CN110687098B - 一种基于聚氨酯的纳米银sers基底的制备方法 - Google Patents

一种基于聚氨酯的纳米银sers基底的制备方法 Download PDF

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CN110687098B
CN110687098B CN201911045971.7A CN201911045971A CN110687098B CN 110687098 B CN110687098 B CN 110687098B CN 201911045971 A CN201911045971 A CN 201911045971A CN 110687098 B CN110687098 B CN 110687098B
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陈国庆
陈律铭
朱纯
马超群
李磊
辜蛟
朱焯炜
高辉
吴亚敏
杨子晨
朱拓
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Abstract

本发明公开了一种基于聚氨酯的纳米银SERS基底的制备方法，属于拉曼光谱技术领域。为了解决SERS基底制备过程复杂、灵敏度底等问题。该方法使用固化后的聚氨酯作为骨架，利用多孔表面结构以及吸附性，将纳米银颗粒吸附在其表面上，得到以结晶紫为探针分子的检测限低至10‑10M的SERS基底。该方法所制备的SERS基底，表面积大，吸附的目标分子数量多，基底易制备，灵敏度高，有利于SERS的定性定量分析。

Description

一种基于聚氨酯的纳米银SERS基底的制备方法
技术领域
本发明涉及一种基于聚氨酯的纳米银SERS基底的制备方法，属于拉曼光谱技术领域。
背景技术
拉曼光谱是识别生物分子最常用的振动光谱。拉曼光谱能提供有价值的信息，在生化分析中具有很大的潜力。此外，这是一种不需要对食品样品进行任何预处理的无损检测技术。由于水的存在不会干扰液体样品的分析，拉曼光谱是识别水样品中所需目标分析物的简单方法。表面增强拉曼散射(SERS)是一种很有应用前景的方法，该方法的灵敏度极高，甚至可以区分检测单个分子，与化学效应相比，电磁效应是增强拉曼信号的一个重要原理，由于局域表面等离子体共振(LSPR)的激发，在粗糙表面附近激发的大量的局部电磁场，对SERS的性能有着显著的影响。具有纳米结构的金属材料具有强烈的SPR效应、生物相容性和高的化学和热稳定性，被认为是SERS检测的可靠材料。高分子材料由于其可靠的稳定性，逐渐成为制作SERS基底的重要材料，但目前公开的利用高分子材料制备SERS基底的技术中，往往制备过程繁琐，因此，提供一种制备方法简单且检测性能优越的SERS基底是非常有必要的。
发明内容
本发明提供了一种基于聚氨酯的纳米银SERS基底的制备方法，本发明以简单易得的聚氨酯为衬底材料，使用固化后的聚氨酯作为骨架，利用其多孔表面性质以及吸附性，将纳米银颗粒吸附在其表面上，得到基于聚氨酯的纳米银SERS基底。
本发明的技术方案如下：
一种基于聚氨酯的纳米银SERS基底的制备方法，包括以下步骤：
(a)使用柠檬酸钠还原硝酸银，制备纳米银溶液；
(b)将聚氨酯A胶与聚氨酯B胶混合后搅拌均匀，静置发泡固化；
(c)将发泡固化后的聚氨酯切成小块浸泡在纳米银溶液中，得到基于聚氨酯的纳米银SERS基底。
在一种实施方式中，所述步骤(a)中，柠檬酸钠溶液的浓度为0.01g/mL。
在一种实施方式中，所述步骤(a)中，硝酸银溶液浓度为200mg/L。
在一种实施方式中，所述步骤(b)中，聚氨酯A胶的成分为异氰酸酯，聚氨酯B胶的成分为组合聚醚。
在一种实施方式中，所述步骤(b)中，聚氨酯A胶与聚氨酯B胶按质量比为1:1混合。
在一种实施方式中，所述步骤(b)中，发泡固化的温度为室温下固化，时间约为2～6h。
在一种实施方式中，所述步骤(c)中，聚氨酯块在纳米银溶液中的浸泡时间为6h以上。
本发明的有益效果：
1、本发明制备出的基于聚氨酯的纳米银SERS基底，能够为SERS信号的测量提供多孔表面结构，并吸附待测目标分子；
2、纳米银颗粒具有表面等离子体共振性能，起到增强拉曼信号的作用；
3、将海绵状的聚氨酯、纳米银结合使用，使其SERS增强优于单独使用聚氨酯或纳米银颗粒，以结晶紫为探针分子的检测限低至10-10M；
4、该方法所制备的SERS基底，表面积大，吸附的目标分子数量多，基底制备工艺简单，灵敏度高，有利于SERS的定性定量分析。
附图说明
图1为制备聚氨酯纳米银SERS基底的流程图。
图2为聚氨酯纳米银基底对不同浓度的CV水溶液的SERS光谱图。
图3为不同浓度的CV水溶液的拉曼光谱图。
图4为不含纳米银的聚氨酯对不同浓度的CV水溶液的SERS光谱图。
图5为纳米银溶液对不同浓度的CV水溶液的SERS光谱图。
图6为使用PDMS代替聚氨酯制备基底对不同浓度的CV水溶液的SERS光谱图。
具体实施方式
本发明使用的聚氨酯A胶和聚氨酯B胶购于博盛科技，聚氨酯A胶的成分为异氰酸酯，聚氨酯B胶的成分为组合聚醚。
实施例1
本发明制备聚氨酯纳米银SERS基底的流程图，如图1所示。
1、制备聚氨酯纳米银SERS基底
(1)使用柠檬酸钠还原硝酸银制备纳米银溶液
a.配制浓度为0.01g/ml的柠檬酸钠水溶液，200mg/L的硝酸银水溶液；
b.取100ml硝酸银溶液，加热至沸腾。迅速滴加3ml柠檬酸钠溶液，边加边搅拌，冷却至室温。
(2)制备聚氨酯
a.取5g聚氨酯A胶与5g聚氨酯B胶，迅速剧烈搅拌；
b.置于室温下2～6h，切成小块后备用。
(3)制备聚氨酯纳米银SERS基底
a.将切好的聚氨酯小块浸泡在制备好的纳米银溶液中，聚氨酯会吸附溶液中的纳米银颗粒；
b.聚氨酯块需在纳米应溶液中浸泡6h以上。
2、使用聚氨酯纳米银基底对不同浓度的CV水溶液进行拉曼测试
使用结晶紫(CV)作为拉曼探针，配制浓度分别为10-10、10-9、10-8、10-7、10-6、10-5、10-4、10-3、10-2摩尔每升的结晶紫(CV)水溶液。将制备好的聚氨酯纳米银基底浸入结晶紫水溶液中数分钟，取出基底后，使用inVia共聚焦拉曼光谱仪获得拉曼光谱，激光光源532nm，功率12.5mw，物镜50倍长焦，曝光时间20s。光束通过显微镜的×50物镜聚焦在样品上，并从滤波片经由每毫米1800刻线的衍射光栅分光后进入到CCD中，拉曼光谱如图2所示，随着浓度的降低，CV的特征峰强度逐渐降低。当CV水溶液的浓度低至10-10摩尔每升时，仍然可以观察到CV的特征峰。
对比例1
直接使用拉曼方法对不同浓度的CV水溶液进行拉曼测试，得到不同浓度的CV水溶液的拉曼光谱图。使用inVia共聚焦拉曼光谱仪获得拉曼光谱，激光光源532nm，功率12.5mw，物镜50倍长焦，曝光时间20s。光束通过显微镜的×50物镜聚焦在样品上，并从滤波片经由每毫米1800刻线的衍射光栅分光后进入到CCD中。如图3所示，随着浓度的降低，CV的特征峰强度逐渐降低。当CV水溶液的浓度低至10-5摩尔每升时，CV的特征峰已经不明显，说明直接使用拉曼方法测试CV水溶液，检测限只能达到10-5摩尔每升。
对比例2
使用没有纳米银溶液中浸泡的固化好的聚氨酯，对不同浓度的CV水溶液进行拉曼测试。将制备好的聚氨酯块浸入结晶紫水溶液中数分钟，取出聚氨酯后，使用inVia共聚焦拉曼光谱仪获得拉曼光谱得到不含纳米银的聚氨酯对不同浓度的CV水溶液的SERS光谱图。如图4所示，随着浓度的降低，CV的特征峰强度逐渐降低。虽然浓度较高时SERS光谱强度较CV水溶液的拉曼光谱有所提高，但当CV水溶液的浓度低至10-5摩尔每升时，CV的特征峰已经不明显。说明没有纳米银颗粒的聚氨酯基底，SERS检测限的提高没用贡献。
对比例3
使用纳米银溶液对不同浓度的CV水溶液进行拉曼测试，将制备好的纳米银溶液与CV水溶液以体积比1：1混合，使用inVia共聚焦拉曼光谱仪获得拉曼光谱，得到纳米银溶液对不同浓度的CV水溶液的SERS光谱图。如图5所示，随着浓度的降低，CV的特征峰强度逐渐降低。当CV水溶液的浓度低至10-6摩尔每升时，CV的特征峰已经不明显。说明了仅使用纳米银溶液作为基底，只能将检测限提高一个数量级。
对比例4
使用高分子材料聚二甲基硅氧烷(PDMS)来替代聚氨酯材料，将固化好的PDMS浸入纳米银溶液中浸泡6h，浸入不同浓度的结晶紫水溶液中数分钟，取出基底使用inVia共聚焦拉曼光谱仪获得拉曼光谱，得到基于高分子材料PDMS的纳米银基底对CV水溶液的SERS光谱图。如图6所示，随着浓度的降低，CV的特征峰强度逐渐降低。当CV水溶液的浓度低至10-6摩尔每升时，CV的特征峰已经不明显。而且PDMS本身具有自己的特征峰，会对CV水溶液的特征峰的观测产生干扰。说明了仅使用PDMS代替聚氨酯作为基底，效果不如聚氨酯纳米银SERS基底。
通过实施例1与对比文件2、3、4的对比可知，本发明中的聚氨酯纳米银基底当CV水溶液的浓度低至10-10摩尔每升时，仍然可以观察到CV的特征峰，说明了聚氨酯纳米银基底对CV的增强系数达到105以上，明显优于只使用纳米银溶液或只是用聚氨酯，或者使用其他的高分子材料。
虽然本发明已以较佳实施例公开如上，但其并非用以限定本发明，任何熟悉此技术的人，在不脱离本发明的精神和范围内，都可做各种的改动与修饰，因此本发明的保护范围应该以权利要求书所界定的为准。

Claims (10)

1.一种纳米银SERS基底的制备方法，其特征在于，该方法包括如下步骤：
将聚氨酯A胶与聚氨酯B胶混合后搅拌均匀，静置发泡固化；
将发泡固化后的聚氨酯切成小块浸泡在纳米银溶液中，得到基于聚氨酯的纳米银SERS基底。
2.根据权利要求1所述的制备方法，其特征在于，所述纳米银溶液的制备是：使用柠檬酸钠还原硝酸银，制备纳米银溶液；其中柠檬酸钠溶液的浓度为0.01g/mL，硝酸银溶液浓度为200mg/L。
3.根据权利要求1所述的制备方法，其特征在于，所述聚氨酯A胶与聚氨酯B胶按质量比为1:1混合。
4.根据权利要求1所述的制备方法，其特征在于，所述发泡固化的温度为室温下固化，时间为2～6h。
5.根据权利要求1所述的制备方法，其特征在于，所述聚氨酯块在纳米银溶液中的浸泡时间为6h以上。
6.按权利要求1-5任一项所述方法制备的基于聚氨酯的纳米银SERS基底。
7.一种检测结晶紫CV的方法，其特征在于，所述方法是利用权利要求6所述的基于聚氨酯的纳米银SERS基底。
8.根据权利要求7所述的方法，其特征在于，将制备好的聚氨酯纳米银基底浸入结晶紫水溶液中数分钟，取出基底后，使用inVia共聚焦拉曼光谱仪获得拉曼光谱，激光光源532nm，功率12.5mw，物镜50倍长焦，曝光时间20s。
9.权利要求6所述的基于聚氨酯的纳米银SERS基底在拉曼光谱技术领域的应用。
10.权利要求6所述的基于聚氨酯的纳米银SERS基底在无损检测技术领域的应用。
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