Synthesis and characterization of fluorinated poly(etherimide)s toughening for carbon fiber‐reinforced epoxy composites

Novel‐fluorinated poly(etherimide)s (FPEIs) with controlled molecular weights were synthesized and characterized, which were used to toughen epoxy resins (EP/FPEI) and carbon fiber‐reinforced epoxy composites (CF/EP/FPEI). Experimental results indicated that the FPEIs possessed outstanding solubility, thermal, and mechanical properties. The thermally cured EP/FPEI resin showed obviously improved toughness with impact strength of 21.1 kJ/m² and elongation at break of 4.6%, respectively. The EP/FPEI resin also showed outstanding mechanical strength with tensile strength of 91.5 MPa and flexural strength of 141.5 MPa, respectively. The mechanical moduli and thermal property of epoxy resins were not affected by blending with FPEIs. Furthermore, CF/EP/FPEI composite exhibited significantly improved toughness with Mode I interlaminar fracture toughness (G_IC) of 899.4 J/m² and Mode II interlaminar fracture toughness (G_IIC) of 1017.8 J/m², respectively. Flexural properties and interlaminar shear strength of the composite were slightly increased after toughening. POLYM. COMPOS., 2010. © 2009 Society of Plastics Engineers     

Curing behavior and thermal and mechanical properties enhancement of tetraglycidyl‐4,4′‐diaminodiphenylmethane/4,4′‐diaminodiphenylsulfone using a liquid crystalline epoxy

A thermosetting resin system, based on tetraglycidyl‐4,4′‐diaminodiphenylmethane, has been developed via copolymerization with 4,4′‐diaminodiphenylsulfone in the presence of a newly synthesized liquid crystalline epoxy (LCE). The curing behavior of LCE‐containing resin system was evaluated using curing kinetics method and Fourier transform infrared spectroscopy. The effect of LCE on the thermal and mechanical properties of modified epoxy systems was studied. Thermogravimetric analysis indicated that the modified resin systems displayed a high T_0.05 and char yield at lower concentrations of LCE (≤5 wt%), suggesting an improved thermal stability. As determined using dynamic mechanical analysis and differential scanning calorimetry, the glass transition value increased by 9.7% compared to that of the neat resin when the LCE content was 5 wt%. Meanwhile, the addition of 5 wt% of LCE maximized the toughness with a 175% increase in impact strength. The analysis of fracture surfaces revealed a possible effect of LCE as a toughener and showed no phase separation in the modified resin system, which was also confirmed by dynamic mechanical analysis. © 2016 Society of Chemical Industry     

Study on the effect of woven sisal fiber mat on mechanical and viscoelastic properties of petroleum based epoxy and bioresin modified toughened epoxy network

Sisal fiber reinforced biocomposites are developed using both unmodified petrol based epoxy and bioresin modified epoxy as base matrix. Two bioresins, epoxidized soybean oil and epoxy methyl soyate (EMS) are used to modify the epoxy matrix for effective toughening and subsequently two layers of sisal fiber mat are incorporated to improve the mechanical and thermomechanical properties. Higher strength and modulus of the EMS modified epoxy composites reveals good interfacial bonding of matrix with the fibers. Fracture toughness parameters K_IC and G_IC are determined and found to be enhanced significantly. Notched impact strength is found to be higher for unmodified epoxy composite, whereas elongation at break is found to be much higher for modified epoxy blend. Dynamic mechanical analysis shows an improvement in the storage modulus for bioresin toughened composites on the account stiffness imparted by fibers. Loss modulus is found to be higher for EMS modified epoxy composite because of strong fiber–matrix interfacial bonding. Loss tangent curves show a strong influence of bioresin on damping behavior of epoxy composite. Strong fiber–matrix interface is found in modified epoxy composite by scanning electron microscopic analysis. © 2015 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2015 , 132, 42699.     

Enhanced mechanical properties and thermal shock resistance of Cf/ZrB2-SiC composite via an efficient slurry injection combined with vibration-assisted vacuum infiltration

An efficient slurry injection combined with vibration-assisted vacuum infiltration process has been developed to fabricate 3D continuous carbon fiber reinforced ZrB₂-SiC ceramics. Homogenous distribution between carbon fiber and ceramic was achieved successfully, leading to an enhancement in mechanical properties. The C_f-PyC/ZrB₂-SiC composite exhibited a typical non-brittle fracture mode with a superior fracture toughness of 6.72 ± 0.21 MPa·m^1/2 and an extraordinary work of fracture of 2270 J/m², respectively, increasing by nearly 14.8 % and 36 % as compared with those of a parent composite fabricated by only slurry injection and slurry infiltration. The enhancement in fracture toughness and work of fracture were attributed to multiple toughening mechanism including crack deflection, PyC coated fiber bundles pull-out and fiber bridging. Moreover, a critical thermal shock temperature difference of 814 °C was achieved, higher than that of traditional ZrB₂-based ceramics. This work presents an efficient approach to fabricate high-performance C_f/UHTCs with uniform architecture.     

Improved thermosets obtained from diglycidyl ether of bisphenol A/4,4′‐diaminodiphenylsulfone based on a new epoxy‐terminated hyperbranched polymer

A new hyperbranched polymer (HBP) with a flexible aromatic skeleton and terminal epoxy groups was synthesized to improve the toughness of diglycidyl ether of bisphenol A. The HBP was characterized using nuclear magnetic resonance, Fourier transfer infrared spectroscopy and gel permeation chromatography. The effect of HBP on the thermomechanical and mechanical properties of modified epoxy systems was studied. For evaluating the efficiency of the modified epoxy systems, composite samples using glass fiber cloth were molded and tested. Using dynamic mechanical analysis, a slight reduction in glass transition temperature (T_g) with increasing HBP content was observed. Analysis of fracture surfaces revealed a possible effect of HBP as a toughener and showed no phase separation in the modified resin systems. The results showed that the addition of 15 phr HBP maximized the toughness of the modified resin systems with 215 and 40% increases in impact and flexural strengths, respectively. T_g and heat resistance of cured modified resin systems decreased slightly with an increase in HBP content and, at 15 phr HBP, only a 2.6% decrease in thermomechanical properties was observed. Meanwhile, a molded composite with HBP showed improved mechanical properties and retention rate at 150 °C as compared to that made with neat resin. © 2015 Society of Chemical Industry     

Biphenyl liquid crystal epoxy containing flexible chain: Synthesis and thermal properties

A biphenyl type liquid crystal epoxy (LCE) monomer 4,4′-di(2,3-epoxyhexyloxy)biphenyl (LCBP4) containing flexible chain was synthesized and the curing behavior was investigated using 4,4′-diaminodiphenylmethane (DDM) as the curing agent. The effect of curing condition on the formation of the liquid crystalline phase was examined. The cured samples show good mechanical properties and thermal stabilities. Moreover, the relationship between thermal conductivity and structure of liquid crystalline domain was also discussed. The samples show high thermal conductivity up to 0.28–0.31 W/(m*K), which is 1.5 times as high as that of conventional epoxy systems. In addition, thermal conductive filler, Al₂O₃, was introduced into LCBP4/DDM to obtain higher thermal conductive composites. When the content of Al₂O₃ was 80 wt%, the thermal conductivity of the composite reached to 1.86 W/(m*K), while that of diglycidyl ether of bisphenol A (Bis-A) epoxy resin/DDM/Al₂O₃ was 1.15 W/(m*K). Compared with Bis-A epoxy resin, the formation of liquid crystal domains in the cured LCE resin enhanced the thermal conductivity synergistically with the presence of Al₂O₃. Furthermore, the introduction of Al₂O₃ also slightly increased the thermal stabilities of the cured LCE.     

Preparation and properties of multiwalled carbon nanotube/epoxy‐amine composites

Different amounts of multiwalled carbon tubes (MWCNTs) were incorporated into an epoxy resin based on diglycidyl ether of bisphenol A and both epoxy precursor and composite were cured with 4,4′‐diamino diphenyl sulfone. Transmission and scanning electron microscopy demonstrated that the carbon nanotubes are dispersed well in the epoxy matrix. Differential scanning calorimetry measurements confirmed the decrease in overall cure by the addition of MWCNTs. A decrease in volume shrinkage of the epoxy matrix caused by the addition of MWCNTs was observed by pressure–volume–temperature measurements. Thermomechanical and dynamic mechanical analysis were performed for the MWCNT/epoxy composites, showing that the T_g was slightly affected, whereas the dimensional stability and stiffness are improved by the addition of MWCNTs. Electrical conductivity measurements of the composite samples showed that an insulator to conductor transition takes place between 0.019 and 0.037 wt % MWCNTs. The addition of MWCNTs induces an increase in both impact strength (18%) and fracture toughness (38%) of the epoxy matrix with very low filler content. © 2012 Wiley Periodicals, Inc. J. Appl. Polym. Sci., 2013     

Effect of deposited carbon nanotubes on interlaminar properties of carbon fiber‐reinforced epoxy composites using a developed spraying processing

Carbon fiber‐reinforced epoxy composites, with incorporated carboxylic multiwall carbon nanotubes (CNTs), were prepared using vacuum‐assisted resin infusion (VARI) molding, and the in‐plane and out‐of‐plane properties, including mode‐I (G_Ic) and mode‐II (G_IIc) interlaminar fracture toughness, interlaminar shear strength (ILSS), tensile, and flexural properties were measured. A novel spraying technique, which sprays a kind of epoxy resin E20 with high viscosity after spraying the CNTs, was adopted to deposit the CNTs on the surface of carbon fiber fabric. The E20 was used to anchor CNTs on the fabric surface, avoiding that the deposited CNTs were removed by the infusing resin during VARI process. The spraying processing, including spraying amount and spraying sequence, was optimized based on the distribution of CNTs on the fibers. After that, three composite specimen groups were fabricated using different carbon fiber fabrics, including as‐received, CNT‐deposited with E20, and CNT‐deposited without E20. The effects of CNTs on the processing quality and mechanical properties of carbon fiber‐reinforced polymer composites were studied. The experimental results show that all studied laminates have uniform thickness with designed values and no obvious defects form inside the laminates. Compared with the composite without CNTs, depositing CNTs with E20 increases by 24% in the average propagation G_Ic, by 11% in the propagation G_IIc and by 12% in the ILSS, while it preserves the in‐plane mechanical properties, However, depositing CNTs without E20 reduces interlaminar fracture toughness. These phenomena are attributed to the differences in the distribution of CNTs and the fiber/matrix interfacial bonding for different spraying processing. POLYM. COMPOS., 2013. © 2012 Society of Plastics Engineers     

Tough and wear-resistant carbon fiber reinforced TiC-based composite prepared by alloyed melt infiltration at low temperatures

To improve the toughness and friction properties of carbon fiber reinforced ceramic matrix composite, a Cu alloy modified carbon fiber reinforced TiC based ceramic matrix composite was designed and prepared by TiCu alloy melt infiltration at low temperatures up to 1100 °C. The as-produced composite was mainly composed of carbon, TiC, Ti₃Cu₄, TiCu₄ and Cu phases. Due to the ductile Cu alloy introduced into the matrix, the composite showed good mechanical performance especially the fracture toughness. The flexural strength reached about 248.36 MPa while the fracture toughness was up to 15.78 MPa·m^1/2. The high toughness of the composite was mainly attributed to the fiber bridging, fiber pull-out, interface debonding, crack propagation and deflection. The tribological performance of the as-produced composite was measured using SiC and 440C stainless steel balls as counterparts, respectively. The as-prepared composite exhibited good wear resistance and the wear mechanism was discussed based on the microstructural observations.     

Preparation and properties of high performance phthalide‐containing bismaleimide modified epoxy matrices

A series of intercrosslinked networks formed by diglycidyl ether of bisphenol A epoxy resin (DGEBA) and novel bismaleimide containing phthalide cardo structure (BMIPP), with 4,4′‐diamino diphenyl sulfone (DDS) as hardener, have been investigated in detail. The curing behavior, thermal, mechanical and physical properties and compatibility of the blends were characterized using differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), dynamic mechanical analysis (DMA), notched Izod impact test, scanning electron microscopy (SEM) and water absorption test. DSC investigations showed that the exothermic transition temperature (T_p) of the blend systems shifted slightly to the higher temperature with increasing BMIPP content and there appeared a shoulder on the high‐temperature side of the exothermic peak when BMIPP content was above 15 wt %. TGA and DMA results indicated that the introduction of BMIPP into epoxy resin improved the thermal stability and the storage modulus (G′) in the glassy region while glass transition temperature (T_g) decreased. Compared with the unmodified epoxy resin, there was a moderate increase in the fracture toughness for modified resins and the blend containing 5 wt % of BMIPP had the maximum of impact strength. SEM suggested the formation of homogeneous networks and rougher fracture surface with an increase in BMIPP content. In addition, the equilibrium water uptake of the modified resins was reduced as BMIPP content increased. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2011     

Mechanically robust,electrically and thermally conductive graphene-based epoxy adhesives

This study develops a facile approach to fabricate adhesives consists of epoxy and cost-effective graphene platelets (GnPs). Morphology, mechanical properties, electrical and thermal conductivity, and adhesive toughness of epoxy/GnP nanocomposite were investigated. Significant improvements in mechanical properties of epoxy/GnP nanocomposites were achieved at low GnP loading of merely 0.5?vol%; for example, Young’s modulus, fracture toughness (K_1C) and energy release rate (G_1C) increased by 71%, 133% and 190%, respectively compared to neat epoxy. Percolation threshold of electrical conductivity is recorded at 0.58?vol% and thermal conductivity of 2.13?W m^?1 K^?1 at 6?vol% showing 4 folds enhancements. The lap shear strength of epoxy/GnP nanocomposite adhesive improved from 10.7?MPa for neat epoxy to 13.57?MPa at 0.375?vol% GnPs. The concluded results are superior to other composites or adhesives at similar fractions of fillers such as single-walled carbon nanotubes, multi-walled carbon nanotubes or graphene oxide. The study promises that GnPs are ideal candidate to achieve multifunctional epoxy adhesives.     

Investigation of thermal behaviour and mechanical property of the functionalised graphene oxide/epoxy resin nanocomposites

ABSTRACT

Graphite oxide (GO) and functionalised graphite oxide (FGO) were successfully prepared with -NH₂-terminated GO in the paper, and their chemical structures were characterised with Fourier transform infrared (FTIR), Energy-Dispersive X-ray Spectroscopy (EDS), UV spectrum analysis and XRD, their microstructures were researched by a scanning electron microscope (SEM) and a transmission electron microscope (TEM), and their thermal properties were characterised by TG. The result showed the carbon residue of FGO was 82.1% and the residual char of GO was 48%, the composite materials were prepared with curing for epoxy resin. The thermal stability, mechanical properties, and morphology after impacting tests of composite materials were investigated using thermogravimetric analysis, tensile and charpy impact tests and SEM. The result showed when the 0.2% FGO was filled into the epoxy, the tensile strength was 55.4?MPa, the impact strength was 17.3?KJ/m², the flexural strength was 82?MPa, and the flexural modulus was 2760?MPa. The mechanical properties of composite materials were higher than those of pure epoxy and improved the strength and toughness of epoxy nanocomposites.     

Rice husk‐derived porous carbon/silica particles as green filler for electronic package application

Bio‐based porous carbon/silica particles (denoted as RH‐carbon/silica) were successfully prepared from agricultural waste rice husk by using acid‐hydrothermal treatment and pyrolysis under nitrogen condition. As green filler, the cure behavior, thermal‐mechanical properties, and thermal conductivity of the epoxy‐carbon/silica biocomposites at different filler contents (5, 9, 17, 29 wt %) were characterized. Because of superior surface properties (surface area, porosity, and silica segment) and high content of carbon component in the RH‐carbon/silica, the characteristics of the biocomposites were significantly improved with the increase of the filler content. At 29 wt % of filler content, the epoxy biocomposites exhibit lower curing temperature (148 °C), lower CTE (42 ppm/°C), higher T_g (123 °C), higher storage modulus (4059 MPa), and higher effective thermal conductivity (0.29 W/mK). In brief, the RH‐carbon/silica particles that can serve not only as reinforcing agent but also as thermal transport medium used in epoxy composite, is a green and high‐performance filler for this purpose. © 2016 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2017 , 134, 44699.     

The Effect of WS2 Nanotubes on the Properties of Epoxy-Based Nanocomposites

In this paper we evaluated the effect of embedding inorganic nanotubes (INT) of tungsten disulfide (WS₂) in an epoxy matrix, on the mechanical, thermal and adhesion properties of the resulting nanocomposites. The nanotube content spanned a range of values (0, 0.1, 0.3, 0.5 and 1.0 wt%), and the nanotube incorporation process consisted of a combination of both distributive (magnetic stirring) and dispersive (ultrasonic mixing) methods. The adhesion of the nanocomposites to an aluminum substrate was characterized by both a single lap shear and a T-peel test. The fracture toughness (K _IC) of the nanocomposites was characterized by a standard compact tension (CT) plane-strain fracture test. The thermal properties of the nanocomposites were determined by dynamic mechanical thermal analysis (DMTA). Overall, the addition of INT-WS₂ was found to improve the shear strength and peel properties of the nanocomposite, and to significantly improve its fracture toughness and glass transition temperature. The extent and character of the nanotube–epoxy interaction were examined by electron microscopy, as was the energy dissipation mechanisms during fracture.     

The mechanical and thermal properties of graphitic carbon nitride (g-C3N4)-based epoxy composites

Numerous ways to reinforce epoxy resin and improve its thermomechanical properties have been attempted using organic and inorganic nanoparticles. In this paper, graphitic carbon nitride (g-C₃N₄) nanoparticles were synthesized and used to improve the mechanical properties and thermal stability of epoxy composites. The g-C₃N₄ was synthesized from cheap melamine powder using a simple one-step thermal treatment, then was used to reinforce the resin at different weight percentages (wt%). X-ray diffraction, scanning electron microscopy (SEM), and Fourier infrared spectroscopy were used to characterize the g-C₃N₄ and ensure its successful synthesis by studying the changes in its crystal structure, morphology, and chemical structure. The filler was dispersed in the resin using a combination of ultrasonication and high shear mixing. The results showed that the mechanical properties were optimum when 0.5 wt% g-C₃N₄ was used. The tensile strength and fracture toughness of the resulting epoxy composite improved by 21.8% and 77.3%, respectively. SEM was used to investigate the morphologies of cracks formed in epoxy composite specimens after the tensile testing. The SEM micrographs of the fracture surface showed a transition from a brittle to a rough morphology, signifying the enhancement in the composites' toughness. Thermogravimetric analysis showed a good improvement in degradation temperature of up to 8.86% while dynamic mechanical analysis showed that the incorporation of g-C₃N₄ did not affect the material's glass transition temperature.     

Interlaminar fracture toughness of woven fabric composite laminates with carbon nanotube/epoxy interleaf films

The Mode I interlaminar fracture behavior of woven carbon fiber/epoxy composite laminates incorporating partially cured carbon nanotube/epoxy composite films has been investigated. Laminates with films containing carbon nanotubes (CNTs) in the as‐received state and functionalized with polyamidoamine were evaluated, as well as laminates with neat epoxy films. Double‐cantilever beam (DCB) specimens were used to measure G_Ic, the critical strain energy release rate (fracture toughness) versus crack length. Post‐fracture microscopic inspection of the fracture surfaces was performed. Results show that initial fracture toughness was improved with the amino‐functionalized CNT/epoxy interleaf films, but the important factor appears to be the polyamidoamine functionalization, not the CNTs. The initial fracture toughness remained relatively unaffected with the incorporation of neat epoxy and as‐received CNT/epoxy interleaf films. Plateau fracture toughness was unchanged with the use of functionalized CNT/epoxy interleaf films, and was reduced with the use of neat epoxy and as‐received CNT/epoxy interleaf films. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2011     

Synthesis and characterization of chlorinated soy oil based epoxy resin/glass fiber composites

Composites with good toughness properties were prepared from chemically modified soy epoxy resin and glass fiber without additional petroleum based toughening agent. Chlorinated soy epoxy (CSE) resin was prepared from soybean oil. The CSE was characterised by spectral, and titration method. The prepared CSE was blended with commercial epoxy resin in different ratios and cured at 85°C for 3 h, and post cured at 225°C for 2 h using m‐phenylene diamine (MPDA) as curing agent. The cure temperatures of epoxy/CSE/MPDA with different compositions were found to be in the range of (151.2–187.5°C). The composite laminates were fabricated using epoxy /CSE/MPDA‐glass fiber at different compositions. The mechanical properties such as tensile strength (248–299 MPa), tensile modulus (2.4–3.4 GPa), flexural strength (346–379 MPa), flexural modulus (6.3–7.8 GPa) and impact strength (29.7–34.2) were determined. The impact strength increased with the increase in the CSE content. The interlaminor fracture toughness (G_IC) values also increased from 0.6953 KJ/m² for neat epoxy resin to 0.9514 KJ/m² for 15%CSE epoxy‐modified system. Thermogravimetric studies reveal that the thermal stability of the neat epoxy resin was decreased by incorporation of CSE. POLYM. COMPOS., 2009. © 2008 Society of Plastics Engineers     

High performance HTLNR/epoxy blend—Phase morphology and thermo-mechanical properties

An attempt was made to toughen diglycidyl ether of bisphenol A (DGEBA) type epoxy resin with liquid natural rubber possessing hydroxyl functionality (HTLNR). Epon 250 epoxy monomer is cured using nadic methyl anhydride as hardener in presence of N, N dimethyl benzyl amine as accelerator. HTLNR of different concentrations up to 20 wt % is used as modifier for epoxy resin. The addition HTLNR to an anhydride hardener/epoxy monomer mixture has given rise to the formation of phase-separated structure, consisting of small spherical liquid natural rubber particles bonded to the surrounding epoxy matrix. The particle size increased with increase in rubber content. The viscoelastic properties of the blends were analyzed using dynamic mechanical thermal analysis. The T_g corresponding to epoxy rich phase was evident from the dynamic mechanical spectrum, while the T_g of the rubber phase was overlapped by the β relaxation of epoxy phase. Glass transition of the epoxy phase decreased linearly as a function of the amount of rubber. The mechanical properties such as impact and fracture toughness were also carefully examined. The impact and fracture toughness increase with HTLNR content. A threefold increase in impact strength was observed with 15 wt % HTLNR/epoxy blend. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2012     

Characterization and role of an elastomeric interphase on carbon fibers reinforcing an epoxy matrix

Oxidized carbon fibers were coated using an on-line filament winding process with an elastomeric adduct crosslinkable and compatible with an epoxy matrix. The coating and modifications of the epoxy network were studied by dynamic mechanical measurements. Assuming that apparent activation energies of the secondary relaxation β_e of the epoxy network and main relaxation α_a of adduct are very different, it is possible at low frequencies to separate the two peaks. The composite material can be described as a three phase system: an epoxy network as matrix, carbon fibers, and a soft interlayer. The mechanical behavior of unidirectional composite materials studied by impact and bending tests is strongly dependent on the presence and the thickness of the coating at the carbon fiber surface.     

High-entropy (Ho0.2Y0.2Dy0.2Gd0.2Eu0.2)2Ti2O7/TiO2 composites with excellent mechanical and thermal properties

High-performance ceramics with low thermal conductivity, high mechanical properties, and idea thermal expansion coefficients have important applications in fields such as turbine blades and automotive engines. Currently, the thermal conductivity of ceramics has been significantly reduced by local doping/substitution or further high-entropy reconfiguration of the composition, but the mechanical properties, especially the fracture toughness, are insufficient and still need to be improved. In this work, based on the high-entropy titanate pyrochlore, TiO₂ was introduced for composite toughening and the high-entropy (Ho_0.2Y_0.2Dy_0.2Gd_0.2Eu_0.2)₂Ti₂O₇-xTiO₂ (x = 0, 0.2, 0.4, 1.0 and 2.0) composites with high hardness (16.17 GPa), Young's modulus (289.3 GPa) and fracture toughness (3.612 MPa·m^0.5), low thermal conductivity (1.22 W·m⁻¹·K⁻¹), and thermal expansion coefficients close to the substrate material (9.5 ×10⁻⁶/K) were successfully prepared by the solidification method. The fracture toughness of the composite toughened sample is 2.25 times higher than that before toughening, which exceeds most of the current low-thermal conductivity ceramics.