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A facile and novel processable method to synthesize the Ni nanoparticles (Ni NPs) by tailoring their size in the matrix of the silicon oxycarbide (SiOC) ceramic system is reported. This method is based on polymer‐derived ceramics (PDCs), instead of the conventional powder route. The specific structural characteristics and magnetic properties of the various Ni NPs/SiOC composites as a function of carbon content are systematically investigated. The magnetic properties are experimentally investigated as a function of NP size and measurement temperature. It is demonstrated that the change in the size of Ni NPs (average from ≈4 to ≈ 19 nm) determines the magnetic nature of superparamagnetism. Zero‐field‐cooled (ZFC) and field‐cooled (FC) magnetization studies under magnetic fields of 100 Oe are performed. The saturatedMversusH(M–H) loops (saturation magnetization) increase and the coercivity decreases with the size reduction of Ni NPs. It is an indicator of the presence of superparamagnetic behavior and single‐domain NP for ceramic materials. 

Abstract In this study, novel ferromagnetic Ni‐containing silicon oxycarbide (SiOC–Ni) was successfully fabricated from a base polysiloxane (PSO) with the addition of nickel 2,4‐pentanedionate. The resultant SiOC–Ni nanocomposite consists of in situ formed Ni nanocrystallites with a small amount of NiO uniformly dispersed in the amorphous SiOC matrix, and the corresponding nanocrystallite size increases with the increase of the pyrolysis temperature. The formation of nickel silicides (Ni_xSi_y) is completely suppressed by the effect of water vapor during the pyrolysis. The fundamental phase evolution process and mechanisms are explained. In an argon atmosphere, the SiOC–Ni materials pyrolyzed at 900°C are stable up to 1000°C with less than 6 wt% weight loss; they exhibit desirable electrical conductivity up to ~900°C with the highest electrical conductivity at ~247 S/m. This series of SiOC–Ni materials also demonstrates exciting ferromagnetic behaviors. Their new semiconducting behavior with soft ferromagnetism presents promising application potentials for magnetic sensors, transformers, actuators, etc.