CN111349892A - 一种银叠加三角形纳米颗粒阵列及其制备方法 - Google Patents
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Abstract
本发明公开了一种银叠加三角形纳米颗粒阵列及其制备方法,将热蒸发工艺和简单成熟的单层聚苯乙烯(PS)球模板相结合,通过对模板处理和两次银沉积,获得了银叠加三角形纳米颗粒阵列。该制备方法具有简单、绿色、重现性好和结构可调等优点,这种结构独特的银纳米颗粒阵列有望在光电等领域得到实用,比如其优异的表面增强拉曼散射性能可应用于环境有机污染物痕量检测上。
Description
技术领域
本发明是一种简单制备银叠加三角形纳米颗粒阵列的方法,属于贵金属微纳结构的制备领域。
背景技术
贵金属纳米粒子具有独特的光学、电学、机械和化学性质,可用于光开关、传感器、非线性光学、表面增强拉曼散射(SERS)、太阳能电池等不同的应用领域。众所周知,金属纳米颗粒的光学吸收和散射是由表面电子的集体振荡引起的,这种振荡被称为表面等离子体共振,它是由入射的电磁辐射激发的。由于表面等离子体共振(SPR)和局域表面等离子体共振(LSPR),周期性纳米结构的光学性质与其尺寸、形状、组成和周围环境密切相关。目前,研究人员对银纳米粒子的LSPR光谱进行了初步研究,系统地分析了其对纳米粒子尺寸、形状、间距的依赖关系。此外,还有纳米环阵列、纳米碗阵列等,这些纳米颗粒阵列的光学性能均依赖于形貌。因此,制备形貌各异的颗粒阵列以满足不同领域的需求是非常重要的。
化学法是制备银纳米颗粒最常用的方法,它是通过化学反应将Ag+还原,方法较为灵活多样,但颗粒容易团聚并且难以控制颗粒的尺寸分布。物理方法很早就用于银纳米颗粒制备,尽管对仪器设备要求较高,但具有产物质量高、能获得周期性阵列的优势。采用物理方法制备银纳米颗粒阵列已有很多报道,但与化学方法相比相当缺乏。
虽然现已报道多种形貌的银纳米颗粒阵列,但是这些颗粒本身都是单层的,阵列的性能如SPR、SERS等则通过改变颗粒尺寸及间距来实现,因而可用于调控的工艺参数较少,并且对性能影响较大的因素如银纳米颗粒尖端效应以及大的比表面积等仍未涉及。此外,采用模板如聚苯乙烯(PS)球是制备银纳米颗粒阵列的主要方法,其工艺路线比较简单,通常都是在银生长前后对模板进行处理或去除,然而至今未见将银生长过程与模板处理相结合的报道。
发明内容
本发明的目的是提供一种银叠加三角形纳米颗粒阵列及其制备方法。
实现本发明目的的技术方案是:一种银叠加三角形纳米颗粒阵列及其制备方法,主要步骤如下:
(1)制备单层PS球胶体薄膜;
(2)获取单层PS球模板/硅片;
(3)在单层PS球模板/硅片上采用热蒸发法沉积银;
(4)加热处理后继续沉积银;
(5)去除单层PS球模板即可获得所述的银叠加三角形纳米颗粒阵列。
较佳的,采用气-液-固相界面自组装方法制备单层PS球胶体薄膜。
具体的,将PS球(直径1 μm)悬浮液(2.5wt%)和乙醇按体积比1:1超声均匀混合,取洁净载玻片,采用气-液-固相界面自组装方法制备单层PS球胶体薄膜。
较佳的,将载有该单层PS球胶体薄膜的载玻片缓慢以45°浸入水中,将所述薄膜附着在硅片上,获得单层PS球模板/硅片。
较佳的,采用热蒸发法沉积银,沉积厚度为100 nm。
较佳的,加热处理温度为110-120℃,时间为10min-30min。
较佳的,加热处理后继续采用热蒸发法沉积银,沉积厚度为100 nm。
较佳的,通过在有机溶剂中浸泡去除单层PS球模板。
具体的,有机溶剂为CH2Cl2,浸泡时间为10 min。
与现有技术相比,本发明的创新之处在于:本发明制备的银叠加三角形纳米颗粒在结构上是独特的,相比单个三角形纳米颗粒,既增大了比表面,又增加了棱角的数量,将提高光电性能。同时,制备方法上也是新颖的,文献中已有在蒸镀银后去球得到三角形银纳米颗粒阵列的报道,而本发明则是继续加热PS球模板和蒸镀银。
本发明的优越之处在下面的附图说明和具体实施方式中将进一步阐述。
附图说明
图1为本发明制备的银叠加三角形纳米颗粒阵列的工艺流程示意图。
图2为本发明实施例1所用直径1μm的PS球模板形貌。
图3为本发明实施例1银叠加三角形纳米颗粒阵列形貌。
图4为本发明实施例1银叠加三角形纳米颗粒阵列对R6G分子的SERS图谱
图5为本发明实施例2制备的银叠加三角形纳米颗粒阵列的形貌图
图6为本发明实施例3制备的银叠加三角形纳米颗粒阵列的形貌图。
具体实施方式
本发明通过将银生长过程与模板处理相结合,获得了结构复杂的银叠加三角形纳米颗粒阵列,此阵列具有更加优异的性能。
本发明合成了银叠加三角形纳米颗粒阵列,即单个三角形颗粒上面叠加一个尺寸较小的三角形颗粒,这样一种结构的表面等离子共振更为复杂,两个三角形之间的光场耦合更多,将大大有利于一些光学性能的提高。
工艺路线如图1所示。首先,组装单层PS球模板并利用热蒸发沉积银;其次,将沉积银后的衬底再进行加热处理和沉积银;最后,去除PS球即可获得银叠加三角形纳米颗粒阵列。颗粒和阵列的结构参数可以通过工艺参数进行调控。该工艺具有简单、绿色、重现性好和可宏量制备的优点,有望得到实际应用。测试表明,银叠加三角形纳米颗粒阵列具有优异的SERS性能。
实施例1
首先,采用文献中报道的气-液-固相界面自组装方法,在洁净的载玻片上制备大尺寸单层PS胶体晶体薄膜并将其转移到硅片上。即将PS球(直径1 μm)悬浮液(2.5wt%)、乙醇按体积比1:1超声均匀混合,取洁净载玻片,在其上方加适量去离子水形成大面积水膜,抽吸PS球混合溶液约0.1mL至水膜表面,PS球自发在气液固界面自组装形成几平方厘米单层胶体晶体薄膜。接着将载有PS球胶体薄膜的载玻片缓慢以45°浸入水中,PS球胶体薄膜就能漂浮到水面,取洁净的硅片,沿水面倾斜进入,将单层胶体薄膜附着在硅片上捞起,获得单层PS球模板/硅片。其次,在PS球模板/硅片上采用热蒸发法进行第一次沉积银,热蒸发仪真空度约2×10-4pa,沉积过程中保持基片静止,沉积厚度为100nm。将沉积银之后的PS球模板/硅片在110℃下加热20min,接着以相同的热蒸发工艺参数第二次沉积银,沉积银厚度仍为100nm。最后,将二次沉积银后的PS球模板/硅片浸泡在CH2Cl2溶剂中10 min去除掉PS球模板,即可获得银叠加三角形纳米颗粒阵列。
采用日本日立公司的S-4800场发射扫描电子显微镜(FESEM)观察样品形貌。采用英国Renishwa公司的In Via激光共焦拉曼光谱仪分析样品的光学性质。
图2为本发明实施例1所用直径1μm的PS球模板形貌。如图所示,PS球呈六方紧密排列,球之间有三角形缝隙。
图 3为本发明实施例1银叠加三角形纳米颗粒阵列形貌。图3a,b对应不同放大倍数SEM像。按照图1所示工艺流程,很明显在PS球之间三角缝隙处能够沉积银,去球后可得到对应的银叠加三角形纳米颗粒阵列,阵列具有十分规则的周期性。每个颗粒都是由上下两个正三角形颗粒叠加而成,三角形三边有轻微弧度。下层颗粒(颜色较暗)尺寸较大,边长约230纳米,上层颗粒尺寸较小,边长约150纳米。上层颗粒尺寸较小是PS球被加热后中间三角缝隙变小导致的。
图4为本发明实施例1银叠加三角形纳米颗粒阵列对R6G分子的SERS图谱。曲线1和2分别对应银叠加三角形纳米颗粒阵列和银三角形纳米颗粒阵列(没有叠加)的SERS谱。可以看出银叠加三角形纳米颗粒阵列具有更大的增强能力。
实施例2
其它工艺参数与实施例1相同。区别是将PS球模板/硅片于110℃下分别加热不同时间,考察银叠加三角形纳米颗粒中上层颗粒的形貌演变。
图 5a和图5b分别对应110℃/10min和110℃/30min热处理条件下得到的银叠加三角形纳米颗粒阵列SEM像。由图可见,短的加热时间对应大的上层颗粒尺寸(图5a),长的加热时间对应小的上层颗粒尺寸(图5b)。因此,可以通过改变模板加热时间(对应PS球之间三角缝隙)调控上层三角颗粒的尺寸。
实施例3
其它工艺参数与实施例2中图5a相同。区别是将初始的(第一次银沉积之前的)PS球模板/硅片于110℃下加热10min,即为第一次模板热处理条件。
图6是第一次模板热处理(110℃/10min)后按照实施例2中图5a工艺参数(第二次模板热处理条件为110℃/10min)制备的银叠加三角形纳米颗粒阵列SEM像。可见,第一次模板热处理能够改变银叠加三角形纳米颗粒的下层颗粒的尺寸,当然上层颗粒尺寸亦随之改变。
根据上述研究结果可知:利用热蒸发银和热处理PS球模板能够制备银叠加三角形纳米颗粒阵列;工艺流程具有简单、绿色、易于宏量制备等优点,有望得到实际应用。
Claims (10)
1.一种银叠加三角形纳米颗粒阵列的制备方法,其特征在于,其步骤如下:
(1)制备单层PS球胶体薄膜;
(2)获取单层PS球模板/硅片;
(3)在单层PS球模板/硅片上采用热蒸发法沉积银;
(4)加热处理后继续沉积银;
(5)去除单层PS球模板即可获得所述的银叠加三角形纳米颗粒阵列。
2.如权利要求1所述的方法,其特征在于,在载玻片上采用气-液-固相界面自组装方法制备单层PS球胶体薄膜。
3.如权利要求1或2所述的方法,其特征在于,在载玻片上采用气-液-固相界面自组装方法制备单层PS球胶体薄膜,其具体步骤如下:将PS球悬浮液和乙醇按体积比1:1超声均匀混合,取洁净载玻片,在载玻片上采用气-液-固相界面自组装方法制备单层PS球胶体薄膜,其中,PS球的直径为1 μm,PS球悬浮液浓度为2.5wt%。
4.如权利要求1所述的方法,其特征在于,获取单层PS球模板/硅片的具体步骤如下:将载有单层PS球胶体薄膜的载玻片缓慢以45°浸入水中,将所述薄膜附着在硅片上,获得单层PS球模板/硅片。
5.如权利要求1所述的方法,其特征在于,采用热蒸发法沉积银,沉积厚度为100 nm。
6.如权利要求1所述的方法,其特征在于,加热处理温度为110-120℃,时间为10min-30min。
7.如权利要求1所述的方法,其特征在于,于110℃下加热20min处理后继续沉积银。
8.如权利要求1所述的方法,其特征在于,加热处理后继续采用热蒸发法沉积银,沉积厚度为100 nm。
9.如权利要求1所述的方法,其特征在于,通过在有机溶剂中浸泡去除单层PS球模板。
10.如权利要求1-9任一所述的方法制备的银叠加三角形纳米颗粒阵列。
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