CN114507846A - 一种表面负载银纳米颗粒的sers基底的制备方法 - Google Patents
一种表面负载银纳米颗粒的sers基底的制备方法 Download PDFInfo
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Abstract
本发明公开了一种表面负载银纳米颗粒的SERS基底的制备方法,包括步骤1:镀银膜石英基底的制备;将干净的石英衬底在丙酮、乙醇、超纯水中分别清洗2‑4次,在石英衬底上沉积Ag膜,并采用厚度检测器对Ag膜厚度进行检测,最终控制Ag膜厚度为10‑800nm;步骤2:将步骤1制备的镀银膜石英基底放置于马弗炉中,加热温度保持为350‑450℃,升温速率控制在1‑10℃/min,加热时间控制在2‑60min;步骤3:将步骤2得到的镀银膜石英衬底置于空气中自然冷却,即得到负载银纳米颗粒的SERS基底。本发明制备的基底灵敏度高,耐高压,增加了SERS的“热点”;负载的银纳米颗粒为自由能最低的单晶面Ag,更容易吸附分子,增强了SERS效果,抗氧化性得到了提高。
Description
技术领域
本发明涉及光谱分析检测技术领域,具体涉及增强拉曼信号领域,尤其是一种表面负载银纳米颗粒的SERS基底的制备方法。
背景技术
后生动物与化能自养生物的共生机制是维持深海生态系统生命活动稳定和可持续的重要因素,已成为深海研究的热点问题之一。磷脂酰乙醇胺(PE)头群可作为古菌共生菌的生物标志物。PE头部基的形成与磷酸乙醇胺(PETA)的形成有关。因此,PETA的微量检测对于深海共生细菌的存在定位和共生细菌代谢物的原位检测具有重要意义。然而,深海细胞外代谢还没有任何原位检测技术手段。传统的检测方法(包括比色法、液相色谱-质谱联用(LC-MS)和核磁共振(NMR))也不能同时检测多组分,耗时长、成本高、灵敏度低。同时,受拉曼检测限的影响,深海微生物代谢物或中间体在低浓度下难以检测。
表面增强拉曼散射(Surface-enhanced Raman Scattering,SERS)主要来自于贵金属(Ag、Au)附近局部电磁场的增强,因此具有超灵敏、快速检测待检测痕量分子的能力。目前常用的拉曼信号增强介质主要有SERS衬底和纳米溶胶。为了满足深海原位实验的需要,需要SERS基底。分散在亚纳米隙基底上的金属纳米结构是增强SERS信号的理想材料。然而,制备间距小于10nm的金属纳米结构并不容易。各种制造技术已被用于创建纳米间隙嵌入结构,如光刻、阴影蒸发和气相沉积。然而,所有这些都是具有挑战性的、昂贵的和耗时的。
发明内容
为了克服现有技术中存在的上述问题,本发明提出一种表面负载银纳米颗粒的SERS基底的制备方法。
本发明解决其技术问题所采用的技术方案是:一种表面负载银纳米颗粒的SERS基底的制备方法,包括如下步骤:
步骤1:镀银膜石英基底的制备;
步骤2:将步骤1制备的镀银膜石英基底放置于马弗炉中,加热温度保持为350-450℃,升温速率控制在1-10℃/min,加热时间控制在2-60min;
步骤3:将步骤2得到的镀银膜石英衬底置于空气中自然冷却,即得到负载银纳米颗粒的SERS基底;
所述步骤1的具体制备方法为:将干净的石英衬底在丙酮、乙醇、超纯水中分别清洗2-4次,在石英衬底上沉积Ag膜,并采用厚度检测器对Ag膜厚度进行检测,最终控制Ag膜厚度为10-800nm。
上述的一种表面负载银纳米颗粒的SERS基底的制备方法,所述步骤1中采用电子束沉积(EBD FU-12PEB)沉积Ag膜。
上述的一种表面负载银纳米颗粒的SERS基底的制备方法,所述步骤1中采用电子束沉积法沉积Ag膜时的速率为1-10A/s。
上述的一种表面负载银纳米颗粒的SERS基底的制备方法,所述步骤2中马弗炉加热温度保持在420-425℃。
上述的一种表面负载银纳米颗粒的SERS基底的制备方法,所述步骤2中马弗炉设置的升温速率为5-10℃/min。
上述的一种表面负载银纳米颗粒的SERS基底的制备方法,所述步骤2中马弗炉设置加热时间为5-30min。
上述的一种表面负载银纳米颗粒的SERS基底的制备方法,所述步骤2中负载的银纳米颗粒之间间隙在5-20nm之间。
本发明的有益效果是:(1)利用简单的高温退火工艺得到了具有类似七星瓢虫形貌的银纳米颗粒的SERS基底,该基底灵敏度高,耐高压,增加了SERS的“热点”;
(2)制备的表面负载银纳米颗粒SERS基底为自由能最低的单晶面Ag(111),更容易吸附分子,增强了SERS效果;
(3)制备的表面负载银纳米颗粒SERS基底在空气中退火,其抗氧化性得到了提高,为未来在极端深海环境中的原位应用铺平了道路。
附图说明
下面结合附图和实施例对本发明进一步说明。
图1为本发明实施例1-实施例5的SERS基底对罗丹明B溶液的检测效果示意图;
图2为本发明实施例4所制样品的的扫描电镜(SEM)图;
图3为本发明实施例4所制样品结构示意图。
具体实施方式
为使本领域技术人员更好的理解本发明的技术方案,下面结合附图和具体实施方式对本发明作详细说明。
【实施例1】
银纳米颗粒SERS基底的制备方案,包括以下步骤:
(1)镀银膜石英基底是通过电子束沉积法制备:将干净的石英衬底在丙酮,乙醇,超纯水中反复洗净,以10A/s的速率在衬底上沉积Ag膜,采用厚度监测器对薄膜厚度进行检测,最终得到厚度为100nm的Ag膜;
(2)取步骤(1)得到的镀银膜石英基底,将步骤(1)制备的镀银膜石英基底放置于马弗炉中,加热温度保持为350℃,升温速率控制在10℃/min,加热时间控制在20分钟,得到负载银纳米颗粒的SERS基底;
(3)将步骤(2)所得的SERS基底,浸润在10-6M罗丹明B溶液中2小时,取出SERS基底干燥后检测。
【实施例2】
(1)镀银膜石英基底是通过电子束沉积法制备:将干净的石英衬底在丙酮,乙醇,超纯水中反复洗净,以10A/s的速率在衬底上沉积Ag膜,采用厚度监测器对薄膜厚度进行检测,最终得到厚度为100nm的Ag膜。
(2)取步骤(1)得到的镀银膜石英基底,将步骤(1)制备的镀银膜石英基底放置于马弗炉中,加热温度保持为375℃,升温速率控制在10℃/min,加热时间控制在20分钟,得到负载银纳米颗粒的SERS基底。
(3)将步骤(2)所得的SERS基底,浸润在10-6M罗丹明B溶液中2小时,取出SERS基底干燥后检测。
【实施例3】
(1)镀银膜石英基底是通过电子束沉积法制备。将干净的石英衬底在丙酮,乙醇,超纯水中反复洗净,以10A/s的速率在衬底上沉积Ag膜。采用厚度监测器对薄膜厚度进行检测,最终得到厚度为100nm的银膜。
(2)取步骤(1)得到的镀银膜石英基底,将步骤(1)制备的镀银膜石英基底放置于马弗炉中,加热温度保持为400℃,升温速率控制在10℃/min,加热时间控制在20分钟,得到负载银纳米颗粒的SERS基底。
(3)将步骤(2)所得的SERS基底,浸润在10-6M罗丹明B溶液中2小时,取出SERS基底干燥后检测。
【实施例4】
(1)镀银膜石英基底是通过电子束沉积法制备。将干净的石英衬底在丙酮,乙醇,超纯水中反复洗净,以10A/s的速率在衬底上沉积Ag膜。采用厚度监测器对薄膜厚度进行检测,最终得到厚度为100nm的银膜。
(2)取步骤(1)得到的镀银膜石英基底,将步骤(1)制备的镀银膜石英基底放置于马弗炉中,加热温度保持为425℃,升温速率控制在10℃/min,加热时间控制在20分钟,得到负载银纳米颗粒的SERS基底。
(3)将步骤(2)所得的SERS基底,浸润在10-6M罗丹明B溶液中2小时,取出SERS基底干燥后检测。
【实施例5】
(1)镀银膜石英基底是通过电子束沉积法制备。将干净的石英衬底在丙酮,乙醇,超纯水中反复洗净,以10A/s的速率在衬底上沉积Ag膜。采用厚度监测器对薄膜厚度进行检测,最终得到厚度为100nm的银膜。
(2)取步骤(1)得到的镀银膜石英基底,将步骤(1)制备的镀银膜石英基底放置于马弗炉中,加热温度保持为450℃,升温速率控制在10℃/min,加热时间控制在20分钟,得到负载银纳米颗粒的SERS基底。
(3)将步骤(2)所得的SERS基底,浸润在10-6M罗丹明B溶液中2小时,取出SERS基底干燥后检测。
实施例1~5制备的银纳米颗粒SERS基底用于罗丹明B溶液的检测的效果见图3,可以看出随着加热温度的升高,SERS效果增强,到温度为425℃时效果最好,超过425℃,效果变差,并对实施例4加热温度为425℃进行扫描电镜实验,扫描电镜图如图2所示,并绘制了实施例4加热温度为425℃时的模型图如图3所示,可见此种方式制备的银纳米颗粒SERS基底表面的银纳米颗粒之间有间隙,且间隙在5-20nm之间。
以上实施例仅为本发明的示例性实施例,不用于限制本发明,本发明的保护范围由权利要求书限定。本领域技术人员可以在本发明的实质和保护范围内,对本发明做出各种修改或等同替换,这种修改或等同替换也应视为落在本发明的保护范围内。
Claims (7)
1.一种表面负载银纳米颗粒的SERS基底的制备方法,其特征在于:包括如下步骤:
步骤1:镀银膜石英基底的制备;
步骤2:将步骤1制备的镀银膜石英基底放置于马弗炉中,加热温度保持为350-450℃,升温速率控制在1-10℃/min,加热时间控制在2-60min;
步骤3:将步骤2得到的镀银膜石英衬底置于空气中自然冷却,即得到负载银纳米颗粒的SERS基底;
所述步骤1的具体制备方法为:将干净的石英衬底在丙酮、乙醇、超纯水中分别清洗2-4次,在石英衬底上沉积Ag膜,并采用厚度检测器对Ag膜厚度进行检测,最终控制Ag膜厚度为10-800nm。
2.根据权利要求1所述的一种表面负载银纳米颗粒的SERS基底的制备方法,其特征在于,所述步骤1中采用电子束沉积(EBD FU-12PEB)沉积Ag膜。
3.根据权利要求2所述的一种表面负载银纳米颗粒的SERS基底的制备方法,其特征在于,所述步骤1中采用电子束沉积法沉积Ag膜时的速率为1-10A/s。
4.根据权利要求1所述的一种表面负载银纳米颗粒的SERS基底的制备方法,其特征在于,所述步骤2中马弗炉加热温度保持在420-425℃。
5.根据权利要求1所述的一种表面负载银纳米颗粒的SERS基底的制备方法,其特征在于,所述步骤2中马弗炉设置的升温速率为5-10℃/min。
6.根据权利要求1所述的一种表面负载银纳米颗粒的SERS基底的制备方法,其特征在于,所述步骤2中马弗炉设置加热时间为5-30min。
7.根据权利要求1所述的一种表面负载银纳米颗粒的SERS基底的制备方法,其特征在于,所述步骤2中负载的银纳米颗粒之间间隙在5-20nm之间。
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