Silicon‐containing ceramics fibers are ideal candidates for thermal resistance due to their incomparable thermo‐stability and chemical stability. Research into anti‐oxidation behavior of silicon‐containing ceramics through metal elements doping is important for the application in extreme high‐temperature environment. Thus, uniform belts‐like Zr‐doped SiOC ceramics fibers were successfully prepared by electrospinning and polymer‐derived ceramics routine with polycarbosilane (PCS) and zirconium butoxide as precursors. The morphology and dimension of the fibers were conveniently controlled by tuning PCS concentration, types of spinning additives and pyrolysis temperature. The ceramics fibers were composed of SiC, ZrO2 and SiO2 crystals, accompanied with amorphous SimZrnCxOy. The structure and compositions realized the excellent thermal stability above 1300°C and the enhanced flexibility. The obtained fibers maintained ultra‐low thermal conductivity of .038–.053 W/(m·K). Thus, the materials were anticipated to be ideal for the thermal insulation up to 1400°C or higher.
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