内包金属铁的富勒烯的功能化修饰及磁性能研究
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摘要
目前纳米磁性材料作为一种安全、高效、经济的医学药用载体,已在癌症研究中表现出广阔的发展空间。作为生物磁性载体材料应具有较小的粒径,较小的毒性,好的磁性,低的造价,稳定的物理化学性能以及良好的生物相容性等特性。
二十世纪末富勒烯被发现以来,内包金属原子簇的富勒烯因其在医药和材料方面有着非常广阔的应用前景,引起了理论和实验科学家的广泛关注。富勒烯是一系列纯碳组成的原子簇的总称。它们是由非平面的五元环、六元环等构成的封闭式空心球形或椭球形结构的共轭烯,Fe@富勒烯就是中心包了铁的球形共轭烯。功能化的Fe@富勒烯具有独特的笼状结构,粒径小,物理化学性能优异且磁性能良好,而且表面接上的功能基团可以显著改善富勒烯在动物体液中的生物相容性和流动性,有利于在外磁场作用下将药物直接输运至病灶,因此有望作为靶向载体材料研究的热点。
为了制备一种新型的磁性靶向载体材料,本文采用化学气相沉积法(CVD)在高温条件下制备了Fe@富勒烯,并采用浓硫酸氧化法对富勒烯进行羟基化后处理。实验通过扫描电子显微镜、X射线衍射分析、红外光谱、紫外光谱及振动样品磁强计等手段对产物的各种结构和性能进行了表征分析。
结果表明：
1)采用化学气相沉积(CVD)法以乙炔为碳源制备的Fe@富勒烯表面形貌较好,平均粒径均在100nm左右,较好的满足了作为靶向载体材料的小粒径要求；产物包裹的铁元素主要以铁单质和四氧化三铁等形态存在,这为其具备顺磁性能提供了可能性；
2)功能化修饰后其形貌和结构有一定程度的变化,石墨化程度和产物纯度还有进一步的提高,同时使Fe@富勒烯被亲水官能团—OH包覆,从而显著提高了Fe@富勒烯在水中的分散性和稳定性,使得富勒烯在生物体液中的流动性和生物相容性得到提高,为产物的生物学应用提供了必要条件；
3)VSM测试表明修饰后样品的饱和磁化强度为13.641emu/g,矫顽力545.77G,与修饰前的的饱和磁化强度17.744emu/g和矫顽力553.86G相比,略有降低,但是依然具有较好的顺磁性,为拓展Fe@富勒烯在磁性靶向载体材料方面的应用提供了重要的理论依据。
With the development of the medicine science, preparing a new type of magnetic material for medicine carrier has attracted great attention. In this work, fullerene related material is selected as a candidate for application in the field of biomedicine. Late-model Fe@fullerene was synthesized under high temperature by using chemical vapor deposition (CVD) method. The products were chemically oxidized using concentrated sulfuric (98%) at 90℃under reflux and further investigated by using different kind of instruments, such as scanning electron microscopy (SEM), X-ray diffraction, X-ray photo electron spectroscopy, infrared absorption spectroscopy, UV-Vis Absorption Spectrum and vibrating sample magnetometer (VSM).
The results showed that:
(1) Fe@ fullerenes were synthesized under 1000℃temperature by CVD method using acetylene as carbon source.The products are all Fe@fullerene with diameters less than 100nm. The iron elements included mostly exists in the metallic iron and Fe3O4 state, which make it possible for Fe@Fllerene to be a kind of paramagnetic body. Simultaneously, XRD investigation indicated that the graphitization degree, purity and stability of physic-chemical properties of the products increased obviously.
(2) Fe@fullerene were coated with hydrophilic functional group-OH through acidification, which effectively improved its distribution and stability in water.
(3) VSM test indicated that the magnetization and coercivity of Fe@ fullerene are 13.641 emu/g and 545.77 G respectively. In comparison with 17.744 emu/g and 553.86G of fullerene before being oxidized by concentrated sulfuric, it had decreased a little. However, the magnetic property of the Fe@fullerene did not changed a lot. All of the results here provided theoretical foundation for the development in exploratory of magnetic carrier materials in the future. Following is the particular results in this work.
二十世纪末富勒烯被发现以来,内包金属原子簇的富勒烯因其在医药和材料方面有着非常广阔的应用前景,引起了理论和实验科学家的广泛关注。富勒烯是一系列纯碳组成的原子簇的总称。它们是由非平面的五元环、六元环等构成的封闭式空心球形或椭球形结构的共轭烯,Fe@富勒烯就是中心包了铁的球形共轭烯。功能化的Fe@富勒烯具有独特的笼状结构,粒径小,物理化学性能优异且磁性能良好,而且表面接上的功能基团可以显著改善富勒烯在动物体液中的生物相容性和流动性,有利于在外磁场作用下将药物直接输运至病灶,因此有望作为靶向载体材料研究的热点。
为了制备一种新型的磁性靶向载体材料,本文采用化学气相沉积法(CVD)在高温条件下制备了Fe@富勒烯,并采用浓硫酸氧化法对富勒烯进行羟基化后处理。实验通过扫描电子显微镜、X射线衍射分析、红外光谱、紫外光谱及振动样品磁强计等手段对产物的各种结构和性能进行了表征分析。
结果表明：
1)采用化学气相沉积(CVD)法以乙炔为碳源制备的Fe@富勒烯表面形貌较好,平均粒径均在100nm左右,较好的满足了作为靶向载体材料的小粒径要求；产物包裹的铁元素主要以铁单质和四氧化三铁等形态存在,这为其具备顺磁性能提供了可能性；
2)功能化修饰后其形貌和结构有一定程度的变化,石墨化程度和产物纯度还有进一步的提高,同时使Fe@富勒烯被亲水官能团—OH包覆,从而显著提高了Fe@富勒烯在水中的分散性和稳定性,使得富勒烯在生物体液中的流动性和生物相容性得到提高,为产物的生物学应用提供了必要条件；
3)VSM测试表明修饰后样品的饱和磁化强度为13.641emu/g,矫顽力545.77G,与修饰前的的饱和磁化强度17.744emu/g和矫顽力553.86G相比,略有降低,但是依然具有较好的顺磁性,为拓展Fe@富勒烯在磁性靶向载体材料方面的应用提供了重要的理论依据。
With the development of the medicine science, preparing a new type of magnetic material for medicine carrier has attracted great attention. In this work, fullerene related material is selected as a candidate for application in the field of biomedicine. Late-model Fe@fullerene was synthesized under high temperature by using chemical vapor deposition (CVD) method. The products were chemically oxidized using concentrated sulfuric (98%) at 90℃under reflux and further investigated by using different kind of instruments, such as scanning electron microscopy (SEM), X-ray diffraction, X-ray photo electron spectroscopy, infrared absorption spectroscopy, UV-Vis Absorption Spectrum and vibrating sample magnetometer (VSM).
The results showed that:
(1) Fe@ fullerenes were synthesized under 1000℃temperature by CVD method using acetylene as carbon source.The products are all Fe@fullerene with diameters less than 100nm. The iron elements included mostly exists in the metallic iron and Fe3O4 state, which make it possible for Fe@Fllerene to be a kind of paramagnetic body. Simultaneously, XRD investigation indicated that the graphitization degree, purity and stability of physic-chemical properties of the products increased obviously.
(2) Fe@fullerene were coated with hydrophilic functional group-OH through acidification, which effectively improved its distribution and stability in water.
(3) VSM test indicated that the magnetization and coercivity of Fe@ fullerene are 13.641 emu/g and 545.77 G respectively. In comparison with 17.744 emu/g and 553.86G of fullerene before being oxidized by concentrated sulfuric, it had decreased a little. However, the magnetic property of the Fe@fullerene did not changed a lot. All of the results here provided theoretical foundation for the development in exploratory of magnetic carrier materials in the future. Following is the particular results in this work.
引文
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