CN103978225A - 一种快速制备稳定性纳米金溶胶的方法 - Google Patents
一种快速制备稳定性纳米金溶胶的方法 Download PDFInfo
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Abstract
本发明公开了一种快速制备稳定性纳米金溶胶的方法,是在超声辐照条件下,将一定量的水和不同浓度的氯金酸、柠檬酸三钠、过氧化氢混合,反应溶液初为无色,后渐渐转为红色,15min后即可得到稳定性好、高SERS活性的纳米金溶胶。本发明的优点是:与已有的技术相比,原料易得、无需加热,且一步反应即可获得SERS活性高的液相纳米金,制备方法更简便快速、而且稳定性高、分散性好。
Description
技术领域
本发明涉及化学领域,具体是一种过氧化氢还原超声波辐照快速制备稳定性纳米金溶胶的方法。
背景技术
金纳米粒子具有较高的电子密度、较好的生物相容性及新奇的光学特性,使之成为纳米科技首选的研究对象之一。在纳米溶胶中,纳米金溶胶具有较高的稳定性、特殊的表面等离子体共振(SPR)特性、较强的表面增强共振拉曼散射(SERS)特性等,其制备新方法备受人们注重。金纳米粒子的制备方法较多,有化学还原、微波、紫外光引发还原、电化学、模板制备法等。纳米金溶胶制备常用柠檬酸三钠热还原法、硼氢化钠还原法。柠檬酸三钠热还原法需要在较高温度下加热,操作不便;硼氢化钠还原法制备的金胶较稳定,但其SERS活性较弱。因此,发展简便快速、高SERS活性、稳定的纳米金溶胶制备方法很有必要。过氧化氢是一种常用的化学试剂,其残留物易被纳米粒子催化分解为水和氧气而对后续研究无影响。目前尚未见用过氧化氢、超声波辐照下制备高SERS活性的纳米金溶胶的报道。
发明内容
本发明的目的是为了克服现有技术的不足而公开一种快速制备稳定性纳米金溶胶的方法。
实现本发明目的的技术方案是:
一种快速制备稳定性纳米金溶胶的方法,具体是:
在超声辐照条件下,将一定量的水和不同浓度的氯金酸、柠檬酸三钠、过氧化氢混合,反应溶液初为无色,后渐渐转为红色,15min后即可得到稳定性好、高SERS活性、稳定的纳米金溶胶。
所述的氯金酸浓度为:1%(质量体积比浓度)、柠檬酸三钠浓度为:60mmol/L、过氧化氢浓度为:30%(质量浓度),
所述氯金酸、柠檬酸三钠和过氧化氢的体积份数比为:氯金酸:柠檬酸三钠:过氧化氢=1:3:0.24。
本发明的优点是:与已有的技术相比,原料易得、无需加热,且一步反应即可获得稳定的液相纳米金溶胶,制备方法更简便快速、而且稳定性高、分散性好、SERS活性高。
附图说明:
图1为本发明的纳米金溶胶1.5mL加水至2.0 mL测量获得的可见光吸收光谱图;
图2为本发明的纳米金溶胶1.5mL加水至2.0 mL测量获得的共振散射光谱图;
图3为本发明的纳米金溶胶1.0 mL+50 mmol/L HCl+0.5μmol/L 罗丹明6G测量获得的拉曼光谱图;
图4为本发明的纳米金溶胶的扫描电镜图。
具体实施方式
实施例:
一种制备纳米金溶胶的方法,包括如下步骤:
取一洁净的100mL锥形瓶,加入47.88 mL 二次蒸馏水,置于SK3300B型超声波仪中,开启仪器开关,然后依次向瓶中加入500μL 1%的氯金酸,1.5 mL 60 mmol/L柠檬酸三钠,120μL 30% H2O2。溶液初期为无色,后渐渐转为红色,15min后,取出溶液,即可获得纳米金溶胶,室温静置 12 h使剩余的H2O2分解后,放入4℃冰箱保存。
本发明制备的纳米金溶胶的可见吸收光谱,在534nm处有最大吸收峰;其共振散射光谱,在302nm、370nm、564nm处有三个共振散射峰;其拉曼光谱图,在1505cm-1处有较强的拉曼位移峰, 其扫描电镜图,金纳米粒子呈球形,平均粒径为20nm。制备的纳米金溶胶在三个月内测定吸收值、共振散射值、拉曼散射值,结果均不变,说明该溶胶稳定性较好。
Claims (3)
1.一种快速制备稳定性纳米金溶胶的方法,其特征是:
在超声辐照条件下,将一定量的水和不同浓度的氯金酸、柠檬酸三钠、过氧化氢混合,反应溶液初为无色,后渐渐转为红色,15min后即可得到稳定性好、高SERS活性的纳米金溶胶。
2.根据权利要求1所述的方法,其特征是:所述的氯金酸浓度为:1%(质量体积比浓度)、柠檬酸三钠浓度为:60mmol/L、过氧化氢浓度为:30%(质量浓度)。
3.根据权利要求1所述的方法,其特征是:所述氯金酸、柠檬酸三钠和过氧化氢的体积份数比为:氯金酸:柠檬酸三钠:过氧化氢=1:3:0.24。
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Citations (5)
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CN101844231A (zh) * | 2010-06-23 | 2010-09-29 | 黑龙江大学 | 贵金属自组装胶体晶体的制备方法 |
CN102166657A (zh) * | 2011-04-11 | 2011-08-31 | 北京化工大学 | 一种快速制备纳米金的方法 |
CN102847951A (zh) * | 2012-07-24 | 2013-01-02 | 浙江理工大学 | 一种过氧化氢酶还原四氯金酸制备金纳米粒子的方法 |
KR20130095957A (ko) * | 2012-02-21 | 2013-08-29 | 한국항공대학교산학협력단 | 초음파 발생 수조를 이용한 금나노유체의 제조방법 |
KR101335152B1 (ko) * | 2013-02-27 | 2013-12-31 | 강원대학교산학협력단 | 음향화학적 환원반응에 의한 금속 나노입자의 제조방법 |
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Publication number | Priority date | Publication date | Assignee | Title |
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CN101844231A (zh) * | 2010-06-23 | 2010-09-29 | 黑龙江大学 | 贵金属自组装胶体晶体的制备方法 |
CN102166657A (zh) * | 2011-04-11 | 2011-08-31 | 北京化工大学 | 一种快速制备纳米金的方法 |
KR20130095957A (ko) * | 2012-02-21 | 2013-08-29 | 한국항공대학교산학협력단 | 초음파 발생 수조를 이용한 금나노유체의 제조방법 |
CN102847951A (zh) * | 2012-07-24 | 2013-01-02 | 浙江理工大学 | 一种过氧化氢酶还原四氯金酸制备金纳米粒子的方法 |
KR101335152B1 (ko) * | 2013-02-27 | 2013-12-31 | 강원대학교산학협력단 | 음향화학적 환원반응에 의한 금속 나노입자의 제조방법 |
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