CN105839062A - 一种复合型多层膜结构银纳米线及其制备方法 - Google Patents
一种复合型多层膜结构银纳米线及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种复合型多层膜结构银纳米线及其制备方法,主要采用物理沉积技术和退火处理相结合的方法,利用磁控溅射技术在二维有序胶体球模板上制备出[Ag 20~30nm/SiO2 3~5nm]n纳米多层膜阵列,并进一步对其在氩气保护下进行退火处理,从而形成复合型多层膜结构表面生长出银纳米线。这种方法制备成本低、耗时少,且具有结构稳定、可控性强、纯度高的特点,将二氧化硅和银结合到一起,二氧化硅可以改变金属周围的电介质环境,而且可以防止银发生氧化,使银纳米线结构存活时间更长。此外,结构具有丰富的热点,有很高的SERS活性,可应用于分子探测与识别技术等领域、电子学、磁学、声学、光学等领域。
Description
技术领域
本发明属于纳米功能材料技术领域。
背景技术
纳米材料具有很多独特的性能和特殊的应用,其结构的特殊性,导致了宏观的声、光、电、磁、热、力学等的物理效应与常规材料有所不同,体现为量子尺寸效应、小尺寸效应、表面效应和宏观隧道效应等,成为了当前人们研究的热点。纳米材料具有较低的光反射系数,能够高效地将太阳能转化为电能和热能,而且作为添加剂还具有增强韧性和强度的功能,在电子学、磁学、声学、光学等领域具有巨大的发展空间和潜在价值。银纳米线作为一维无机纳米材料已经在偏光器件、光子晶体、催化剂以及生物和化学传感器等领域得到了广泛地应用。目前已经开发了很多制备银纳米线的方法,然而大部分方法工艺比较复杂,成本高,对反应设备要求比较高而且能量消耗大。
发明内容
为了解决现有的银纳米线的制备方法工艺复杂成本高,对反应设备要求比较高而且能量消耗大的问题,本发明提供了一种复合型多层膜结构银纳米线,其生长于结构为20~30nm的银和3~5nm的二氧化硅循环沉积n个周期形成的[Ag 20~30nm/SiO2 3~5nm]n纳米多层膜阵列表面;其中5≥n≥1,优选n=4。
所述复合型多层膜结构银纳米线的制备方法具体步骤如下:
步骤一、利用自组装技术制备聚苯乙烯二维有序胶体球序列模板,其中胶体球呈六方密堆排列,胶体球直径为200-700nm;
步骤二、采用磁控溅射技术向二维有序胶体球模板上依次沉积20-30nm的银和3-5nm的二氧化硅,循环沉积n个周期,形成[Ag 20~30nm/SiO2 3~5nm]n纳米多层膜阵列;其中5≥n≥1,优选n=4。
步骤三、将上一步制得的[Ag 20~30nm/SiO2 3~5nm]n纳米多层膜阵列浸泡在四氢呋喃或氯仿、甲苯等有机溶剂中去掉聚苯乙烯二维有序胶体球序列模板,然后在保护气氛下进行800-900℃退火处理1-2小时。
本发明步骤二中进行磁控溅射时采用直流溅射制备银层,采用交流溅射制备SiO2层。在正式镀膜之前,要预溅射20分钟左右。靶材和基底之间的距离为20厘米。在共溅射期间基底被旋转并且真空室的本底气压为2.4×10-4Pa。Ag靶和SiO2靶的溅射功率分别是20瓦和72瓦。在薄膜沉积的时期,工作气压为0.6Pa并且Ag和SiO2的溅射速率分别为0.06纳米每秒和0.01纳米每秒。
本发明的有益效果:
1、这种基底制备方法过程简单,耗时少,成本低。
2、复合型多层膜银纳米线结构稳定,可控性强,纯度高。
3、对复合型多层膜银纳米线结构进行表面增强拉曼(SERS)性能检测,该结构具有丰富的热点,有很高的SERS活性,可应用于分子探测与识别技术、电子学、磁学、声学、光学等领域。
4、单质银在所有金属中具有最高的导电性和导热性,在许多应用领域,都具有潜在的用途,但是银的缺点在于化学稳定性和生物相容性较差,不能满足检测要求。而二氧化硅是一种化学惰性的、热稳定的、生物相容的绝缘体,二氧化硅不吸光,也不会干扰磁场,可保持结合的材料本身的性质,将二氧化硅和银结合到一起,二氧化硅可以改变金属周围的电介质环境,而且可以防止银发生氧化,使银纳米线结构存活时间更长。
附图说明
图1是利用磁控溅射技术在二维有序胶体球模板上制备出[Ag20~30nm/SiO23~5nm]n纳米多层膜阵列的示意图。
图2是本发明实施例1中[Ag30nm/SiO25nm]4纳米多层膜阵列侧面的SEM图。
图3是本发明实施例1中[Ag30nm/SiO25nm]4纳米多层膜阵列正面的SEM图。
图4和图5是本发明实施例1中将[Ag30nm/SiO25nm]4纳米多层膜阵列在氩气保护下,900℃退火处理后形成的复合型多层膜银纳米线结构SEM图。
图6是本发明实施例1中制备的复合型多层膜结构银纳米线mapping图。
具体实施方式
实施例1
首先采用自组装技术制备单层的二维有序胶体球模板,在附图1中a为胶体球模板示意图。具体步骤是:硅片衬底放到含有氨水、过氧化氢和水(体积比为1:2:6)的混合溶液中煮沸五分钟,然后依次用去离子水和乙醇溶液超声清洗三次。将其中一片硅片浸泡在10%的十二烷基硫酸钠溶液中24小时,得到亲水的衬底表面,其余的放在去离子水中保存用来做胶体球模板衬底。取体积比为1:1的聚苯乙烯溶液和去离子水混合,然后取一滴混合溶液滴在用十二烷基硫酸钠溶液浸泡过的硅片衬底上,待溶液均匀晕开之后,缓慢的倾斜浸入装有去离子水的容器中,由于水表面张力作用,在水的表面形成一层聚苯乙烯胶体小球的单层膜,再快速在单层膜周围滴入浓度为2%的十二烷基硫酸钠溶液,使其形成高度有序紧密堆积的胶体球模板,稍静止2分钟左右,再用保存在去离子水中的硅片衬底将单层膜捞起来,用滤纸吸去多余的水之后,在空气中自然挥发干燥后即可在硅衬底表面形成单层的聚苯乙烯小球二维有序阵列,中胶体球呈六方密堆排列,胶体球直径为200~700nm。
由图3所示,采用磁控溅射技术向二维有序胶体球模板上依次沉积30nm的银和5nm的二氧化硅,循环沉积4个周期,形成[Ag30nm/SiO25nm]4纳米多层膜阵列。如图2中SEM图所示,4层[Ag30nm/SiO25nm]纳米帽子形成了一个柱状结构,由于材料的属性不同相邻的银层之间由二氧化硅层隔开,二氧化硅层有效的避免了银层之间发生团聚。
为防止有机物质的干扰,将上面制得的[Ag30nm/SiO25nm]4纳米多层膜阵列浸泡在四氢呋喃溶液中两个小时,去掉胶体球模板后在氩气保护下进行900℃退火处理1小时,紧密排列的小球之间存在缺陷,当加热后,银会从缺陷中被烧出来,在多层膜上面形成了无序的纳米线结构,如附图4和图5所示,可看出产物为复合型多层膜结构的纳米线,而图6的mapping验证了纳米线中的元素含量大多为银。由此可知,我们将[Ag 30nm/SiO2 5nm]4纳米多层膜阵列退火处理后得到了复合型多层膜结构银纳米线。
本实施例中所用的磁控溅射系统是ATC 1800-F,USA AJA高真空多靶溅射仪,它是一种直流溅射和射频溅射相结合的磁控镀膜仪。通常采用直流溅射制备金属薄膜,采用交流溅射制备氧化物薄膜。通过溅射Ag和SiO2靶材制备复合型纳米图纹结构缝隙阵列基底。在正式镀膜之前,要预溅射20分钟左右。靶材和基底之间的距离为20厘米。在共溅射期间基底被旋转并且真空室的本底气压为2.4×10-4Pa。Ag靶和SiO2靶的溅射功率分别是20瓦和72瓦。在薄膜沉积的时期,工作气压为0.6Pa并且Ag和SiO2的溅射速率分别为0.06纳米每秒和0.01纳米每秒。
实施例2
本实施例与实施例1的不同之处在于采用磁控溅射技术向二维有序胶体球模板上依次沉积20-30nm的银和3-5nm的二氧化硅,循环沉积周期可为1~5个周期。所达到的技术效果与实施例1相同。
实施例3
本实施例与实施例1的不同之处在于[Ag 30nm/SiO2 5nm]n纳米多层膜阵列浸泡在四氢呋喃或氯仿、甲苯等有机溶剂中去掉聚苯乙烯二维有序胶体球序列模板。所达到的技术效果与实施例1相同。
实施例4
本实施例与实施例1的不同之处在于在氩气保护下进行800-900℃退火处理1-2小时。所达到的技术效果与实施例1相同,即在经过退火处理后,银会从缺陷中被烧出来,在多层膜上面形成了无序的纳米线结构。
本发明实施例1中磁控溅射的条件和参数是本领域常用的条件和参数,实施例1中磁控溅射步骤中所采用的条件和设定的参数为本领域常用的条件和参数,因此该条件参数仅作为实施本发明的优选方案,除实施例1中所使用的条件外,其他条件和参数制备出的[Ag20~30nm/SiO2 3~5nm]n复合结构经过800-900℃退火处理1-2小时也可达到本发明相同的技术效果。
Claims (9)
1.一种复合型多层膜结构银纳米线,其特征在于,其生长于结构为20~30nm的银和3~5nm的二氧化硅循环沉积n个周期形成的[Ag 20~30nm/SiO2 3~5nm]n纳米多层膜阵列的表面;其中5≥n≥1。
2.根据权利要求1所述的复合型多层膜结构银纳米线,其特征在于,其结构为30nm的银和5nm的二氧化硅循环沉积形成。
3.根据权利要求1所述的复合型多层膜结构银纳米线,其特征在于,[Ag 20~30nm/SiO23~5nm]n纳米多层膜阵列中的n=4。
4.一种权利要求1所述复合型多层膜结构银纳米线的制备方法,具体步骤如下:
步骤一、利用自组装技术制备聚苯乙烯二维有序胶体球序列模板,其中胶体球呈六方密堆排列,胶体球直径为200-700nm;
步骤二、采用磁控溅射技术向二维有序胶体球模板上依次沉积20-30nm的银和3-5nm的二氧化硅,循环沉积n个周期,形成[Ag 20~30nm/SiO2 3~5nm]n纳米多层膜阵列;其中5≥n≥1。
步骤三、将上一步制得的[Ag 20~30nm/SiO2 3~5nm]n纳米多层膜阵列浸泡在有机溶剂中去掉聚苯乙烯二维有序胶体球序列模板,然后在保护气氛下进行800-900℃退火处理1-2小时。
5.根据权利要求4所述的复合型多层膜结构银纳米线的制备方法,其特征在于,所述的有机溶剂为四氢呋喃、氯仿或甲苯。
6.根据权利要求4所述的复合型多层膜结构银纳米线的制备方法,其特征在于,退火处理的温度为900℃。
7.根据权利要求4所述的复合型多层膜结构银纳米线的制备方法,其特征在于,步骤二中进行磁控溅射时采用直流溅射制备银层,采用交流溅射制备二氧化硅层。
8.根据权利要求4所述的复合型多层膜结构银纳米线的制备方法,其特征在于,在磁控溅射期间基底被旋转并且真空室的本底气压为2.4×10-4Pa;Ag靶和SiO2靶的溅射功率分别是20瓦和72瓦。
9.根据权利要求4所述的复合型多层膜结构银纳米线的制备方法,其特征在于,在磁控溅射后的薄膜沉积的时期,工作气压为0.6Pa并且Ag和SiO2的溅射速率分别为0.06纳米每秒和0.01纳米每秒。
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