CN111650177B - 一种实现单分子探测的碲化镓基表面增强拉曼基底及其制备方法 - Google Patents
一种实现单分子探测的碲化镓基表面增强拉曼基底及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种实现单分子探测的碲化镓基表面增强拉曼基底及其制备方法,基底结构从下至上依次为Au孔阵列层,二维薄层GaTe层和Au纳米颗粒层,本发明在SiO2/Si基底层上,通过热蒸发的方法生长Ti层或Cr层,利用光刻和微纳加工方法制备Au孔阵列层,利用机械剥离的方法制备二维薄层GaTe层,并利用转移平台转移到Au孔阵列层上,最后将基底浸没在HAuCl4溶液中制备Au纳米颗粒层。本发明得益于GaTe材料较高的缺陷密度,在二维薄层GaTe层上自组装形成的金纳米颗粒层覆盖率能达到98%,此基底对R6G分子的最低探测浓度达到10‑16M,超过了绝大部分的表面增强拉曼散射基底,具有较好的稳定性和可重复性,具有实用化前景。
Description
技术领域
本发明专利涉及一种基底以及制备方法,具体地说是一种实现单分子探测的碲化镓基表面增强拉曼基底及其制备方法。
背景技术
光子与材料相互作用时发生的非弹性散射称为拉曼散射。由于散射前后光子的能量差仅与分子自身能级有关,因此基于拉曼散射的拉曼光谱是一种对分子结构高度敏感的探测手段。分子在一些表面上具有显著拉曼散射增强效应的现象称为表面增强拉曼散射(SERS)。经过数十年的发展,SERS已经取得了非凡的进展,在多种需要痕量分析的领域得到了广泛的应用,包括生物医疗、环境监测、食品安全、安防等。但目前SERS在应用上依然存在一些问题,主要在于SERS基底的诸多性能之间存在一定的矛盾性,往往需要舍此就彼,如无序结构的SERS基底通常在稳定性、均一性和可重复性方面表现比较差,而采用纳米光刻或者纳米打印工艺制备的有序基底受到加工工艺的限制,不易制备间距小于10nm的器件以获得最大化的电磁耦合。
二维层状材料的发现为SERS基底的制备提供了一个新的方向。二维材料SERS基底具有良好的均一性、稳定性和可重复性,对某些分子如非硫醇芳香族分子的探测能力也强于传统基底。作为SERS领域研究最多的二维材料,石墨烯(graphene)基底已经获得比肩传统基底的SERS增强能力,实现对罗丹明6G(rhodamine 6G,R6G)分子的单分子探测。除石墨烯之外,基于其他二维材料的SERS基底也有所报道,如氮化硼、二硫化钼等。目前石墨烯是用作SERS基底最多的二维材料,但据PengqiLu等人的报道,GaTe二维材料拥有比石墨烯材料更好的潜在探测性能:在相似的基底结构下,GaTe基底对R6G分子的极限探测浓度为10- 11M,而石墨烯基底只有8×10-7M。因此研发以GaTe二维材料作为基底的具有单分子探测能力的SERS基底具有实际应用价值。
发明内容
本发明的正是针对现有技术的不足之处所作的改进,提供了一种提高GaTe基SERS基底的探测能力,实现单分子探测的碲化镓基表面增强拉曼基底及其制备方法。
本发明是采用以下技术方案来实现的:
本发明公开了一种新型的碲化镓GaTe基表面增强拉曼基底,所述的基底结构从下至上依次为Au孔阵列层,二维薄层GaTe层和Au纳米颗粒层。
作为进一步地改进,本发明所述的二维薄层GaTe层与Au孔阵列层形成异质结构。
作为进一步地改进,在所述的二维薄层GaTe层(2)上自组装形成的Au纳米颗粒层(3)。
作为进一步地改进,本发明所述的基底结构从下至上依次为SiO2/Si基底层、Ti或Cr层、Au孔阵列层,二维薄层GaTe层和Au纳米颗粒层。
作为进一步地改进,本发明所述的二维薄层GaTe层为3-5nm,较薄的GaTe层有利于提高Au孔阵列层与Au纳米颗粒层之间局域等离激元的耦合,从而提高基底的拉曼散射增强能力。
作为进一步地改进,本发明所述的Au孔阵列层的孔周期为4-20um,孔直径为2-10um,孔深度为80-120nm,孔截面形状为圆形。以上参数有利于降低制备难度,获得较强的表面电场,从而较好地平衡制备难度与探测能力。
本发明还公开了一种新型的碲化镓GaTe基表面增强拉曼基底的制备方法,在SiO2/Si基底层上,通过热蒸发的方法生长Ti层或Cr层,利用光刻和微纳加工方法制备Au孔阵列层,利用机械剥离的方法制备二维薄层GaTe层,并利用转移平台转移到Au孔阵列层上,最后将基底浸没在HAuCl4溶液中制备Au纳米颗粒层。
作为进一步地改进,本发明所述的GaTe单晶需要保存在惰性氛围中,制备和转移过程需要快速完成,以降低GaTe层的氧化,提高基底探测能力,制备Au颗粒时的浸没时间为240-960秒,该参数能有效提高基底探测能力。
本发明的有益效果是:
得益于GaTe材料较高的缺陷密度,在二维薄层GaTe层上自组装形成的金纳米颗粒层覆盖率能达到98%,因此能在金颗粒之间产生极强的局域表面等离激元。二维薄层GaTe层下方的Au孔阵列层经过孔周期、孔直径、孔深度的参数优化后,也能产生极强的局域表面等离激元。由于二维GaTe层非常薄,金纳米颗粒层和Au孔阵列层产生的局域等离激元能高效地耦合在一起,增强了GaTe表面的电场强度,从而大幅提升了拉曼散射增强效果。作为拉曼散射增强效果得到提升的体现,此基底对R6G分子的最低探测浓度达到10-16M,超过了绝大部分的表面增强拉曼散射基底。本基底同时具有较好的稳定性和可重复性,具有实用化前景。
附图说明
图1是SERS基底制备流程示意图;
图2是SERS基底对R6G分子的变浓度探测实验结果图,右侧图像是R6G浓度为10-16M时的拉曼信号图;
图1中1是Au孔阵列层,2是二维薄层GaTe层,3是Au纳米颗粒层。
具体实施方式
本发明公开了一种新型的碲化镓GaTe基表面增强拉曼基底,基底结构从下至上依次为SiO2/Si基底层、Ti或Cr层、Au孔阵列层1,二维薄层GaTe层2和Au纳米颗粒层3,二维薄层GaTe层2与Au孔阵列层1形成的异质结构,制备方法为在SiO2/Si基底层上,通过热蒸发的方法生长Ti层或Cr层,通过光刻和微纳加工制备Au孔阵列层1,利用机械剥离的方法制备二维薄层GaTe层2,并利用转移平台转移到Au孔阵列层1上,最后将基底浸没在HAuCl4溶液中制备Au纳米颗粒层3。
下面结合说明书附图,通过具体实施例对本发明的技术方案作进一步地说明:
本发明公开了一种新型的GaTe基表面增强拉曼基底,器件结构由下至上分别为SiO2/Si基底层、Ti层、Au孔阵列层1、二维薄层GaTe层2和Au纳米颗粒层3。二维薄层GaTe层2为3-5nm,Au孔阵列层1的孔周期为12um,孔直径为6um,孔深度为100nm,孔截面形状为圆形,二维薄层GaTe层2与Au孔阵列层1形成的异质结构,二维薄层GaTe层2上自组装形成的Au纳米颗粒层3。
本发明的简要制备步骤如下:
1)在SiO2/Si基底层上生长Ti或Cr层,再制备Au孔阵列层1;
2)制备薄层的GaTe二维材料;
3)将制备好的二维薄层GaTe层2转移到Au孔阵列层1上;
4)在二维薄层GaTe层2上制备金颗粒,形成Au纳米颗粒层3。
下面结合说明书附图,通过具体实施例对本发明的技术方案作进一步地说明:
制作流程
图1是制备流程示意图。
A.SiO2(300nm)/Si基底层的准备和清洗
将SiO2(300nm)/Si片切成1cm*1cm规格,在乙醇和去离子水中各超声数分钟后吹干即可。SiO2(300nm)/Si片也可替换为其他衬底,如硅片和金属片等。
B.制备Au孔阵列层1
在清洗完毕的SiO2(300nm)/Si片上热蒸发生长15nmTi层。从冰箱中取出AZ5350光刻胶并放入通风柜,在暗室环境下通风10分钟。10分钟后将流片放入匀胶机进行匀胶,在500rpm(round per minute)转速下匀胶10秒,4000rpm转速下匀胶60秒。匀胶完毕后将流片100℃前烘5分钟。使用相应光刻掩膜板进行3.6秒的汞灯曝光,然后显影45秒,显影期间需要不停搅动显影液使得显影均匀。取出流片,用去离子水洗去残留显影液,氮气枪吹干后100℃后烘坚膜5分钟,完成光刻。随后使用电子束蒸发在流片上镀金100nm。蒸镀完成后立即放入丙酮中,使用丙酮去除流片上的光刻胶,完成剥离。为了取得更好的剥离效果,可对丙酮加热或超声,超声时长不宜超过10s。剥离完成后,使用去离子水冲洗去除剩余的丙酮,并将流片放于100℃热板上加热10min,烘干表面水分。
C.GaTe二维材料的制备和转移
GaTe单晶需要保存在惰性气体氛围下。二维GaTe材料通过机械剥离法进行制备:用思高胶带粘住GaTe的两面,然后撕开,使GaTe一分为二。不断重复这个过程直到胶带上的GaTe足够薄。将粘有二维GaTe的胶带粘在PDMS薄膜上后撕去,二维GaTe薄膜即粘留在PDMS薄膜上。最后利用转移平台将PDMS薄膜上的GaTe转移到Au孔阵列层上,二维薄层GaTe层2为3-5nm。二维薄层GaTe层2的制备和转移需要快速完成以降低氧化的影响。
D.GaTe层上Au纳米颗粒层3的制备
将GaTe层/Au孔阵列层1/Ti层/SiO2/Si结构浸没在0.2mg/ml的HAuCl4溶液中,一段时间后取出,用乙醇润洗并吹干。浸没时间一般为960秒,探测极低浓度分子时可以降低至240秒。
至此便完成了SERS基底的整个制作流程。
测试及结果
通过以上工艺过程,获得了完整的SERS基底。
为了测试基底性能,使用R6G分子对SERS基底进行定量表征测试。将不同浓度的溶液滴在SERS基底上,20分钟后用乙醇洗去,氮气吹干。然后用显微共焦拉曼光谱仪进行拉曼测试,激发光波长为532nm。图2是SERS基底对R6G分子的变浓度实验结果,右侧是R6G浓度为10-16M时的拉曼信号图谱,拉曼峰位清晰可见。
以上所述的仅是本发明的优选实施方式,应当指出,对于本技术领域的普通技术人员来说,在不脱离本发明核心技术特征的前提下,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 (1)
1.一种新型的碲化镓GaTe基表面增强拉曼基底,其特征在于,所述的基底结构从下至上依次为Au孔阵列层(1),二维薄层GaTe层(2)和Au纳米颗粒层(3),所述的二维薄层GaTe层(2)与Au孔阵列层(1)形成异质结构,所述的二维薄层GaTe层(2)上自组装形成的Au纳米颗粒层(3),所述的二维薄层GaTe层(2)为3-5nm,所述的Au孔阵列层(1)的孔周期为4-20um,孔直径为2-10um,孔深度为80-120nm,孔截面形状为圆形,所述的新型的碲化镓GaTe基表面增强拉曼基底的制备方法为:在SiO2/Si基底层上,通过热蒸发的方法生长Ti层或Cr层,利用光刻和微纳加工方法制备Au孔阵列层(1),利用机械剥离的方法制备二维薄层GaTe层(2),并利用转移平台转移到Au孔阵列层(1)上,最后将基底浸没在HAuCl4溶液中制备Au纳米颗粒层(3),所述的GaTe单晶需要保存在惰性氛围中,制备和转移过程需要快速完成,制备Au颗粒时的浸没时间为240-960秒。
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