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采用高分辨电子显微镜(HREM)和扫描透射电子显微镜(STEM)成像、能谱分析(EDX)和电子能量损失谱(EELS)研究 CoFe2O4 铁氧体纳米颗粒在硅气凝胶基质中的情况。

A transmission electron microscopy study of CoFe2O4 ferrite nanoparticles in silica aerogel matrix using HREM and STEM imaging and EDX spectroscopy and EELS.

机构信息

Dipartimento di Scienze Chimiche and INSTM, Università di Cagliari, Monserrato, Cagliari, Italy.

出版信息

Microsc Microanal. 2010 Apr;16(2):200-9. doi: 10.1017/S1431927610000061. Epub 2010 Mar 4.


DOI:10.1017/S1431927610000061
PMID:20199712
Abstract

Magnetic nanocomposite materials consisting of 5 and 10 wt% CoFe2O4 nanoparticles in a silica aerogel matrix have been synthesized by the sol-gel method. For the CoFe2O4-10wt% sample, bright-field scanning transmission electron microscopy (BF STEM) and high-resolution transmission electron microscopy (HREM) images showed distinct, rounded CoFe2O4 nanoparticles, with typical diameters of roughly 8 nm. For the CoFe2O4-5wt% sample, BF STEM images and energy dispersive X-ray (EDX) measurements showed CoFe2O4 nanoparticles with diameters of roughly 3 +/- 1 nm. EDX measurements indicate that all nanoparticles consist of stoichiometric CoFe2O4, and electron energy-loss spectroscopy measurements from lines crossing nanoparticles in the CoFe2O4-10wt% sample show a uniform composition within nanoparticles, with a precision of at best than +/-0.5 nm in analysis position. BF STEM images obtained for the CoFe2O4-10wt% sample showed many "needle-like" nanostructures that typically have a length of 10 nm and a width of 1 nm, and frequently appear to be attached to nanoparticles. These needle-like nanostructures are observed to contain layers with interlayer spacing 0.33 +/- 0.1 nm, which could be consistent with Co silicate hydroxide, a known precursor phase in these nanocomposite materials.

摘要

由 5wt%和 10wt%CoFe2O4 纳米颗粒组成的磁性纳米复合材料已通过溶胶-凝胶法合成。对于 CoFe2O4-10wt%样品,明场扫描透射电子显微镜(BF STEM)和高分辨率透射电子显微镜(HREM)图像显示出明显的、圆形的 CoFe2O4 纳米颗粒,典型直径约为 8nm。对于 CoFe2O4-5wt%样品,BF STEM 图像和能量色散 X 射线(EDX)测量显示 CoFe2O4 纳米颗粒的直径约为 3±1nm。EDX 测量表明所有纳米颗粒都由化学计量比的 CoFe2O4 组成,并且 CoFe2O4-10wt%样品中穿过纳米颗粒的线的电子能量损失光谱测量表明纳米颗粒内的组成均匀,分析位置的精度最好优于±0.5nm。对于 CoFe2O4-10wt%样品获得的 BF STEM 图像显示出许多“针状”纳米结构,其通常具有 10nm 的长度和 1nm 的宽度,并且经常似乎附着在纳米颗粒上。这些针状纳米结构被观察到包含具有 0.33±0.1nm 层间距的层,这与这些纳米复合材料中的 Co 硅酸盐氢氧化物相吻合,这是一种已知的前体相。

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