CN110554020A - 一种SPR在近红外的Ag-TiS2复合SERS基底及其制备方法 - Google Patents
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Abstract
本发明公开了一种SPR在近红外的Ag‑TiS2复合SERS基底及其制备方法，属于复合纳米功能材料技术领域。本发明目的是改善TiS2表面增强拉曼散射活性，获得在近红外区有较强拉曼活性的基底，本发明为Ag和TiS2的复合材料，该复合结构是将Ag和TiS2通过共溅射的方式沉积在200nm的聚苯乙烯小球六方密排阵列上获得。通过改变TiS2的溅射功率，调控Ag‑TiS2活性基底在近红外区的SPR。拉曼光谱证明Ag‑TiS2SERS活性基底的增强因子可以达到109，说明这种由半金属‑金属组成的基底具有卓越的SERS活性。
Description
技术领域
本发明属于复合纳米功能材料技术领域。
背景技术
当入射光与金属表面自由电子的运动发生共振时产生表面等离子体共振(surface plasmonresonance，SPR)。SPR自从被发现以来，主要研究集中在贵金属中，如银，金等。但是单一的纳米材料的性能具有局限性，所以复合纳米材料的研究得到了重视和发展。复合材料能够极大的改善材料本身的性能，提高材料的应用范围和价值。TiS2有类似金属的能带结构，较高的载流子浓度，迁移率和导电性能，以及在光照下产生表面等离子特性。但是TiS2很弱的表面增强拉曼散射活性限制了其在拉曼散射领域的应用，因此设计和研究Ag-TiS2复合SERS活性基底，可以拓展SERS技术理论和应用的范围。
发明内容
为了改善TiS2表面增强拉曼散射活性，获得在近红外区有较强拉曼活性的基底，本发明公开了一种SPR在近红外的Ag-TiS2表面增强拉曼散射活性基底，该基底为Ag和TiS2的复合材料，该复合结构是将Ag和TiS2通过共溅射的方式沉积在200nm的聚苯乙烯小球六方密排阵列上获得。
通过改变TiS2的溅射功率，调控Ag-TiS2活性基底在近红外区的SPR。拉曼光谱证明Ag-TiS2SERS活性基底的增强因子可以达到109，说明这种由半金属-金属组成的基底具有卓越的SERS活性。
该复合材料的制备步骤为：
(1)清洗硅片。将硅片放入烧杯中，在烧杯中分别加入体积比为1:2:6的氨水、过氧化氢和去离子水的混合溶液中。将烧杯放在烤焦台上加热至沸腾，并保持5～10min。冷却后将液体倒出，依次用去离子水，无水乙醇反复超声15min。
(2)制备六方密排的聚苯乙烯小球阵列。将直径200nm聚苯乙烯小球和无水乙醇的按照体积比为1:1混合，再通过超声处理使聚苯乙烯小球均匀分散。用移液枪将聚苯乙烯小球分散液滴在大块的硅片，使分散液均匀分布在硅片上，将大硅片缓慢倾斜的滑入液面平稳的器皿中，在水面上形成密排的聚苯乙烯小球阵列。最后用清洗后的硅片将浮在水面上的小球阵列缓慢的捞起来，吸水干燥后备用。
(3)制备活性基底。将步骤(2)中制备的带有聚苯乙烯小球阵列的基底放入磁控溅射腔体内。工作条件为：真空度2×10-4Pa，溅射气压0.6Pa，气流量为25sccm，溅射气体为纯度是99.99％的氩气。Ag的溅射速率为21.6W，TiS2的溅射功率为100W～200W，优选150W。共溅射时间为20min，溅射完成后获得SPR在近红外的Ag-TiS2表面增强拉曼散射活性基底。本发明的有益效果：
利用磁控溅射沉积技术在聚苯乙烯胶体球上共溅射制备Ag-TiS2复合纳米结构形成稳定的周期性结构阵列。制备方法简单，实验周期短，应用范围广。通过改变TiS2的溅射功率精确调控Ag-TiS2复合纳米基底在近红外的SPR吸收峰，同时Ag-TiS2复合纳米基底的表面增强拉曼散射活性会随之改变。
附图说明
图1TiS2的溅射功率为100W的Ag-TiS2复合纳米基底的SEM图像
图2TiS2的溅射功率为150W的Ag-TiS2复合纳米基底的SEM图像
图3TiS2的溅射功率为200W的Ag-TiS2复合纳米基底的SEM图像。
图4Ag-TiS2复合纳米基底的紫外吸收图谱。
图5Ag-TiS2复合纳米基底的拉曼光谱。
具体实施方式
下面以具体实施例的方式对本发明技术方案做进一步解释和说明。
(1)清洗硅片。将硅片并放入烧杯中，在烧杯中分别加入体积比为1:2:6的氨水、过氧化氢和去离子水的混合溶液中。将烧杯放在烤焦台上加热至沸腾，并保持5～10min，冷却后将液体倒出，依次用去离子水，无水乙醇反复超声15min。
(2)制备六方密排的聚苯乙烯小球阵列。直径200nm聚苯乙烯小球和无水乙醇的按照体积比为1:1混合，再通过超声处理使聚苯乙烯小球均匀分散，用移液枪将聚苯乙烯小球分散液滴在大块的硅片，使分散液均匀分布在硅片上，将大硅片缓慢倾斜的滑入液面平稳的器皿中，在水面上形成密排的聚苯乙烯小球阵列，最后用清洗后的硅片将浮在水面上的小球阵列缓慢的捞起来，吸水干燥后备用。
(3)制备活性基底。将步骤(2)制备带有聚苯乙烯小球阵列的硅片放入磁控溅射腔体内。工作条件为：真空度2×10-4Pa，溅射气压0.6Pa，气流量为25sccm，溅射气体为纯度是99.99％的氩气。Ag的溅射速率为21.6W，TiS2的溅射功率分别设定为100W、150W和200W。溅射时间为20min，溅射完成后获得SPR在近红外的Ag-TiS2表面增强拉曼散射活性基底。
Ag-TiS2复合纳米基底的形貌如图1～3所示，溅射功率不同，纳米结构的表面粗糙度不同，纳米缝隙尺寸不同，其中在TiS2溅射功率为150W的产品粗糙度最高。
用紫外吸收光谱测试Ag-TiS2复合纳米基底的吸收光谱。如图4所示，当TiS2溅射功率从100W变为200W时，SPR向近红外区红移。在图5中，SERS信号先增加在减小，在TiS2溅射功率为150W时，SERS信号最强。这是因为当激发光照射在复合纳米结构表面时，Ag-TiS2(150W)粗糙的表面和纳米缝隙产生的热点最丰富，且其的增强因子可达到109。
Claims (5)
1.一种SPR在近红外的Ag-TiS2表面增强拉曼散射活性基底，其特征在于，该基底为Ag和TiS2的复合材料，该复合结构是将Ag和TiS2通过共溅射的方式沉积在200nm的聚苯乙烯小球六方密排阵列上获得。
2.如权利要求1所述的SPR在近红外的Ag-TiS2表面增强拉曼散射活性基底的制备方法，具体步骤如下：
1)清洗硅片；
2)制备制备六方密排的聚苯乙烯小球阵列；
3)将步骤2)中制备的带有聚苯乙烯小球阵列的基底放入磁控溅射腔体内，工作条件为：真空度2×10-4Pa，溅射气压0.6Pa，气流量为25sccm，溅射气体为纯度是99.99％的氩气。Ag的溅射速率为21.6W，TiS2的溅射功率为100W～200W，共溅射时间为20min，溅射完成后获得SPR在近红外的Ag-TiS2表面增强拉曼散射活性基底。
3.根据权利要求2所述的SPR在近红外的Ag-TiS2表面增强拉曼散射活性基底的制备方法，其特征在于，
步骤1)具体步骤为：将硅片放入烧杯中，在烧杯中分别加入体积比为1:2:6的氨水、过氧化氢和去离子水的混合溶液中。将烧杯放在烤焦台上加热至沸腾，并保持5～10min。冷却后将液体倒出，依次用去离子水，无水乙醇反复超声15min。
4.根据权利要求2所述的SPR在近红外的Ag-TiS2表面增强拉曼散射活性基底的制备方法，其特征在于，
步骤2)具体步骤为：将直径200nm聚苯乙烯小球和无水乙醇的按照体积比为1:1混合，再通过超声处理使聚苯乙烯小球均匀分散。用移液枪将聚苯乙烯小球分散液滴在大块的硅片，使分散液均匀分布在硅片上，将大硅片缓慢倾斜的滑入液面平稳的器皿中，在水面上形成密排的聚苯乙烯小球阵列。最后用清洗后的硅片将浮在水面上的小球阵列缓慢的捞起来，吸水干燥后备用。
5.根据权利要求2所述的SPR在近红外的Ag-TiS2表面增强拉曼散射活性基底的制备方法，其特征在于，TiS2的溅射功率为150W。
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