Topological Polymer Networks-Enabled Mechanically Strong Polyamide-Imide Aerogel Fibers for Thermal Insulation in Harsh Environments.

Aerogel fibers have sparked substantial interest as attractive candidates for thermal insulation materials. Developing aerogel fibers with the desired porous structure, good knittability, flame retardancy, and high- and low-temperature resistance is of great significance for practical applications; however, that is very challenging, especially by using an efficient method. Herein, mechanically strong and flexible aerogel fibers with remarkable thermal insulation performance are reported, which are achieved by constructing stiff-soft topological polymer networks and a multilevel hollow porous structure. The combination of polyamide-imide (PAI) with stiff chains and polyurethane (PU) with soft chains is first found to be able to form a topological entanglement architecture. More importantly, multilevel hollow pores can be constructed synchronously through just a one-step and green wet-spinning process. The resultant PAI/PU@340 aerogel fibers show an ultrahigh breaking strength of 94.5 MPa and superelastic property with a breaking strain of 20%. Furthermore, they can be knitted into fabrics with a low thermal conductivity of 25 mW/(m·K) and exhibit attractive thermal insulation property under extremely high (300 °C) and low temperatures (-191 °C), implying them as promising candidates for next-generation thermal insulation materials.

Significantly Enhanced Mechanical, Thermal, and Ablative Properties of the Lightweight Carbon Fabric/Phenol-Formaldehyde Resin/Siloxane Aerogels Ternary Interpenetrating Network.

Lightweight ablative thermal protection materials (TPMs), which can resist long-term ablation in an oxidizing atmosphere, are urgently required for aerospace vehicles. Herein, carbon fabric/phenol-formaldehyde resin/siloxane aerogels (CF/PFA/SiA) nanocomposite with interpenetrating network multiscale structure was developed via simple and efficient sol-gel followed by atmospheric pressure drying. The ternary networks structurally interpenetrating in macro-, micron-, and the nanoscales, chemically cross-linking at the molecular scale, and silica layer generated by in situ heating synergistically bring about low density (∼0.3 g cm-3), enhanced mechanical properties, thermal stability, and oxidation resistance, and a low thermal conductivity of 81 mW m-1 K-1. More intriguingly, good thermal protection with near-zero surface recession at 1300 °C for 300 s and remarkable thermal insulation with a back-side temperature below 60 °C at 20 mm thickness. The interpenetrating network strategy can be extended to other porous components with excellent high-temperature properties, such as ZrO2 and SiC, which will facilitate the improvement of lightweight ablative TPMs. Moreover, it may open a new avenue for fabricating multifunctional binary, ternary, and even multiple interpenetrating network materials.

A Passive-Active Anti/Deicing Coating Integrating Superhydrophobicity, Thermal Insulation, and Photo/Electrothermal Conversion Effects.

Anti/deicing coatings that combine active and passive methods can utilize various energy sources to achieve anti/deicing effects. However, poor photothermal or electrothermal performance and inevitable heat loss often reduce their anti/deicing efficiency. Herein, copper sulfide loaded activated biochar (AC@CuS) as photo/electric material, polydimethylsiloxane as hydrophobic component, thermally expandable microspheres as foaming agent, and an anti/deicing coating integrating thermal insulation, superhydrophobicity, photo/electrothermal effects was successfully constructed. Benefiting from the synergistic effect of superhydrophobicity and thermal insulation, the freezing time of water droplets on the coating surface is extended from 150 to 2140 s, showing excellent passive anti-icing performance. AC@CuS exhibits photo/electrothermal effects, and porous expanded microspheres reduce heat loss, which endows the coating with desirable photo/electrothermal conversion performance. Under the conditions of 0.2 W/cm2 electric power density (EPD) and 0.1 W/cm2 optical power density (OPD), the temperature of the coating increases from 24 to 96.4 and 113 °C, respectively. Interestingly, with a coheating of 0.05 W/cm2 weaker OPD and 0.05 W/cm2 lower EPD, the ice on the coating surface can be quickly melted in 2.5 min, showing synergistic deicing performance. In addition, the WCA of the prepared coating remains above 150° after mechanical damage, rain impact, UV irradiation, chemical corrosion, and high-temperature treatment, and good superhydrophobic durability ensures the anti/deicing durability of the coating.

Cellulose-derived carbon scaffolds with bidirectional gradient Fe3O4 distribution: Integration of green EMI shielding and thermal management.

Cellulose papers (CPs) possess a pore structure, rendering them ideal precursors for carbon scaffolds because of their renewability. However, achieving a tradeoff between high electromagnetic shielding effectiveness and low reflection coefficient poses a tremendous challenge for CP-based carbon scaffolds. To meet the challenge, leveraging the synergistic effect of gravity and evaporation dynamics, laminar CP-based carbon scaffolds with a bidirectional gradient distribution of Fe3O4 nanoparticles were fabricated via immersion, drying, and carbonization processes. The resulting carbon scaffold, owing to the bidirectional gradient structure of magnetic nanoparticles and unique laminar arrangement, exhibited excellent in-plane electrical conductivity (96.3 S/m), superior electromagnetic shielding efficiency (1805.9 dB/cm2 g), low reflection coefficients (0.23), and a high green index (gs, 3.38), suggesting its green shielding capabilities. Furthermore, the laminar structure conferred upon the resultant carbon scaffold a surprisingly anisotropic thermal conductivity, with an in-plane thermal conductivity of 1.73 W/m K compared to a through-plane value of only 0.07 W/m K, confirming the integration of thermal insulation and thermal management functionalities. These green electromagnetic interference shielding materials, coupled with thermal insulation and thermal management properties, hold promising prospects for applications in sensitive devices.

Preparation and Properties of Elastic Mullite Fibrous Porous Materials with Excellent High-Temperature Resistance and Thermal Stability.

Mullite fiber felt is a promising material that may fulfill the demands of advanced flexible external thermal insulation blankets. However, research on the fabrication and performance of mullite fiber felt with high-temperature resistance and thermal stability is still lacking. In this work, mullite fibers were selected as raw materials for the fabrication of mullite fibrous porous materials with a three-dimensional net structure. Said materials' high-temperature resistance and thermal stability were investigated by assessing the effects of various heat treatment temperatures (1100 °C, 1300 °C, and 1500 °C) on the phase composition, microstructure, and performance of their products. When the heat treatment temperature was below 1300 °C, both the phase compositions and microstructures of products exhibited stability. The compressive rebound rate of the product before and after 1100 °C reached 92.9% and 84.5%, respectively. The backside temperature of the as-prepared products was 361.6 °C when tested at 1500 °C for 4000 s. The as-prepared mullite fibrous porous materials demonstrated excellent high-temperature resistance, thermal stability, thermal insulation performance, and compressive rebound capacity, thereby indicating the great potential of the as-prepared mullite fibrous porous materials in the form of mullite fiber felt within advanced flexible external thermal insulation blankets.

Performance Evaluation of Thermal Insulation Materials from Sheep's Wool and Hemp Fibres.

In the current work, the performance properties of natural-fibre-based thermal insulation materials were examined. For this purpose, three different compositions of natural fibres were prepared: pure sheep wool (SW), wool and industrial hemp (SW/HF) fibres, and pure industrial hemp (HF) fibres. Low-melt bicomponent polylactide (PLA) fibres were used as a binding material. For specimens prepared from natural fibres, the dependence of the thermal conductivity, the tensile strength along and across the direction of product formation, and the short-term water absorption on the density of the specimens and the flammability parameters were determined. In addition, to reduce the water absorption and flammability, the specimens were coated with hydrophobic agents and flame retardants. The obtained research results were also statistically processed. The analysis of the results showed that the thermal conductivity of natural-fibre-based thermal insulation materials varied within the range of 0.0333 ÷ 0.0438 W/(m·K), the tensile strength varied from 2.5 to 130 kPa, the short-term water absorption varied from 0.5 to 8.5 kg/m2, and the water vapour diffusion resistance factor varied from 2.537 to 2.667. It was additionally determined that all the studied products were flammable. The water absorption and flammability values were significantly reduced by the use of hydrophobic agents and flame retardants.

Biomimetic Leaf-Vein Aerogel for Electromagnetic Wave Absorption and Thermal Superinsulation.

Electromagnetic protection in extreme environments requires materials with excellent thermal insulation capability and mechanical property to withstand severe temperature fluctuations and complex external stresses. Achieving strong electromagnetic wave absorption (EMA) while sustaining these exceptional properties remains a significant challenge. Herein, a facile approach is demonstrated to fabricate a biomimetic leaf-vein MXene/CNTs/PI (MCP) aerogel with parallel venations through bidirectional freeze-casting method. Due to its multi-arch lamellar structure and parallel venations within the aerogel layers, the ultralight MCP aerogel (16.9 mg·cm-3) achieves a minimum reflection loss (RLmin) of -75.8 dB and a maximum effective absorption bandwidth (EABmax) of 7.14 GHz with an absorber content of only 2.4 wt%, which also exhibits superelasticity and structural stability over a wide temperature range from -196 to 400 °C. Moreover, this unique structure facilitates rapid heat dissipation within the layers, while significantly impeding heat transfer between adjacent layers, achieving an ultralow thermal conductivity of 15.3 mW·m-1·K-1 for thermal superinsulation. The combination of excellent EMA performance, robust structural stability, and thermal superinsulation provides a potential design scheme under extreme conditions, especially in aerospace applications.

Mixed-Dimensional Assembly Strategy to Construct Reduced Graphene Oxide/Carbon Foams Heterostructures for Microwave Absorption, Anti-Corrosion and Thermal Insulation.

Considering the serious electromagnetic wave (EMW) pollution problems and complex application condition, there is a pressing need to amalgamate multiple functionalities within a single substance. However, the effective integration of diverse functions into designed EMW absorption materials still faces the huge challenges. Herein, reduced graphene oxide/carbon foams (RGO/CFs) with two-dimensional/three-dimensional (2D/3D) van der Waals (vdWs) heterostructures were meticulously engineered and synthesized utilizing an efficient methodology involving freeze-drying, immersing absorption, secondary freeze-drying, followed by carbonization treatment. Thanks to their excellent linkage effect of amplified dielectric loss and optimized impedance matching, the designed 2D/3D RGO/CFs vdWs heterostructures demonstrated commendable EMW absorption performances, achieving a broad absorption bandwidth of 6.2 GHz and a reflection loss of - 50.58 dB with the low matching thicknesses. Furthermore, the obtained 2D/3D RGO/CFs vdWs heterostructures also displayed the significant radar stealth properties, good corrosion resistance performances as well as outstanding thermal insulation capabilities, displaying the great potential in complex and variable environments. Accordingly, this work not only demonstrated a straightforward method for fabricating 2D/3D vdWs heterostructures, but also outlined a powerful mixed-dimensional assembly strategy for engineering multifunctional foams for electromagnetic protection, aerospace and other complex conditions.

Tree-Inspired Structurally Graded Aerogel with Synergistic Water, Salt, and Thermal Transport for High-Salinity Solar-Powered Evaporation.

Solar-powered interfacial evaporation is an energy-efficient solution for water scarcity. It requires solar absorbers to facilitate upward water transport and limit the heat to the surface for efficient evaporation. Furthermore, downward salt ion transport is also desired to prevent salt accumulation. However, achieving simultaneously fast water uptake, downward salt transport, and heat localization is challenging due to highly coupled water, mass, and thermal transport. Here, we develop a structurally graded aerogel inspired by tree transport systems to collectively optimize water, salt, and thermal transport. The arched aerogel features root-like, fan-shaped microchannels for rapid water uptake and downward salt diffusion, and horizontally aligned pores near the surface for heat localization through maximizing solar absorption and minimizing conductive heat loss. These structural characteristics gave rise to consistent evaporation rates of 2.09 kg m-2 h-1 under one-sun illumination in a 3.5 wt% NaCl solution for 7 days without degradation. Even in a high-salinity solution of 20 wt% NaCl, the evaporation rates maintained stable at 1.94 kg m-2 h-1 for 8 h without salt crystal formation. This work offers a novel microstructural design to address the complex interplay of water, salt, and thermal transport.

Improving Pore Characteristics, Mechanical Properties and Thermal Performances of Near-Net Shape Manufacturing Phenolic Resin Aerogels.

Thermally stable high-performance phenolic resin aerogels (PRAs) are of great interest for thermal insulation because of their light weight, fire retardancy and low thermal conductivity. However, the drawbacks of PRA synthesis, such as long processing time, inherent brittleness and significant shrinkage during drying, greatly restrict their wide applications. In this work, PRAs were synthesized at ambient pressure through a near-net shape manufacturing technique, where boron-containing thermosetting phenolic resin (BPR) was introduced into the conventional linear phenolic resin (LPR) to improve the pore characteristics, mechanical properties and thermal performances. Compared with the traditional LPR-synthesized aerogel, the processing time and the linear shrinkage rate during the drying of the PRAs could be significantly reduced, which was attributed to the enhanced rigidity and the unique bimodal pore size distribution. Furthermore, no catastrophic failure and almost no mechanical degradation were observed on the PRAs, even with a compressive strain of up to 60% at temperatures ranging from 25 to 200 °C, indicating low brittleness and excellent thermo-mechanical stability. The PRAs also showed outstanding fire retardancy. On the other hand, the PRAs with a density of 0.194 g/cm3 possessed a high Young's modulus of 12.85 MPa and a low thermal conductivity of 0.038 W/(m·K).

Rice Husk-Based Insulators: Manufacturing Process and Thermal Potential Assessment.

The development of bio-insultation materials has attracted increasing attention in building energy-saving fields. In tropical and hot-humid climates, building envelope insulation is important for an energy efficient and comfortable indoor environment. In this study, several experiments were carried out on a bio-insulation material, which was prepared by using rice husk as a raw material. Square rice husk-based insultation panels were developed, considering the ASTM C-177 dimensions, to perform thermal conductivity coefficient tests. The thermal conductivity coefficient obtained was 0.073 W/(m K), which is in the range of conventional thermal insulators. In a second phase of this study, two experimental enclosures (chambers) were constructed, one with rice husk-based insulation panels and the second one without this insulation. The measures of the temperatures and thermal flows through the chambers were obtained with an electronic module based on the ARDUINO platform. This module consisted of three DS18B20 temperature sensors and four Peltier plates. Daily temperature and heat flux data were collected for the two chambers during the dry season in Panama, specifically between April and May. In the experimental chamber that did not have rice husk panel insulation on the roof, a flow of up to 28.18 W/m2 was observed, while in the chamber that did have rice husk panels, the presence of a flow toward the interior was rarely observed. The rice husk-based insulation panels showed comparable performance with conventional insulators, as a sustainable solution that takes advantage of a local resource to improve thermal comfort and the reduction of the environmental impact.

Large-Scale Engineerable Films Tailored with Cellulose Nanofibrils for Lighting Management and Thermal Insulation.

Fibrillated cellulose-based nanocomposites can improve energy efficiency of building envelopes, especially windows, but efficiently engineering them with a flexible ability of lighting and thermal management remains highly challenging. Herein, a scalable interfacial engineering strategy is developed to fabricate haze-tunable thermal barrier films tailored with phosphorylated cellulose nanofibrils (PCNFs). Clear films with an extremely low haze of 1.6% (glass-scale) are obtained by heat-assisted surface void packing without hydrophobization of nanocellulose. PCNF gel cakes serve here as templates for surface roughening, thereby resulting in a high haze (73.8%), and the roughened films can block heat transfer by increasing solar reflection in addition to a reduced thermal conduction. Additionally, obtained films can tune distribution of light from visible to near-infrared spectral range, enabling uniform colored lighting and inhibiting localized heating. Furthermore, an integrated simulation of lighting and cooling energy consumption in the case of office buildings shows that the film can reduce the total energy use by 19.2-38.1% under reduced lighting levels. Such a scalable and versatile engineering strategy provides an opportunity to endow nanocellulose-reinforced materials with tunable optical and thermal functionalities, moving their practical applications in green buildings forward.

Flexible and Thermally Insulating Porous Materials Utilizing Hollow Double-Shell Polymer Fibers.

The global climate change is mainly caused by carbon dioxide (CO2) emissions. To help reduce CO2 emissions and conserve thermal energy, sustainable materials based on flexible thermal insulation are developed to minimize heat flux, drawing inspiration from natural systems such as polar bear hairs. The unique structure of hollow double-shell fibers makes it possible to achieve low thermal conductivity in the material while retaining exceptional elasticity, allowing it to adapt to insulation systems of any shape. The layered system of porous mats reaches a thermal conductivity coefficient of 0.031 W∙m⁻¹âˆ™K⁻¹ and enables to reduce the heat transfer. The results achieved using scanning thermal microscopy (SThM) correlate with the simulated heat flow in the case of individual fibers. This research study brings new insights into the energy efficiency of domestic environments, thereby addressing the growing demand for sustainable and high-performance insulation materials for saving energy loss and reducing pollution footprint.

Research on Thermal Stability and Flammability of Wood Scob-Based Loose-Fill Thermal Insulation Impregnated with Multicomponent Suspensions.

Loose-fill thermal composite insulation produced from surface-modified wood scobs has been explored as a potential fire-resistant material for building envelopes. This work involves fire resistance behavior comparisons between four coating systems consisting of liquid glass, liquid glass-tung oil, liquid glass-expandable graphite, and liquid glass-tung oil-expandable graphite. The techniques of thermogravimetric and differential thermogravimetric analyses, gross heat combustion via a calorimetric bomb, cone calorimetry, SEM imaging of char residues, and energy dispersive spectrometry for elemental analysis, as well as propensity to undergo continuous smoldering, were implemented. The coating technique resulted in greater thermal stability at a higher temperature range (500-650 °C) of the resulting loose-fill thermal composite insulation, reduced flame-damaged area heights after the exposure of samples at 45° for 15 s and 30 s, with a maximum of 49% decreased gross heat combustion, reduced heat release and total smoke release rates, improved char residue layer formation during combustion and changed smoldering behavior due to the formation of homogeneous and dense carbon layers. The results showed that the highest positive impact was obtained using the liquid glass and liquid glass-expandable graphite system because of the ability of the liquid glass to cover the wood scob particle surface and form a stable and strong expanding carbon layer.

Construction of chitosan/alginate aerogels with three-dimensional hierarchical pore network structure via hydrogen bonding dissolution and covalent crosslinking synergistic strategy for thermal management systems.

To replace traditional petrochemical-based thermal insulation materials, in this work, the chitosan (CHI)/alginate (ALG) (CA) aerogels with three-dimensional hierarchical pore network structure were constructed by compositing CHI and ALG using a synergistic strategy of hydrogen bonding dissolution and covalent crosslinking. The structure and properties were further regulated by crosslinking the CA aerogels with epichlorohydrin (ECH). The CA aerogels exhibited various forms of covalent crosslinking, hydrogen bonding and electrostatic interactions, with hydrogen bonding content reaching 79.12 %. The CA aerogels showed an excellent three-dimensional hierarchical pore network structure, with an average pore size minimum of 15.92 nm. The structure regulation of CA aerogels obtained excellent compressive properties, with an increase of stress and strain by 137.61 % and 45.05 %, which can support a heavy object 5000 times its weight. Additionally, CA aerogels demonstrate excellent thermal insulation properties and low thermal conductivity, comparable to commercially available insulation materials. More importantly, CA aerogels have good cyclic insulation stability and thermal properties, and they have a flame retardancy rating of V-0, which shows the stability of insulation properties and excellent safety. CA aerogels provide new ideas for the development of biomass thermal insulation materials and are expected to be candidates for thermal management applications.

Integration of N- and P- elements in sodium alginate aerogels for efficient flame retardant and thermal insulating properties.

In the field of building energy conservation, the development of biodegradable biomass aerogels with excellent mechanical performance, flame retardancy and thermal insulation properties is of particular importance. Here, a directional freeze-drying method was used for fabricating composite sodium alginate (SA) aerogels containing functionalized ammonium polyphosphate (APP) flame retardant. In particular, APP was coated with melamine (MEL) and phytic acid (PA) by a supramolecular assembly process. Through optimizing the flame retardant addition, the SA-20 AMP sample exhibited excellent flame retardant and thermal insulation properties, with the limiting oxygen index of 38.2 % and the UL-94 rating of V-0. Such aerogels with anisotropic morphology demonstrated a low thermal conductivity of 0.0288 (W/m·K) in the radial direction (perpendicular to the lamellar structure). In addition, as-obtained aerogels displayed remarkable water stability and mechanical properties, indicating significant potential for practical applications.

Upcycling of industrial footwear waste into nonwoven fibrous structures with thermal and acoustic insulation properties.

The footwear industry significantly impacts the environment, from raw material extraction to waste disposal. Transforming waste into new products is a viable option to mitigate the environmental consequences, reducing the reliance on virgin raw materials. This work aims to develop thermal and acoustic insulation materials using polyester waste from footwear industry. Two nonwoven and two compressed nonwoven structures, comprising 80% polyester waste and 20% commercial recycled polyester (matrix), were produced. The materials were created through needle-punching and compression molding techniques. The study included the production of sandwich and monolayer nonwoven structures, which were evaluated considering area weight, thickness, air permeability, mechanical properties, morphology using field emission scanning electron microscopy, and thermal and acoustic properties. The nonwoven samples presented high tensile strength (893 kPa and 629 kPa) and the highest strain (79.7% and 73.3%) and compressed nonwoven structures showed higher tensile strength (2700 kPa and 1291 kPa) but reduced strain (25.8% and 40.8%). Nonwoven samples showed thermal conductivity of 0.041 W/K.m and 0.037 W/K.m. Compressed nonwoven samples had higher values at 0.060 W/K.m and 0.070 W/K.m. While the sample with the highest conductivity exceeds typical insulation levels, other samples are suitable for thermal insulation. Nonwoven structures exhibited good absorption coefficients (0.640-0.644), suitable for acoustic insulation. Compressed nonwoven structures had lower values (0.291-0.536), unsuitable for this purpose. In summary, this study underscores the potential of 100% recycled polyester structures derived from footwear and textile industry waste, showcasing remarkable acoustic and thermal insulation properties ideal for the construction sector.

Multiphase Symbiotic Engineered Elastic Ceramic-Carbon Aerogels with Advanced Thermal Protection in Extreme Oxidative Environments.

Elastic aerogels can dissipate aerodynamic forces and thermal stresses by reversible slipping or deforming to avoid sudden failure caused by stress concentration, making them the most promising candidates for thermal protection in aerospace applications. However, existing elastic aerogels face difficulties achieving reliable protection above 1500 °C in aerobic environments due to their poor thermomechanical stability and significantly increased thermal conductivity at elevated temperatures. Here, a multiphase sequence and multiscale structural engineering strategy is proposed to synthesize mullite-carbon hybrid nanofibrous aerogels. The heterogeneous symbiotic effect between components simultaneously inhibits ceramic crystalline coarsening and carbon thermal etching, thus ensuring the thermal stability of the nanofiber building blocks. Efficient load transfer and high interfacial thermal resistance at crystalline-amorphous phase boundaries on the microscopic scale, coupled with mesoscale lamellar cellular and locally closed-pore structures, achieve rapid stress dissipation and thermal energy attenuation in aerogels. This robust thermal protection material system is compatible with ultralight density (30 mg cm-3), reversible compression strain of 60%, extraordinary thermomechanical stability (up to 1600 °C in oxidative environments), and ultralow thermal conductivity (50.58 mW m-1 K-1 at 300 °C), offering new options and possibilities to cope with the harsh operating environments faced by space exploration.

A Review of High-Temperature Aerogels: Composition, Mechanisms, and Properties.

High-temperature aerogels have garnered significant attention as promising insulation materials in various industries such as aerospace, automotive manufacturing, and beyond, owing to their remarkable thermal insulation properties coupled with low density. With advancements in manufacturing techniques, the thermal resilience of aerogels has considerable improvements. Notably, polyimide-based aerogels can endure temperatures up to 1000 °C, zirconia-based aerogels up to 1300 °C, silica-based aerogels up to 1500 °C, alumina-based aerogels up to 1800 °C, and carbon-based aerogels can withstand up to 2500 °C. This paper systematically discusses recent advancements in the thermal insulation performance of these five materials. It elaborates on the temperature resistance of aerogels and elucidates their thermal insulation mechanisms. Furthermore, it examines the impact of doping elements on the thermal conductivity of aerogels and consolidates various preparation methods aimed at producing aerogels capable of withstanding temperatures. In conclusion, by employing judicious composition design strategies, it is anticipated that the maximum tolerance temperature of aerogels can surpass 2500 °C, thus opening up new avenues for their application in extreme thermal environments.

Fabrication of the SiC/HfC Composite Aerogel with Ultra-Low Thermal Conductivity and Excellent Compressive Strength.

Aerogels, as a new type of high-temperature-resistant insulation material, find extensive application in aerospace, high-temperature industrial furnaces, new energy batteries, and various other domains, yet still face some limitations such as inadequate temperature resistance and pronounced brittleness. In this work, SiC/HfC composite aerogels were prepared through a combination of sol-gel method, atmospheric pressure drying technique, and carbothermal reduction reaction. The effects of different molar ratios, calcination time, and temperatures on the microstructural features and physicochemical properties of the resulting SiC/HfC composite aerogels were investigated. The aerogel exhibited an elevated BET-specific surface area of 279.75 m2/g, while the sample displayed an extraordinarily low thermal conductivity of 0.052 W/(m·K). Most notably, the compressive strength reached an outstanding 5.93 MPa after a carbonization temperature of 1500 °C, far exceeding the values reported in prior aerogel studies. This research provided an innovative approach for advancing the development of carbide aerogels in the realm of high-temperature applications.