La-Zn substituted M-type Ba hexaferrite powders were prepared by sol-gel (Mx) and organometallic precursor (Sk) methods with Fe/Ba ratio of 11.6 and 10.8, respectively. The compositions (LaZn)xBa 1 − x Fe 12 − x O 19 with 0.0 ≤ x ≤ 0.6 were annealed at 975 • C/2 h. The cationic site preferences of nonmagnetic La 3+ instead of Ba 2+ ions and Zn 2+ instead of Fe 3+ ions were determined by Mössbauer spectroscopy. The La 3+ ions substitute the large Ba 2+ ions at 2a site and for x ≥ 0.4 also at 4f 2 site. The nearly all Zn 2+ ions are placed at the 4f 1 sites. The thermomagnetic analysis of χ(ϑ) confirms that only the small substitutions for x ≤ 0.4 can be taken as a singlephase hexaferrites. The coercivity H c almost does not change at x = 0.2 for (Mx) samples and further decrease up to x = 0.6. For (Sk) samples at substitution x = 0.2 the values of H c are decreasing and at higher x the values nearly do not change. The Curie points, T c , slowly decrease with x for both (Mx) and (Sk) samples.