Dedicated to Prof. Dr. Josef Breu on the occasion of his 60th birthdayPhase-pure 6 nm spinel MnFe 2 O 4 nanoparticles with high specific surface area of 145 m 2 g À 1 were successfully prepared via microwave-assisted non-aqueous sol-gel synthesis. The phase evolution during postsynthetic thermal treatment was investigated systematically by various methods, including powder X-ray diffraction (PXRD), pair distribution function (PDF) analysis, and Raman spectroscopy. Our results show that the material decomposes to non-spinel binary compounds α-Mn 2 O 3 and α-Fe 2 O 3 at temperatures between 400 and 600 °C. The application potential of MnFe 2 O 4 nanoparticles with 3d 5 Mn(II) and Fe(III) ions with respect to the magnetic properties was demonstrated by superconducting quantum interference device (SQUID) magnetometry, with the as-synthesized nanoparticles reaching a high saturation magnetization of 2.62 μ B per formula unit (63.5 Am 2 kg À 1 ) at 10 K. We further highlight the visiblelight response of synthesized powders, making the materials promising for light-related applications, e. g. photocatalytic hydrogen evolution. An important additional feature of MnFe 2 O 4 nanoparticles is their good dispersibilty in polar or non-polar media, as a result of postsynthetic colloidal stabilization with betaine hydrochloride, oleic acid combined with oleylamine, or citric acid.