Abstract. Hematite nanoparticles were prepared by a procedure consisting in sonication of μ 3 -oxo trinuclear iron(III) acetate of composition [Fe 3 O(OOCCH 3 ) 6 (H 2 O) 3 ]NO 3 •4H 2 O, {Fe 3 O}NO 3 as iron source, in strong basic conditions followed by thermal treatment at 600˚C. The formation of the hematite was confi rmed by IR spectroscopy, X-ray powder diffraction and Raman spectroscopy while, the shape and size of the nanoparticles and their agglomeration were evidenced and estimated on the basis of the images taken with TEM techniques.Keywords: hematite, nanoparticles, iron oxides, sonochemistry. There are various forms of iron oxides [7]. They differ in composition, in the valence of Fe and, above all, in crystal structure. The most stable and wide spread oxide phase of iron is α-Fe 2 O 3 , where Fe has the lower Gibbs free energy [8]. Hematite has hexagonal structure of the corundum type with a close-packed oxygen lattice in which twothirds of the octahedral sites are occupied by Fe(III) ions. Bulk hematite is antiferromagnetic till Morin temperature (TM) (~260 K). Between TM and Neel temperature (TN) (~ 950K) it is weak ferromagnetic and above TN the hematite is paramagnetic [9,11]. These transitions are infl uenced by particle size, shape and crystallinity [9][10][11]. Particles smaller than 16 nm have a superparamagnetic behaviour at room temperature [12].Hematite nanoparticles proved to be effective catalyst in numerous reactions such as the decomposition of soot and NO x in diesel exhausts [13], oxidation of CO [14], photocatalytic degradation of salicylic acid [15], and FischerTropsch synthesis [16]. An iron-based solid catalyst is also normally used as a Lewis acid catalyst and/or support in homogeneous and heterogeneous catalysis [17]. Hematite nanoparticles could be applicable in water treatment technology for removing metal [18]. Hematite has a bandgap of 2-2.2 eV thus being semiconductor suitable for photocatalytic water-splitting with hydrogen formation [19].The hematite nanoparticles could be obtained by different routes: co-precipitation [20], microemulsion method [20,21], thermal decomposition [20,22] Our approach in this study is to obtain hematite nanoparticles using μ 3 -oxo homotrinuclear {Fe 3 O}NO 3 acetate as an iron source and easy sonochemical route as a synthesis procedure. The obtained product was characterized by adequate techniques (FTIR, energy-dispersive X-ray spectroscopy, Raman spectroscopy, wide angle X-ray spectroscopy, transmission electron microscopy), in order to evaluate the formed structure.