CN109440104A - 超疏水表面sers基底的制备及产品和应用 - Google Patents

超疏水表面sers基底的制备及产品和应用 Download PDF

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CN109440104A
CN109440104A CN201811202166.6A CN201811202166A CN109440104A CN 109440104 A CN109440104 A CN 109440104A CN 201811202166 A CN201811202166 A CN 201811202166A CN 109440104 A CN109440104 A CN 109440104A
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sers substrate
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何丹农
卢静
李砚瑞
金彩虹
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Shanghai National Engineering Research Center for Nanotechnology Co Ltd
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Abstract

本发明涉及到一种超疏水表面SERS基底的制备及产品和应用，将硅片/玻片基底清洁处理，通过加入适量酸溶液调整质量比范围为1：1.1‑1:1.4的硝酸锌和六亚甲基四胺混合溶液的pH值至5.4‑6.2后；将处理的基片放入其中，在80‑100℃条件下油浴反应后取出，乙醇清洗后在50℃下烘干；将烘干的基底放入磁控溅射系统，沉积一定厚度的金/银纳米薄膜，即可获得有超疏水表面结构的SERS基底。本发制备的超疏水SERS基底可以在无需额外清理的条件下用于不同分子的快速检测，对SERS基底在实际环境中的应用具有重要意义。

Description

超疏水表面SERS基底的制备及产品和应用
技术领域
本发明属于表面分析和纳米结构制备领域，具体涉及到一种超疏水表面SERS基底的制备及产品和应用。
背景技术
SERS（Surface-enhanced Raman scattering）中文意义为表面增强拉曼散射。SERS技术能够用极低浓度的分子探测，因而在环境监测、食品安全、生物医药等领域具有广泛的应用。基于贵金属粒子的SERS基底制备技术近些年得到了快速发展，不同金、银纳米颗粒及复合结构的成功制备，有效提升了SERS基底的灵敏度；制备技术的发展，使得大面积均匀的SERS基底制备成为可能。但SERS基底实际检测过程中，表面会有待检测分子的残留，会影响SERS基底再次使用时的“指纹”识别特征。基于此，具有自清洁能力的疏水表面在SERS基底制备中开始受到关注。
朱利等在ZL2016101279548中提供了一种疏水表面固相单层均匀SERS基底的制备方法，主要是通过将疏水材料硅烷化后再沉积上金属纳米颗粒，该方案主要改进了金属颗粒在疏水材料表面分布不均匀问题。
而在文献报导中，不少研究人员开始将仿生结构疏水表面与SERS基底制备结合起来，极大促进了可回收SERS基底的发展。王等采用激光烧蚀的方法在硅基底上构建疏水结构后沉积银纳米薄膜，获得的具有低黏附性超疏水表面的SERS基底，可探测浓度低至10-14M的罗丹明6G溶液,在乙醇溶液中浸泡后即可重复使用（Low-adhesive superhydrophobicsurface-enhanced Raman spectroscopy substrate fabricated by femtosecond laserablation for ultratrace molecular detection，J. Mater. Chem. B, 2017,5, 777-784）。高等采用电化学沉积法，在铜箔上制备了具有疏水结构的Cu(OH)2纳米针阵列，在吸附了银纳米颗粒进一步修饰后，获得了具有再次使用前免洗特性的SERS基底。(Superhydrophobic “wash free” 3D nanoneedle array for rapid, recyclable andsensitive SERS sensing in real environment, Sensors and Actuators B 267(2018) 129–135)。
但上述制备的疏水表面SERS基底的技术方案，制备工艺复杂、可重复性较差，在批量生产和大范围内使用上存在较多问题。
发明内容
针对超疏水表面SERS基底制备技术工艺复杂、可重复性差的问题，本发明的目的在于提供一种超疏水表面SERS基底的制备方法。
本发明的再一目的在于：提供一种上述方法制备的超疏水表面SERS基底产品。
本发明的又一目的在于：提供一种上述产品的应用。
本发明目的通过下述方案实现：一种超疏水表面SERS基底的制备方法，通过在硅片/玻璃基底表面构建纳米结构ZnO形成疏水表面后溅射金/银纳米薄膜的方式得到超疏水表面SERS基底，包括如下步骤：
1）对硅片/玻璃片基底进行清洗及预处理，具体包括：用丙酮、乙醇、去离子水依次超声清洗后在浓盐酸浸泡，取出后用去离子水冲洗干净，氮气枪吹干；
2）配置生成疏水结构的反映溶液：具体包括：按1：1.1-1:1.4物质量比称取硝酸锌和六亚钾基四铵，加入去离子水后搅拌生成混合溶液，加入适量酸溶液调整缓和溶液的pH值5.4-6.2，包括5.4、5.5、5.6、5.7、5.8、5.9、6.0、6.1、6.2；
3）将步骤1）中预处理过的基底放入步骤2）所获得的混合溶液，在80-100℃油浴反应后取出，用乙醇清洗后烘干，得干燥后的基底；
4) 将步骤3）中干燥后的基底放入磁控溅射系统，溅射一定厚度的金/银纳米薄膜，即可获得超疏水表面SERS基底。
其中，步骤1）中的超声清洗时间为10分钟，浓盐酸浸泡时间不少于20分钟。
步骤2）中混合溶液中硝酸锌的浓度为1.25mM。
步骤2）中调节混合溶液pH值的酸溶液为盐酸、硝酸、硫酸、氢氟酸。
步骤3）中油浴反应时间为1.5-2小时；烘干温度控制在40-60°C。
步骤4）中金/银纳米薄膜的厚度为10-20nm。
本发明提供一种超疏水表面SERS基底，根据上述任一所述方法制备得到。
本发明提供一种超疏水表面SERS基底在拉曼检测中的应用。
与现有的技术方案相比，本发明的有益效果为：
本发明通过在硅片/玻璃基底表面构建纳米结构ZnO形成疏水表面后溅射金/银纳米薄膜的方式，获得了能够可回收使用的具有超疏水表面结构的SERS基底。该疏水SERS基底可以在无需额外清理的条件下用于不同分子的快速检测，且制备方法简单，工艺易控，对大规模制备适用于各种实际环境的疏水SERS基底具有重要作用。
附图说明
图1为实施例2交替测试罗丹明溶液（10-7mol/L）和液晶5CB分子的拉曼谱图。
具体实施方式
下面对本发明的实施例作详细说明，本实施例在以本发明技术方案为前提下进行实施，给出了详细的实施方式和具体的操作过程，但本发明的保护范围不限于下述的实施例。
实施例1
1）将购买的玻片切割为2cm*2cm的基片，用丙酮、乙醇、去离子水依次分别超声清洗10分钟取出，在浓盐酸中浸泡20分钟后取出，用去离子水冲洗干净后高纯氮气吹干备用；
2）称取0.5mmol硝酸锌和0.7mmol六亚甲基四胺,加如40mL去离子水搅拌形成混合溶液，加入适量硝酸调整溶液PH值为5.4-6.2之间，更优的为5.8；
3）将步骤1中预处理过的玻片放入步骤2中制成的混合溶液中，在80℃下油浴反应1.5小时后取出，乙醇清洗后在60°C下烘干；
4）将步骤3中干燥后的基底放入磁控溅射系统，溅射20纳米厚的银纳米薄膜。即可获得超疏水表面SERS基底。
实施例2
1）将购买的硅片切割为2cm*2cm的基片，用丙酮、乙醇、去离子水依次分别超声清洗10分钟取出，在浓盐酸中浸泡20分钟后取出，用去离子水冲洗干净后用、高纯氮气吹干备用；
2）称取0.5mmol硝酸锌和0.6mmol六亚甲基四胺,加如40mL去离子水搅拌形成混合溶液，加入适量氢氟酸调整溶液PH值在5.4-6.2之间，更优的为5.8；.
3）将步骤1中预处理过的玻片放入步骤2中制成的混合溶液中，在90℃下油浴反应2小时后取出，乙醇清洗后50℃烘干；
4）将步骤3中干燥后的基底放入磁控溅射系统，溅射15纳米厚的银纳米薄膜。即可获得超疏水表面SERS基底。
实施例3
1）将购买的玻片切割为2cm*2cm的基片，用丙酮、乙醇、去离子水依次分别超声清洗10分钟取出，在浓盐酸中浸泡20分钟后取出，用去离子水冲洗干净后用、高纯氮气吹干备用；
2）称取0.5mmol硝酸锌和0.55mmol六亚甲基四胺,加如40mL去离子水搅拌形成混合溶液，加入适量盐酸调整溶液PH值在5.4-6.2之间， 更优的为5.8；
3）将步骤1中预处理过的玻璃基底放入步骤2中制成的混合溶液中，在100℃温度的油浴中反应1.5小时后取出，乙醇清洗后40℃烘干；
4）将步骤3中干燥后的基底放入磁控溅射系统，溅射20纳米度的金纳米薄膜，即可获得超疏水表面SERS基底。
实施例4
1）将购买的硅片切割为2cm*2cm的基片，用丙酮、乙醇、去离子水依次分别超声清洗10分钟取出，在浓盐酸中浸泡20分钟后取出，用去离子水冲洗干净后用、高纯氮气吹干备用；
2）称取0.5mmol硝酸锌和0.65mmol六亚甲基四胺,加如40mL去离子水搅拌形成混合溶液，加入适量氢氟酸调整溶液PH值在5.4-6.2之间， 更优的为5.8；
3）将步骤1中预处理过的玻璃基底放入步骤2中制成的混合溶液中，在80℃温度的油浴中反应2小时后取出，乙醇清洗后60℃烘干；
4）将步骤3中干燥后的基底放入磁控溅射系统，溅射15纳米厚的金纳米薄膜，即可获得超疏水表面SERS基底。
实施例5
1）将购买的波片切割为2cm*2cm的硅片，用丙酮、乙醇、去离子水依次分别超声清洗10分钟取出，在浓盐酸中浸泡20分钟后取出，用去离子水冲洗干净后用、高纯氮气吹干备用；
2）称取0.5mmol硝酸锌和0.65mmol六亚甲基四胺,加如40mL去离子水搅拌形成混合溶液，加入适量硫酸调整溶液PH值在5.4-6.2之间，更优的为5.8；
3）将步骤1中预处理过的玻璃基底放入步骤2中制成的混合溶液中，在85℃下油浴中1.5小时后取出，乙醇清洗后50℃烘干。
4）将步骤3中干燥后的基底放入磁控溅射系统，溅射10纳米厚的银纳米薄膜。即可获得超疏水表面SERS基底。
实施例6
将购买的硅片切割为2cm*2cm的硅片，用丙酮、乙醇、去离子水依次分别超声清洗10分钟取出，在浓盐酸中浸泡20分钟后取出，用去离子水冲洗干净后用、高纯氮气吹干备用；
2）称取0.5mmol硝酸锌和0.55mmol六亚甲基四胺,加如40mL去离子水搅拌形成混合溶液，加入适量氢氟酸调整溶液PH值在5.4-6.2之间， 更优的为5.8；
3）将步骤1中预处理过的玻璃基底放入步骤2中制成的混合溶液中，在85℃下油浴反应2小时后取出，乙醇清洗后50℃下烘干。
4） 将步骤3中干燥后的基底放入磁控溅射系统，溅射10纳米厚的金纳米薄膜，即可获得超疏水表面SERS基底。

Claims (9)

1.一种超疏水表面SERS基底的制备方法，通过在硅片/玻璃基底表面构建纳米结构ZnO形成疏水表面后溅射金/银纳米薄膜的方式得到超疏水表面SERS基底，包括如下步骤：
1) 对硅片/玻璃片基底进行清洗及预处理，包括：用丙酮、乙醇、去离子水依次超声清洗后在浓盐酸浸泡，取出后用去离子水冲洗干净，氮气枪吹干；
2)配置生成疏水结构的反映溶液，包括：按质量比范围为1：1.1-1:1.4称取硝酸锌和六亚钾基四铵，加入去离子水后搅拌生成混合溶液，加入适量酸溶液调整混合溶液的pH值至5.4-6.2；
3)将步骤1）中预处理过的基底放入步骤2）获得的混合溶液中，在80-100℃油浴反应后取出，用乙醇清洗后烘干，得干燥后的基底；
4)将步骤3）干燥后的基底放入磁控溅射系统，溅射一定厚度的金/银纳米薄膜，即可获得超疏水表面SERS基底。
2.根据权利要求1所述的制备方法，其特征在于步骤1）中的超声清洗时间为10分钟，浓盐酸浸泡时间不少于20分钟。
3.根据权利要求1所述的制备方法，其特征在于步骤2）中，所述的混合溶液中硝酸锌的浓度为1.25mM。
4.根据权利要求1或3所述的制备方法，其特征在于步骤2）中调节混合溶液pH值的酸溶液为盐酸、硝酸、硫酸、氢氟酸。
5.根据权利要求4所述的制备方法，调整混合溶液的pH值至5.8。
6.根据权利要求1所述的制备方法，其特征在于：步骤3）中油浴反应时间为1.5-2小时；烘干温度控制在40-60°C。
7.根据权利要求1所述的制备方法，其特征在于：步骤4）中金/银纳米薄膜的厚度为10-20nm。
8.一种超疏水表面SERS基底，其特征在于根据权利要求1-7任一所述方法制备得到。
9.一种根据权利要求8所述超疏水表面SERS基底在拉曼检测中的应用。
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