High-performance thermal insulation materials with broad application prospects have attracted great attention. The introduction of new microstructures into thermal protection materials can significantly improve the thermal insulation performance. The tubular microstructure has obvious advantages such as thermal insulation, lightweight, mechanical, and other properties. Therefore, the microtubular structure has become an important reference microstructure for the development of high-performance thermal insulation materials. In this paper, the carbon/ZrO2 aerogel composite microtube superfoams with excellent thermal protection properties were prepared by a vacuum filtration and high-temperature carbonization method. The ZrO2 aerogel precursor solution can be quickly and uniformly adsorbed on the inner and outer walls of cellulose microtubules. These adsorbed ZrO2 aerogel precursor solution films can be converted into ZrO2 alcohol gel shells under the acceleration and promotion effect of citric acid at 65 °C. The micromorphology of the ZrO2 aerogel shell on the inner and outer walls of the composite microtubes can be efficiently controlled by the concentration of the ZrO2 aerogel precursor solution and the carbonization temperature. The carbon/ZrO2 aerogel composite microtube superfoam exhibits a lower thermal conductivity, lower density, good mechanical properties, and high ablation resistance. The thermal conductivity of the carbon/ZrO2 aerogel composite microtube superfoam is as low as 0.040 ± 0.001 W m-1 K-1. The residual rate of the carbon/ZrO2 aerogel composite microtube superfoam is still as high as 84.33% after butane flame ablation for up to 3600 seconds.
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