CN114990494B - 一种金纳米层包覆银纳米棒阵列的松塔结构sers基底及其制备方法 - Google Patents
一种金纳米层包覆银纳米棒阵列的松塔结构sers基底及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种金纳米层包覆银纳米棒阵列的松塔结构SERS基底及其制备方法,属于纳米技术领域。该SERS基底的制备方法包括:利用倾斜角沉积技术制备均一性和重复度高的银纳米棒阵列结构,再通过动态阴影沉积技术蒸镀不同厚度的金纳米层,获得不同形貌的金层包覆银纳米棒阵列的“松塔”结构SERS基底。该SERS基底具有更好的化学稳定性和更高的SERS活性,比单一金属结构检测更有优势。本发明的“松塔”结构SERS基底具有十分优异的表面增强拉曼散射能力,制备过程简单、灵敏度高、增强效果显著、可修饰性及可重复性强、可大规模生产。
Description
技术领域
本发明属于纳米技术领域,涉及一种生化检测芯片,具体涉及一种金纳米层包覆银纳米棒阵列的松塔结构SERS基底及其制备方法。
背景技术
表面增强拉曼光谱(SERS)通过激发局域表面等离子体激元放大电磁场,从而获得分子结构信息以及灵敏的检测限。SERS技术被广泛认为是一种可以提供分子指纹信息的一种分析表征技术,主要是由于粗糙贵金属表面等离子体共振促使拉曼信号指数式增强的现象,其增强机制归因于电磁增强和化学增强。因为SERS具有灵敏度高、水干扰小、速度快等优点,这使得SERS技术成为时下研究热门,并在生物医学、食品安全以及环境监测等众多领域得到应用。然而,SERS技术和其他技术一样,既有它的优势也存在灵敏度不高、稳定性差等问题,研究者们尝试从新型SERS活性基底方面弥补其缺点和不足,拓宽SERS的应用范围。
发明内容
本发明的目的之一是提供一种金纳米层包覆银纳米棒阵列的松塔结构SERS基底的制备方法,工艺简单可靠。
本发明的目的之二是提供上述制备方法制得的金纳米层包覆银纳米棒阵列的松塔结构SERS基底,进行痕量物质检测时灵敏度高。
为实现上述目的,本发明采用的技术方案如下:
第一方面,本发明提供一种金纳米层包覆银纳米棒阵列的松塔结构SERS基底的制备方法,包括以下步骤:
(1)在电子束蒸发系统中,利用倾斜角沉积技术在洁净的玻璃片上制备银纳米棒阵列结构;
(2)利用动态阴影沉积效应在步骤(1)制备的银纳米棒阵列上蒸镀不同厚度的金纳米层;
(3)定量检测。
优选的,步骤(1)具体步骤如下:将玻璃片按设备要求尺寸进行切割,超声清洗后固定在沉积室中,对沉积室抽真空使内部压力小于5×10-7Torr;通过电子束蒸发系统,的沉积速率,先后沉积一层20nm钛薄膜和100-200nm银薄膜,然后旋转样品台使得基底法线与沉积方向夹角为85-87°,通过电子束蒸发,以0.1-0.3nm/s的速度生长实际棒长为990nm的银纳米棒阵列。
更优选的,所述超声清洗的步骤是:将切割后的玻璃片加入乙醇中,超声波清洗3-5min,重复三次,氮气吹干。
优选的,步骤(2)具体步骤如下:设置蒸汽源入射角度相对于样品台法线为θ=86°,以速率为0.05-0.1nm/s生长不同厚度的金纳米层,沉积开始时样品台面自转角度ψ启用,自转速率为1°/s。
优选的,步骤(3)具体步骤如下:设置激光波长、功率、积分时间,对基底上被测物进行扫描,得到的表面增强拉曼光谱中某处特征峰不随被测物浓度改变而受到影响,此特征峰即作为定量检测的参考峰。
第二方面,本发明还提供上述制备方法制得的金纳米层包覆银纳米棒阵列的松塔结构SERS基底。
通过SEM电镜分析,该SERS基底表面具有不同厚度的金纳米层和均匀分布的银纳米棒阵列结构。该“松塔”结构SERS基底具有十分优异的表面增强拉曼散射能力,检测限低,灵敏度高。
与现有技术相比,本发明具有如下有益效果:
1.制备过程简单、灵敏度高、增强效果显著、可修饰性及可重复性强、可大规模生产,且能检测较低浓度的探针分子,显示其较高灵敏度。
2.本发明制备的周期性纳米复合阵列结构是一种新颖的等离子体结构,相邻的金银结构单元间的间隙能构成“热点”,从而提高耦合能力,大幅度增强SERS效应。而金纳米层结构大大增加了提供的化学吸附的表面位点,这也显著的增强了SERS信号,从而提高SERS检测灵敏度。
附图说明
图1是本发明金纳米层包覆银纳米棒“松塔”结构的SERS基底的制备示意图;
图2是本发明金纳米层包覆银纳米棒“松塔”结构的扫描电子显微镜照片。其中,A是该复合基底的俯视图,B是该复合基底的截面图,右侧均为高倍率放大图;
图3是本发明金纳米层包覆银纳米棒“松塔”结构检测不同浓度BPE分子的表面增强拉曼图谱;
图4是本发明金纳米层包覆银纳米棒“松塔”结构检测BPE的浓度与强度的工作曲线;
图5是本发明金纳米层包覆银纳米棒“松塔”结构检测不同浓度BaP分子的表面增强拉曼图谱;
图6是本发明金纳米层包覆银纳米棒“松塔”结构检测BaP的浓度与强度的工作曲线。
具体实施方式
下面将结合本发明实施例中的附图,对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
实施例1
步骤一,将玻璃片切割成0.8cm×0.8cm,放入乙醇中,再转移到超声波清洗机中清洗5min,重复三次,氮气吹干后固定在沉积室中;在压力小于5×10-7Torr真空沉积室中,通过电子束蒸发系统,利用倾斜角沉积技术在清洗干净的玻璃片上先后以0.2nm/s和0.3nm/s的速率沉积一层20nm的钛薄膜和一层100nm的银薄膜,然后旋转样品台使得基底法线与沉积方向夹角为86°,通过电子束蒸发,以0.3nm/s的速度生长实际棒长为990nm的银纳米棒阵列。
步骤二,设置蒸汽源入射角度相对于样品台法线为θ=86°,利用动态阴影沉积效应在银纳米棒阵列上以速率为0.05nm/s生长150nm金纳米层,沉积开始时样品台面自转角度ψ启用,自转速率为1°/s;以上参数均为机器端设置参数,且该速率与膜厚由石英晶体微天平在镀膜过程中实时监控。
步骤三,定量检测,选定激光波长为785nm、功率30mw、积分时间10s,以目的产物为SERS活性基底对不同浓度的BPE(反式1,2-双(4-吡啶基)乙烯)进行检测,得到一系列BPE的表面增强拉曼光谱图,并确定其检出限。
测试例1:电子显微镜扫描
对实施例1得到的金纳米层包覆银纳米棒“松塔”结构SERS基底进行扫描电子显微镜观察,得到表征结果如图2所示。其中金纳米层包覆于银纳米棒尖处,利用Image J计算出纳米棒的直径约为D=64±10nm,两个相邻棒之间的距离为l=78±10nm,纳米棒的长度为L=1100±50nm,所得的纳米复合结构的生长方向为68±2°。
测试例2:对BPE的检测应用分析
将一定量浓度范围为1×10-11~1×10-6M的BPE滴定于实施例1得到的金纳米层包覆银纳米棒“松塔”结构SERS基底表面,静置吸附,在空气中自然干燥后,利用光谱仪进行SERS性能测试,得到如图3和图4的拉曼光谱仪表征结果。图3为该复合结构对不同浓度BPE分子的表面增强拉曼图谱。图4为在1200cm-1特征峰处峰值强度与溶液浓度的线性拟合曲线,说明该复合基底的灵敏度高,可以检测到10-13M BPE。
实施例2
步骤一,将玻璃片切割成0.8cm×0.8cm,加入乙醇中,再转移到超声波清洗机中清洗5min,重复三次,氮气吹干后固定在沉积室中;在压力小于5×10-7Torr真空沉积室中,通过电子束蒸发,利用倾斜角沉积技术在清洗干净的玻璃片上先后以0.2nm/s和0.3nm/s的速率沉积一层20nm的钛薄膜和一层100nm的银薄膜,然后旋转样品台使得基底法线与沉积方向夹角为86°,通过电子束蒸发,以0.3nm/s的速度生长实际棒长为990nm的银纳米棒阵列。
步骤二,设置蒸汽源入射角度相对于样品台法线为θ=86°,利用动态阴影沉积效应在银纳米棒阵列上以速率为0.05nm/s生长150nm金纳米层,沉积开始时样品台面自转角度ψ启用,自转速率为1°/s;以上参数均为机器端设置参数,且该速率与膜厚由石英晶体微天平在镀膜过程中实时监控。
步骤三,定量检测,选定激光波长为785nm、功率30mw、积分时间10s,以目的产物为SERS活性基底对不同浓度的BaP(苯并芘)进行检测,得到一系列BaP的表面增强拉曼光谱图,确定其检出限。
测试例1:对BaP的SERS检测
为了进一步探索“松塔”结构基底检测方法的通用性以及其SERS性质,使用该基底检测不同浓度的BaP溶液。图5光谱中,不同浓度BaP水溶液在“松塔”结构上获得的SERS光谱特征峰位基本一致,即使在低浓度的情况下,BaP的主要特征峰也没用发生明显的偏移情况,这表明了“松塔”结构不会对BaP分子造成分子结构的改变。如图6所示,当BaP水溶液浓度为1-100ppb这一浓度范围时,特征峰1234cm-1均可被检出,随着浓度的降低,AuNL@AgNR“松塔”结构上存在的BaP分子就越少,因此探测器捕捉到的BaP分子指纹信息就相对减少,故得到的SERS特征峰强度也逐渐减小,这一现象表明浓度与峰强之间存在着一种线性递增的关系。1-100ppb浓度范围内,位于1234cm-1特征峰处峰值强度与BaP溶液浓度的关系为,I1234=0.352CBaP+15.341,R2=0.973,基于拉依达原则得知BaP水溶液的LOD为1ppb,其满足了环境污染物中BaP检测需求。表明“松塔”结构对BaP检测的高灵敏度。
以上所述仅仅是本发明的优选实施方案,应当指出,对于本技术领域的普通技术人员来说,在不脱离本发明原理的前提下,还可以做出若干改进和润饰,这些改进和润饰也应视为本发明的保护范围。
Claims (5)
1.一种金纳米层包覆银纳米棒阵列的松塔结构SERS基底的制备方法,其特征在于,包括以下步骤:
(1)在电子束蒸发系统中,利用倾斜角沉积技术在洁净的玻璃片上制备银纳米棒阵列结构;
(2)利用动态阴影沉积效应在步骤(1)制备的银纳米棒阵列上蒸镀不同厚度的金纳米层;具体步骤如下:设置蒸汽源入射角度相对于样品台法线为θ = 86°,以速率为0.05 -0.1 nm/s生长不同厚度的金纳米层,沉积开始时样品台面自转角度ψ启用,自转速率为1°/s;
(3)定量检测。
2.根据权利要求1所述的一种金纳米层包覆银纳米棒阵列的松塔结构SERS基底的制备方法,其特征在于,步骤(1)具体步骤如下:将玻璃片按设备要求尺寸进行切割,超声清洗后固定在沉积室中,对沉积室抽真空使内部压力小于5×10-7 Torr;通过电子束蒸发系统,在清洗干净的玻璃片上以0.1 - 0.3 nm/s的沉积速率,先后沉积一层20 nm钛薄膜和100 -200 nm银薄膜,然后旋转样品台使得基底法线与沉积方向夹角为85-87°,通过电子束蒸发,以0.1 - 0.3 nm/s的速度生长实际棒长为990 nm的银纳米棒阵列。
3.根据权利要求2所述的一种金纳米层包覆银纳米棒阵列的松塔结构SERS基底的制备方法,其特征在于,所述超声清洗的步骤是:将切割后的玻璃片加入乙醇中,超声波清洗3-5min,重复三次,氮气吹干。
4.根据权利要求1所述的一种金纳米层包覆银纳米棒阵列的松塔结构SERS基底的制备方法,其特征在于,步骤(3)具体步骤如下:设置激光波长、功率、积分时间,对基底上被测物进行扫描,得到的表面增强拉曼光谱中某处特征峰不随被测物浓度改变而受到影响,此特征峰即作为定量检测的参考峰。
5.权利要求1至4任一项所述的制备方法制得的金纳米层包覆银纳米棒阵列的松塔结构SERS基底。
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