CN108274018A - 一种以铜纳米线为模板制备银纳米管的方法 - Google Patents

一种以铜纳米线为模板制备银纳米管的方法 Download PDF

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CN108274018A
CN108274018A CN201711390658.8A CN201711390658A CN108274018A CN 108274018 A CN108274018 A CN 108274018A CN 201711390658 A CN201711390658 A CN 201711390658A CN 108274018 A CN108274018 A CN 108274018A
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copper nano
template
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silver
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张广维
吴雪卫
陈剑宇
孙志鹏
李谊
马延文
仪明东
黄艳琴
罗孟成
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Nanjing Post and Telecommunication University
Nanjing University of Posts and Telecommunications
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    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/16—Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/05—Metallic powder characterised by the size or surface area of the particles
    • B22F1/054—Nanosized particles
    • B22F1/0547—Nanofibres or nanotubes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
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    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
    • C23C18/1601—Process or apparatus
    • C23C18/1633—Process of electroless plating
    • C23C18/1655—Process features
    • C23C18/1657—Electroless forming, i.e. substrate removed or destroyed at the end of the process
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
    • C23C18/1601—Process or apparatus
    • C23C18/1633—Process of electroless plating
    • C23C18/1689—After-treatment
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
    • C23C18/31—Coating with metals
    • C23C18/42—Coating with noble metals
    • C23C18/44—Coating with noble metals using reducing agents

Abstract

本发明公开了一种以铜纳米线为模板制备银纳米管的方法，所述方法以铜纳米线为模板，以硝酸银为银源进行化学镀银，退火过程后采用蚀刻液去除铜纳米线，即可制得银纳米管。本发明所述方法以铜纳米线为模板，以硝酸银为镀液的银源，经退火和蚀刻液洗涤去除模板等过程制得以纳米管，整个过程能耗少，且操作简便，适合大规模生产。

Description

一种以铜纳米线为模板制备银纳米管的方法
技术领域
本发明属于材料化学领域，涉及一种纳米材料制备与应用传感技术，具体为一种以铜纳米线为模板制备银纳米管的方法。
背景技术
纳米材料在尺寸和结构上的特异性，使得纳米材料具有很多不同于常规材料的特殊性质，比如较高的晶体缺陷密度、界面所占体积百分数很大、极细的晶粒尺寸等，这些结构上独特性质使得纳米材料的电学、光学、热学、力学、磁学等性能，无论在宏观或微观方面都与常规大块材料大不相同。在众多的纳米材料中，管状纳米结构材料如银纳米管因其独特的物理、化学性能在光、电、催化和存储等领域表现出重要的应用价值。如果对其内壁、外壁或者端口进行修饰，会进一步表现出独特的性能。现有的银纳米管制备方法存在步骤繁琐、制备成本高、对设备要求高等弊端，因此，如何低成本的大规模制备银纳米管成为一项具有重大意义的课题。
发明内容
解决的技术问题：为了克服现有技术的缺陷，获得一种操作简便、能耗少、适合大规模制备管状纳米结构材料，本发明提供了一种以铜纳米线为模板制备银纳米管的方法。
技术方案：一种以铜纳米线为模板制备银纳米管的方法，所述方法以铜纳米线为模板，以硝酸银为银源进行化学镀银，退火过程后采用蚀刻液去除铜纳米线，即可制得银纳米管。
优选的，所述方法具体包括以下步骤：
(1)将铜纳米线原料分散至镀液中，所述镀液中硝酸银和三乙烯四胺的摩尔比例为1:1～1:2，0～60℃水浴条件条件下搅拌反应10～60min；
(2)将步骤(1)得到的铜金异质结构100～300℃条件下退火处理1～10h；
(3)将退火处理后的样品分散至蚀刻液中反应6～24小时制得，所述蚀刻液为含有二价铜离子的盐酸溶液或三氯化铁溶液。
优选的，所述铜纳米线的直径为50-100nm，长度为10-20μm。
优选的，步骤(1)的镀液中硝酸银和三乙烯四胺的摩尔比例为1:1～1:2。
优选的，步骤(3)中所述盐酸为质量分数36％的浓盐酸。
优选的，步骤(3)中二价铜离子与盐酸的摩尔比例为1:2～1:4。
本发明以铜纳米线为模板制备银纳米管方法的原理在于：以铜纳米线为模板，通过置换反应进行化学镀银，再蚀刻铜芯，得到银纳米管。
有益效果：(1)本发明所述方法以铜纳米线为模板，以硝酸银为镀液的银源，经退火和蚀刻液洗涤去除模板等过程制得以纳米管，整个过程能耗少，且操作简便，适合大规模生产；(2)本发明所述方法制备获得的银纳米管具有外壁光滑，长径比高，产率高，可重复性强等优点。
附图说明
图1是本发明所述方法制得的银纳米管的TEM图。
具体实施方式
以下实施例进一步说明本发明的内容，但不应理解为对本发明的限制。在不背离本发明精神和实质的情况下，对本发明方法、步骤或条件所作的修改和替换，均属于本发明的范围。若未特别指明，实施例中所用的技术手段为本领域技术人员所熟知的常规手段。
实施例1
(1)称取5g硝酸银溶解在250mL水中，加入9mL三乙烯四胺配置成镀液待用；
(2)称取0.5g铜纳米线加入镀液中，冰水浴条件下反应10min，抽滤后待用；
(3)将上述抽滤后得到的样品在马弗炉中退火处理10h；
(4)称取3g无水硫酸铜分散至100mL的36％浓盐酸中配置成蚀刻液；
(5)将退火后的异质结构分散至蚀刻液中反应1h，依次用去离子水和乙醇洗涤抽滤后得到银纳米管。
实施例2
(1)称取5g硝酸银溶解在250mL水中，加入6mL三乙烯四胺配置成镀液待用；
(2)称取0.5g铜纳米线加入镀液中，30℃条件下反应10min，抽滤后待用；
(3)将上述抽滤后得到的样品在马弗炉中退火处理10h；
(4)称取3g无水硫酸铜分散至100mL的36％浓盐酸中配置成蚀刻液；
(5)将退火后的异质结构分散至蚀刻液中反应1h，依次用去离子水和乙醇洗涤抽滤后得到银纳米管。
实施例3
(1)称取5g硝酸银溶解在250mL水中，加入6mL三乙烯四胺配置成镀液待用；
(2)称取0.5g铜纳米线加入镀液中，60℃条件下反应10min，抽滤后待用；
(3)将上述抽滤后得到的样品在马弗炉中退火处理10h；
(4)称取3g无水硫酸铜分散至100mL的36％浓盐酸中配置成蚀刻液；
(5)将退火后的异质结构分散至蚀刻液中反应1h，依次用去离子水和乙醇洗涤抽滤后得到银纳米管。
实施例4
(1)称取5g硝酸银溶解在250mL水中，加入6mL三乙烯四胺配置成镀液待用；
(2)称取0.5g铜纳米线加入镀液中，冰水浴条件下反应10min，抽滤后待用；
(3)将上述抽滤后得到的样品在马弗炉中退火处理10h；
(4)称取10g三氯化铁分散至200mL去离子水中配置成蚀刻液；
(5)将退火后的异质结构分散至蚀刻液中反应1h，依次用去离子水和乙醇洗涤抽滤后得到银纳米管。
实施例5
(1)称取5g硝酸银溶解在250mL水中，加入6mL三乙烯四胺配置成镀液待用；
(2)称取0.5g铜纳米线加入镀液中，30℃条件下反应10min，抽滤后待用；
(3)将上述抽滤后得到的样品在马弗炉中退火处理10h；
(4)称取10g三氯化铁分散至200mL去离子水中配置成蚀刻液；
(5)将退火后的异质结构分散至蚀刻液中反应1h，依次用去离子水和乙醇洗涤抽滤后得到银纳米管。
实施例6
(1)称取5g硝酸银溶解在250mL水中，加入6mL三乙烯四胺配置成镀液待用；
(2)称取0.5g铜纳米线加入镀液中，60℃条件下反应10min，抽滤后待用；
(3)将上述抽滤后得到的样品在马弗炉中退火处理10h；
(4)称取10g三氯化铁分散至200mL去离子水中配置成蚀刻液；
(5)将退火后的异质结构分散至蚀刻液中反应1h，依次用去离子水和乙醇洗涤抽滤后得到银纳米管。
结果分析：由图1可知，本发明所制备银纳米管外径在100nm左右，且直径均匀，外壁光滑。

Claims (6)

1.一种以铜纳米线为模板制备银纳米管的方法，其特征在于，所述方法以铜纳米线为模板，以硝酸银为银源进行化学镀银，退火过程后采用蚀刻液去除铜纳米线，即可制得银纳米管。
2.根据权利要求1所述的一种以铜纳米线为模板制备银纳米管的方法，其特征在于，所述方法具体包括以下步骤：
(1)将铜纳米线原料分散至镀液中，所述镀液中硝酸银和三乙烯四胺的摩尔比例为1:1～1:2，0～60℃水浴条件下搅拌反应10～60min；
(2)将步骤(1)得到的铜金异质结构100～300℃条件下退火处理1～10h；
(3)将退火处理后的样品分散至蚀刻液中反应6～24小时制得，所述蚀刻液为含有二价铜离子的盐酸溶液或三氯化铁溶液。
3.根据权利要求1所述的一种以铜纳米线为模板制备银纳米管的方法，其特征在于，所述铜纳米线的直径为50-100nm，长度为10-20μm。
4.根据权利要求1所述的一种以铜纳米线为模板制备银纳米管的方法，其特征在于，步骤(1)的镀液中硝酸银和三乙烯四胺的摩尔比例为1:1～1:2。
5.根据权利要求1所述的一种以铜纳米线为模板制备银纳米管的方法，其特征在于，步骤(3)中所述盐酸为质量分数36％的浓盐酸。
6.根据权利要求1所述的一种以铜纳米线为模板制备银纳米管的方法，其特征在于，步骤(3)中二价铜离子与盐酸的摩尔比例为1:2～1:4。
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