Search Results (13)

Thermal protection materials with excellent performance are critical for hypersonic vehicles. Carbon fiber/phenolic resin composites (C_f/Ph) have been widely used as thermal protection materials due to their high specific strength and ease of processing. However, oxidative failure limits the extensive applications of C_f/Ph in harsh environments. In this paper, a novel hafnium carbide (HfC) and boron carbide (B₄C)-modified C_f/Ph was fabricated via an impregnating and compression molding route. The synergistic effect of HfC and B₄C on the thermal stability, flexural strength, microstructure, and phase evolution of the ceramizable composite was studied. The resulting ceramizable composites exhibited excellent resistance to oxidative corrosion and ablation behavior. The residual yield at 1400 °C and the flexural strength after heat treatment at 1600 °C for 20 min were 46% and 54.65 MPa, respectively, with an increase of 79.59% in flexural strength compared to that of the composites without ceramizable fillers. The linear ablation rate (LAR) and mass ablation rate (MAR) under a heat flux density of 4.2 MW/m² for the 20 s were as low as −8.33 × 10⁻³ mm/s and 3.08 × 10⁻² g/s. The ablation mechanism was further revealed. A dense B–C–N–O–Hf ceramic layer was constructed in situ as an efficient thermal protection barrier, significantly reducing the corrosion of the carbon fibers. Full article

Ceramizable silicone rubber (CSR) composed of silicone rubber matrix and inorganic fillers can be transformed into a dense flame-retardant ceramic upon encountering high temperatures or flames. Conventionally, CSR can be sintered into a dense ceramic at temperatures above 1000 °C, which is higher than the melting point of a copper conductor used in a power cable. In this study, the vulcanization process and mass ratio of inorganic fillers of CSR were studied to lower its ceramization temperature to 950 °C. The electrical and mechanical properties of CSRs and their ceramic bulks were studied with various ratios of wollastonite and muscovite. It was found that the CSR samples could be successfully fabricated using a two-step vulcanization technique (at 120 °C and 150 °C, respectively). As a high ratio of muscovite filler was introduced into the CSR, the sample presented a high dc electrical resistivity of 6.713 × 10¹⁴ Ω·cm, and a low dielectric constant of 4.3 and dielectric loss of 0.025 at 50 Hz. After the thermal sintering (at 950 °C for 1 h) of the CSR sample with a high ratio of muscovite, the ceramic sample exhibits a dense microstructure without any pores. The ceramic also demonstrates excellent insulating properties, with a volume resistivity of 8.69 × 10¹¹ Ω·cm, and a low dielectric loss of 0.01 at 50 Hz. Meanwhile, the three-point bending strength of the ceramic sample reaches a value of 110.03 MPa. This study provides a potential route to fabricate CSR used for fire-resistant cables. Full article

In this study, a heat-resistant adhesive was prepared using molybdenum-phenolic (Mo-PF) resin as the matrix and TiB₂ particle as the ceramizable filler for bonding Al₂O₃ ceramic substrates. Firstly, Fourier transform infrared (FTIR) was used to characterize the chemical structure of the Mo-PF. Subsequently, thermo gravimetric analysis (TGA) and shear strength testing were employed to investigate the effects of heat treatment in different atmospheres on the thermal stability and residual bonding properties of the adhesive. To further explore the bonding mechanism of the adhesive after heat treatment in different atmospheres, scanning electron microscopy (SEM), compressive strength testing, and X-ray diffraction (XRD) were utilized to analyze the microstructure, mechanical strength, and composition evolution of the adhesive at different temperatures. The bonding strength of Al₂O₃ joints showed a trend of initially decreasing and then increasing after different temperature heat treatment in air, with the shear strength reaching a maximum value of 25.68 MPa after treatment at 1200 °C. And the bonding strength of Al₂O₃ joints decreased slowly with the increase of temperature in nitrogen. In air, the ceramicization reaction at a high temperature enabled the mechanical strength of the adhesive to rise despite the continuous pyrolysis of the resin. However, the TiB₂ filler in nitrogen did not react, and the properties of the adhesive showed a decreasing tendency with the pyrolysis of the resin. Full article

Hypersonic vehicles encounter hostile service environments of thermal/mechanical/chemical coupling, so thermal protection materials are crucial and essential. Ceramizable composites have recently attracted intensive interest due to their ability to provide large-area thermal protection for hypersonic vehicles. In this work, a novel ceramizable composite of quartz fiber/benzoxazine resin modified with fused SiO₂ and h-BN was fabricated using a prepreg compression molding technique. The effects of the fused SiO₂ and h-BN contents on the thermal, mechanical, and ablative properties of the ceramizable composite were systematically investigated. The ceramizable composite with an optimized amount of fused SiO₂ and h-BN exhibited superb thermal stability, with a peak degradation temperature and residue yield at 1400 °C of 533.2 °C and 71.5%, respectively. Moreover, the modified ceramizable composite exhibited excellent load-bearing capacity with a flexural strength of 402.2 MPa and superior ablation resistance with a linear ablation rate of 0.0147 mm/s at a heat flux of 4.2 MW/m², which was significantly better than the pristine quartz fiber/benzoxazine resin composite. In addition, possible ablation mechanisms were revealed based on the microstructure analysis, phase transformation, chemical bonding states, and the degree of graphitization of the ceramized products. The readily oxidized pyrolytic carbon (PyC) and the SiO₂ with a relatively low melting point were converted in situ into refractory carbide. Thus, a robust thermal protective barrier with SiC as the skeleton and borosilicate glass as the matrix protected the composite from severe thermochemical erosion and thermomechanical denudation. Full article

New trends in the circular economy and sustainability are pointing towards the gradual elimination of standard flame retardants such as phosphorus compounds or halogenated compounds. New solutions are therefore being sought in this area and ceramizable composites could be an interesting alternative. Weak rheological properties are one of the main disadvantages of ceramizable composites. This study tested ceramizable composites composed of styrene-butadiene rubber (SBR) as a polymer matrix and mica as a mineral filler and aimed to improve the viscoelastic properties of silicone oil as a plasticizer. To characterize this composite’s mechanical properties before and after ceramization, the viscoelastic properties were tested with a dynamic oscillating rheometer and the thermal behavior with a cone calorimeter. This paper also provides results showing differences (via the abovementioned properties) between vulcanization with sulfur and that with peroxide for the ceramizable composites based on SBR. The presented results, showing changes in mechanical properties, dynamic viscosity or flammability, among others, allow a better understanding of elastomeric composites with ceramizable flame-retardant systems. Such composites can find a wide range of applications, from lagging for electrical cables to building elements such as floor coverings and fire barriers. Full article

Carbon fiber fabric-reinforced phenolic resin composites are widely used as thermal protection materials for thermal protection systems in hypersonic vehicles and capsules. In this work, carbon fiber fabric-reinforced boron phenolic resin composites modified with MoSi₂ and B₄C were prepared via a compression molding technique. The high-temperature performance of the composites as well as the oxidation behavior of the carbon fibers was studied. The results indicate that the incorporation of B₄C improves the performance of composites at high temperatures. The residual weight rate of composites with 15 phr B₄C (BP-15) sufficiently increased from 23.03% to 32.91% compared with the composites without B₄C (BP-0). After being treated at 1400 °C for 15 min, the flexural strength of BP-15 increased by 17.79% compared with BP-0. Compared with BP-0, the line ablation rate and mass ablation rate of BP-15 were reduced by 53.96% and 1.56%, respectively. In addition, MoSi₂ and B₄C particles had a positive effect on the oxidation of carbon fibers in the composites. After treatment at 1400 °C, the diameter of the as-received carbon fiber was reduced by 31.68%, while the diameter of the carbon fiber in BP-0 and BP-15 decreased by 15.12% and 6.14%, respectively. At high temperatures, the liquid B₂O₃ from B₄C and MoSi₂-derived complex-phase ceramics (MoB, MoB₂, Mo₂C, Mo_4.8Si₃C_0.6) acted as an oxygen barrier, effectively mitigating the oxidation degree of the carbon fibers. Full article

The reliable mechanical properties of ceramizable silicone rubber composites during pyrolysis are necessary for their application in the fire-resistant fields. The effects of liquid-phase amount on the mechanical properties of silicone rubber composites are investigated. The results show a positive correlation between the liquid-phase amount and the flexural strength of the residual products pyrolysis below 800 °C. The nano-γ-Al₂O₃ in the fillers reacts with liquid B₂O₃ to form aluminum borate above 800 °C, which consumes the liquid phase and strengthens the residual products to a certain extent. Increasing the B₂O₃ addition and introducing nano-γ-Al₂O₃ can control the liquid-phase amount in the range of 15% to 30%, which makes the composites have better residual strength and support performance. The residual strength of composites pyrolysis at 500 °C to 1000 °C is higher than 2.50 MPa, and the maximum is up to 18.7 MPa at 1000 °C. Full article

Flame-retardant coatings have drawn much attention in recent years. In this study, an inorganic sodium silicate-based intumescent flame-resistance coating with an excellent flameproof properties is developed by mainly utilizing sodium silicate as the ceramizable binder, via hydrolysis and self-condensation reaction. Fly ash, metakaoline, and wollastonite behave as supplement cementing materials. Major formulation encompasses the combination of the ammonium polyphosphate and pentaerythritol as the flame-retardant additives, and aluminum hydroxide or expandable graphite as the intumescence-improving filler agents. Expandable graphite was found to play an important role in the eventual performance of flame-resistance testing. The results showed that solid interaction forces can be formed between metakaoline and sodium silicate, resulting in a similar material to geopolymer with excellent physical properties. After high-temperature flame testing, a densely complex protective layer of carbon-char created on top of the robust silicon dioxide networks offers notable flame resistance. An optimal ratio in this inorganic intumescent coating contains sodium silicate—metakaoline (weight ratio = 9:1)—ammonium polyphosphate and pentaerythritol, aluminum hydroxide (3, 3, 10 wt.%)—expandable graphite (1 wt.%), which can create 4.7 times higher expansion ratio compared with neat sodium silicate matrix. The results of flame testing demonstrate only 387.1 °C and 506.3 °C on the back surface of steel substrate after one and three hours flaming (>1000 °C) on the other surface, respectively, which could meet the requirements according to the level of fire rating. Full article

Ceramizable composite is a kind of polymer matrix composite that can turn into ceramic material at a high temperature. It can be used for the ceramic insulation of a metal conductor because of its processability. However, poor low-temperature ceramization performance is a problem of ceramizable composites. In this paper, ceramizable composites were prepared by using silicone rubber as a matrix. Ceramic samples were sintered at different temperatures no more than 1000 °C, according to thermogravimetric analysis results of the composites. The linear contraction and flexural strength of the ceramics were measured. The microstructure and crystalline phase of ceramics were analyzed using scanning electron microscope (SEM) and X-ray diffraction (XRD). The results show that the composites turned into ceramics at 800 °C, and a new crystal and continuous microstructure formed in the samples. The flexural strength of ceramics was 46.76 MPa, which was more than twice that of similar materials reported in other research sintered at 1000 °C. The maximum flexural strength was 54.56 MPa, when the sintering temperature was no more than 1000 °C. Moreover, glass frit and nano silica played important roles in the formation of the ceramic phase in this research. A proper content of nano silica could increase the strength of the ceramic samples. Full article

The article illustrates the impact of basalt filler in the form of flakes and fibres on the toxicity of gaseous products that formed during the thermal decomposition of silicone rubber composites. The values of specific emissions of gases were determined with the help of the IR spectroscopy and further applied to calculate the toxicometric index. The presented method of measuring the concentrations of gaseous products resulting from thermal decomposition consists in the application of a fluidised bed reactor, which makes it possible to conduct the decomposition of a sample at a precisely assumed temperature value and imitate the conditions of a real fire. At a temperature lower than 700 °C, the gases resulting from the thermal decomposition of composites are particularly toxic due to the presence of significant concentrations of formaldehyde that does not undergo oxidation to more stable inorganic products. At a temperature of 600 °C the toxicity of gases for the samples with ceramizable additives and without them was similar. In the first case, there appeared to be a positive synergistic effect of mineral and basalt additives, and the basalt additives themselves increased the toxicity of gases. At higher temperatures of decomposition, the exponentially increasing rate of the oxidation reaction in the gaseous phase results in the lack of significant differences between the toxicity of gases for the samples with and without basalt additives. The toxicometric index value at temperatures of 700 °C and 800 °C was by one or two orders of magnitude higher, respectively, than the one that was observed in the temperature range of 500–600 °C, as inorganic components appear in the place of formaldehyde. Full article

This article illustrates the impact of basalt filler, both in the form of basalt flakes and basalt fibers, on thermal and mechanical properties, as well as on the fire hazard, of silicone rubber (SR) composites, including ceramizable composites. In addition to basalt filler, ceramizable composites contain mineral fillers in their composition in the form of silica and calcium carbonate, inorganic fluxes such as zinc borate and glass frit, and melamine cyanurate as a flame retardant. The obtained composites were analyzed from the point of view of their morphology, rheological and thermal properties, flammability, and mechanical properties before and after the ceramization process. The obtained research results indicate that the basalt filler has an unambiguous impact on the improvement of thermal properties and the reduction of flammability in the analyzed composites. The results of morphological analyses of ceramizable composites before and after the process of their ceramization indicate a definite impact of the basalt filler on the structure of the formed ceramic layer. An increase in its homogeneity exerts a direct impact on the improvement of its mechanical parameters. Full article

Synergistic effects of different fillers are widely utilized in polymer technology. The combination of various types of fillers is used to improve various properties of polymer composites. In this paper, a synergistic effect of flame retardants was tested to improve the performance of ceramizable composites. The composites were based of styrene-butadiene rubber (SBR) used as polymer matrix. Three different types of flame retardants were tested for synergistic effect: Mica (phlogopite) high aspect-ratio platelets, along with low softening point temperature glass frit (featuring ceramization effect), and melamine cyanurate, a commonly used flame retardant promoting carbonaceous char. In order to characterize the properties of the composites, combustibility, thermal stability, viscoelastic properties, micromorphology, and mechanical properties were tested before and after ceramization. The results obtained show that the synergistic effect of ceramization promoting fillers and melamine cyanurate was especially visible with respect to the flame retardant properties resulting in a significant improvement of fire resistance of the composites. Full article

Ceramizable silicone rubber (MVQ)/halloysite (HNT) composites were fabricated by incorporation of three different borates, including sodium tetraborate decahydrate, ammonium pentaborate, and zinc borate into MVQ matrix, respectively. The composites without any borates were also prepared as control. The effect of the borates on the mechanical and electrical properties of MVQ/HNT composites was investigated. The ceramic residues were obtained from the decomposition of the composites after sintering at 1000 °C. The effect of the borates on the linear shrinkage, weight loss, and flexural and impact strength of the residues was also studied. The fracture surfaces of the composites and their corresponding residues were observed by SEM. The proposed ceramizable mechanism of the composites by incorporation of different borates was revealed by XRD analysis. Full article