CN107866560B - 一种分支网状金纳米材料的制备方法 - Google Patents

一种分支网状金纳米材料的制备方法 Download PDF

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CN107866560B
CN107866560B CN201711258431.8A CN201711258431A CN107866560B CN 107866560 B CN107866560 B CN 107866560B CN 201711258431 A CN201711258431 A CN 201711258431A CN 107866560 B CN107866560 B CN 107866560B
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杜明明
李银晓
曾淦宁
王杰
盛加楠
王国梁
斯鹏松
李清彪
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Abstract

一种分支网状金纳米材料的制备方法：分别配制柠檬酸三钠水溶液、氯金酸水溶液、硼氢化钠水溶液，将柠檬酸三钠水溶液和氯金酸水溶液混合，再加入硼氢化钠水溶液，室温搅拌反应10～60s，之后静置1～4h，得到近球形金溶胶；在所得近球形金溶胶中加入离子液体[BMIM][BF4]，搅拌0.5～2min，之后静置0.2～1.0h，即得分支网状金纳米材料；本发明首次报道了利用离子液体诱导水相中的近球形金纳米快速形成分支网状的金纳米材料，工艺简单，产率高，离子液体用量少；由于分支网状金纳米材料在近红外有强烈的特征吸收，因此在医疗和光学领域等方面具有潜在的应用价值。

Description

一种分支网状金纳米材料的制备方法
(一)技术领域
本发明涉及一种分支网状金纳米材料的制备方法。
(二)背景技术
纳米材料是指在三维空间中至少有一维处于纳米尺寸(0.1-100nm)或由它们作为基本单元构成的材料，按照维数纳米材料可以分为零位、一维和二维纳米材料(Nanotechnology,18(2007))。由于纳米材料晶粒尺寸很小，晶面原子的比例很大使其表现出量子尺寸效应、表面效应、宏观量子隧道效应以及介电限域效应等，从而使得纳米颗粒的热、磁、光、敏感特性和表面稳定性等不同于常规的材料。
贵金属纳米颗粒的物理化学性能与其形貌息息相关，在过去的十多年中，金纳米颗粒的形貌调控主要集中在近球形(J Nanopart Res,13(2011)4957-4968)、三角片(AdvFunct Mater,16(2006)1209-1214)、金纳米线(J Am Chem Soc,130(2008)8902-8903)、金纳米棒(J Am Chem Soc,124(2002)14316-14317)等。研究人员在合成粒度分度窄的球形金纳米颗粒，超细的金纳米线以及高产率的三角片和金纳米棒等方面做了大量的工作。因为它们的新颖特性在光学、医疗、催化等领域具有潜在的应用价值。因此，金纳米颗粒的形貌调控已经引起了很大的关注，它们为基础研究和技术应用提供了新的可能性。目前金纳米颗粒形貌调控方法有光化学法、晶种辅助法、水相化学还原法、电化学法、表面活性剂辅助法以及生物法等等，而探寻新的金纳米颗粒形貌调控方法也是研究者重要关注的方向之一。
(三)发明内容
本发明的目的是提供一种分支网状的金纳米材料的制备方法。本发明首先以硼氢化钠为还原试剂，柠檬酸三钠为保护剂制备近球形金溶胶，然后在所得近球形金溶胶中加入离子液体，即可快速合成分支网状的金纳米材料，所得分支网状金纳米材料产率高。
本发明的技术方案如下：
一种分支网状金纳米材料的制备方法，所述的制备方法为：
(1)分别配制0.1～1.0mmol/L(优选0.5mmol/L)柠檬酸三钠水溶液、0.1～1.0mmol/L(优选0.5mmol/L)氯金酸水溶液、1.0～10.0mol/L(优选4mmol/L)硼氢化钠水溶液，将柠檬酸三钠水溶液和氯金酸水溶液混合，再加入硼氢化钠水溶液，室温搅拌反应10～60s，之后静置1～4h，得到近球形金溶胶；
所述柠檬酸三钠水溶液、氯金酸水溶液、硼氢化钠水溶液的体积比为1：0.5～2：0.1～1.5，优选1：1：0.5；
(2)在步骤(1)所得近球形金溶胶中加入离子液体[BMIM][BF4]，搅拌0.5～2min，之后静置0.2～1.0h，即得分支网状金纳米材料；
所述离子液体[BMIM][BF4]与所述近球形金溶胶的体积比为0.05～1.0：50，优选0.1～0.2：50。
本发明所述室温为20～35℃。
本发明的有益效果在于：本发明首次报道了利用离子液体诱导水相中的近球形金纳米快速形成分支网状的金纳米材料，工艺简单，产率高，离子液体用量少。由于分支网状金纳米材料在近红外有强烈的特征吸收，因此在医疗和光学领域等方面具有潜在的应用价值。
(四)附图说明
图1：实施例1制备的分支网状金纳米材料的TEM图，图中的标尺为50nm；
图2：实施例1制备的分支网状金纳米材料的紫外-可见-近红外的光吸收光谱图，横坐标为Wavelength(nm)，纵坐标为吸收强度Absorption(a.u.)。
(五)具体实施方式
下面结合具体实施例对本发明作进一步的说明，但本发明的保护范围并不仅限于此。
实施例1
配制0.5mmol/L的柠檬酸三钠水溶液，0.5mmol/L的氯金酸水溶液，4mol/L的硼氢化钠水溶液。分别量取20mL柠檬酸三钠溶液和氯金酸溶液，加入100mL锥形瓶中混合，再向其中加入10mL 4mol/L的硼氢化钠溶液，室温搅拌反应30s后，静置2h，得到金溶胶。向金溶胶中加入0.1mL离子液体[BMIM][BF4]，搅拌1min后静置0.5h，得到分支网状金纳米材料。
通过TEM进行形貌分析，从图1中可以看出有大量的分支网状金纳米材料的生成，从紫外-可见-近红外的光吸收光谱图(图2)中可以看出，在700-1000nm的近红外波段存在着一个明显的吸收峰，该峰为分支网状金纳米材料的吸收峰。
实施例2
按照实施例1制备金溶胶，并向其中加入0.2mL离子液体[BMIM][BF4]，搅拌1min后静置0.5h，得到分支网状金纳米材料，并利用TEM进行形貌分析，与实施例1相比，金纳米材料分支更多网状结构更密集。
对比例1
按照实施例1制备金溶胶。将侧柏植物树叶(生物质)晒干、研磨粉碎，取1g侧柏叶粉末加去离子水100mL，搅拌2h过滤后得到滤液。取10mL滤液加入金溶胶中，搅拌0.5h，后加入0.1mL离子液体[BMIM][BF4]，搅拌1min后静置0.5h，并利用TEM进行形貌分析，未见分支网状金纳米材料形成。这一结果说明，通过植物生物质修饰后的金纳米材料，离子液体不能将其诱导形成分支网状金纳米材料。
对比例2
将侧柏植物树叶(生物质)晒干、研磨粉碎，取1g侧柏叶粉末加去离子水100mL，搅拌2h过滤后得到滤液，取30mL滤液置于100mL锥形瓶中，并加入20mL 0.5mmol/L氯金酸水溶液，搅拌1h后，可得近球形的金溶胶，向金溶胶中加入0.1mL离子液体[BMIM][BF4]，搅拌1min后静置0.5h，并利用TEM进行形貌分析，未见分支网状金纳米材料形成。这一结果说明，通过植物生物质制备的金纳米材料，离子液体同样也不能将其诱导形成分支网状金纳米材料。这是因为植物生物质对金纳米颗粒的保护作用更加强，而柠檬酸三钠是一种较弱的保护剂，因此离子液体可以将其保护的球形金纳米颗粒诱导形成分支网状金纳米材料。

Claims (6)

1.一种分支网状金纳米材料的制备方法，其特征在于，所述的制备方法为：
(1)分别配制0.1～1.0mmol/L柠檬酸三钠水溶液、0.1～1.0mmol/L氯金酸水溶液、1.0～10.0mol/L硼氢化钠水溶液，将柠檬酸三钠水溶液和氯金酸水溶液混合，再加入硼氢化钠水溶液，室温搅拌反应10～60s，之后静置1～4h，得到近球形金溶胶；
所述柠檬酸三钠水溶液、氯金酸水溶液、硼氢化钠水溶液的体积比为1：0.5～2：0.1～1.5；
(2)在步骤(1)所得近球形金溶胶中加入离子液体[BMIM][BF4]，搅拌0.5～2min，之后静置0.2～1.0h，即得分支网状金纳米材料；
所述离子液体[BMIM][BF4]与所述近球形金溶胶的体积比为0.05～1.0：50。
2.如权利要求1所述的分支网状金纳米材料的制备方法，其特征在于，步骤(1)中，所述柠檬酸三钠水溶液的浓度配制为0.5mmol/L。
3.如权利要求1所述的分支网状金纳米材料的制备方法，其特征在于，步骤(1)中，所述氯金酸水溶液的浓度配制为0.5mmol/L。
4.如权利要求1所述的分支网状金纳米材料的制备方法，其特征在于，步骤(1)中，所述硼氢化钠水溶液的浓度配制为4mmol/L。
5.如权利要求1所述的分支网状金纳米材料的制备方法，其特征在于，步骤(1)中，所述柠檬酸三钠水溶液、氯金酸水溶液、硼氢化钠水溶液的体积比为1：1：0.5。
6.如权利要求1所述的分支网状金纳米材料的制备方法，其特征在于，步骤(2)中，所述离子液体[BMIM][BF4]与所述近球形金溶胶的体积比为0.1～0.2：50。
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