CN111321373A - 多个等离激元共振特性的金/银纳米岛膜及其制备方法 - Google Patents

多个等离激元共振特性的金/银纳米岛膜及其制备方法 Download PDF

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CN111321373A
CN111321373A CN202010117209.1A CN202010117209A CN111321373A CN 111321373 A CN111321373 A CN 111321373A CN 202010117209 A CN202010117209 A CN 202010117209A CN 111321373 A CN111321373 A CN 111321373A
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张明娣
吕且妮
戴海涛
何剑涛
薛永祥
葛宝臻
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Abstract

本发明公开了一种多个等离激元共振特性的金/银纳米岛膜及其制备方法，其步骤如下：(1)在ITO玻璃上以一定速度蒸镀一定厚度的金/银薄膜；(2)将薄膜放置于高温退火炉中，在氮气保护下退火，即可得到金/银纳米岛膜。本发明制备得到的金纳米岛膜具有三个LSPR，中心波长分别位于316nm,407nm及可调的540nm～600nm。银纳米岛膜具有两个LSPR，中心波长分别位于354nm及可调的440nm～580nm，该制备方法具有步骤简洁，操作简单，并可制备面积大的纳米岛膜，且重复性高的特点，可结合表面增强光谱学研究，用于多光谱探测，识别等领域。

Description

多个等离激元共振特性的金/银纳米岛膜及其制备方法
技术领域
本发明属于纳米岛膜的制备领域，涉及一种具备多个LSPR特性的金/银纳米岛膜及其制备方法，具体涉及一种通过控制蒸镀速度和金/银膜的厚度，进而影响高温退火时的奥斯瓦尔德熟化过程，形成具有多个LSPR的金/银纳米岛膜的方法。
背景技术
纳米金/银材料，由于其优异的小尺寸效应、特有的光学效应以及生物相容性，在食品、生物医学以及环境监测分析方面得到广泛的应用。金/银纳米岛膜的均一性和可重复性，使其在作为表面增强荧光，表面增强拉曼散射的增强衬底的同时，有助于光谱信号的定量分析。目前已提出多种方法用于金/银纳米岛膜的制备，如化学自组装法，电子束刻蚀法，纳米压印法，机械法等。其中，电子束刻蚀技术、纳米压印法、机械法等均需要特殊仪器，成本高、耗时长。化学自组装方法在衬底面积和均一性上都无法很好的满足增强需求。利用奥斯瓦尔德熟化过程对金/银薄膜进行退火，可以得到大面积且均匀性好的纳米岛膜，这种方法操作简单，可重复性高。当增强波长分辨时，通常需要利用电子束刻蚀方法，在同一衬底上刻蚀不同大小的纳米结构，使其具有多个LSPR，这增加了制备成本，且延长了制备时间。因此，需要一种操作简单、成本低廉、重复性高，且可制备具有多个LSPR的金/银纳米岛膜的制备方法。
发明内容
本发明目的是克服现有技术的缺陷，提出一种操作简单，成本低，重复性高，且可制备具有多个等离激元共振特性的金/银纳米岛膜的制备方法，以满足波长分辨的表面增强光谱学需求。
该方法的原理是对蒸镀形成的纳米薄膜进行高温退火，通过奥斯瓦尔德熟化过程形成纳米颗粒。在合适的蒸镀速度，薄膜厚度和退火温度下，金纳米岛膜具有三个LSPR，其中心波长分别位于316nm，407nm，及可调的540nm～600nm，银纳米岛膜具有两个LSPR，其中心波长分别位于354nm和可调的440nm～580nm。
第一个技术方案是金/银纳米岛膜的制备方法，包括以下步骤：
步骤一、将ITO玻璃分别浸泡在酒精和去离子水中，并超声清洗15min,氮气吹干备用；
步骤二、将干净的ITO玻璃以及金/银靶材放入多源有机气相沉积系统的腔体中，抽真空至3×10-4Pa；
步骤三、以7A/4min速度给钨舟加电流，同时观察膜厚检测仪显示的蒸镀速度；
步骤四、达到所需蒸镀速度后，预蒸镀10nm厚度，待速度稳定后打开挡板开始蒸镀，得到所需膜厚，关闭挡板；
步骤五、将薄膜从蒸镀腔取出进行退火(或存放于水氧含量低于0.1ppm的手套箱中备用)，退火过程分为三步：以5℃/min的速度升温到退火温度，在退火温度下保持30min，再从退火温度降温到室温；
步骤六、通过控制步骤四中的蒸镀速度和薄膜厚度，即可得到具有可调等离激元共振(LSPR)的金/银纳米岛膜。
所述步骤四中蒸镀速度为
Figure BDA0002391858730000021
金薄膜厚度为4nm～8nm；银薄膜厚度为6nm～10nm。
所述步骤五中金薄膜退火温度是350℃，银薄膜退火温度是300℃。
所述靶材纯度为99.999％。
第二个技术方案是由上述方法制备金/银纳米岛膜，金纳米岛膜具有三个LSPR，其中心波长分别位于316nm、407nm及可调的540nm～600nm；银纳米岛膜具有两个LSPR，中心波长分别位于354nm和可调的440nm～580nm。
该金岛膜具有三个LSPR，银岛膜具有两个LSPR，可以用于表面增强光谱学研究中的多光谱增强或波长分辨的光谱识别。该金/银纳米岛膜具有制备工艺简单，成本低，重复性高，并可大面积制备等特点，有广泛的推广使用价值。
附图说明
图1为本发明实施例1所获得四种金纳米岛膜的紫外可见吸收光谱图；
图2为本发明实施例1所获得四种金纳米岛膜的SEM图；
图3为本发明实施例2所获得四种银纳米岛膜的紫外可见吸收光谱图；
图4为本发明实施例2所获得四种银纳米岛膜的SEM图。
具体实施方式
为使本发明的目的、技术方案和优点更加清楚，下面对本发明实施方式作进一步地详细描述。
下面以图1和图2所示的四种金纳米岛膜的紫外可见吸收光谱图和SEM图为例，阐述本发明的金纳米岛膜及其制备方法的具体过程：
实施例1：
步骤1、将ITO玻璃分别浸泡在酒精和去离子水中，并超声清洗15min,氮气吹干备用；
步骤2、将干净的ITO玻璃以及金靶材放入多源有机气相沉积系统的腔体中，抽真空至3×10-4Pa。以7A/4min速度给钨舟加电流，同时观察膜厚检测仪显示的蒸镀速度。当速度达到
Figure BDA0002391858730000031
后，预蒸镀10nm厚度，待速度稳定后打开挡板开始蒸镀，待膜厚分别达到①5nm,②6nm,③7nm,④8nm后关闭挡板；
步骤3、将薄膜从蒸镀腔取出，立即放入管式炉中，在氮气保护下进行退火。退火过程为：以5℃/min的速度升温到350℃，保持30min，再从该温度降到室温，该降温过程有内置风扇辅助。得到具有三个LSPR的四种金纳米岛膜，其LSPR的中心波长分别为316nm,407nm,以及①560nm,②576nm,③585nm，④592nm。
若在步骤2中，当速度达到
Figure BDA0002391858730000032
后，预蒸镀10nm厚度，待速度稳定后打开挡板开始蒸镀，待膜厚分别达到①4nm,②5nm,③6nm,④7nm后关闭挡板；按步骤3，即可得到具有三个LSPR的四种金纳米岛膜，其LSPR的中心波长分别为316nm,407nm,以及①552nm,②560nm,③576nm,④585nm。
若在步骤2中，当速度达到
Figure BDA0002391858730000033
后，预蒸镀10nm厚度，待速度稳定后打开挡板开始蒸镀，待膜厚分别达到①5nm,②6nm,③7nm和④8nm后关闭挡板；按步骤3，即可得到具有三个LSPR的四种金纳米岛膜，其LSPR的中心波长分别为316nm,407nm,以及①556nm,②569nm,③575nm,④583nm。
若在步骤2中，当速度达到
Figure BDA0002391858730000034
后，预蒸镀10nm厚度，待速度稳定后打开挡板开始蒸镀，待膜厚分别达到①4nm,②6nm,③7nm和④8nm后关闭挡板；按步骤3，即可得到具有三个LSPR的四种金纳米岛膜，其LSPR的中心波长分别为316nm,407nm,以及①557nm,②582nm,③593nm,④600nm。
下面以图3和图4所示的四种银纳米岛膜的紫外可见吸收光谱图和SEM图为例，阐述本发明的银纳米岛膜及其制备方法的具体过程：
实施例2：
步骤1、将ITO玻璃分别浸泡在酒精和去离子水中，并超声清洗15min,氮气吹干备用；
步骤2、将干净的ITO玻璃以及银靶材放入多源有机气相沉积系统的腔体中，抽真空至3×10-4Pa。以7A/4min速度给钨舟加电流，同时观察膜厚检测仪显示的蒸镀速度。当达到一定速度后，预蒸镀10nm厚度，待速度稳定后打开挡板开始蒸镀，待膜厚达到一定厚度后关闭挡板，本次实施例中，蒸镀速度和薄膜厚度为①
Figure BDA0002391858730000041
8nm；②
Figure BDA0002391858730000042
8nm；③
Figure BDA0002391858730000043
9nm；④
Figure BDA0002391858730000044
9nm；
步骤3、将薄膜从蒸镀腔取出，立即放入管式炉中，在氮气保护下进行退火。退火过程为，以5℃/min的速度升温到300℃，保持30min，再从300℃降到室温，该降温过程有内置风扇辅助。得到具有两个LSPR的四种银纳米岛膜，其LSPR的中心波长分别为354nm以及①507nm,②515nm,③525nm，④539nm。
本领域技术人员可以理解附图只是一个优选实施例，上述本发明实施例序号仅仅为了描述，不代表实施例的优劣。
以上所述仅为本发明的较佳实施例，并不用以限制本发明，凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。

Claims (5)

1.多个等离激元共振特性的金/银纳米岛膜的制备方法，其特征在于，该方法包括以下步骤：
步骤一、将ITO玻璃分别浸泡在酒精和去离子水中，并超声清洗，氮气吹干备用；
步骤二、将干净的ITO玻璃以及金/银靶材放入多源有机气相沉积系统的腔体中，抽真空至3×10-4Pa；
步骤三、以7A/4min速度给钨舟加电流，同时观察膜厚检测仪显示的蒸镀速度；
步骤四、达到所需蒸镀速度后，预蒸镀10nm厚度，待速度稳定后打开挡板开始蒸镀，得到所需膜厚，关闭挡板；
步骤五、将薄膜从蒸镀腔取出进行退火，退火过程分为三步：以5℃/min的速度升温到退火温度，在退火温度下保持30min，再从退火温度降温到室温；
步骤六、最终金/银纳米岛膜上可调的LSPR是通过控制步骤四中的蒸镀速度和薄膜厚度得到的。
2.根据权利要求1所述的制备方法，其特征在于，蒸镀速度为
Figure FDA0002391858720000011
金薄膜厚度为4nm～8nm，银薄膜厚度为6nm～10nm。
3.根据权利要求1所述的制备方法，其特征在于，金薄膜退火温度是350℃，银薄膜退火温度是300℃。
4.根据权利要求1所述的制备方法，其特征在于，金/银靶材的纯度为99.999％。
5.根据权利要求1至4中任一项所述的方法制备金/银纳米岛膜，其特征在于，金纳米岛膜具有三个LSPR，其中心波长分别位于316nm、407nm及可调的540nm～600nm；银纳米岛膜具有两个LSPR，其中心波长分别位于354nm及可调的440nm～580nm。
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