CN113046708B - 一种磁场调控纳米阵列结构的制备方法及其应用 - Google Patents
一种磁场调控纳米阵列结构的制备方法及其应用 Download PDFInfo
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Abstract
本发明公开了一种磁场调控纳米阵列结构的制备方法及其应用,涉及纳米复合材料微加工技术领域,包括以下制备步骤:(1)清洗硅片;(2)六方密排聚苯乙烯微球阵列结构制备;(3)球状包覆阵列结构制备;(4)周期性纳米孔洞阵列结构制备;(5)银纳米周期阵列制备;(6)纳米阵列结构;本发明纳米阵列结构SERS活性强,灵敏度高,对于新型纳米光子学器件、自标定测量都有积极意义。
Description
技术领域
本发明涉及纳米复合材料微加工技术领域,尤其涉及一种磁场调控纳米阵列结构的制备方法及其应用。
背景技术
表面增强拉曼散射(Surface-enhancement Raman scattering,SERS)是基于粗糙金属表面产生强烈拉曼散射的现象,是一种无损特征性识别的探测方法。SERS技术的光谱不仅具有普通拉曼光谱测量过程中特异性强、不损坏样品等特点,同时具有更高的探测极限,它弥补了传统拉曼信号探测时信号弱的缺点,因此SERS技术作为一种强大的分析工具已经被广泛应用于化学化工、生命科学、国防安全、表面科学等领域。
目前,现有技术中通常采用化学刻蚀等方法进行SERS基底的制备,例如,一种在中国专利文献上公开的“一种纳米金属球碗阵列结构的制备方法”,其公告号CN103626119A,其公开了一种纳米金属球碗阵列结构的制备方法,包括以下步骤:(1)对基片进行亲水性处理;(2)选择直径大小均匀一致的纳米乳胶溶液,利用旋涂法或提拉法在步骤(1)中经过亲水处理的极片上自组装单层紧密排列的纳米球阵列;(3)在步骤(2)所得到的纳米球阵列上,镀金属膜;(4)利用具有粘性、易固化成型或易操作低成本的材料将步骤(3)中表面镀金属膜的纳米阵列从基片上剥离下来;(5)利用具有腐蚀性的有机溶剂或反应离子刻蚀技术将步骤(4)中剥离下来的纳米球去除掉,即获得纳米金属球碗阵列结构。然而,该发明采用化学刻蚀法虽然制备步骤简单,但基底表面微结构均匀性较差,导致SERS光谱的稳定性和重现性较差。
发明内容
本发明是为了克服上述问题,提出了一种磁场调控纳米阵列结构的制备方法及其应用。
为了实现上述目的,本发明采用以下技术方案:
一种磁场调控纳米阵列结构的制备方法,包括以下制备步骤:
(1)清洗硅片;
(2)通过自组装的方法制备得到六方密排聚苯乙烯微球阵列结构;
(3)将六方密排聚苯乙烯微球阵列结构进行一次刻蚀制备得到溅射衬底;
(4)将溅射衬底表面进行垂直溅射,得到球状包覆阵列结构;
(5)将溅射完成的球状包覆阵列结构粘结转移到胶带表面;
(6)将胶带置于有机溶剂中进行聚苯乙烯微球溶解;
(7)对溶解后胶带表面纳米阵列结构进行二次刻蚀制备得到周期性纳米孔洞阵列结构;
(8)将周期性纳米孔洞阵列结构置于含银离子溶液中,调节光照促进反应,控制生长在纳米阵列结构表面的银纳米粒子,制备得到银纳米周期阵列;
(9)施加垂直于银纳米周期阵列的磁场,制备得到纳米阵列结构。
本发明在制备过程中,首先利用自组装的方法制备得到六方密排聚苯乙烯微球阵列结构,该阵列结构中每个聚苯乙烯微球周围均匀排列有六个聚苯乙烯微球,随后对聚苯乙烯微球进行刻蚀,使得聚苯乙烯微球的体积缩小到一定程度,为后续的磁控溅射留出空间,从而制备得到溅射衬底,随后对溅射衬底表面进行垂直溅射,得到球状包覆阵列结构,之后将球状包覆阵列结构转移到胶带表面,使得中间小孔朝上,漏出聚苯乙烯微粒,随后用有机溶剂将聚苯乙烯微球溶解,再通过二次蚀刻制备得到了一种中间带有大孔洞,大孔洞周围带有六个大小相同的小孔洞,形同类似于纽扣的高度有序且重复性好呈轴对称的周期性纳米孔洞阵列结构,大孔洞形成是由于胶体粒子与衬底接触使得薄膜不能生长。小孔形成是由于聚苯乙烯微粒相邻部分的阴影效应使局部薄膜生长速度较低,薄膜厚度较小,因此刻蚀使该部分最先被刻穿。随后将周期性纳米孔洞阵列结构置于含银离子溶液中,光照下在表面发生等离激元诱导反应,生成的Ag纳米粒子均匀地分布于小孔洞周围,这是由于促进化学反应的热点及电子在磁场下发生移动。最后在磁场作用下,Ag纳米粒子生长形貌实现纳米尺寸上的移动,由于洛伦兹力作用使得热点集中于周期性纳米孔洞阵列结构的半边,而制备得到纳米阵列结构。
本发明纳米阵列结构SERS活性强,灵敏度高,对于新型纳米光子学器件、自标定测量都有积极意义。
作为优选,步骤(1)中所述清洗硅片为将硅片置于体积比为1:2-3:5-6的氨水、过氧化氢和去离子水的混合溶液中,加热至沸腾5-10min后,冷却,将硅片依次采用去离子水和无水乙醇超声10-20min。
作为优选,步骤(2)所述六方密排聚苯乙烯微球阵列结构中聚苯乙烯微球的直径为200-500nm。
作为优选,步骤(3)中所述一次刻蚀为等离子刻蚀,刻蚀气体为体积比O2:Ar=4-5:1的混合气体,刻蚀后聚苯乙烯微球的直径为180-450nm,聚苯乙烯微球之间的间距为20-50nm。
作为优选,步骤(4)中所述垂直溅射靶材包括金,溅射厚度为310-330nm。
作为优选,步骤(6)中所述有机溶剂为四氢呋喃、二氯甲烷、三氯甲烷、甲苯、二甲基甲酰胺中的一种或几种。
作为优选,步骤(7)中所述二次刻蚀为等离子刻蚀,刻蚀气体为体积比O2:Ar=4-5:1的混合气体,刻蚀时间为3-4min。
本发明将刻蚀后聚苯乙烯微球的直径和间距以及二次刻蚀时间进行严格限定,使得制备得到的周期性纳米孔洞阵列结构中大孔洞直径在100nm左右,孔洞太小,不会形成明显作用的局域电场,对化学反应无明显影响。孔洞太大,则会使整体结构受到破坏。
作为优选,步骤(8)中所述含银离子溶液为0.1-0.5mmol/ml的硝酸银和100-120mmol/ml的柠檬酸钠混合溶液;所述光照光源为620-630nm红光,照射功率为3-5W,光源距离样品的距离为5-15cm,光照反应时间为5-8min。
作为优选,步骤(9)中所述磁场强度为300-500高斯。
一种上述方法制备得到的纳米阵列结构在检测肝癌细胞标志物中的应用。
因此,本发明具有如下有益效果:本发明纳米阵列结构SERS活性强,灵敏度高,对于新型纳米光子学器件、自标定测量都有积极意义。
附图说明
图1是本发明实施例1制备得到的周期性纳米孔洞阵列结构SEM图。
图2是本发明实施例1制备得到的银纳米周期阵列SEM图。
图3是本发明实施例1制备得到的纳米阵列结构SEM图。
图4是本发明对比例1制备得到的周期性纳米孔洞阵列结构SEM图。
图5是本发明对比例2制备得到的周期性纳米孔洞阵列结构SEM图。
图6是本发明实施例1中制备得到的周期性纳米孔洞阵列结构和最终产物纳米阵列结构SERS对比表征图。
图7是本发明实施例1制备得到的纳米阵列结构进行肝癌细胞标志物AFP检测时SERS表征图。
具体实施方式
下面结合具体实施方式对本发明做进一步的描述。
总实施例:一种磁场调控纳米阵列结构的制备方法,包括以下制备步骤:
(1)将硅片置于体积比为1:2-3:5-6的氨水、过氧化氢和去离子水的混合溶液中,加热至沸腾5-10min后,冷却,将硅片依次采用去离子水和无水乙醇超声10-20min进行硅片清洗;
(2)通过自组装的方法制备得到六方密排聚苯乙烯微球阵列结构,所述六方密排聚苯乙烯微球阵列结构中聚苯乙烯微球的直径为200-500nm;
(3)将六方密排聚苯乙烯微球阵列结构进行一次刻蚀,刻蚀气体为体积比O2:Ar=4-5:1的混合气体,制备得到溅射衬底制备得到溅射衬底;刻蚀后聚苯乙烯微球的直径为180-450nm,聚苯乙烯微球之间的间距为20-50nm;
(4)将溅射衬底表面进行垂直溅射金,溅射厚度为310-330nm,得到球状包覆阵列结构;
(5)将溅射完成的球状包覆阵列结构粘结转移到胶带表面;
(6)将胶带置于有机溶剂中进行聚苯乙烯微球溶解;所述有机溶剂为四氢呋喃、二氯甲烷、三氯甲烷、甲苯、二甲基甲酰胺中的一种或几种
(7)对溶解后胶带表面纳米阵列结构进行二次刻蚀,刻蚀气体为体积比O2:Ar=4-5:1的混合气体,刻蚀时间为3-4min,制备得到周期性纳米孔洞阵列结构;
(8)将周期性纳米孔洞阵列结构置于0.1-0.5mmol/ml的硝酸银和100-120mmol/ml的柠檬酸钠混合溶液中,调节光照,光照光源为620-630nm红光,照射功率为3-5W,光源距离样品的距离为5-15cm,光照反应时间为5-8min,控制生长在纳米阵列结构表面的银纳米粒子,制备得到银纳米周期阵列;
(9)施加300-500高斯、垂直于银纳米周期阵列的磁场,制备得到纳米阵列结构。
实施例1:一种磁场调控纳米阵列结构的制备方法,包括以下制备步骤:
(1)将硅片置于体积比为1:2:6的氨水、过氧化氢和去离子水的混合溶液中,加热至沸腾5min后,冷却,将硅片依次采用去离子水和无水乙醇超声20min进行硅片清洗;
(2)通过自组装的方法制备得到六方密排聚苯乙烯微球阵列结构,所述六方密排聚苯乙烯微球阵列结构中聚苯乙烯微球的直径为500nm;
(3)将六方密排聚苯乙烯微球阵列结构进行一次刻蚀,刻蚀气体为体积比O2:Ar=4:1的混合气体,制备得到溅射衬底制备得到溅射衬底;刻蚀后聚苯乙烯微球的直径为460nm,聚苯乙烯微球之间的间距为20nm;
(4)将溅射衬底表面进行垂直溅射金,溅射厚度为320nm,得到球状包覆阵列结构;
(5)将溅射完成的球状包覆阵列结构粘结转移到胶带表面;
(6)将胶带置于四氢呋喃中进行聚苯乙烯微球溶解;
(7)对溶解后胶带表面纳米阵列结构进行二次刻蚀,刻蚀气体为体积比O2:Ar=4-5:1的混合气体,刻蚀时间为3min,制备得到周期性纳米孔洞阵列结构,(如图1所示);
(8)将周期性纳米孔洞阵列结构置于0.2mmol/ml的硝酸银和110mmol/ml的柠檬酸钠混合溶液中,调节光照,光照光源为620nm红光,照射功率为4W,光源距离样品的距离为10cm,光照反应时间为7min,控制生长在纳米阵列结构表面的银纳米粒子,制备得到银纳米周期阵列,(如图2所示);
(9)施加400高斯、垂直于银纳米周期阵列的磁场,制备得到纳米阵列结构。
实施例2:一种磁场调控纳米阵列结构的制备方法,包括以下制备步骤:
(1)将硅片置于体积比为1:3:5的氨水、过氧化氢和去离子水的混合溶液中,加热至沸腾10min后,冷却,将硅片依次采用去离子水和无水乙醇超声10min进行硅片清洗;
(2)通过自组装的方法制备得到六方密排聚苯乙烯微球阵列结构,所述六方密排聚苯乙烯微球阵列结构中聚苯乙烯微球的直径为400nm;
(3)将六方密排聚苯乙烯微球阵列结构进行一次刻蚀,刻蚀气体为体积比O2:Ar=5:1的混合气体,制备得到溅射衬底制备得到溅射衬底;刻蚀后聚苯乙烯微球的直径为350nm,聚苯乙烯微球之间的间距为30nm;
(4)将溅射衬底表面进行垂直溅射金,溅射厚度为310nm,得到球状包覆阵列结构;
(5)将溅射完成的球状包覆阵列结构粘结转移到胶带表面;
(6)将胶带置于四氢呋喃中进行聚苯乙烯微球溶解;
(7)对溶解后胶带表面纳米阵列结构进行二次刻蚀,刻蚀气体为体积比O2:Ar=4:1的混合气体,刻蚀时间为4min,制备得到周期性纳米孔洞阵列结构;
(8)将周期性纳米孔洞阵列结构置于0.5mmol/ml的硝酸银和120mmol/ml的柠檬酸钠混合溶液中,调节光照,光照光源为630nm红光,照射功率为5W,光源距离样品的距离为5cm,光照反应时间为5min,控制生长在纳米阵列结构表面的银纳米粒子,制备得到银纳米周期阵列;
(9)施加300高斯、垂直于银纳米周期阵列的磁场,制备得到纳米阵列结构。
实施例3:一种磁场调控纳米阵列结构的制备方法,包括以下制备步骤:
(1)将硅片置于体积比为1:2:5的氨水、过氧化氢和去离子水的混合溶液中,加热至沸腾8min后,冷却,将硅片依次采用去离子水和无水乙醇超声15min进行硅片清洗;
(2)通过自组装的方法制备得到六方密排聚苯乙烯微球阵列结构,所述六方密排聚苯乙烯微球阵列结构中聚苯乙烯微球的直径为200nm;
(3)将六方密排聚苯乙烯微球阵列结构进行一次刻蚀,刻蚀气体为体积比O2:Ar=5:1的混合气体,制备得到溅射衬底制备得到溅射衬底;刻蚀后聚苯乙烯微球的直径为180nm,聚苯乙烯微球之间的间距为50nm;
(4)将溅射衬底表面进行垂直溅射金,溅射厚度为330nm,得到球状包覆阵列结构;
(5)将溅射完成的球状包覆阵列结构粘结转移到胶带表面;
(6)将胶带置于四氢呋喃中进行聚苯乙烯微球溶解;
(7)对溶解后胶带表面纳米阵列结构进行二次刻蚀,刻蚀气体为体积比O2:Ar=4:1的混合气体,刻蚀时间为3.5min,制备得到周期性纳米孔洞阵列结构;
(8)将周期性纳米孔洞阵列结构置于0.1mmol/ml的硝酸银和100mmol/ml的柠檬酸钠混合溶液中,调节光照,光照光源为630nm红光,照射功率为3W,光源距离样品的距离为5cm,光照反应时间为8min,控制生长在纳米阵列结构表面的银纳米粒子,制备得到银纳米周期阵列;
(9)施加500高斯、垂直于银纳米周期阵列的磁场,制备得到纳米阵列结构。
将实施例1制备得到的纳米阵列结构进行SEM表征,结构如图3所示,图中可知,本发明制备得到的纳米阵列结构中的集中于周期性纳米孔洞阵列结构的半边,(图中虚线区域)。
对比例1:与实施例1的区别在于,二次刻蚀时间为5min,超过限定范围。
对比例2:与实施例1的区别在于,二次刻蚀时间为2min,小于限定范围。
将对比例1-2制备得到的纳米阵列结构进行SEM表征,结构如图4-5所示,图中可知,二次刻蚀时间在限定范围外,无法形成完好的六孔结构。
将实施例1中制备得到的周期性纳米孔洞阵列结构和最终产物纳米阵列结构分别作为基底进行SERS检测,结果如图6所示,图中曲线从上至下依次为最终产物纳米阵列结构和周期性纳米孔洞阵列结构作为基底时SERS活性,对比可知,本发明最终产物纳米阵列结构具有更高的SERS活性。
将实施例1制备得到的矩形有序纳米阵列结构用于肝癌细胞标志物AFP检测;以5,5′-Dithiobis (succinimidyl-2-nitrobenzoate) (DSNB)为探针分子,连接AFP抗体,以其1335cm-1的峰为参考,实现对AFP的定量识别,结果如图7所示,图中曲线浓度从上至下为依次为4ng/ml、2ng/ml、1ng/ml、0.5ng/ml、0ng/ml,图中可知峰位移动量与AFP抗原浓度的对数成正比,从而能够实现定量测量。
本发明中所用原料、设备,若无特别说明,均为本领域的常用原料、设备;本发明中所用方法,若无特别说明,均为本领域的常规方法。
以上所述,仅是本发明的较佳实施例,并非对本发明作任何限制,凡是根据本发明技术实质对以上实施例所作的任何简单修改、变更以及等效变换,均仍属于本发明技术方案的保护范围。
Claims (7)
1.一种磁场调控纳米阵列结构的制备方法,其特征在于,包括以下制备步骤:
(1)清洗硅片;
(2)通过自组装的方法制备得到六方密排聚苯乙烯微球阵列结构;
(3)将六方密排聚苯乙烯微球阵列结构进行一次刻蚀制备得到溅射衬底;
(4)将溅射衬底表面进行垂直溅射,得到球状包覆阵列结构;
(5)将溅射完成的球状包覆阵列结构粘结转移到胶带表面;
(6)将胶带置于有机溶剂中进行聚苯乙烯微球溶解;
(7)对溶解后胶带表面纳米阵列结构进行二次刻蚀制备得到周期性纳米孔洞阵列结构;
(8)将周期性纳米孔洞阵列结构置于含银离子溶液中,调节光照促进反应,控制生长在纳米阵列结构表面的银纳米粒子,制备得到银纳米周期阵列;
(9)施加垂直于银纳米周期阵列的磁场,制备得到纳米阵列结构;
步骤(9)中,所述磁场的磁场强度为300-500高斯;
步骤(4)中,垂直溅射靶材包括金,溅射厚度为310-330nm;
步骤(7)中,所述二次刻蚀为等离子刻蚀,刻蚀气体为体积比O2:Ar=4-5:1的混合气体,刻蚀时间为3-4min。
2.根据权利要求1所述的一种磁场调控纳米阵列结构的制备方法,其特征在于,步骤(1)中所述清洗硅片为将硅片置于体积比为1:2-3:5-6的氨水、过氧化氢和去离子水的混合溶液中,加热至沸腾5-10min后,冷却,将硅片依次采用去离子水和无水乙醇超声10-20min。
3.根据权利要求1所述的一种磁场调控纳米阵列结构的制备方法,其特征在于,步骤(2)所述六方密排聚苯乙烯微球阵列结构中聚苯乙烯微球的直径为200-500nm。
4.根据权利要求1所述的一种磁场调控纳米阵列结构的制备方法,其特征在于,步骤(3)中所述一次刻蚀为等离子刻蚀,刻蚀气体为体积比O2:Ar=4-5:1的混合气体,刻蚀后聚苯乙烯微球的直径为180-450nm,聚苯乙烯微球之间的间距为20-50nm。
5.根据权利要求1所述的一种磁场调控纳米阵列结构的制备方法,其特征在于,步骤(6)中所述有机溶剂为四氢呋喃、二氯甲烷、三氯甲烷、甲苯、二甲基甲酰胺中的一种或几种。
6.根据权利要求1所述的一种磁场调控纳米阵列结构的制备方法,其特征在于,步骤(8)中所述含银离子溶液为0.1-0.5mmol/ml的硝酸银和100-120mmol/ml的柠檬酸钠混合溶液;所述光照光源为620-630nm红光,照射功率为3-5W,光源距离样品的距离为5-15cm,光照反应时间为5-8min。
7.一种如权利要求1-6任一所述方法制备得到的纳米阵列结构在检测肝癌细胞标志物中的应用。
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