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The chemical structure of the surface of glass fibers, including silanized fibers, was studied. Highly efficient heat-resistant composites were obtained by impregnating silanized glass fiber with a polysulfone solution, and the effect of modification of the surface of glass fibers on the physical, mechanical and thermophysical properties of the composite materials was studied. As a result of the study, it was found that the fiber-to-polymer ratio of 70/30 wt.% showed the best mechanical properties for composites reinforced with pre-heat-treated and silanized glass fibers. It has been established that the chemical treatment of the glass fibers with silanes makes it possible to increase the mechanical properties by 1.5 times compared to composites reinforced with initial fibers. It was found that the use of silane coupling agents made it possible to increase the thermal stability of the composites. Mechanisms that improve the interfacial interaction between the glass fibers and the polymer matrix have been identified. It has been shown that an increase in adhesion occurs both due to the uniform distribution of the polymer on the surface of the glass fibers and due to the improved wettability of the fibers by the polymer. An interpenetrating network was formed in the interfacial region, providing a chemical bond between the functional groups on the surface of the glass fiber and the polymer matrix, which was formed as a result of treating the glass fiber surface with silanes, It has been shown that when treated with aminopropyltriethoxysilane, significant functional unprotonated amino groups NH+/NH2+ are formed on the surface of the fibers; such free amino groups, oriented in the direction from the fiber surface, form strong bonds with the matrix polymer. Based on experimental data, the chemical structure of the polymer/glass fiber interface was identified.
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In this study, the interlaminar fracture toughness and impact strength of polyethersulfone reinforced with continuous carbon fibers were studied. Interlaminar fracture toughness tests were performed using the double cantilever beam method. It was shown that surface modification using the thermal oxidation method of the carbon fibers can strongly increase the interlaminar fracture toughness of the obtained composites. Thus, the maximum value reached 1.72 kJ/m2, which was 40% higher than the fracture toughness of the composites reinforced with initial carbon fibers. Moreover, fractographic analysis using a scanning electron microscope allowed us to highlight the main reasons for the dependence of fracture toughness on fiber content and surface modification conditions of the carbon fibers. It was shown that the main factor that allowed for an increase in fracture toughness was the enhanced interfacial interaction between the fibers and polymer matrix. Additionally, it was found that expectedly, there was a good correlation between interlaminar fracture toughness and interlaminar shear strength results. However, a negative influence of surface modification on the impact properties of composites was found. Such behavior occurred because of higher structural stability and lower exposure to delamination in multiple layers of the composites reinforced with the modified carbon fibers. It was found that impact energy reached ~150 kJ/m2 for the polyethersulfone-based composites reinforced with initial fibers, while the composites reinforced with modified carbon fibers showed impact energy values of only ~80 kJ/m2. Nevertheless, surface modification of carbon fibers using the thermal oxidation method can be an effective method for improving the performance properties of polyethersulfone-based composite materials.
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The paper is devoted to the study of thermal and mechanical behavior and structural features of the polysulfone solution impregnated unidirectional carbon fiber yarns depending on fabrication conditions and appearance for optimum production method of the composites. The effect of producing conditions, such as polysulfone solution concentration, drying and post-heating temperatures, and the residual solvent content on the structure, mechanical, and thermal properties of the carbon fiber-reinforced composites was studied. The polysulfone solution impregnated carbon fiber yarns show relatively high mechanical properties, realizing up to 80% of the carbon fibers' tensile strength, which can be attributed to good wettability and uniform polymer matrix distribution throughout the entire volume of the composites. It was found that the composites impregnated with 40 wt.% of the polysulfone solution showed lower porosity and higher mechanical properties. The results of a dynamic mechanical analysis indicate that residual solvent has a significant effect on the composites' thermal behavior. The composites heated to 350 °C for a 30 min showed higher thermal stability compared to ones dried at 110 °C due to removal of residual solvent during heating. The impregnated carbon fiber yarns can be used for the further producing bulk unidirectional composites by compression molding and the proposed method can be easily transformed to continuous filament production, for example for further use in 3-D printing technology.
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In this study, the mechanical and thermophysical properties of carbon fiber-reinforced polyethersulfone are investigated. To enhance the interfacial interaction between carbon fibers and the polymer matrix, the surface modification of carbon fibers by thermal oxidation is conducted. By means of AFM and X-ray spectroscopy, it is determined that surface modification changes the morphology and chemical composition of carbon fibers. It is shown that surface modification dramatically increases the mechanical properties of the composites. Thus, flexural strength and the E-modulus of the composites reinforced with modified fibers reached approximately 962 MPa and 60 GPa, respectively, compared with approximately 600 MPa and 50 GPa for the composites reinforced with the initial ones. The heat deflection temperatures of the composites reinforced with the initial and modified fibers were measured. It is shown that composites reinforced with modified fibers lose their stability at temperatures of about 211 °C, which correlates with the glass transition temperature of the PES matrix. The thermal conductivity of the composites with different fiber content is investigated in two directions: in-plane and transverse to layers of carbon fibers. The obtained composites had a relatively high realization of the thermal conductive properties of carbon fibers, up to 55-60%.
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This work evaluated the fracture toughness of the low-temperature carbonized elastomer-based composites filled with shungite and short carbon fibers. The effects of the carbonization temperature and filler content on the critical stress intensity factor (K1c) were examined. The K1c parameter was obtained using three-point bending tests for specimens with different l/b ratio (notch depth to sample thickness) ranging from 0.2 to 0.4. Reliable detection of the initiation and propagation of cracks was achieved using an acoustic sensor was attached to the samples during the bending test. The critical stress intensity factor was found to decrease linearly with increasing carbonization temperature. As the temperature increased from 280 to 380 °C, the K1c parameter was drastically reduced from about 5 to 1 MPa·m1/2 and was associated with intense outgassing during the carbonization step that resulted in sample porosity. The carbon fiber addition led to some incremental toughening; however, it reduced the statistical dispersion of the K1c values.
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The structure of self-reinforced composites (SRCs) based on ultra-high molecular weight polyethylene (UHMWPE) was studied by means of Wide-Angle X-ray Scattering (WAXS), X-ray tomography, Raman spectroscopy, Scanning Electron Microscopy (SEM) and in situ tensile testing in combination with advanced processing tools to determine the correlation between the processing conditions, on one hand, and the molecular structure and mechanical properties, on the other. SRCs were fabricated by hot compaction of UHMWPE fibers at different pressure and temperature combinations without addition of polymer matrix or softener. It was found by WAXS that higher compaction temperatures led to more extensive melting of fibers with the corresponding reduction of the Herman's factor reflecting the degree of molecular orientation, while the increase of hot compaction pressure suppressed the melting of fibers within SRCs at a given temperature. X-ray tomography proved the absence of porosity while polarized light Raman spectroscopy measurements for both longitudinal and perpendicular fiber orientations showed qualitatively the anisotropy of SRC samples. SEM revealed that the matrix was formed by interlayers of molten polymer entrapped between fibers in SRCs. Moreover, in situ tensile tests demonstrated the increase of Young's modulus and tensile strength with increasing temperature.
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Carbonized elastomer-based composites (CECs) possess a number of attractive features in terms of thermomechanical and electromechanical performance, durability in aggressive media and facile net-shape formability, but their relatively low ductility and strength limit their suitability for structural engineering applications. Prospective applications such as structural elements of micro-electro-mechanical systems MEMS can be envisaged since smaller principal dimensions reduce the susceptibility of components to residual stress accumulation during carbonization and to brittle fracture in general. We report the results of in situ in-SEM study of microdeformation and fracture behavior of CECs based on nitrile butadiene rubber (NBR) elastomeric matrices filled with carbon and silicon carbide. Nanostructured carbon composite materials were manufactured via compounding of elastomeric substance with carbon and SiC fillers using mixing rolling mill, vulcanization, and low-temperature carbonization. Double-edge notched tensile (DENT) specimens of vulcanized and carbonized elastomeric composites were subjected to in situ tensile testing in the chamber of the scanning electron microscope (SEM) Tescan Vega 3 using a Deben microtest 1 kN tensile stage. The series of acquired SEM images were analyzed by means of digital image correlation (DIC) using Ncorr open-source software to map the spatial distribution of strain. These maps were correlated with finite element modeling (FEM) simulations to refine the values of elastic moduli. Moreover, the elastic moduli were derived from unloading curve nanoindentation hardness measurements carried out using a NanoScan-4D tester and interpreted using the Oliver-Pharr method. Carbonization causes a significant increase of elastic moduli from 0.86 ± 0.07 GPa to 14.12 ± 1.20 GPa for the composite with graphite and carbon black fillers. Nanoindentation measurements yield somewhat lower values, namely, 0.25 ± 0.02 GPa and 9.83 ± 1.10 GPa before and after carbonization, respectively. The analysis of fractography images suggests that crack initiation, growth and propagation may occur both at the notch stress concentrator or relatively far from the notch. Possible causes of such response are discussed, namely, (1) residual stresses introduced by processing; (2) shape and size of fillers; and (3) the emanation and accumulation of gases in composites during carbonization.
Assuntos
Elastômeros/química , Nanocompostos/química , Carbono/química , Compostos Inorgânicos de Carbono/química , Simulação por Computador , Módulo de Elasticidade , Análise de Elementos Finitos , Dureza , Teste de Materiais , Microscopia Eletrônica de Varredura , Nanocompostos/ultraestrutura , Compostos de Silício/química , Estresse Mecânico , Resistência à TraçãoRESUMO
Thermally stable composites obtained by the low-temperature carbonization of an elastomeric matrix filled with hard dispersed silicon carbide particles were obtained and investigated. Evolution of the microstructure and of mechanical and thermal characteristics of composites during thermal degradation and carbonization processes in a wide range of filling from 0 to 450 parts per hundred rubber was studied. For highly filled composites, the compressive strength values were found to be more than 200 MPa; Young's modulus was more than 15 GPa. The thermal conductivity coefficient of composites was up to 1.6 W/(m·K), and this magnitude varied slightly in the temperature range of 25-300 °C. Coupled with the high thermal stability of the composites, the observed properties make it possible to consider using such composites as strained friction units instead of reinforced polymers.
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Since obtaining a highly oriented structure based on a large-scale commercial ultra-high molecular weight polyethylene (UHMWPE) is considered very difficult due to its high molecular weight and melting index, modifying the structure of these cheap commercial UHMWPE brands into a supra-molecular structure with fiber-forming properties by adding a small amount of polyethylene wax (PE-wax) will provide the possibility to obtain highly oriented UHMWPE products with enhanced mechanical and tribological properties. In this work, highly oriented UHMWPE/PE-wax films were prepared. The PE-wax affected the UHMWPE as an intermolecular lubricant. The obtained lamellar structure of the UHMWPE/PE-wax composites had a better processability. The UHMWPE and UHMWPE/PE-wax structures for the xerogels and the films were studied by using differential scanning calorimetry and scanning electron microscopy. The PE-wax presence enhanced the mechanical properties of the UHMWPE/PE-wax films to a high degree. The highest average value of the tensile strength was 1320 MPa (an increase of 78%) obtained by adding a PE-wax content of 1.0 wt.%, and the highest average value of the Young's modulus was 56.8 GPa (an increase of 71%) obtained by adding a PE-wax content of 2.0 wt.%. The addition of the PE-wax increased the work of fracture values of the UHMWPE/PE-wax films up to 233%. The formation of the cavities was observed in the virgin UHMWPE films more than in the UHMWPE/PE-wax films, and the whitening of the oriented films was related to the crystallization process more than to the cavitation phenomenon. The coefficient of friction of the oriented UHMWPE/PE-wax films improved by 33% in comparison with the isotropic UHMWPE, and by 7% in comparison with the oriented virgin UHMWPE films.
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The effect of thermal treatment of glass fibers (GF) on the mechanical and thermo-mechanical properties of polysulfone (PSU) based composites reinforced with GF was investigated. Flexural and shear tests were used to study the composites' mechanical properties. A dynamic mechanical analysis (DMA) and a heat deflection temperature (HDT) test were used to study the thermo-mechanical properties of composites. The chemical structure of the composites was studied using IR-spectroscopy, and scanning electron microscopy (SEM) was used to illustrate the microstructure of the fracture surface. Three fiber to polymer ratios of initial and preheated GF composites (50/50, 60/40, 70/30 (wt.%)) were studied. The results showed that the mechanical and thermo-mechanical properties improved with an increase in the fiber to polymer ratio. The interfacial adhesion in the preheated composites enhanced as a result of removing the sizing coating during the thermal treatment of GF, which improved the properties of the preheated composites compared with the composites reinforced with initial untreated fibers. The SEM images showed a good distribution of the polymer on the GF surface in the preheated GF composites.
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The properties of hybrid self-reinforced composite (SRC) materials based on ultra-high molecular weight polyethylene (UHMWPE) were studied. The hybrid materials consist of two parts: an isotropic UHMWPE layer and unidirectional SRC based on UHMWPE fibers. Hot compaction as an approach to obtaining composites allowed melting only the surface of each UHMWPE fiber. Thus, after cooling, the molten UHMWPE formed an SRC matrix and bound an isotropic UHMWPE layer and the SRC. The single-lap shear test, flexural test, and differential scanning calorimetry (DSC) analysis were carried out to determine the influence of hot compaction parameters on the properties of the SRC and the adhesion between the layers. The shear strength increased with increasing hot compaction temperature while the preserved fibers' volume decreased, which was proved by the DSC analysis and a reduction in the flexural modulus of the SRC. The increase in hot compaction pressure resulted in a decrease in shear strength caused by lower remelting of the fibers' surface. It was shown that the hot compaction approach allows combining UHMWPE products with different molecular, supramolecular, and structural features. Moreover, the adhesion and mechanical properties of the composites can be varied by the parameters of hot compaction.
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Interfacial interaction is one of the most important factors that affect the mechanical properties of the fiber reinforced composites. The effect of fabrics' sizing removal from glass fibers' surface by thermal treatment on the mechanical characteristics of polyethersulfone based composites at different fiber to polymer weight ratios was investigated. Three fiber to polymer weight ratios of 50/50, 60/40, and 70/30 were studied. Flexural and shear tests were carried out to illustrate the mechanical properties of the composites; the structure was studied using Fourier-transform infrared spectroscopy and scanning electron microscopy. It was shown that solution impregnation of glass fabrics with polyethersulfone before compression molding allows to achieve good mechanical properties of composites. The thermal treatment of glass fabrics before impregnation results in an increase in flexural and shear strength for all the composites due to the improvement of fiber-matrix interaction.
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The paper studies new high-temperature thermoplastic impregnated unidirectional carbon fiber composites. The research focuses on the effect of thermal and chemical oxidation of the carbon fibers surface on the interfacial interaction between fibers and polysulfone and polyphenylene sulfide as well as thermal and mechanical properties of the composites. The research reveals the interaction between carbon fibers and the polymer matrix depend both on the type of surface treatment and nature of the polymer. The chemical oxidation of carbon fibers results in good interfacial interaction, and the best mechanical properties were observed for tows impregnated with polyphenylene sulfide.
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Carbon fabrics are widely used in polymer based composites. Nowadays, most of the advanced high-performance composites are based on thermosetting polymer matrices such as epoxy resin. Thermoplastics have received high attention as polymer matrices due to their low curing duration, high chemical resistance, high recyclability, and mass production capability in comparison with thermosetting polymers. In this paper, we suggest thermoplastic based composite materials reinforced with carbon fibers. Composites based on polysulfone reinforced with carbon fabrics using polymer solvent impregnation were studied. It is well known that despite the excellent mechanical properties, carbon fibers possess poor wettability and adhesion to polymers because of the fiber surface chemical inertness and smoothness. Therefore, to improve the fiber-matrix interfacial interaction, the surface modification of the carbon fibers by thermal oxidation was used. It was shown that the surface modification resulted in a noticeable change in the functional composition of the carbon fibers' surface and increased the mechanical properties of the polysulfone based composites. Significant increase in composites mechanical properties and thermal stability as a result of carbon fiber surface modification was observed.
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Bulk oriented films based on ultrahigh molecular weight polyethylene (UHMWPE) with a drawing ratio of 35 were prepared by using a low solvent concentration. Bulk oriented films were filled with fluorinated multi-walled carbon nanotubes (FMWCNTs). The structure of bulk oriented films on UHMWPE, which were manufactured at different stages of orientation, was investigated by scanning electron microscope (SEM) and differential scanning calorimetry (DSC). The addition of FMWCNTs at a concentration of 0.05 wt % in bulk oriented UHMWPE films led to an increase in the tensile strength by 10% (up to 1020 ± 23 MPa) compared to unfilled oriented films. However, the addition of FMWCNTs at a concentration of more than 0.5 wt % led to a decrease in tensile strength due to excessive accumulation of nanotubes and hindering of self-diffusion of UHMWPE macromolecules. The multiple increase in tensile strength, doubling the hardness, the formation of fibrillar structure, and the presence of carbon nanotubes led to a significant increase in tribological properties in bulk oriented films. Bulk oriented UHMWPE/1% FMWCNT films can be operated at a maximum contact pressure that is 18 times higher and exhibit a specific wear rate more than an order of magnitude and less than the traditional UHMWPE of isotropic structure. Bulk oriented UHMWPE/1% FMWCNT films have an extremely low dry coefficient of friction (COF) of 0.075 at a contact pressure of 31 MPa. The developed bulk oriented films can be used for manufacturing frictional surfaces for sliding bearings, or for acetabular cups for knee and hip endoprostheses.