Itoh Hiroyuki, Sugimoto Tadao
Institute of Multidisciplinary Research for Advanced Materials, Tohoku University, Katahira 2-1-1, Aobaku, Sendai 980-8577, Japan.
J Colloid Interface Sci. 2003 Sep 15;265(2):283-95. doi: 10.1016/s0021-9797(03)00511-3.
As an application of the gel-sol method especially developed for the synthesis of general monodisperse particles in large quantities, uniform hematite (alpha-Fe2O3), magnetite (Fe3O4), and maghemite (gamma-Fe2O3) particles, precisely controlled in size, aspect ratio, and internal structure, have been prepared. For the synthesis of uniform ellipsoidal single-crystal particles of alpha-Fe2O3, a highly condensed suspension of fine beta-FeOOH particles doped with a prescribed amount of PO4(3-) ion in their interiors was aged at 140 degrees C for 24 h with seed particles of alpha-Fe2O3 in an acidic medium containing optimum concentrations of HCl and NaNO3. Systematic control of the aspect ratio and mean size was achieved by regulating the concentration of PO4(3-) ion incorporated into the beta-FeOOH particles and the number of seeds added. The resulting hematite particles were converted into magnetite by reduction in a H2 stream at 330 degrees C for 6 h; the magnetite was then oxidized to maghemite in an air stream at 240 degrees C for 2 h. Magnetite and maghemite thus prepared retained the original shape of the hematite. On the other hand, polycrystalline hematite particles of different sizes and aspect ratios were also prepared by aging a condensed Fe(OH)3 gel in the presence of different concentrations of SO4(2-) ion and seeds. The polycrystalline hematite particles were similarly converted into magnetite and then maghemite. The magnetic properties of these magnetite and maghemite particles were analyzed as a function of their mean particle volume, aspect ratio, and internal structure.
作为一种专门为大量合成一般单分散颗粒而开发的凝胶-溶胶法的应用,已经制备出尺寸、纵横比和内部结构得到精确控制的均匀赤铁矿(α-Fe₂O₃)、磁铁矿(Fe₃O₄)和磁赤铁矿(γ-Fe₂O₃)颗粒。为了合成均匀的α-Fe₂O₃椭球形单晶颗粒,将内部掺杂规定量PO₄³⁻离子的细β-FeOOH颗粒的高度浓缩悬浮液,在含有最佳浓度HCl和NaNO₃的酸性介质中,于140℃下与α-Fe₂O₃籽晶一起老化24小时。通过调节掺入β-FeOOH颗粒中的PO₄³⁻离子浓度和添加的籽晶数量,实现了纵横比和平均尺寸的系统控制。所得赤铁矿颗粒在330℃的H₂气流中还原6小时转化为磁铁矿;然后磁铁矿在240℃的空气流中氧化2小时转化为磁赤铁矿。这样制备的磁铁矿和磁赤铁矿保留了赤铁矿的原始形状。另一方面,还通过在不同浓度的SO₄²⁻离子和籽晶存在下老化浓缩的Fe(OH)₃凝胶,制备了不同尺寸和纵横比的多晶赤铁矿颗粒。这些多晶赤铁矿颗粒同样被转化为磁铁矿,然后再转化为磁赤铁矿。分析了这些磁铁矿和磁赤铁矿颗粒的磁性能与其平均颗粒体积、纵横比和内部结构的关系。