CN113976904A - 一种微腔内光激发化学诱导生长贵金属纳米粒子的方法 - Google Patents
一种微腔内光激发化学诱导生长贵金属纳米粒子的方法 Download PDFInfo
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Abstract
本发明公开了一种微腔内光激发化学诱导生长贵金属纳米粒子的方法,包括以下步骤:(1)利用磁控溅射技术,在清洗后的硅片表面溅射生成Au膜,得金衬底;(2)对衬底进行退火处理;(3)利用磁控溅射技术,在退火后的衬底上表面依次溅射生成Au膜、SiO2膜,按需重复前面步骤,在衬底上表面形成多层Au/SiO2复合层;(4)将待腐蚀样品沿着某一条线解理出来以获得光滑的截面;将截面朝下放入腐蚀液中腐蚀SiO2膜,腐蚀后用清水洗涤腐蚀面,得金纳米空腔结构;(5)将金纳米空腔结构放入硝酸银溶液中,滴加柠檬酸钠溶液,在红光照射下,诱导银纳米粒子的生长。本发明工艺步骤简单,可操作性强,得到的贵金属纳米粒子分散、稳定。
Description
技术领域
本发明涉及纳米材料制备技术领域,尤其是涉及一种微腔内光激发化学诱导生长贵金属纳米粒子的方法。
背景技术
纳米材料的性能取决于其尺寸、结构、组成及排列方式等,而尺寸大小又是影响性能的主要因素。贵金属纳米粒子由于粒径小、比表面积大以及其它许多独特的性质,其被广泛应用于感光分析、表面拉曼效应增强等诸多领域。
稳定和单分散的贵金属纳米粒子是获得良好性能的前提以及实现生物探针良好的工作灵敏度的前提,通过对纳米颗粒的尺寸、形状和多层结构的控制得到相应的物理、化学性质一直是材料科学以及相关领域的热点。
发明内容
本发明是为了提供了一种微腔内光激发化学诱导生长贵金属纳米粒子的方法,工艺步骤简单,可操作性强,得到的银纳米粒子分散、稳定,且生长在狭长的纳米通道内,反应势垒将大大降低,可大大改善催化效果。
为了实现上述目的,本发明采用以下技术方案:一种微腔内光激发化学诱导生长贵金属纳米粒子的方法,包括以下步骤:
(1)利用磁控溅射技术,在清洗后的硅片表面溅射生成Au膜,得金衬底。
(2)对衬底进行退火处理。通过退火以加强金膜与硅片之间的附着力,保证结构的稳定性。
(3)利用磁控溅射技术,在退火后的衬底上表面依次溅射生成Au膜、SiO2膜,按需重复前面步骤,在衬底上表面形成多层Au/SiO2复合层。
(4)将复合层结构沿着某一条线解理出来以获得光滑的截面;将截面朝下放入腐蚀液中腐蚀SiO2膜,腐蚀后用清水洗涤腐蚀面,得金纳米空腔结构。
(5)将金纳米空腔结构放入硝酸银溶液中,滴加柠檬酸钠溶液,在红光照射下,诱导银纳米粒子的生长。
本发明通过腐蚀液对SiO2膜进行选择性腐蚀,使Au膜之间产生不同的间隙和空腔(微腔结构),达到一个热点增强的效果,利用结构中的不同间隙诱导生长出尺寸大小可控的金属纳米粒子;本发明的方法过程较为简单,易于操作,而且诱导生长出来的纳米粒子都是单分散的、稳定的,并且生长的纳米粒子在狭长的纳米通道内,反应势垒将大大降低,大大改善催化效果这种方法,本发明适用于多种金属纳米粒子的生长,例如Au、Ag、Pt等金属纳米粒子。
作为优选,所述清洗后的硅片通过以下方法得到:将硅片放入烧杯中,用酒精超声洗涤5min,再用去离子水超声洗涤5~15min。
作为优选,步骤(1)中,所述Au膜厚度为20~100nm。
作为优选,步骤(2)中,退火步骤为:将衬底温度从室温逐渐升温至400℃,保温1h。
作为优选,步骤(3)中,SiO2膜厚度为10~60nm,Au膜厚度为20~100nm。
作为优选,磁控溅射生成SiO2膜的工艺参数为:溅射功率50W,真空度0.6Pa,通入氩气流量为25sccm,垂直溅射;磁控溅射生成Au膜的工艺参数为:溅射功率10W,真空度0.6Pa,通入氩气流量为25sccm,垂直溅射。
作为优选,步骤(4)中,所述腐蚀液为10~30%氢氟酸溶液。
作为优选,步骤(5)中,所述硝酸银溶液浓度为0.5~2mM,柠檬酸钠溶液浓度为20~50mM,光照波长为400~700nm,生长时间为0.5~2h。
因此,本发明具有如下有益效果:工艺简单,易于操作,且诱导生长出来的纳米粒子都是单分散的、稳定的,并且生长的纳米粒子在狭长的纳米通道内,反应势垒将大大降低,大大改善催化效果这种方法,本发明适用于多种金属纳米粒子的生长,例如Au、Ag、Pt等金属纳米粒子。
附图说明
图1是实施例1中步骤(4)、步骤(5)的工艺示意图。
图2是实施例1中得到的Au/SiO2复合层电镜图。
图3是实施例1中得到的金纳米空腔结构电镜图。
图4是实施例1得到的银纳米粒子电镜图。
图5是实施例2得到的银纳米粒子电镜图。
图6是实施例3得到的银纳米粒子电镜图.
具体实施方式
下面结合附图和具体实施方式对本发明做进一步的描述。
实施例1
(1)利用磁控溅射技术,在清洗后的硅片表面溅射生成厚度为50nm的Au膜,得金衬底。
(2)对衬底进行退火处理,退火步骤为:将衬底温度从室温逐渐升温至400℃,保温1h。
(3)利用磁控溅射技术,在退火后的衬底上表面依次溅射生成厚度为50nm的Au膜、厚度为28nm的SiO2膜,按需重复前面步骤,在衬底上表面形成多层Au/SiO2复合层(如图2所示),得待腐蚀样品,其中,磁控溅射生成SiO2膜的工艺参数为:溅射功率50W,真空度0.6Pa,通入氩气流量为25sccm,垂直溅射;磁控溅射生成Au膜的工艺参数为:溅射功率10W,真空度0.6Pa,通入氩气流量为25sccm,垂直溅射。
(4)将待腐蚀样品沿着某一条线解理出来以获得光滑的截面;将截面朝下放入腐蚀液(10%氢氟酸溶液)中腐蚀SiO2膜,腐蚀后用清水洗涤腐蚀面,得金纳米空腔结构(如图1、图3所示)。
(5)将金纳米空腔结构放入适量浓度为1mM的硝酸银溶液中,滴加适量浓度为34mM的柠檬酸钠溶液,在700nm的红光照射下,诱导银纳米粒子的生长,生长时间为0.5h(如图1所示)。
本实施例中生成的银纳米粒子如图4所示。
实施例2
实施例2与实施例1不同之处在于:步骤(5)中,诱导银纳米粒子的生长,生长时间为1h,其余与实施例1完全相同。
本实施例中生成的银纳米粒子如图5所示。
实施例3
实施例3与实施例1不同之处在于:步骤(5)中,在633nm的红光照射下,诱导银纳米粒子的生长,生长时间为1h,其余与实施例1完全相同。
本实施例中生成的银纳米粒子如图6所示。
从图4、图5、图6可以看出,诱导生长出来的银纳米粒子都是单分散的、稳定的。
以上所述的实施例只是本发明的一种较佳的方案,并非对本发明作任何形式上的限制,在不超出权利要求所记载的技术方案的前提下还有其它的变体及改型。
Claims (8)
1.一种微腔内光激发化学诱导生长贵金属纳米粒子的方法,其特征在于,包括以下步骤:
(1)利用磁控溅射技术,在清洗后的硅片表面溅射生成Au膜,得金衬底;
(2)对衬底进行退火处理;
(3)利用磁控溅射技术,在退火后的衬底上表面依次溅射生成Au膜、SiO2膜,按需重复前面步骤,在衬底上表面形成多层Au/SiO2复合层;
(4)将复合层结构沿着某一条线解理出来以获得光滑的截面;将截面朝下放入腐蚀液中腐蚀SiO2膜,腐蚀后用清水洗涤腐蚀面,得金纳米空腔结构;
(5)将金纳米空腔结构放入硝酸银溶液中,滴加柠檬酸钠溶液,在红光照射下,诱导银纳米粒子的生长。
2.根据权利要求1所述的一种微腔内光激发化学诱导生长贵金属纳米粒子的方法,其特征在于,所述清洗后的硅片通过以下方法得到:将硅片放入烧杯中,用酒精超声洗涤5~15min,再用去离子水超声洗涤5~15min。
3.根据权利要求1或2所述的一种微腔内光激发化学诱导生长贵金属纳米粒子的方法,步骤(1)中,所述Au膜厚度为20~100nm。
4.根据权利要求1所述的一种微腔内光激发化学诱导生长贵金属纳米粒子的方法,其特征在于,步骤(2)中,退火步骤为:将衬底温度从室温逐渐升温至400℃,保温1h。
5.根据权利要求1所述的一种微腔内光激发化学诱导生长贵金属纳米粒子的方法,其特征在于,步骤(3)中,SiO2膜厚度为10~60nm,Au膜厚度为20~100nm。
6.根据权利要求1或5所述的一种微腔内光激发化学诱导生长贵金属纳米粒子的方法,其特征在于,磁控溅射生成SiO2膜的工艺参数为:溅射功率50W,真空度0.6Pa,通入氩气流量为25sccm,垂直溅射;磁控溅射生成Au膜的工艺参数为:溅射功率10W,真空度0.6Pa,通入氩气流量为25sccm,垂直溅射。
7.根据权利要求1所述的一种微腔内光激发化学诱导生长贵金属纳米粒子的方法,其特征在于,步骤(4)中,所述腐蚀液为10~30%氢氟酸溶液。
8.根据权利要求1所述的一种微腔内光激发化学诱导生长贵金属纳米粒子的方法,其特征在于,步骤(5)中,所述硝酸银溶液浓度为0.5~2mM,柠檬酸钠溶液浓度为20~50mM,光照波长为400~700nm,生长时间为0.5~2h。
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