CN108247039B - 一种金纳米带的制备方法 - Google Patents
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Abstract
本发明公开了一种金纳米带的制备方法。该制备方法的具体步骤如下：(1)将阳离子调节剂、四氯金酸和还原剂在水中混合搅拌10～30min，得到正电荷覆盖的金粒子溶液；(2)向上述正电荷覆盖的金粒子溶液中加入巯基型阴离子调节剂，室温下搅拌10～25小时，得到金纳米带。本发明方法简单，可以合成不同尺寸纳米金粒子形成的纳米带，并获得较好的单分散性，为纳米技术领域中纳米粒子表面控制剂的选择及不同形貌的纳米材料可控制备提供了重要的指导依据。
Description
技术领域
本发明涉及一维纳米材料制备技术领域，具体的说，涉及一种金纳米带的制备方法。
背景技术
亚纳米-纳米范围内的金属纳米材料已经在催化、传感和医学诊断中得到越来越多的应用，其中粒径和粒子空间特征在功能特性中起着关键作用。如有报道通过硫醇盐实现纳米簇的构建，携带生物药剂，在风湿性关节炎、支气管哮喘、疟疾、医疗护理等方面起到缓慢释放药物的作用。还有报道利用聚合物实现纳米粒子从单分散型演变成几个纳米的字符串的可控微观结构构建方法。
纳米带是不同于纳米粒子、纳米管的新一维纳米结构。根据不同形状或结构的金属纳米粒子的电磁场增强理论研究表明：不论是三角形粒子、椭圆形粒子还是纳米粒子二聚体，在光谱中容易形成热点的都是纳米材料的棱角、边缘等区域，因此纳米带的边缘均易成为光谱增强的热点，这样的电子特性使得金属纳米带在具备很大的应用前景。
目前氧化物等半导体材料的纳米带研究较多，而金属尤其是贵金属的纳米带研究较少，如何通过简单的化学合成法可控制备金属纳米带仍是一个有意义的研究方向。
发明内容
针对以上技术问题，本发明利的目的在于提供一种新颖的金纳米带的制备方法。该方法通过静电引力作用，将独立的不同尺寸的金纳米粒子串成纳米带，工艺简单，反应条件温和，容易控制。
本发明中，首先是在合成金纳米粒子的过程中引入阳离子调节剂，覆盖在纳米金表面，再加入具有强结合力的巯基型阴离子调节剂，通过阳离子调节剂和阴离子调节剂之间的静电引力作用，将独立的不同尺寸纳米金粒子形成纳米带；本发明形成的纳米带具有较好的单分散性。
本发明的技术方案具体介绍如下。
本发明提供一种金纳米带的制备方法，具体步骤如下：
(1)将阳离子调节剂、四氯金酸和还原剂在水中混合搅拌10～30min，得到正电荷覆盖的金粒子溶液；
(2)向上述正电荷覆盖的金粒子溶液中加入巯基型阴离子调节剂，室温下搅拌10～25小时，得到金纳米带。
本发明中，步骤(1)中，阳离子调节剂、四氯金酸和还原剂的摩尔比为100：(28-35)：(40-60)。
本发明中，步骤(1)中，阳离子调节剂为十六烷基三甲基溴化铵或十八烷基三甲基溴化铵；还原剂为硼氢化钠。
本发明中，步骤(1)中，正电荷覆盖的金粒子溶液中的金粒子的尺寸在2-20nm之间。
本发明中，步骤(2)中，巯基型阴离子调节剂为巯基丙酸或巯基丁酸。
本发明中，步骤(2)中，巯基型阴离子调节剂和正电荷覆盖的金粒子溶液的体积比1:10～1:5。
和现有技术相比，本发明的有益效果在于：
1、方法简单，适用范围光，可以将不同尺寸纳米金粒子形成纳米带，并获得较好的单分散性。
2、本发明通过阴阳离子调节剂的相互作用来控制金粒子彼此相接却又能保持一定间距。而根据不同形状或结构的金属纳米粒子的电磁场增强理论研究表明：在光谱中容易形成热点的都是纳米材料的棱角、边缘等区域，因此纳米带的边缘以及粒子-粒子彼此之间均易成为光谱增强的热点，这样的电子特性使得金属纳米带在具备很大的应用前景。
附图说明
图1为金纳米带的球差电镜图(a)及示意图(b)。
具体实施方式
下面结合具体的实施例对本发明的技术方案做进一步的描述，但本发明并不限于下述实施例。
本发明实施例中所用的各种原料，如无特殊说明，均为市售。
实施例1
(1)～8纳米金粒子的制备
首先100毫升浓度为0.10摩尔/升的十六烷基三甲基溴化铵溶液中加入5毫升0.030摩尔/升的四氯金酸溶液以及浓度为0.50摩尔/升的硼氢化钠溶液4毫升，搅拌20分钟，得到十六烷基三甲基溴化铵覆盖的金粒子溶液；
(2)金纳米带的制备
在上述金粒子溶液中，加入7毫升的巯基丙酸，室温下搅拌10个小时。搅拌过程中巯基丙酸根替代原本吸附在纳米粒子表面的溴离子，进而与十六烷基三甲基铵正离子进行静电结合，长链正离子易形成头尾相接的双体，从而依次将单个的纳米粒子通过表面上组装的正负离子静电引力结合成金纳米带带。
(3)纳米带形貌表征
通过球差电镜对纳米金带的尺寸和形貌进行表征，观察到的金纳米带呈细致而紧密排布且粒子粒径为～8nm，如图1所示。
实施例2
(1)～12纳米金粒子的制备
首先100毫升浓度为0.10摩尔/升的十六烷基三甲基溴化铵溶液中加入5毫升0.028摩尔/升的四氯金酸溶液以及浓度为0.55摩尔/升的硼氢化钠溶液4毫升，搅拌20分钟，得到十六烷基三甲基溴化铵覆盖的金粒子溶液；
(2)金纳米带的制备
在上述金粒子溶液中，加入10毫升的巯基丙酸，室温下搅拌10个小时。搅拌过程中巯基丙酸根替代原本吸附在纳米粒子表面的溴离子，进而与十六烷基三甲基铵正离子进行静电结合，长链正离子易形成头尾相接的双体，从而依次将单个的纳米粒子通过表面上组装的正负离子静电引力结合成金纳米带带。
(3)纳米带形貌表征
通过球差电镜对纳米金带的尺寸和形貌进行表征，观察到的金纳米带呈细致而紧密排布，粒子粒径～17nm。
Claims (1)
1.一种金纳米带的制备方法，其特征在于，具体步骤如下：
(1)将阳离子调节剂、四氯金酸和还原剂在水中混合搅拌10～30min，得到正电荷覆盖的金粒子溶液；
(2)向上述正电荷覆盖的金粒子溶液中加入巯基型阴离子调节剂，室温下搅拌10～25小时，得到金纳米带；
步骤(1)中，阳离子调节剂、四氯金酸和还原剂的摩尔比为100：(28-35)：(40-60)；阳离子调节剂为十六烷基三甲基溴化铵或十八烷基三甲基溴化铵；还原剂为硼氢化钠；正电荷覆盖的金粒子溶液中的金粒子的尺寸在2-20nm之间；
步骤(2)中，巯基型阴离子调节剂为巯基丙酸或巯基丁酸；巯基型阴离子调节剂和正电荷覆盖的金粒子溶液的体积比1:10～1:5。
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