A comparison of the interfacial, thermal, and ablative properties between spun and filament yarn type carbon fabric/phenolic composites

In the present paper, the interfacial, thermal, and ablative properties of phenolic composites reinforced with spun yarn type carbon fabrics (spun C/P composite) and filament yarn type carbon fabrics (filament C/P composite) heat-treated at 1100 °C have been extensively compared. The interlaminar shear strength, crack growth rate, and fracture surface were studied to evaluate the interfacial characteristics of the composites using short-beam shear test, double cantilever beam test, and scanning electron microscopy, respectively. The thermal conductivity and the coefficient of thermal expansion were also measured in the longitudinal and transverse directions, respectively. To explore the ablative characteristics of the composites in terms of insulation index, erosion rate, and microscopic pattern of ablation, an arc plasma torch was used. The interfacial properties of the spun C/P composite are significantly greater than those of the filament C/P composite, with qualitative support of fracture surface observations. It has been investigated that the presence of protruded fibers in the phenolic matrix of the spun C/P composite may play an important role in enhancing the properties due to a fiber bridging effect. The longitudinal thermal conductivity of the spun C/P composite is about 7% lower than that of the filament C/P counterpart. It has been found from the ablation test using arc plasma torch flame that the erosion rate is 14% higher than that of the filament C/P counterpart. Consequently, all the experimental results suggest that use of spun yarn type carbon fabrics heat-treated at low carbonization temperature as reinforcement in a phenolic composite may significantly contribute to improving the interfacial, thermal, and ablative properties of C/P composites.     

Effect of temperature and layer thickness on these strengths of carbon bonding for carbon/carbon composites

In order to apply carbon/carbon composites (C/Cs) to various hot structures, secondary bonding techniques effective at elevated temperatures are frequently required. In the present study, carbon bonding between lamination type C/Cs was formed by the carbonation of polymer adhesive, and the strength of the bonding was evaluated at temperatures up to 2273 K in a vacuum using the double-notched shear method. The results revealed that bonding strength increased with increasing temperature and became higher than the inter-laminar shear strength of the substrate C/C when the bonding layer was thin. The enhancement of carbon bonding strength with increasing temperature was shown to be caused mainly by the evaporation of absorbed gases, probably water, up to temperatures of 1800 K with a slight additional contribution of thermal residual stress. It was also shown that heat treatment at higher temperatures made the bonding stronger.     

Thermophysical properties of carbon/carbon composites and physical mechanism of thermal expansion and thermal conductivity

Five different carbon/carbon composites (C/C) have been prepared and their thermophysical properties studied. These were three needled carbon felts impregnated with pyrocarbons (PyC) of different microstructures, chopped fibers/resin carbon + PyC, and carbon cloth/PyC. The results show that the X-Y direction thermal expansion coefficient (CTE) is negative in the range 0-100 °C with values ranging from −0.29 to −0.85 × 10⁻⁶/K. In the range 0-900 °C, their CTE is also very low, and the CTE vs. T curves have almost the same slope. In the same temperature range composites prepared using chopped fibers show the smallest CTE values and those using the felts show the highest. The microstructure of the PyC has no obvious effect on the CTE for composites with the same preform architecture. Their expansion is mainly caused by atomic vibration, pore shrinkage and volatilization of water. However, the PyC structure has a large effect on thermal conductivity (TC) with rough laminar PyC giving the highest value and isotropic PyC giving the lowest. All five composites have a high TC, and values in the X-Y direction (25.6-174 W/m K) are much larger than in the Z direction (3.5-50 W/m K). Heat transmission in these composites is by phonon interaction and is related to the preform and PyC structures.     

Thermal diffusivity of 3D C/SiC composites from room temperature to 1400 °C

A 3D C/SiC composite and a bulk CVD SiC material were prepared. The effects of the CVD SiC coating and the heat treatment on the longitudinal and transverse thermal diffusivity of the C/SiC composites were investigated. The thermal diffusivity of the C/SiC composites could be well fitted by a multinomial function from room temperature to 1400 °C which includes a power term, an exponential term and a constant term. The exponential term affected the thermal diffusivity and led to its increase above 1200 °C with activation energy of 77 kcal/mol. The microstructure change in the composites was the reason that the thermal diffusivity was increased above 1200 °C. The longitudinal thermal diffusivity of the composite was twice or more than the transverse one and increased more rapidly by the exponential term. The former was decreased by the CVD SiC coating, but the latter was increased by it. The heat treatment could increase the thermal diffusivity and make the exponential term disappeared in the functions. The functional curve before the treatment intersected that after the treatment at the treatment temperature.     

Mechanical, thermal and ablative properties of interply continuous/spun hybrid carbon composites

The mechanical and thermal properties of interply hybrid carbon fiber (continuous and spun fabric)/phenolic composite materials have been studied. Hybrid carbon/phenolic composites (hybrid CP) with continuous carbon fabric of high tensile, flexural strength and spun carbon fabric of better interlaminar shear strength and lower thermal conductivity are investigated in terms of mechanical properties as well as thermal properties.Through hybridization, tensile strength and modulus of spun type carbon fabric reinforced phenolic composites (spun CP) increased by approximately 28% and 20%, respectively. Hybrid CP also exhibits better interlaminar shear strength than continuous carbon fabric/phenolic composites (continuous CP).The in-plane thermal conductivity of hybrid CP is 4-8% lower than that of continuous CP. As continuous filament type carbon fiber volume fraction increases, the transversal thermal conductivity of hybrid CP decreases.The erosion rate and insulation index were examined using torch test. Spun CP has a higher insulation index than continuous CP and hybrid CP over the entire temperature range. Hybrid CP with higher content of spun fabric exhibits higher insulation index as well as lower erosion rate.     

Electrical and mechanical properties of granular-fibrous carbon-carbon composites with recycled carbon fibres

In the following study, the electrical and mechanical properties of granular-fibrous carbon-carbon composites with short recycled carbon fibres have been investigated. The examined composites contained from 0 to 12?wt% of three types of recycled carbon fibres that differ in length. The conducted study has proven that it is not the type of applied fibre, but rather the resultant porosity of composites that exerts the predominant influence on the electrical resistivity and mechanical properties of the tested materials. The curve fitting revealed mathematical formulas correlating the studied properties with the apparent density of the composite samples. Owing to the addition of the shortest carbon fibres, the mechanical and electrical properties were significantly improved (50.14% and 24.06% increase in modulus of elasticity and flexural strength respectively for the sample with 12?wt% of the shortest fibres). A 21.39% decline in the resistivity ($?=161.26\mu \Omega ?\mathrm{m}$) of the composite containing 4% of shortest fibres was noted in comparison with the reference sample. Unlike powdered fibres, the addition of longer fibres caused an increase in porosity and deterioration of microstructure, which resulted in a significant decline in the key properties of the investigated composites.     

Thermal and ablative properties of binary carbon nanotube and nanodiamond reinforced carbon fibre epoxy matrix composites

The thermal and ablative properties of carbon nanotube (CNT) and nanodiamond (ND) reinforced carbon fibre epoxy matrix composites were investigated by simulating shear forces and high temperatures using oxyacetylene torch apparatus. Three types of composite specimens—(i) carbon fibre epoxy matrix composite (CF/Epoxy), (ii) carbon fibre epoxy matrix composite containing 0.1 wt-% CNTs and 0.1 wt-% NDs, and (iii) carbon fibre epoxy matrix composite containing 0.2 wt-% CNTs and 0.2 wt-% NDs—were explored. The ablative response of composites was studied through pre- and post-burnt SEM analysis and further related with thermogravimetric analysis, weight loss profile and thermal conductivity measurements. The novel nanofiller composites showed marked improvement in their thermal and ablative properties. A 22% and 30% increase in thermal conductivity was observed for composites containing 0.1 wt-% CNTs/0.1 wt-% NDs and 0.2 wt-% CNTs/0.2 wt-% NDs respectively. These nanofillers also improved the thermal stability of thermosetting epoxy matrix, and an increase of 13% and 20% was recorded in the erosion rate of composites containing 0.1 wt-% CNTs/0.1 wt-% NDs and 0.2 wt-% CNTs/0.2 wt-% NDs respectively. This improvement is due to the increased char yield produced by the increase in the loading of nanofillers, i.e. CNTs and NDs. Insulation index and insulation to density performance have also been improved due to increased thermal conductivity and char yield.     

An RTM densification method of manufacturing carbon-carbon composites using Primaset PT-30 resin

This paper presents a development of carbon-carbon (C-C) composite by resin transfer molding (RTM) process. The RTM was used for both manufacturing of the resin matrix composite part as well as impregnation of the carbonized parts. Materials chosen were heat-treated T300 2-D carbon fabric and Primaset PT-30 cyanate ester. The PT-30 resin has a char yield similar to that of phenolics, very low volatiles, low viscosity at processing temperatures, and no by-products during cure, and hence, an excellent choice for RTM process. The process consists of RTM of the composite part, carbonization, RTM impregnation, and re-carbonization. The last two steps were repeated to achieve the desired density. The measured density and mechanical properties of just two times-densified C-C composite panels were superior to or nearly the same as the data in the literature by other processes. The RTM densification is about twice as fast as the resin solution method and it is environment friendly.     

Effect of carbonization rate on the properties of a PAN/phenolic-based carbon/carbon composite

The effect of carbonization rate in a wide range (1, 100 and 1000 °C/min) on the properties of a PAN/phenolic-based carbon/carbon (C/C) composite was studied. The results indicated that the composite processed at a higher carbonization rate had a higher porosity level, more large pores and a more graphitic structure than that processed at a lower carbonization rate. After second graphitization the bending properties of composites carbonized at 1 °C/min and 1000 °C/min were comparable. The composite carbonized at 1000 °C/min had the highest fracture energy. The composite carbonized at 100 °C/min showed the worst mechanical performance among three. The large increase in carbonization rate can be beneficial to the industry from an economic point of view.     

Numerical modeling of the carbonization process in the manufacture of carbon/carbon composites

A method for the numerical simulation of the carbonization process is introduced. A general model for the transient analyses of heat and mass transfer together with stress and displacement predictions is constructed using two-dimensional FEM (finite element method) for arbitrary geometry. The established model is applied to the carbonization of a single-phase, homogeneous, isotropic phenolic foam, and an anisotropic, two-phase composite material. A damage model is introduced to account for the development of shrinkage cracks, and a CDM (continuum damage mechanics) model is implemented for the calculation of mechanical property degradation due to crack evolution. The established model is verified by comparison with experimental results, and is applied to various numerical examples.     

Size control and characterization of spherical carbon aerogel particles from resorcinol-formaldehyde resin

Spherical resorcinol-formaldehyde (RF) aerogel particles were synthesized by emulsion polymerization of resorcinol with formaldehyde in a slightly basic aqueous solution, followed by supercritical drying with carbon dioxide. RF carbon aerogel particles were prepared by carbonizing of the RF aerogel particles at a high temperature under a nitrogen atmosphere. By changing the viscosity of the RF sol added to the cyclohexane containing a surface-active agent for preparation of the spherical RF hydrogels, we investigated the influence of the apparent viscosity of the RF sol on the size of the generated RF carbon aerogel particles. We could successfully prepare the RF carbon aerogel particles with a truly spherical shape and control their size in the range from about 10 to 500 μm by changing the apparent viscosity of the RF sol. The spherical RF carbon aerogel particles with an average diameter of 20 μm have a BET surface area of about 800 m²/g and a uniform mesopore radius of 1.78 nm.     

Thermophysical properties of densified pitch based carbon/carbon materials—I. Unidirectional composites

Unidirectional carbon/carbon composites were developed using high-pressure impregnation/carbonization technique with PAN and pitch based carbon fibers of varying microstructure as reinforcements and different types of pitches as matrix precursors. The composites have been given final heat treatment to 2500-2700 °C. Microstructure of these composites has been evaluated using scanning electron microscope and polarized light optical microscope. Thermophysical properties, i.e., thermal conductivity, coefficient of thermal expansion and specific heat have been evaluated. It is found that the type of fibers and matrix present in the composites influences the absorption (specific heat) and transmission (conductivity) of thermal energy. The temperature dependence of thermal diffusion, specific heat, thermal conductivity and coefficient of thermal expansion has been studied and correlated with microstructure of carbon/carbon composites.     

Thermophysical properties of densified pitch based carbon/carbon materials—II. Bidirectional composites

Bidirectional carbon/carbon composites were developed using high-pressure impregnation/carbonization technique with PAN based carbon fabric as reinforcement and coal tar and synthetic pitches as matrix precursors. Microstructure of these composites has been evaluated using scanning electron microscope and polarized light optical microscope. Thermophysical properties i.e. thermal conductivity and specific heat have been evaluated both at room temperature and between 40 and 300 °C. The temperature dependence of thermal diffusion, specific heat and thermal conductivity has been studied and correlated with microstructure of carbon/carbon composites. It is found that the specific heat of carbon/carbon composites shows increase with temperature with an inverse slope in the temperature range of 150-200 °C. Accordingly, though the thermal conductivity decrease with temperature due to increased phonon interactions, it shows reversible action between 150 and 200 °C.     

A TEM study of microstructure of carbon fiber/polycarbosilane-derived SiC composites

The structures of two types of mesophase pitch-based carbon fibers (M30 and M70) reinforced SiC composites, prepared by the polycarbosilane impregnation-pyrolysis process, were investigated using transmission electron microscopy (TEM). It was found that M70 possessed a highly-ordered graphite structure despite occasional misorientation of some crystallites. However, the skin of M70 was less ordered than the interior of M70. The structure of M30 was uniform throughout, and was less ordered than that of M70. The fiber and matrix in M70/SiC bonded weakly, whereas the fiber and matrix in M30/SiC bonded tightly and locked together. This difference in the interface feature originates from the difference of the surface crystalline structures of M30 and M70, and is formed during the first impregnation-pyrolysis cycle of polycarbosilane.     

Evolution of chemistry and morphology during the carbonization and combustion of rice husk

Both fine carbon/silica and pure silica powders can be obtained by carbonization and combustion of rice husk under non-isothermal conditions, and the products can be used for preparation of high-quality ceramic materials. Studies on the morphology, chemical and physical characteristics of products were carried out by N₂-adsorptionmeter, SEM, XRD, FTIR, ICP-MS and EA. Results indicate that decreasing the heating rate increased the specific surface area, pore volume and pore diameter. At a heating rate of 5 °C/min, the specific surface areas of both the carbon/silica and pure silica powders were 261 and 235 m²/g, and the average pore diameters were 2.2 and 5.4 nm, respectively. The products obtained from various heating rates were all amorphous. Thermogravimetric analysis was employed to study the reaction characteristics during carbonization or combustion, indicating that decomposition process of rice husk could be divided into three temperature zones. This results of the study can also provide the important information on the recovery of biomass material from rice husk.     

Surface properties of carbon micro-coils oxidized by a low concentration of oxygen gas

Vapor-grown carbon micro-coils were oxidized under a low O₂ flow-rate for introducing oxygen-containing functional groups on the surface. The surface characteristics were then examined. The O1s/C1s intensity ratios of the XPS spectra measured on the surface increased on using the oxidation treatment. The maximum O1s/C1s ratio of 11.4 at.% was obtained under the following conditions: (a) the flow-rate of the mixed gas of O₂+Ar (O₂/Ar=1/10) was 82.5 sccm; (b) the oxidation temperature was 600°C; and (c) the treatment time was 30 min. The maximum O1s/C1s ratio is about 3.5 times that of the source carbon coils. The specific surface area significantly increased due to the oxidation treatment and attained a maximum value of 1050 m² g⁻¹, which is about 10 times that of the source carbon coils. As the specific surface area increased, the surface morphology of the carbon coils became more complicated on a nanometer scale.