Abstract We report studies of the structural and microstructural properties of Sr₃Co₂Fe₂₄O₄₁ in bulk form and as thick films. The precursor powders for the bulk form were prepared following the sol-gel auto-combustion method. The prepared pellets were synthesized at 1200 °C to produce Sr₃Co₂Fe₂₄O₄₁. The XRD spectra of the bulks showed the characteristic peaks corresponding to the Z-type hexaferrite structure as a main phase and second phases of CoFe₂O₄ and Sr₃Fe₂O_7-x. The microstructure analysis of the cross-section of the bulk pellets revealed a hexagonal sheet structure. Large areas were observed of packages of hexagonal sheets where the separate hexagonal particles were ordered along the c axis. Sr₃Co₂Fe₂₄O₄₁ thick films were deposited from a suspension containing the Sr₃Co₂Fe₂₄O₄₁ powder. The microstructural analysis of the thick films showed that the particles had the perfect hexagonal shape typical for hexaferrites.