CN105575578A - 一种二氧化硅包覆磁性纳米粒子制备方法 - Google Patents

一种二氧化硅包覆磁性纳米粒子制备方法 Download PDF

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CN105575578A
CN105575578A CN201510763593.1A CN201510763593A CN105575578A CN 105575578 A CN105575578 A CN 105575578A CN 201510763593 A CN201510763593 A CN 201510763593A CN 105575578 A CN105575578 A CN 105575578A
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郝青
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Shaanxi Yuhang Electronic Co Ltd
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Shaanxi Yuhang Electronic Co Ltd
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
    • H01F1/10—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials non-metallic substances, e.g. ferrites, e.g. [(Ba,Sr)O(Fe2O3)6] ferrites with hexagonal structure
    • H01F1/11—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials non-metallic substances, e.g. ferrites, e.g. [(Ba,Sr)O(Fe2O3)6] ferrites with hexagonal structure in the form of particles
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
    • H01F1/34—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials non-metallic substances, e.g. ferrites
    • H01F1/36—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials non-metallic substances, e.g. ferrites in the form of particles

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  • Engineering & Computer Science (AREA)
  • Power Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Dispersion Chemistry (AREA)
  • Silicon Compounds (AREA)
  • Compounds Of Iron (AREA)

Abstract

一种二氧化硅包覆磁性纳米粒子制备方法，属于磁性纳米材料制备领域。提供一种操作简单，反应条件温和，产物具有超顺磁特性的二氧化硅包覆磁性纳米粒子制备方法。所述方法由多元醇法制得四氧化三铁纳米粒子，利用水解法在其表面生成了一层无定型二氧化硅包覆层。该制备方法过程简单，反应条件温和，Fe3O4/SiO2复合纳米粒子的饱和磁化强度为9.23emu·g-1，在常温下呈现超顺磁特性。

Description

一种二氧化硅包覆磁性纳米粒子制备方法
技术领域
本发明属于磁性纳米材料制备领域。
背景技术
四氧化三铁纳米粒子具有优异的磁性能和良好的生物相容性，在细胞分离、靶向给药、癌症热疗、磁共振成像等领域有广阔的应用前景，是当今纳米生物医学领域的研究热点之一。生物医学应用对四氧化三铁纳米粒子的表面性质有很高的要求。未经表面修饰的四氧化三铁纳米粒子亲水性差，易团聚，表面缺少活性基团，不能满足生物医学应用的要求。二氧化硅无毒无害、亲水性好、具有良好的生物相容性，易于实现表面功能化，做为四氧化三铁纳米粒子的表面修饰材料受到广泛关注。目前，制备SiO2包覆Fe304纳米粒子的方法主要微乳液法，反应在由水相、油相和表面活性剂组成的尺寸均匀的微乳液滴中进行，得到的纳米粒子形态规则、粒径分布较窄，但是操作复杂、大量表面活性剂难以分离。
发明内容
本发明的目的是提供一种操作简单，反应条件温和，产物具有超顺磁特性的二氧化硅包覆磁性纳米粒子制备方法。
本发明通过以下技术方案予以实现：一种二氧化硅包覆磁性纳米粒子制备方法，包括Fe304纳米粒子的制备和SiO2包覆Fe304纳米粒子的制备两步骤；
所述Fe304纳米粒子的制备步骤为，取一定的乙酰丙酮铁和三甘醇加入到回流加热反应装置中，在磁力搅拌和Ar气保护的条件下，将装置缓慢加热至沸腾，并保持回流一段时间。冷却后向反应溶液中加入乙酸乙醇使生成的四氧化三铁纳米粒子产生絮凝，磁性分离黑色产物，清洗数次，分散到乙醇中，即得到稳定的Fe3O4乙醇胶体溶液；
所述SiO2包覆Fe304纳米粒子的制备步骤为，在室温机械搅拌的条件下，向150mL的锥形瓶中加人一定量的Fe304胶体、去离子水、无水乙醇和正硅酸乙醇(TEOS)，然后加入氨水(质量分数26％)催化TEOS水解、缩合，反应12h后将产物磁性分离，用超纯水洗涤多次彻底除去未反应的原料，即得到Fe3O4/SiO2复合纳米粒子。
本发明具有如下有益效果：
该制备方法过程简单，反应条件温和，Fe3O4/SiO2复合纳米粒子的饱和磁化强度为9.23emu·g-1，在常温下呈现超顺磁特性。
具体实施方式
下面结合具体实施例对本发明做进一步说明。
具体实施例：本发明所述制备过程包括Fe304纳米粒子的制备和SiO2包覆Fe304纳米粒子的制备两步骤；
所述Fe304纳米粒子的制备步骤为，取一定的乙酰丙酮铁和三甘醇加入到回流加热反应装置中，在磁力搅拌和Ar气保护的条件下，将装置缓慢加热至沸腾，并保持回流一段时间。冷却后向反应溶液中加入乙酸乙醇使生成的四氧化三铁纳米粒子产生絮凝，磁性分离黑色产物，清洗数次，分散到乙醇中，即得到稳定的Fe3O4乙醇胶体溶液；
所述SiO2包覆Fe304纳米粒子的制备步骤为，在室温机械搅拌的条件下，向150mL的锥形瓶中加人一定量的Fe304胶体、去离子水、无水乙醇和正硅酸乙醇(TEOS)，然后加入氨水(质量分数26％)催化TEOS水解、缩合，反应12h后将产物磁性分离，用超纯水洗涤多次彻底除去未反应的原料，即得到Fe3O4/SiO2复合纳米粒子。
对制备的复合纳米粒子进行测试，其饱和磁化强度为9.23emu·g-1，在常温下呈现超顺磁特性，复合纳米粒子尺寸均匀，包覆层厚度可控，并保持了内核的超顺磁性，在生物医药、环境治理和工业催化等领域有广阔的应用前景。
以上内容是结合具体的实施方式对本发明所做的进一步详细说明，不能认定本发明的具体实施只局限于这些说明。对于本发明所属技术领域的普通技术人员来说，在不脱离本发明构思的前提下，还可以做出若干简单推演或替换，都应当视为属于本发明的保护范围。

Claims (1)

1.一种二氧化硅包覆磁性纳米粒子制备方法，其特征在于：包括Fe304纳米粒子的制备和SiO2包覆Fe304纳米粒子的制备两步骤；
（1）所述Fe304纳米粒子的制备步骤为，取一定的乙酰丙酮铁和三甘醇加入到回流加热反应装置中，在磁力搅拌和Ar气保护的条件下，将装置缓慢加热至沸腾，并保持回流一段时间。冷却后向反应溶液中加入乙酸乙醇使生成的四氧化三铁纳米粒子产生絮凝，磁性分离黑色产物，清洗数次，分散到乙醇中，即得到稳定的Fe3O4乙醇胶体溶液；
（2）所述SiO2包覆Fe304纳米粒子的制备步骤为，在室温机械搅拌的条件下，向150mL的锥形瓶中加人一定量的Fe304胶体、去离子水、无水乙醇和正硅酸乙醇(TEOS)，然后加入氨水(质量分数26％)催化TEOS水解、缩合，反应12h后将产物磁性分离，用超纯水洗涤多次彻底除去未反应的原料，即得到Fe3O4/SiO2复合纳米粒子。
CN201510763593.1A 2015-11-11 2015-11-11 一种二氧化硅包覆磁性纳米粒子制备方法 Pending CN105575578A (zh)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106876075A (zh) * 2017-03-09 2017-06-20 东南大学 一种磁性材料及其制备方法
CN113398848A (zh) * 2021-06-24 2021-09-17 苏州市德赫亚新纺织科技有限公司 一种可回收氧化壳聚糖包覆Fe304磁性微球的制备方法
US11348711B2 (en) * 2017-09-27 2022-05-31 Fujifilm Corporation Core-shell particle, fired product of core-shell particle, manufacturing method of core-shell particle, epsilon type iron oxide-based compound particle, manufacturing method of epsilon type iron oxide-based compound particle, magnetic recording medium, and manufacturing method of magnetic recording medium

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106876075A (zh) * 2017-03-09 2017-06-20 东南大学 一种磁性材料及其制备方法
US11348711B2 (en) * 2017-09-27 2022-05-31 Fujifilm Corporation Core-shell particle, fired product of core-shell particle, manufacturing method of core-shell particle, epsilon type iron oxide-based compound particle, manufacturing method of epsilon type iron oxide-based compound particle, magnetic recording medium, and manufacturing method of magnetic recording medium
CN113398848A (zh) * 2021-06-24 2021-09-17 苏州市德赫亚新纺织科技有限公司 一种可回收氧化壳聚糖包覆Fe304磁性微球的制备方法

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Application publication date: 20160511