Ceramic fibers have the advantages of low density, high strength, high temperature resistance, and excellent mechanical vibration resistance. In this work, sol-gel and electrospinning were used to prepare ultra-fine rareearth-zirconate high-entropy ceramic (HEC) fibers with the composition of ((La 0.25 Nd 0.25 Sm 0.25 Gd 0.25 ) 0.75 Yb 0.25 ) 2 Zr 2 O 7 . The decomposition process and microscopic morphology of the fibers were characterized by thermogravimetry/differential scanning calorimetry, Fourier transform infrared and scanning electron microscope. The results indicated that defective fluorite-structured fibers with a smooth surface were obtained by calcining at 900-1000 • C, while fibers with the pyrochlore structure and the diameter within 140 nm were obtained by calcining at temperature higher than 1100 • C. The HEC fibers still maintain a continuous microstructure on the surface after calcination. In addition, the porous ceramics prepared from HEC fibers have a comparatively low thermal conductivity (0.22 ± 0.05 W m −1 K −1 , 25 • C). These promising properties indicate that the HEC fibers could be candidate materials for thermal-insulation application.

The order-disorder transition (ODT) of A2B2O7 compounds obtained enormous attention owing to the potential application for thermal barrier coating (TBC) design. In this work, the influence of ODT on the mechanical and thermophysical properties of dual-phase A2B2O7 high-entropy ceramics was investigated by substituting Ce4+ and Hf4+ with different ionic radii on B-sites (Zr4+). The X-ray diffraction (XRD), Raman, and transmission electron microscopy (TEM) results show that $$r_{\rm{A}^{3+}}/r_{\rm{B}^{4+}}=1.47$$ r A 3 + / r B 4 + = 1.47 is the critical value of ODT phase boundary with different doping B-site ion contents, and the energy dispersive spectroscopy (EDS) results further indicate the uniform distribution of elements. Interestingly, owing to the high intrinsic disorder derived from high-entropy effect, the A2B2O7 high-entropy ceramics exhibit unreduced modulus (E0 ≈ 230 GPa) and enhanced mechanical properties (HV ≈ 10 GPa, KIC ≈ 2.3 MPa·m0.5). A2B2O7 high-entropy ceramics exhibit excellent thermal stability with relatively high thermal expansion coefficients (TECs) (Hf0.25, 11.20×10−6 K−1, 1000 °C). Moreover, the matching calculation implied that the ODT further enhances the phonon scattering coefficient, leading to a relatively lower thermal conductivity of (La0.25Eu0.25Gd0.25Yb0.25)2(Zr0.85Ce0.15)2O7 (1.48–1.51 W/(m·K), 100–500 °C) compared with other components. This present work provides a novel composition design principle for high-entropy ceramics, as well as a material selection rule for high-temperature insulation applications.

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Excessive sintering shrinkage leads to severe deformation and cracking, affecting the microstructure and properties of porous ceramics. Therefore, reducing sintering shrinkage and achieving near‐net‐size forming is one of the effective ways to prepare high‐performance porous ceramics. Herein, low‐shrinkage porous mullite ceramics were prepared by foam‐gelcasting using kyanite as raw material and aluminum fluoride (AlF3) as additive, through volume expansion from phase transition and gas generated from the reaction. The effects of AlF3 content on the shrinkage, porosity, compressive strength, and thermal conductivity of mullite‐based porous ceramics were investigated. The results showed that with the increase of content, the sintering shrinkage decreased, the porosity increased, and mullite whiskers were produced. Porous mullite ceramics with 30 wt% AlF3 content exhibited a whisker structure with the lowest shrinkage of 3.5%, porosity of 85.2%, compressive strength of 3.06 ± 0.51 MPa, and thermal conductivity of 0.23 W/(m·K) at room temperature. The temperature difference between the front and back sides of the sample reached 710°C under high temperature fire resistance test. The low sintering shrinkage preparation process effectively reduces the subsequent processing cost, which is significant for the preparation of high‐performance porous ceramics.