Mechanical properties of carbon woven reinforced epoxy matrix composites. A study on the influence of matrix modification with polysulfone

An experimental investigation has been carried out to study the influence of thermoplastic addition on the mechanical properties of woven carbon fiber/epoxy matrix composites. As toughening agent bisphenol‐A polysulfone, PSu, has been added to the epoxy matrix. Flexural tests haved been performed to characterize the mechanical behavior of unmodified and PSu‐modified bulk tetra‐ and bifunctional epoxy matrices and also for the corresponding woven carbon fiber, CF, composite materials. Three‐point notched flexural tests been used to investigate the influence of polysulfone addition in the mode‐I fracture properties of the bulk epoxy matrices, relating them to their microstructural features investigated by atomic force microscopy (AFM). The double‐cantilever bea (DCB) and the end‐notched flexural (ENF) tests have been applied to characterize the interlaminar fracture toughness of the corresponding composites. For composites, the flexural properties were simmilar independent of the funcetionality of the epoxy matrix and of the thermoplastic content. Nevertheless, PSu addition to the epoxy matrix celarly enhanced the ode‐I and II interlaminar fracture toughness of the corresponding composites, the immprovement being higher for the composites manufactured with the bifunctional epoxy matrix at every thermoplastic content because of the lower crosslink density of the epoxy matrix.     

Influence of polyethersulfone modification of a tetrafunctional epoxy matrix on the fracture behavior of composite laminates based on woven carbon fibers

In this study, the influence of poly(ethersulfone) (PES) as a modifying agent of a tetrafunctional epoxy matrix (TGDDM) on the mechanical behavior of composite laminates based on woven carbon fibers has been investigated. Dynamic mechanical experiments were performed on neat matrix resins and on their corresponding laminate composites. Mode-I and Mode-II fracture toughness tests for the bulk matrices and their composites, respectively, and also flexural and short beam shear tests (SBS) were carried out. Atomic force microscopy (AFM) and scanning electron microscopy (SEM) were used to investigate the morphologies obtained. A nanoscopic phase separation was obtained after PES addition, which was not able to stabilize the fracture process, leading, as a consequence, to a poor extent of improvement on fracture toughness properties. Polym. Compos. 25:480–488, 2004. © 2004 Society of Plastics Engineers.     

A comparative study on the influence of epoxy sizings on the mechanical performance of woven carbon fiber-epoxy composites

In the present work the effect of epoxy sizings on the fracture behavior of woven carbon fiber tetrafunctional epoxy composites has been investigated. Three-point flexural, short beam shear (SBS) and Mode-II interlaminar fracture toughness (ENF) tests have been carried out. Wettability and Atomic Force Microscopy (AFM) studies have been performed on commercial sized, desized and 0.7 wt% TGDDM and 0.7 wt% DGEBA sized carbon fibers. Dynamic mechanical thermal analysis and Scanning Electron Microscopy (SEM) studies were also carried out on the different carbon fiber/epoxy composites. The used sizing treatments provided composites with improved mechanical properties due to the enhancement achieved in the fiber-matrix adhesion. Polym. Compos. 25:319–330, 2004. © 2004 Society of Plastics Engineers.     

Mechanical properties of glass fiber composites with an epoxy resin modified by a liquid crystalline epoxy

The effect of liquid crystalline networks on epoxy + glass fiber composites is investigated. The matrix obtained from in‐situ curing of liquid crystalline (LC) diglycidyl ether of 4,4‐dihydroxybiphenol (DGE‐DHBP) with diglycidyl ether of bisphenol F (DGEBP‐F) by anhydride curing agent was used as the matrix for polymer composites. Impact, tensile, and flexural testing results are compared between the unmodified and modified systems. The interlaminar fracture toughness of commposites in the shear mode was determined by end notch flexure (ENF) tests. Scanning electron microscopy is used to study the fracture surfaces to understand the mechanism of fracture and interphase formation between the fiber and the matrix.     

Control of morphologies and mechanical properties of thermoplastic‐modified epoxy matrices by addition of a second thermoplastic

Ternary mixtures based on stoichiometric mixtures of the diglycidyl ether of bisphenol‐A (DGEBA) and 4,4′‐diaminodiphenyl sulfone (DDS) and two miscible thermoplastics, poly(methyl methacrylate) (PMMA) and the poly(hydroxy ether of bisphenol‐A) (phenoxy), were investigated by optical microscopy (OM), atomic force microscopy (AFM) and dynamic mechanical analysis (DMA). Mechanical testing was used to study the ultimate behavior. All the modified epoxy mixtures were heterogeneous. DMA has been shown to be an excellent technique for detecting the morphologies generated after curing when the loss modulus is used for analysis. Morphology varied with the thermoplastic content on the mixtures. The addition of a second thermoplastic in small amounts changed the morphological features from particulated to co‐continuous and from that to phase‐inverted morphologies. A significant increase in fracture toughness was observed above all for the mixtures with some level of co‐continuity within the epoxy‐rich matrix. Phase inversion led to poor strength and also fracture toughness. Copyright © 2003 Society of Chemical Industry     

Microstructural,mechanical, and thermal characteristics of recycled cellulose fiber‐halloysite‐epoxy hybrid nanocomposites

Epoxy hybrid‐nanocomposites reinforced with recycled cellulose fibers (RCF) and halloysite nanotubes (HNTs) have been fabricated and investigated. The dispersion of HNTs was studied by synchrotron radiation diffraction (SRD) and transmission electron microscopy (TEM). The influences of RCF/HNTs dispersion on the mechanical properties and thermal properties of these composites have been characterized in terms of flexural strength, flexural modulus, fracture toughness, impact toughness, impact strength, and thermogravimetric analysis. The fracture surface morphology and toughness mechanisms were investigated by SEM. Results indicated that mechanical properties increased because of the addition of HNTs into the epoxy matrix. Flexural strength, flexural modulus, fracture toughness, and impact toughness increased by 20.8, 72.8, 56.5, and 25.0%, respectively, at 1 wt% HNTs load. The presence of RCF dramatically enhanced flexural strength, fracture toughness, impact strength, and impact toughness of the composites by 160%, 350%, 444%, and 263%, respectively. However, adding HNTs to RCF/epoxy showed only slight enhancements in flexural strength and fracture toughness. The inclusion of 5 wt% HNTs into RCF/epoxy ecocomposites increased the impact toughness by 27.6%. The presence of either HNTs or RCF accelerated the thermal degradation of neat epoxy. However, at high temperature, samples reinforced with RCF and HNTs displayed better thermal stability with increased char residue than neat resin. POLYM. COMPOS. 2012. © 2012 Society of Plastics Engineers     

Influence of processing conditions and physicochemical interactions on morphology and fracture behavior of a clay/thermoplastic/thermosetting ternary blend

This study provides information on the mechanical behavior of epoxy‐poly(methyl methacrylate) (PMMA)‐clay ternary composites, which have been prepared using the phase separation phenomenon of PMMA and the introduction of organophilic‐modified montmorillonites (MMTs), the continuous matrix being the epoxy network. Two dispersion processing methods are used: a melt processing without any solvent and an ultrasonic technique with solvent and a high‐speed stirrer. TEM analysis shows that phase separation between PMMA and the epoxy network was obtained in the shape of spherical nodules in the presence of the clay in both process methods used. Nanoclay particles were finely dispersed inside thermosetting matrix predominantly delaminated when ultrasonic blending was used; whereas micrometer‐sized aggregates were formed when melt blending was used. The mechanical behavior of the ternary nanocomposites was characterized using three‐point bending test, dynamic mechanical analysis (DMA), and linear elastic fracture mechanics. The corresponding fracture surfaces were examined by scanning electron microscopy to identify the relevant fracture mechanisms involved. It was evidenced that the better dispersion does not give the highest toughness because ternary nanocomposites obtained by melt blending present the highest fracture parameters (K_Ic). Some remaining disordered clay tactoids seem necessary to promote some specific toughening mechanisms. © 2010 Wiley Periodicals, Inc. J Appl Polym Sci, 2010     

Poly(methyl methacrylate)‐modified vinyl ester thermosets: Morphology,volume shrinkage,and mechanical properties

Thermoset materials obtained from styrene/vinyl ester resins of different molecular weights modified with poly(methyl methacrylate) (PMMA) were prepared and studied. Scanning electron microscopy and transmission electron microscopy micrographs of the fracture surfaces allowed the determination of a two‐phase morphology of the modified networks. Depending on the molecular weight of the vinyl ester oligomer, the initial content of the PMMA additive, and the selected curing temperature, different morphologies were obtained, including the dispersion of thermoplastic‐rich particles in a thermoset‐rich matrix, cocontinuous structures, and the dispersion of thermoset‐rich particles in a thermoplastic‐rich matrix (phase‐inverted structure). Density measurements were performed to determine the effect of the PMMA‐modifier concentration and curing temperature on the volume shrinkage of the final materials. The development of cocontinuous or thermoplastic‐rich matrices was not too effective in controlling the volume shrinkage of the studied vinyl ester systems. The evaluation of the dynamic mechanical behavior, flexural modulus, compressive yield stress, and fracture toughness showed that the addition of PMMA increased the fracture resistance without significantly compromising the thermal or mechanical properties of the vinyl ester networks. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci 2007     

Fracture toughness improvement of epoxy resins with short carbon fibers

This study examined the thermal stability and fracture toughness of diglycidylether of bisphenol-A (DGEBA)/short carbon fiber (SCF) composites using several techniques. The thermal stability of the DGEBA/SCF composites was similar to that of neat epoxy resin. The fracture toughness of the composites was significantly improved relative to the neat resin. The SEM micrographs indicated that a relatively rough surface with shear deformation and tortuous cracks was formed, thereby preventing deformation and crack propagation and inducing higher fracture toughness in the DGEBA/SCF composites.     

Morphology,viscoelastic properties,and mechanical behavior of epoxy resin modified with hydroxyl‐terminated poly(ether ether ketone) oligomer with pendent tert‐butyl groups

Hydroxyl‐terminated poly (ether ether ketone) with pendent tert‐butyl groups (PEEKTOH) synthesized from 4,4′‐difluorobenzophenone and tert‐butyl hydroquinone was blended with diglycidyl ether of bisphenol‐A (DGEBA) epoxy resin. A diamine, 4,4′‐diaminodiphenyl sulfone (DDS) was used as the curing agent. The thermal and mechanical properties, fracture toughness, and morphology of the blends were investigated. Morphological analysis of the blends revealed a particulate structure with PEEKTOH phase dispersed in the epoxy matrix. Unlike classical polymer blend systems, increase in concentration of PEEKTOH does not increase the domain size. Instead, a decrease is obtained. The fracture toughness increased with the addition of oligomer without much decrease in tensile and flexural strengths. Addition of 15 phr oligomer gave maximum toughness. The dispersed PEEKTOH initiated several mechanisms that improved the fracture toughness of the blends. The cross‐link density calculated from the storage modulus in the rubbery plateau region decreased with the increase in PEEKTOH. The thermal stability of epoxy resin remained unaffected even after blending with PEEKTOH. POLYM. ENG. SCI., 45:1645–1654, 2005. © 2005 Society of Plastics Engineers     

Influence of fiber modification on interfacial adhesion and mechanical properties of pineapple leaf fiber‐epoxy composites

Three kinds of surface treatment, that is, the alkalization (5% w/v NaOH aqueous solution), the deposition of diglycidyl ether of bisphenol A (DGEBA) from toluene solution (1% w/v DGEBA), and the alkalization combined with the deposition of DGEBA (5% w/v NaOH/1% w/v DGEBA) were applied to modify interfacial bonding and to enhance mechanical properties of pineapple leaf fiber (PALF) reinforced epoxy composites. The fiber strength and strain were measured by single fiber test and the fiber strength variation was assessed using Weibull modulus. Furthermore, a fragmentation test was used to quantify the interfacial adhesion of PALF‐epoxy composite. It was verified that the interfacial shear strength of modified PALFs was substantially higher than that of untreated PALF by almost 2–2.7 times because of the greater interaction between the PALFs and epoxy resin matrix. The strongest interfacial adhesion was obtained from the fibers that had been received the alkalization combined with DGEBA deposition. Moreover, the flexural and impact properties of unidirectional PALF‐epoxy composites were greatly enhanced when reinforced with the modified PALFs due to an improvement in interfacial adhesion, particularly in the synergetic use of 5% NaOH and 5% NaOH/1% DGEBA. © 2008 Wiley Periodicals, Inc. J Appl Polym Sci, 2008     

Preparation of hyperbranched epoxy resin containing nitrogen heterocycle and its toughened and reinforced composites

Low‐viscosity hyperbranched epoxy resin‐containing nitrogen heterocycle (HTPE) is synthesized from epichlorohydrin (ECH), dimethylol propionic acid (DMPA), and tris(2‐hydrooxyethyl)‐isocyanurate. The structure and properties of HTPE are characterized by FTIR, GPC, and molecular simulation. The performance of HTPE/diglycidyl ether of bisphenol‐A (DGEBA) composites first increase and then decrease with the increase of the content and molecular weight of HTPE. Compared to those of pure DGEBA, the impact strength, fracture toughness, tensile, and flexural strength of HTPE‐2/DGEBA composite can be enhanced by about 192%, 39%, 18%, and 23%, respectively. The absence of microphase separation and the presence of lots of “protonema” on the fracture surface of the composites are explicated by an in situ reinforcing and toughening mechanism. The intramolecular cavity of HTPE and the strong interaction between HTPE and DGEBA are two key factors to toughening and reinforcing DGEBA. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2012     

Influence of multiwalled carbon nanotubes on the processing behavior of epoxy powder compositions and on the mechanical properties of their fiber reinforced composites

This study reports the preparation of advanced carbon fiber composites with a nanocomposite matrix prepared by dispersing multiwall carbon nanotubes (CNTs) in a powder type epoxy oligomer with two different processing techniques (1) master batch dilution technique and (2) direct mixing (with the help of twin‐screw extruder in both cases). The master batch technique shows a better efficiency for the dispersion of the CNTs aggregates. The rheological results demonstrate that the incorporation of the CNTs into the epoxy oligomer leads, as expected, to a marked increase in the viscosity and of the presence of a yield stress point that also depends on the processing technique adopted. Carbon fiber (CFRP) and glass fiber (GFRP) composite materials were produced by electrostatic spraying of the epoxy matrix formulations on the carbon and glass fabric, respectively, followed by calendering and mold pressing. The mechanical properties of the obtained epoxy/CNT‐matrix composite materials, such as interlaminar fracture toughness, flexural strength, shear storage and loss moduli are discussed in terms of the processing techniques and fabric material. The incorporation of 1 wt% CNTs in the epoxy matrix results in a relevant increase of the fracture toughness, flexural strength and modulus of both CFRP and GFRP. POLYM. COMPOS., 37:2377–2383, 2016. © 2015 Society of Plastics Engineers     

Incorporation of silicon dioxide nanoparticles at the carbon fiber‐epoxy matrix interphase and its effect on composite mechanical properties

Functionalized silicon dioxide nanoparticles (nano‐fSiO₂) were uniformly deposited on the surface of carbon fibers (CFs) using a coating process which consisted of immersing the fibers directly in a suspension of nano‐fSiO₂ particles and epoxy monomers in 1‐methyl‐2‐pyrrolidinone (NMP). The 0° flexural properties, 90° flexural properties, and Interlaminar shear strength (ILSS) mechanical properties of unidirectional epoxy composites made with nano‐fSiO₂+epoxy sized carbon fibers, with control fibers, and with epoxy‐only sized fibers were measured and compared. An obvious increase of the fiber/matrix adherence strength was obtained with the nano‐fSiO₂+epoxy coating. The nano‐fSiO₂+epoxy sized CF/epoxy composites showed a relative increase of 15%, 50%, and 22% in comparison to control fibers, for the Interlaminar shear strength, the 90^° flexural strength and the 90° flexural modulus, respectively, but little e difference was measured between the different systems for the 0° flexural properties. The observation of the fracture surfaces by scanning electron microscopy of composite fracture confirmed the improvement of the interfacially dependent mechanical properties. POLYM. COMPOS., 38:1474–1482, 2017. © 2015 Society of Plastics Engineers     

Strengthening and toughening effects of layered double hydroxide and hyperbranched polymer on epoxy resin

The effects of organically modified layered double hydroxide (O-LDH) and epoxy functionalized hyperbranched aliphatic polyester (E1), on the mechanical strength, thermal property and toughness of diglycidyl ether of bisphenol A (DGEBA) epoxy resin were studied in detail. The crystalline structure and morphology of the nanocomposites composed of DGEBA/O-LDH and DGEBA/E1/O-LDH were investigated by wide angle X-ray diffraction analysis and transmission electron microscopy observation. Both results showed that the LDH nanosheets were sufficiently exfoliated and randomly dispersed in the epoxy matrix. The thermal and mechanical properties were compared with the corresponding neat polymer matrix. The enhancement in strength and toughness was achieved by the addition of O-LDH and E1, respectively, and confirmed in terms of fracture surface analysis by scanning electron microscopy.     

Concentration effect of γ‐glycidoxypropyltrimethoxysilane on the mechanical properties of glass fiber–epoxy composites

In this study, glass fibers were modified using γ‐glycidoxypropyltrimethoxysilane of different concentrations to improve the interfacial adhesion at interfaces between fibers and matrix. Effects of γ‐glycidoxypropyltrimethoxysilane on mechanical properties and fracture behavior of glass fiber/epoxy composites were investigated experimentally. Mechanical properties of the composites have been investigated by tensile tests, short beam tests, and flexural tests. The short‐beam method was used to measure the interlaminar shear strength (ILSS) of laminates. The tensile and flexural properties of composites were characterized by tensile and three‐point bending tests, respectively. The fracture surfaces of the composites were observed with a scanning electron microscope. On comparing the results obtained for the different concentrations of silane solution, it was found that the 0.5% GPS silane treatment provided the best mechanical properties. The ILSS value of heat‐cleaned glass fiber reinforced composite is enhanced by ∼59% as a result of the glass fiber treatment with 0.5% γ‐GPS. Also, an improvement of about 37% in tensile strength, about 78% in flexural strength of the composite with the 0.5% γ‐GPS treatment of glass fibers was observed. POLYM. COMPOS., 2009. © 2008 Society of Plastics Engineers     

Toughness and strength improvement of diglycidyl ether of bisphenol‐A by low viscosity liquid hyperbranched epoxy resin

This article reports on the use of low viscosity liquid thermosetting hyperbranched poly(trimellitic anhydride‐diethylene glycol) ester epoxy resin (HTDE) as an additive to an epoxy amine resin system. Four kinds of variety molecular weight and epoxy equivalent weight HTDE as modifiers in the diglycidyl ether of bisphenol‐A (DGEBA) amine systems are discussed in detail. It has been shown that the content and molecular weight of HTDE have important effect on the performance of the cured system, and the performance of the HTDE/DGEBA blends has been maximum with the increase of content and molecular weight or generation of HTDE. The impact strength and fracture toughness of the cured systems with 9 wt % second generation of HTDE are 58.2 kJ/m² and 3.20 MPa m^1/2, which are almost three and two times, respectively, of DGEBA performance. Furthermore, the tensile and flexural strength can be enhanced about 20%. The glass transition temperature and Vicat temperature, however, are found to decrease to some extent. The fracture surfaces are evaluated by using scanning electron microscopy, which showed that the homogeneous phase structure of the HTDE blends facilitates an enhanced interaction with the polymer matrix to achieve excellent toughness and strength enhancement of the cured systems, and the “protonema” phenomenon in SEM has been explained by in situ reinforcing and toughening mechanism and molecular simulation. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 101: 2504–2511, 2006     

Mechanical,thermal, and viscoelastic response of novel in situ CTBN/POSS/epoxy hybrid composite system

The present study focuses on the preparation of a novel hybrid epoxy nanocomposite with glycidyl polyhedral oligomeric silsesquioxane (POSS) as nanofiller, carboxyl terminated poly(acrylonitrile‐co‐butadiene) (CTBN) as modifying agent and diglycidyl ether of bisphenol A (DGEBA) as matrix polymer. The reaction between DGEBA, CTBN, and glycidyl POSS was carefully monitored and interpreted by using Fourier transform infrared (FTIR) and differential scanning calorimetry (DSC). An exclusive mechanism of the reaction between the modifier, nanofiller, and the matrix is proposed herein, which attempts to explains the chemistry behind the formation of an intricate network between POSS, CTBN, and DGEBA. The mechanical properties, such as tensile strength, and fracture toughness, were also carefully examined. The fracture toughness increases for epoxy/CTBN, epoxy/POSS, and epoxy/CTBN/POSS hybrid systems with respect to neat epoxy, but for hybrid composites toughening capability of soft rubber particles is lost by the presence of POSS. Field emission scanning electron micrographs (FESEM) of fractured surfaces were examined to understand the toughening mechanism. The viscoelastic properties of epoxy/CTBN, epoxy/POSS, and epoxy/CTBN/POSS hybrid systems were analyzed using dynamic mechanical thermal analysis (DMTA). The storage modulus shows a complex behavior for the epoxy/POSS composites due to the existence of lower and higher crosslink density sites. However, the storage modulus of the epoxy phase decreases with the addition of soft CTBN phase. The T_g corresponding to epoxy‐rich phase was evident from the dynamic mechanical spectrum. For hybrid systems, the T_g is intermediate between the epoxy/rubber and epoxy/POSS systems. Finally, TGA (thermo gravimetric analysis) studies were employed to evaluate the thermal stability of prepared blends and composites. POLYM. COMPOS., 37:2109–2120, 2016. © 2015 Society of Plastics Engineers     

Toughening of epoxy/polycaprolactone composites via reaction induced phase separation

A series of melt processable thermoset/thermoplastic blends were prepared by mixing bisphenol‐A diglycidyl ether (Epon‐828)/diaminodiphenyl sulfone (DGEBA/DDS) system with two grades of polycaprolactone resin. Phase separation behavior of the blends was investigated by means of optical microscopy, microstructure by scanning electron microscopy (SEM), and thermo‐mechanical properties. The toughness of polycaprolactone modified epoxies was measured by instrumented falling weight impact (IFWI) testing. Various blend morphologies were observed depending upon the cured epoxy network/thermoplastic composition. Spinodal decomposition as characterized by modulated structure of unique periodicity and phase connectivity was found to be the probable mechanism of phase separation. SEM examination of fracture surfaces indicated a strong adhesion between the epoxy‐rich and polycaprolactone‐rich phases. Optimum improvement in failure energy was obtained for the compositions containing 10‐20% polycaprolactone without significantly compromising the elastic modulus and the thermo‐mechanical stability of the epoxy. In light of morphological evidences, a possible toughening effect was postulated in terms of tearing of the thermoplastic component and induced plastic deformation of the epoxy matrix.     

Preparation and properties of MWCNTs/poly(acrylonitrile‐ styrene‐butadiene)/epoxy hybrid composites

Poly(acrylonitrile‐styrene‐butadiene) (ABS) was used to modify diglycidyl ether of bisphenol‐A (DGEBA) type epoxy resin, and the modified epoxy resin was used as the matrix for making multiwaled carbon tubes (MWCNTs) reinforced composites and were cured with diamino diphenyl sulfone (DDS) for better mechanical and thermal properties. The samples were characterized by using infrared spectroscopy, pressure volume temperature analyzer (PVT), thermogravimetric analyzer (TGA), dynamic mechanical analyzer (DMA), thermo mechanical analyzer (TMA), universal testing machine (UTM), and scanning electron microscopy (SEM). Infrared spectroscopy was employed to follow the curing progress in epoxy blend and hybrid composites by determining the decrease of the band intensity due to the epoxide groups. Thermal and dimensional stability was not much affected by the addition of MWCNTs. The hybrid composite induces a significant increase in both impact strength (45%) and fracture toughness (56%) of the epoxy matrix. Field emission scanning electron micrographs (FESEM) of fractured surfaces were examined to understand the toughening mechanism. FESEM micrographs reveal a synergetic effect of both ABS and MWCNTs on the toughness of brittle epoxy matrix. © 2012 Wiley Periodicals, Inc. J. Appl. Polym. Sci., 2013