数微米的均匀尺寸一维纳米线。
实施例12
称取0.033g CH3COOAg、0.1g乙烯基吡咯烷酮与0.02g CTAB,溶解于20mL水中,将溶液搅拌均匀;将所得溶液转移至50mL反应釜中,在烘箱中加热200℃,反应5h,得到反应产物;将制备的反应产物进行离心洗涤,得到Ag-AgBr样品,为直径约40nm,长度为数十微米的均匀尺寸一维纳米线。
对比例1
称取0.034gAgNO3与0.12g CTAB,溶解于20mL水中,将溶液搅拌均匀;将所得溶液转移至50mL反应釜中,在烘箱中加热200℃,反应10h,得到反应产物;
将制备的反应产物进行离心洗涤,得到如图9所示的Ag-AgBr样品。由图9可以看出,在无PVP表面活性剂参与的条件下,合成的Ag-AgBr样品的结构为较大直径颗粒。
上述说明仅为本发明的优选实施例,并非是对本发明的限制,尽管参照前述实施例对本发明进行了详细的说明,对于本领域技术人员来说,其依然可以对前述各实施例所记载的技术方案进行修改,或者对其中部分技术特征进行等同替换。凡在本发明的精神和原则之内,所作的任何修改、等同替换、改型等,均应包含在本发明的保护范围之内。
Claims (6)
1.一种Ag-AgX纳米线的制备方法,其特征在于,包括以下步骤:
(1)将摩尔比为1:2~10:0.05~0.6的可溶性银源与表面活性剂A和表面活性剂B混合溶解于水中,搅拌均匀,然后180~220℃加热反应5~20 h;
(2)将反应得到的反应液进行离心洗涤,获得产物;
其中,所述可溶性银源为硝酸银、醋酸银;
所述表面活性剂A为聚乙烯吡咯烷酮、N-甲基吡咯烷酮、乙烯基吡咯烷酮或2-吡咯烷酮中的任一种;所述表面活性剂B为含有卤素离子的阳离子表面活性剂或卤化盐;
所述X为Cl、Br、I。
2.根据权利要求1所述的制备方法,其特征在于,所述步骤(1)中AgNO3与表面活性剂A和表面活性剂B的摩尔比为1:3~5:0.12~0.28。
3.根据权利要求1所述的制备方法,其特征在于,可溶性银源与表面活性剂A以及表面活性剂B溶解于水中后的总摩尔浓度为0.03~0.12 mol/L。
4.根据权利要求1所述的制备方法,其特征在于,所述表面活性剂B为十八烷基三甲基溴化铵、十八烷基三甲基氯化铵、十八烷基三甲基碘化铵、十六烷基三甲基溴化铵、十六烷基三甲基氯化铵、十六烷基三甲基碘化铵、十四烷基三甲基溴化铵、十四烷基三甲基氯化铵、十四烷基三甲基碘化铵、十二烷基三甲基溴化铵、十二烷基三甲基氯化铵、十二烷基三甲基碘化铵、十烷基三甲基溴化铵、十烷基三甲基氯化铵、十烷基三甲基碘化铵、八烷基三甲基溴化铵、八烷基三甲基氯化铵、八烷基三甲基碘化铵、六烷基三甲基溴化铵、六烷基三甲基氯化铵、六烷基三甲基碘化铵、四丁基溴化铵、四丁基氯化铵、四丁基碘化铵。
5.根据权利要求1所述的制备方法,其特征在于,所述卤化盐为溴化钠、氯化钠、碘化钾。
6.采用权利要求1至5任一项所述的制备方法制备得到的Ag-AgX纳米线,其特征在于,所述纳米线的形貌为一维结构,直径为25~120 nm,长度为几百纳米至几十微米。
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