CN101408513A - 表面规则凹凸起伏的样品台及其制作方法 - Google Patents
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Abstract
表面规则凹凸起伏的样品台及其制作方法属于SERS(表面增强拉曼光谱)检测技术领域。现有技术采用真空金属溅射的方式在样品台基板上形成规则分布的探针，需要采用昂贵的设备，操作过程需要精确控制。本发明之表面规则凹凸起伏的样品台的结构为，在平面基板上格状分布粒度在150～250nm范围的球状物，球状物表面有金属镀层，所有球状物背离基板一侧的表面共同构成样品台规则凹凸起伏表面。制作方法是将样品台基板水平放置于盛有挥发性溶剂的容器底部，倒入粒度在150～250nm范围的球状物，静置直至溶剂完全挥发，球状物自然沉积在基板上并呈格状分布，将容器放入镀液中，在球状物表面形成金属镀层。应用于SERS检测技术领域。
Description
技术领域
本发明涉及一种表面规则凹凸起伏的样品台及其制作方法，应用于SERS(表面增强拉曼光谱)检测，属于SERS(表面增强拉曼光谱)检测技术领域。
背景技术
根据不同物质拉曼光谱也不同这一现象，拉曼光谱检测技术被用来进行物质检测。然而，由于拉曼散射强度非常弱，当检测微量的物质时必须进行散射增强，所采取的措施就是表面增强，于是SERS(表面增强拉曼光谱)检测技术诞生。所谓表面增强就是处理样品台表面，从而提高散射强度。现有处理样品台表面的技术方案是，在超高真空系统中采用电子溅射的方式将金属颗粒如颗粒银溅射到平面基板上，在这一过程中，金属蒸汽中的纳米级金属颗粒沿晶格方向在基板上生长，最终在基板上形成规则分布的探针。这一措施使得拉曼光谱检测技术达到ng的量级，应用于腐蚀、催化的中间产物的检测，金属及热分解过程分析，毒品的鉴定，蔬菜、水果表面农药残留的检测，墨迹中微量成分的分析等。
发明内容
所述现有技术需要采用昂贵的设备，操作过程需要精确控制溅射浓度、溅射时间、溅射方向倾斜角、电场强度等参数，否则要么处理欠缺，不能实现表面增强，要么处理过度，探针长平，同样未能实现表面增强，还会出现探针长歪、分布不规则，降低增强效果的情况。为了实现SERS检测技术所采用的样品台表面处理的简易化，我们提出了一项称为表面规则凹凸起伏的样品台及其制作方法的技术方案。
本发明之表面规则凹凸起伏的样品台的结构为，在平面基板上格状分布粒度在150～250nm范围的球状物，球状物表面有金属镀层，所有球状物背离基板一侧的表面共同构成样品台规则凹凸起伏表面。
本发明之表面规则凹凸起伏的样品台的制作方法为，将样品台基板水平放置于盛有挥发性溶剂的容器底部，倒入粒度在150～250nm范围的球状物，静置直至溶剂完全挥发，球状物自然沉积在基板上并呈格状分布，将容器放入镀液中，在球状物表面形成金属镀层。
上述技术方案的技术效果表现在，只需采用常规的器具和普通的化工技术即可完成具有表面增强效果的SERS检测技术所需的样品台的制作。采用本发明之样品台用于构成脱氧核糖核酸的四种碱基腺嘌呤、胞嘧啶、鸟嘌呤、胸腺嘧啶的SERS检测，获得了各自具有明显特征谱峰的拉曼光谱图，不仅能够判断碱基混合物中碱基的种类，还能够根据特征谱峰强度判断每种碱基的含量。
附图说明
图1本发明之表面规则凹凸起伏的样品台局部表面形态示意图，该图兼作为摘要附图。图2是腺嘌呤(adenine，A)拉曼光谱图。图3是鸟嘌呤(guanine，G)拉曼光谱图。图4是胞嘧啶(cytosine，C)拉曼光谱图。图5是胸腺嘧啶(thymine，T)拉曼光谱图。图6是腺嘌呤(adenine，A)、鸟嘌呤(guanine，G)、胞嘧啶(cytosine，C)和胸腺嘧啶(thymine，T)拉曼光谱对比图。
具体实施方式
本发明之表面规则凹凸起伏的样品台的结构为，在平面基板上格状分布粒度在150～250nm范围的球状物，平面基板材料为玻璃，球状物材料为聚苯乙烯或者聚丙烯，表面金属镀层为银层或者金层，所有球状物背离基板一侧的表面共同构成样品台规则凹凸起伏表面，见图1所示。
本发明之表面规则凹凸起伏的样品台的制作方法为，将样品台基板水平放置于盛有挥发性溶剂的容器底部，所述挥发性溶剂采用无水乙醇，倒入粒度在150～250nm范围的球状物，静置直至溶剂完全挥发，球状物自然沉积在基板上并呈格状分布，将容器放入镀液中，所述镀液采用硝酸银，浓度为10～20％(wt)，经光照硝酸银分解，分解出的银沉积在球状物表面上，形成金属镀层，光照时间为30～60秒，金属镀层的厚度在80～120nm范围内。
采用本发明之样品台用于构成脱氧核糖核酸的四种碱基腺嘌呤、胞嘧啶、鸟嘌呤、胸腺嘧啶的SERS检测，采用功率为200mW、波长为514.5nm的氩离子激光为光源，获得了各自具有明显特征谱峰的拉曼光谱图，见图2～5所示，从图中可以看出，腺嘌呤(adenine，A)的特征谱峰在722.3cm-1和1331.8cm-1波数处，胞嘧啶(cytosine，C)的特征谱峰在792.7cm-1和1275.6cm-1波数处，鸟嘌呤(guanine，G)的特征谱峰在649.9cm-1、1267.2cm-1和1360.1cm-1波数处，胸腺嘧啶(thymine，T)的特征谱峰在617.7cm-1、983.7cm-1和1368.6cm-1波数处。四种碱基的特征谱峰并没有出现重叠，见图6所示，据此完全可以鉴别出这四种碱基，并且每种碱基的谱峰强度又与各自的含量相关，所以还可以测出每种碱基的含量。
Claims (8)
1、一种表面规则凹凸起伏的样品台，其特征在于，在平面基板上格状分布粒度在150～250nm范围的球状物，球状物表面有金属镀层，所有球状物背离基板一侧的表面共同构成样品台规则凹凸起伏表面。
2、根据权利要求1所述的表面规则凹凸起伏的样品台，其特征在于，平面基板材料为玻璃。
3、根据权利要求1所述的表面规则凹凸起伏的样品台，其特征在于，球状物材料为聚苯乙烯或者聚丙烯。
4、根据权利要求1所述的表面规则凹凸起伏的样品台，其特征在于，表面金属镀层为银层或者金层。
5、一种表面规则凹凸起伏的样品台的制作方法，其特征在于，将样品台基板水平放置于盛有挥发性溶剂的容器底部，倒入粒度在150～250nm的球状物，静置直至溶剂完全挥发，球状物自然沉积在基板上并呈格状分布，将容器放入镀液中，在球状物表面形成金属镀层。
6、根据权利要求5所述的表面规则凹凸起伏的样品台的制作方法，其特征在于，所述挥发性溶剂采用无水乙醇。
7、根据权利要求5所述的表面规则凹凸起伏的样品台的制作方法，其特征在于，所述镀液采用硝酸银，浓度为10～20％(wt)，经光照硝酸银分解，分解出的银沉积在球状物表面上，形成金属镀层，光照时间为30～60秒。
8、根据权利要求7所述的表面规则凹凸起伏的样品台的制作方法，其特征在于，金属镀层的厚度在80～120nm范围内。
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Cited By (9)
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| CN102759520A (zh) * | 2012-05-14 | 2012-10-31 | 北京化工大学 | 一种具有表面增强拉曼散射效应的活性基底的制备方法 |
| CN103213938A (zh) * | 2013-04-16 | 2013-07-24 | 上海大学 | 金纳米帽阵列表面增强拉曼活性基底及其制备方法 |
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