Mullite–Nickel Magnetic Nanocomposite Fibers Obtained from Electrospinning Followed by Thermal Reduction

Mullite–nickel nanocomposite fibers with Ni nanoparticles of controllable size, dispersion, and consequent magnetic properties were fabricated using sol–gel/electrospinning method, followed by thermal reduction. The fibers were electrospun from an aqueous solution containing sol–gel mullite precursor and nickel nitrate. These fibers were then heat treated in the reducing atmosphere between 550°C and 750°C to achieve fine‐dis persed metallic Ni nanoparticles (NPs). After the Ni 2+ was reduced to Ni NPs at 750°C for 10 h, the fibers were then directly transformed to the mullite fibers at 1000°C without the undesirable intermediate spinel phase. In many high‐temperature applications, mullite is the desired phase than spinel. If not fully reduced, the Ni 2+ cations induce early precipitation of spinel phase before mullite can be formed. This spinel phase was a solid solution between Al 2 NiO 4 and Al‐Si spinels, which later reacted with the residual silica and formed a mixture of mullite and spinel at 1400°C. The formation of spinel phase was suppressed or fully eliminated with chemically reducing Ni 2+ to metal NPs. The average size of nickel NPs within the fibers was ~20 nm, insensitive of the Ni concentration and reducing temperature. However, the Ni NPs on the fiber surface grew as large as ~80 nm due to fast surface diffusion. The magnetic nanocomposites exhibited ferromagnetism with saturation magnetization ( M s ) close to pure nickel of the same nominal weight, but coercivity ( H c ) much smaller than the bulk nickel, indicating the nature of bimodal magnetic nanoparticle distributions. The majority of small Ni NPs (~20 nm) within the fibers exhibited superparamagnetism, while the minor portion of relatively large NPs (50–80 nm) showed ferromagnetism.