CN112974830A - 一种具有富集和sers检测生物分子的银修饰氧化铁纳米环的制备方法 - Google Patents
一种具有富集和sers检测生物分子的银修饰氧化铁纳米环的制备方法 Download PDFInfo
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Abstract
一种具有富集和SERS性能的银/氧化铁纳米环制备方法,包括:将无水三氯化铁溶解于去离子水中,形成溶液a;将磷酸二氢钠和无水硫酸钠溶解于去离子水中,形成溶液b;将溶液b倒入溶液a中形成溶液c;加热溶液c,之后离心分离收集产物,洗涤干燥,得到三氧化二铁纳米环;将三氧化二铁纳米环,赖氨酸和硝酸银溶解于去离子水中,形成溶液d;将硼氢化钠溶解于去离子水中,形成溶液e;将溶液e倒入溶液d中,形成溶液f;搅拌溶液f一段时间,之后离心分离收集产物,洗涤干燥后得到产物。本发明的方法以三氧化二铁为底物,通过赖氨酸将贵金属锚定在磁性金属氧化物表面,改善了溶液中低浓度生物分子SERS检测难的问题。
Description
技术领域
本发明具体涉及一种具有富集和SERS检测性能的银/氧化铁纳米环的制备方法。
背景技术
表面增强拉曼散射(SERS)是借助贵金属纳米结构表面产生的一种表征技术,其因具有灵敏度高、响应速度快和可以提供分子指纹信息的而受到人们的广泛关注。因此,制备SERS增强信号好、操作简单和价格便宜的SERS基底成为拓展SERS应用的策略之一。常见的SERS基底是通过化学法合成的贵金属(如金、银等)胶体基底,该基底价格便宜且易大规模制备,但易受环境和样品影响,纳米颗粒发生团聚,SERS增强效果减弱。相比于传统的SERS基底,与功能材料相结合的SERS基底(如:聚合物复合金属SERS基底、二维材料复合金属SERS基底、以及金属/金属氧化物SERS基底)具有独特的物理、化学性质,可以获得更好的增强效果,其中磁性金属氧化物因其独特的性质引起了人们的广泛关注。研究发现磁性复合SERS 基底可以利用其磁性对待测物分子进行富集,因而制备比表面积大、SERS热点多的磁性复合 SERS基底仍然成为SERS领域研究的热点之一。基于此,我们合成了银纳米颗粒修饰的氧化铁纳米环,由于磁性环状金属氧化物的超大比表面积,与分子的良好亲和力,有利于吸附目标分子,从而实现待测物分子低浓度的超灵敏检测。
发明内容
本发明的目的是提供一种具有富集和SERS检测性能的银修饰氧化铁纳米环,通过银/ 纳米环较大的比表面可以提供更多的SERS活性位点,改善常规SERS基底难以检测低浓度生物分子的问题,
为实现上述发明目的,本发明的技术方案具体如下:
一种具有富集和SERS检测性能的银修饰氧化铁纳米环的制备方法,包括以下步骤:
S1:将无水三氯化铁溶解于去离子水中,搅拌均匀,形成溶液a;
将磷酸二氢钠和无水硫酸钠溶解于去离子水中,搅拌均匀,形成溶液b;
S2:将溶液b倒入溶液a中,搅拌均匀,形成溶液c;加热溶液c一段时间,之后离心
分离收集产物,洗涤,得到三氧化二铁纳米环;
S3:将三氧化二铁纳米环,赖氨酸和硝酸银溶解于去离子水中,搅拌均匀,形成溶液
d;将硼氢化钠溶解于去离子水中,搅拌均匀,形成溶液e;
S4:将溶液e倒入溶液d中,搅拌均匀,形成溶液f;搅拌溶液f一段时间,之后离心分离收集产物,洗涤干燥后得到产物;
作为优选的技术方案,所述步骤S2具体包括:溶液c体积定容至80mL,将溶液c转移至反应釜中220℃加热48h,之后通过离心分离收集产物,然后用去离子水和无水乙醇将产物洗涤数次,得尺寸形貌均匀的三氧化二铁纳米环。
作为优选的技术方案,所述步骤S3中,将溶液d超声30min,三氧化二铁环和硝酸银的摩尔比为1:1。
本发明还提供了由上述方法制备的具有富集和SERS检测性能的银修饰氧化铁纳米环复合材料。
与现有技术相比,本发明的有益效果:
本发明的方法以三氧化二铁为底物,通过赖氨酸原位还原将银纳米颗粒修饰在三氧化二铁纳米环表面,通过把银修饰三氧化二铁环上来改善银纳米颗粒易发生团聚,SERS增强效果弱的问题;
本发明的方法通过将银纳米粒子和氧化铁结合,利用氧化铁材料较强的磁性富集能力,合成了兼具富集和SERS检测能力的银修饰氧化铁纳米环复合材料,改善了银纳米颗粒对低浓度生物分子检测难的问题。
附图说明
图1(左)Fe2O3纳米环的X-射线粉末衍射图(XRD);(右)Fe2O3纳米环的扫描电镜图(SEM);
图2(左)Ag@Fe2O3的X-射线粉末衍射图(XRD);(右)Ag@Fe2O3的透射电镜图 (TEM);
图3Ag@Fe2O3检测不同浓度R6G的SERS光谱图。
具体实施方式:
下面将结合本发明实施例中的附图,对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
实施例
1、前驱物的合成方法:
将无水三氯化铁(0.26g)溶解于去离子水中,搅拌均匀,形成溶液a;再将磷酸二氢钠(0.0017 g)和无水硫酸钠(0.0062g)溶解于去离子水中,搅拌均匀,形成溶液b;然后将溶液b倒入溶液a中,搅拌均匀,形成溶液c;转移至反应釜中加热24h,冷却至室温后离心分离收集产物,洗涤干燥,即可得到三氧化二铁纳米环。图1为在上述实验条件下通过溶剂热所得的产物的XRD(图1左)和扫描电镜图(图1右)。XRD图表明所得产物为较好结晶性的Fe2O3,扫描电镜图表明所得产物为环状结构。
2、银修饰氧化铁组装的复合材料:
将三氧化二铁纳米环,赖氨酸和硝酸银溶解于去离子水中,搅拌均匀,形成溶液d;将硼氢化钠溶解于去离子水中,搅拌均匀,形成溶液e;将溶液e倒入溶液d中,搅拌均匀,形成溶液f;搅拌溶液f一段时间,之后离心分离收集产物,洗涤干燥后得到产物;图2为通过加入NaBH4反应2h后的得到的产物的XRD(图2左)和透射电镜图TEM(图2右)。XRD 图表明所得产物为Ag@Fe2O3,TEM图(图2右)表明所得产物成功将银纳米颗粒修饰在氧化铁纳米环上。图3表明Ag@Fe2O3具有SERS活性且对R6G的检测可以低至1×10-8M。
Claims (6)
1.一种具有富集和SERS检测性能的银修饰氧化铁纳米环的制备方法,包括以下步骤:
S1:将无水三氯化铁溶解于去离子水中,搅拌均匀,形成溶液a;将磷酸二氢钠和无水硫酸钠溶解于去离子水中,搅拌均匀,形成溶液b;
S2:将溶液b倒入溶液a中,搅拌均匀,形成溶液c;加热溶液c一段时间,之后离心分离收集产物,洗涤,得到三氧化二铁纳米环;
S3:将三氧化二铁纳米环,赖氨酸和硝酸银溶解于去离子水中,搅拌均匀,形成溶液d;将硼氢化钠溶解于去离子水中,搅拌均匀,形成溶液e;
S4:将溶液e倒入溶液d中,搅拌均匀,形成溶液f;搅拌溶液f一段时间,之后离心分离收集产物,洗涤干燥后得到产物。
2.根据权利要求1所述的方法,其特征在于,所述步骤S2包括:将溶液c体积定容至80mL,转移至反应釜中反应一段时间,之后通过离心分离收集产物,然后用去离子水和无水乙醇将产物洗涤数次,得尺寸形貌均匀的三氧化二铁纳米环。
3.根据权利要求2所述的方法,其特征在于,所述反应温度是220℃,反应时间是48h。
4.根据权利要求1所述的方法,其特征在于,所述步骤S3中还包括将溶液d超声30min。
5.根据权利要求1所述的方法,其特征在于,所述步骤S3中,三氧化二铁环和硝酸银的摩尔比为1:1。
6.由以上任一权利要求所述方法制备的具有富集和SERS检测性能的银修饰氧化铁纳米环复合材料。
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