Ceramic aerogels show excellent thermal insulation and
functional
performance for their unique nanoporous structure. However, conventional
ceramic aerogels often undergo structural collapse and performance
deterioration in high-temperature environments due to sintering, crystallization,
and/or phase transition. Here, we designed a TiCN/SiBCN ceramic aerogel
in which the TiCN phase was in situ formed through a carbothermal
reaction during pyrolysis. Benefiting from its unique pearl-necklace-like
structure, the TiCN/SiBCN aerogel exhibits a high specific surface
area (248 m2/g), a low thermal conductivity (0.08 W/m·K),
and a considerable compressive strength (2.2 MPa). The formation of
a stable TiCN phase endows the aerogel with significant resistance
to thermal decomposition and crystallization up to 1800 °C. Moreover,
the TiCN/SiBCN aerogel retains high surface area and low thermal conductivity
after thermal treatment, indicative of the stability and reliability
of the nanoporous structure. The TiCN/SiBCN ceramic aerogel with superior
thermal and structural stability is an ideal candidate for structural
and functional applications in high-temperature environments.