CN110405226B - 一种水溶性银微纳米晶及其可控制备方法 - Google Patents
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Abstract
一种水溶性银微纳米晶及其可控制备方法，涉及银微纳米晶制备技术领域。包括反应前驱液的配制和室温快速还原反应两个过程，首先配制硝酸银溶液，然后将抗坏血酸(VC)固体加入到硝酸银溶液中，最后在室温下通过快速还原反应得到水溶性银微纳米晶；也可以在配制硝酸银溶液时加入表面活性剂的水溶液。本发明所制备的Ag微纳米晶是由无数Ag纳米颗粒构成的微晶，通过改变表面活性剂的种类和用量可分别获得准球状(不添加表面活性剂)、树枝晶状(采用蓝月亮洗手液LYL作为表面活性剂)和颗粒链状Ag微纳米晶(采用硬脂酸微乳液ALA作为表面活性剂)。本发明所获得的产物水溶性、分散性和稳定性好，可望用于水性抗菌涂料生产行业。
Description
技术领域
本发明涉及银微纳米晶制备技术领域，具体是涉及一种水溶性银微纳米晶及其可控制备方法。
背景技术
水溶性Ag纳米粉体在抗菌涂料生产中起着关键的作用。银(Ag)微纳米晶由于其优异的光学、催化和抗菌等性质，以及在表面等离子体共振、表面增强拉曼散射和抗菌等方面应用广泛。Ag纳米晶所具备的独特的性质是由其尺寸和形貌决定的，因此不同尺寸和形貌的银纳米晶的合成一直备受关注，例如球形、立方体、三棱柱、片状、棒状和线状等银纳米晶。
已报道的诸多形态Ag纳米晶通常均是在氯仿和甲酰胺等有机相中，同时利用PVP、SDS和CTAB为修饰剂来控制Ag纳米晶形貌。该方法尽管重复性好，形态可控，但是此方法获得的Ag纳米晶表面常包覆有机配体，水溶性较差，从而大大限制了其在生物医学、催化和水性功能涂料等方面的实际应用。而已有以硼氢化钠、抗坏血酸和柠檬酸钠等还原剂在水相中合成的Ag纳米晶尺寸小、分散性差和易氧化等。
发明内容
本发明针对已有制备水溶性银微纳米晶中所存在的不足之处，提供一种水溶性银微纳米晶及其可控制备方法。采用自制的水溶性阴离子表面活性剂——蓝月亮洗手液(LYL)和硬脂酸微乳液(ALA)，来可控制备Ag纳米晶生长，为水性抗菌功能涂料生产提供助剂保障。
为了实现上述目的，本发明所采用的技术方案为：一种水溶性银微纳米晶的可控制备方法，包括反应前驱液的配制和室温快速还原反应两个过程，首先配制硝酸银溶液，然后将抗坏血酸(VC)固体加入到硝酸银溶液中，最后在室温下通过快速还原反应得到水溶性银微纳米晶；
或者，首先配制硝酸银溶液，然后加入表面活性剂的水溶剂，均匀混合后，再将抗坏血酸(VC)固体加入到混合溶液中，最后在室温下通过快速还原反应得到水溶性银微纳米晶。
作为本发明可控制备方法的优选技术方案，方法包括如下步骤：
1)、将50-200mL浓度为0.01-0.1mol/L的AgNO3溶液和0-25mL浓度为0.1-0.4mol/L的表面活性剂的水溶液混合后得到活性反应前驱体溶液；
2)、将0.1-0.6g的VC固体加入到反应前驱体溶液中，通过快速还原反应得到水溶性银微纳米晶。
进一步优选地，可控制备方法中，快速还原反应时间为1-5min。步骤2)中得到的水溶性银微纳米晶溶液体系的pH值为6-7.5。VC的使用量与AgNO3的体积和浓度有关，当AgNO3的体积一定时，随着VC固体的使用量增加，反应所需时间缩短。
本发明在室温下，采用自制的LYL和ALA绿色水性试剂来调控Ag微纳米晶的生成，整个工艺原料易得、方法简便易行，操作简单而且产率高。
与现有技术相比，本发明的有益效果表现在：
1)、本发明的可控制备方法得到的Ag微纳米晶是由无数Ag纳米颗粒构成的微晶，通过改变表面活性剂的种类和用量可分别获得准球状(不添加表面活性剂)、树枝晶状(采用蓝月亮洗手液LYL作为表面活性剂)和颗粒链状Ag微纳米晶(采用硬脂酸微乳液ALA作为表面活性剂)。
2)、本发明利用廉价绿色的水性修饰剂来调控Ag纳米晶组装和生长，得到了光学性能优异的银微纳米材料，为高性能抗菌助剂生产提供了新的策略。整个制备工艺简单、所需原料易得且产率高，获得的产物水溶性、分散性和稳定性好，可望用于水性抗菌涂料生产行业。
附图说明
图1为实施例1-4制备的水溶性银微纳米晶的外观形态、微观形态及化学组成。
图2为实施例1-3制备的水溶性银微纳米晶的XRD对比分析图。
图3为实施例1-3制备的水溶性银微纳米晶的UV-vis谱图。
具体实施方式
以下结合实施例和附图对本发明的水溶性银微纳米晶及其可控制备方法作出进一步的详述。本发明方法所得产物的结构、形态性能分别采用场发射扫描电子显微镜(FE-SEM，SU8010)、X射线粉末衍射(XRD,D3500)和紫外-可见光谱仪(Vb300)来表征和分析。
实施例1
一种水溶性银微纳米晶的制备方法，步骤如下：
将100mL浓度为0.01mol/L的AgNO3溶液和0.2g的VC固体混合均匀，通过还原反应2min得到水溶性银微纳米晶。
实施例2
一种水溶性银微纳米晶的制备方法，步骤如下：
1)、将100mL浓度为0.01mol/L的AgNO3溶液和10mL浓度为0.2mol/L的蓝月亮洗手液LYL的水溶液混合后得到活性反应前驱体溶液。
2)、将0.4g的VC固体加入到反应前驱体溶液中，通过还原反应3min得到水溶性银微纳米晶。
实施例3
一种水溶性银微纳米晶的制备方法，步骤如下：
1)、将100mL浓度为0.01mol/L的AgNO3溶液和10mL浓度为0.2mol/L的硬脂酸微乳液ALA的水溶液混合后得到活性反应前驱体溶液。
2)、将0.4g的VC固体加入到反应前驱体溶液中，通过还原反应3min得到水溶性银微纳米晶。
实施例4
一种水溶性银微纳米晶的制备方法，步骤如下：
1)、将100mL浓度为0.01mol/L的AgNO3溶液和10mL浓度为0.4mol/L的硬脂酸微乳液ALA的水溶液混合后得到活性反应前驱体溶液。
2)、将0.6g的VC固体加入到反应前驱体溶液中，通过还原反应1min得到水溶性银微纳米晶。
实施例5
制备产物的形态结构分析：
图1为实施例1-4制备的水溶性银微纳米晶的外观形态、微观形态及化学组成。通过图1可以看出，实施例1不添加表面活性剂所制备的产物为浅黄色Ag微晶(见图1E)。采用扫描电子显微镜对上述产物进行表征可知，该实验获得的产物的形状为准球状，直径可达2μm(见图1A及图1F左上图)。XRD测试结果表明，得到的产物为Ag微纳米晶(见图2)。
实施例2利用蓝月亮洗手液LYL作为表面活性剂所制备的为浅灰色产物(见图1E)。扫描电镜观察结果表明，灰色产物形状为树枝状(见图1B及图1F右上图)。
实施例3利用硬脂酸微乳液ALA作为表面活性剂所制备的为浅黑色产物(见图1E)。扫描电镜观察结果表明，浅黑色产物形状为颗粒链状(见图1C及图1F左下图)。
最后，通过在实施例3的基础上，增大表面活性剂的添加量，实施例4所制备的产物颜色呈深黑色(见图1E)，扫描电镜观察结果表明，深黑色产物形状仍然为颗粒链状(见图1D)，较之实施例3，可以看出，随着表面活性剂的添加量的增大，所制备产物的颗粒链的尺寸逐渐变大。
基于上述实验结果，Ag微纳米晶形成过程可以看成由以下3个过程组成：
首先，VC发生氧化反应释放出电子(e)(见反应式子(1))；
接着，Ag+将与电子结合发生还原反应生成Ag0纳米颗粒(见反应式子(2))；
最后，若干Ag纳米颗粒在LYL和ALA形态控制剂作用下自组装形成各种形态Ag微纳米晶。
上述还原反应生成Ag可用下面两个式子来表示。
Ag++e→Ag0 (2)
实施例6
Ag微纳米晶的结构与可见光吸收特征。
首先，利用X衍射手段对各种颜色和形态的Ag微纳米晶产物进行物相分析并与块体Ag标准XRD衍射普(PDF，No.040783)进行比较后得知，实施例1-3所得到的准球状、树枝状和颗粒链状Ag微纳米晶物相纯度很高(见图2及图1F右下图)。
通过UV-vis.比较分析结果(见图3)可知，准球状Ag微纳米晶吸收波长约为420nm。树枝状Ag微纳米晶吸收峰有两个，分别位于310nm和420nm处。而颗粒链状Ag微纳米晶吸收峰也有两个，分别位于315nm和370nm处。Ag微纳米晶不同的光吸收特征峰与其尺寸大小和微结构有关。
以上内容仅仅是对本发明的构思所作的举例和说明，所属本技术领域的技术人员对所描述的具体实施例做各种各样的修改或补充或采用类似的方式替代，只要不偏离发明的构思或者超越本权利要求书所定义的范围，均应属于本发明的保护范围。
Claims (4)
1.一种水溶性银微纳米晶的可控制备方法，其特征在于，包括反应前驱液的配制和室温快速还原反应两个过程，首先配制硝酸银溶液，然后加入表面活性剂的水溶剂，均匀混合后，再将抗坏血酸(VC)固体加入到混合溶液中，最后在室温下通过快速还原反应得到水溶性银微纳米晶；采用硬脂酸微乳液ALA作为表面活性剂制备的水溶性银微纳米晶的微观形态呈颗粒链状。
2.如权利要求1所述的可控制备方法，其特征在于，包括如下步骤：
1）、将50-200 mL浓度为0.01-0.1 mol/L的AgNO3溶液和0-25 mL浓度为0.1-0.4 mol/L的表面活性剂的水溶液混合后得到活性反应前驱体溶液，表面活性剂的添加量不为0；
2）、将0.1-0.6 g的VC固体加入到反应前驱体溶液中，通过快速还原反应得到水溶性银微纳米晶。
3.如权利要求2所述的可控制备方法，其特征在于，快速还原反应时间为1-5 min。
4.如权利要求2所述的可控制备方法，其特征在于，步骤2）中得到的水溶性银微纳米晶溶液体系的pH值为6-7.5。
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