本文与传统的柠檬酸盐方法不同，首次直接以柠檬酸铁为起始物质，经由络合物型溶胶凝胶过程非醇盐法制得超细的铁棕磁粉。使用ＤＴＡ、ＸＲＤ、ＦＴＩＲ、ＳＥＭ、ＢＥＴ以及磁天平等测试手段，表征了试样的特性，证明产物为纳米晶γＦｅ２Ｏ３，具有良好的磁性，ＸＲＤ给出了原始晶粒的精确尺寸３０．４ｎｍ，并与ＢＥＴ所测平均团粒尺寸１４７ｎｍ加以比较。讨论了络合物型溶胶凝胶过程的最适宜工艺条件和某些反应机理。 In this paper, different from the traditional citrate method, the ferric-ferromagnetic powder with ultrafine iron powder was prepared directly from ferric citrate through the non-alkoxide method of complex sol-gel process. The properties of the samples were characterized by DTA, XRD, FT-IR, SEM, BET and magnetic balance test. The results show that the product is nanocrystalline γ-Fe2O3 with good magnetic properties. XRD gives the exact size of the original grains 30.4 nm, and compared with the BET measured average particle size of 147 nm. The optimum conditions and some reaction mechanisms of the complex sol-gel process are discussed.