摘要
我们用水解法合成了不同粒径的纳米α-Fe_2O_3(粒径为10-63nm)，还利用水热法合成了不同粒径的纳米α-FeOOH(粒径为12.8-31.6nm)。利用X射线粉末衍射(XRD)、透射电镜(TEM)、场发射扫描电镜(FESEM)、红外光谱(IR)、热重-差热(TG-DTA)、紫外-可见光谱(UV-VIS)和磁性测试等实验表征手段，对合成的纳米α-Fe_2O_3和α-FeOOH进行了物理化学性质与尺寸效应关系的研究。在纳米α-Fe_2O_3体系中，随着粒径的减小，纳米α-Fe_2O_3表现出晶格膨胀，轴比c／a增加。这一结论明显的与早期文献研究的结果不同，这些研究认为在小粒径时，α-Fe_2O_3具有高的晶格对称性。对纳米α-Fe_2O_3的表面水合作用的研究发现，表面水合作用与粒径有强烈的依赖关系，粒径越小，其表面水合作用越强。纳米α-Fe_2O_3由于表面水合作用和晶格膨胀的缘故，其晶格振动，电子跃迁和磁性行为明显地发生变化。在这个工作中，我们首次报道了随着粒径的减小，540cm~(-1)垂直模式的振动频率发生红移，同时在可见光范围内，双激发跃迁的能量发生蓝移。粒子的矫顽力也随着尺寸的减小而明显减小。在纳米α-FeOOH体系中，我们重点研究了尺寸效应对纳米α-FeOOH受热失水过程中的影响，根据实验结果，不同于其他文献报道对失水过程的划分，我们发现纳米α-FeOOH的失水过程可划分为四个阶段。同时我们详细分析了各失水过程与粒径的依赖关系，研究发现在失去物理吸附水时，随着粒径的减小，DTA吸热峰对应的温度
α- Fe_2O_3 nanocrystals (10-63nm) with controlled diameters were successfully prepared by hydrolysis mothod, and different particle size of α-FeOOH nanocrystals (12.8-31.6nm) were prepared using hydrothermal mothod. The finite size effects in α-Fe_2O_3 nanocrystals and α-FeOOH nanocrystals were probed by X-ray diffraction (XRD) , infrared spectroscopy (IR) , thermogravimetric analysis (TG-DTA) , UV-visible spectrum (UV-VIS) , and magnetization measurements. With a size reduction, α-Fe_2O_3 nanocrystals showed a lattice expansion and an enlarged axial ratio of c/a that is in apparent contradiction to the previous conjecture of high lattice symmetry for α- Fe_2O_3 nanocrystals at small sizes. The surface terminations of α- Fe_2O_3 nanocrystals were found to be highly hydrated with a size dependence. The lattice vibrations, electronic transitions, and magnetic properties of α- Fe_2O_3 nanocrystals were significantly modified by surface hydration and lattice expansion. The finite size effects that occurred in α-Fe_2O_3 nanocrystals at small sizes were first
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