Fracture toughness of silica particulate‐filled epoxy composite

The relationship between the postcuring conditions and fracture toughness on three silica particulate‐filled epoxy composites was investigated. The glass transition temperature, T_g, and the fragility parameter, m, derived from the thermo‐viscoelasticity, were used to characterize the composites, which were postcured under various conditions. The glass transition temperature and fragility both depended on both of the curing conditions and the volume fraction of silica particles. The glass transition temperature increased with the postcuring time and temperature, while the fragility generally decreased as the volume fraction increased. There was no direct correlation between the glass transition temperature and fragility. The fracture toughness depended on both the glass transition temperature and fragility. The composites with a high glass transition temperature and low fragility had high fracture toughness. These results indicate that the glass transition temperature and fragility are useful parameters for estimating the fracture toughness of the silica particulate‐filled epoxy composites. © 2002 Wiley Periodicals, Inc. J Appl Polym Sci 86: 2261–2265, 2002     

Synthesis of modified silica spheres used for the preparation of dual ultraviolet‐ and thermo‐cured epoxyacrylate/silica composites

To investigate the interfacial effect on properties of epoxyacrylate–silica composites, submicron‐sized silica spheres were synthesized by sol–gel reaction under a basic environment and their surfaces were endowed with vinyl functional groups by further modification with 3‐methacryloxypropyl trimethoxy silane. The pure silica (PS) and the modified silica (MPS) spheres were characterized by Fourier transform infrared, ²⁹Si‐ and ¹³C‐nuclear magnetic resonance (NMR), scanning electron microscope (SEM), and particle size analyzer. The silica spheres were then added to the presynthesized difunctional epoxyacrylate resin with one vinyl group and one epoxide group at each end, in addition to the photo‐ and thermo‐curing agents. After cure, thermal and mechanical properties of the obtained epoxyacrylate–silica composites were measured and compared. Tensile mechanical properties including initial modulus, ultimate tensile strength, and elongation at break, as well as the fracture energy of the epoxyacrylate–silica composite were all increased by increasing the content of silica spheres. Moreover, the composites filled with MPS had stronger interfacial strength between silica sphere and matrix than those with PS and thus exhibited an additional increase of tensile mechanical properties and fracture toughness. The increase of fracture toughness was owing to the crack deflection and particle–matrix debonding as evidenced by SEM pictures on the fracture surface. POLYM. ENG. SCI., 2012. © 2012 Society of Plastics Engineers     

Impact behavior of particles filled‐glass/polyester composite plates

The aim of the study is to lay bare the impact behavior of filled composite plates experimentally. The woven glass/polyester‐matrix composite plates filled with 0% (unfilled), 10%, and 20% SiC_p ceramic particles were manufactured by hand lay‐up method. The low velocity drop impact testing is conducted to the composite samples subjected to increasing impact energies that were ranged from approximately 2.5 to 22.5 J. With this use of increasing impact energies, it was possible to examine the impact response and damage mechanism until perforation of the composite plates. An energy profiling method was used in order to identify the perforation thresholds of composites. It is concluded that addition of particles to resin, until a certain ratio, increases the perforation thresholds of the woven glass/polyester. The perforation threshold of 10% filled composite is about 37% higher than that of the 20% filled composite and 6% higher than ones of the unfilled composite. POLYM. COMPOS., 2011. © 2011 Society of Plastics Engineers     

Tribological behavior of micrometer‐ and nanometer‐Al2O3‐particle‐filled poly(phthalazine ether sulfone ketone) copolymer composites used as frictional materials

Micrometer‐ and nanometer‐Al₂O₃‐particle‐filled poly(phthalazine ether sulfone ketone) (PPESK) composites with filler volume fractions ranging from 1 to 12.5 vol % were prepared by hot compression molding. We evaluated the tribological behaviors of the PPESK composites with the block‐on‐ring test rig by sliding PPESK‐based composite blocks against a mild carbon steel ring under dry‐friction conditions. The effects of different temperatures on the wear rate of the PPESK composites were also investigated with a ball‐on‐disc test rig. The wear debris and the worn surfaces of the PPESK composites were investigated with scanning electron microscopy, and the structures of the PPESK composites were analyzed with IR spectra. The lowest wear rate, 7.31 × 10^?6 mm³ N^?1 m^?1, was obtained for the composite filled with 1 vol %‐nanometer Al₂O₃ particles. The composite with nanometer particles exhibited a higher friction coefficient (0.58–0.64) than unfilled PPESK (0.55). The wear rate of 1 vol %‐nanometer‐Al₂O₃‐particle‐filled PPESK was stable and was lower than that of unfilled PPESK from the ambient temperature to 270°C. We anticipate that 1 vol %‐nanometer‐Al₂O₃‐particle‐filled PPESK can be used as a good frictional material. We also found that micrometer‐Al₂O₃‐particle‐filled PPESK had a lower friction coefficient at a filler volume fraction below 5%. The filling of micrometer Al₂O₃ particles greatly increased the wear resistance of PPESK under filler volume fractions from 1 to 12.5%. © 2005 Wiley Periodicals, Inc. J Appl Polym Sci 95: 993–1001, 2005     

Noticeable viscosity reduction of polycarbonate melts caused jointly by nano‐silica filling and TLCP fibrillation

Nano‐SiO₂ was introduced into in‐situ composites of polycarbonate (PC) and a thermotropic liquid crystalline polymer (TLCP) using a twin‐screw extruder. The rheology of these composites was characterized with capillary rheometry, and the morphology of the dispersed TLCP observed with scanning electron microscopy. The rheological data revealed that the viscosity decrease of PC melts by only the addition up to 20 wt% TLCP remained smaller than 30%, while it became ～48% upon further addition of only about 1 wt% nano‐SiO₂ and larger than 60% upon ～9 wt% nano‐SiO₂ filling, in contrast to a 50% viscosity increase of PC melts with increase in nanosilica loading up to ～9 wt%. These silica‐filled composites exhibited markedly low viscosity, especially at relatively high shear rates. The morphology of TLCP extracted from unfilled and silica‐filled composites indicated that the largest viscosity reduction was correlated well with the fibrillation of TLCP droplets enhanced by nano‐SiO₂. The TLCP/SiO₂/PC composites exhibited rheological hybrid effect with fillers at nanometer scale. POLYM. ENG. SCI., 47:757–764, 2007. © 2007 Society of Plastics Engineers     

Nanosilica filled poly(glycerol‐sebacate‐citrate) elastomers with improved mechanical properties,adjustable degradability,and better biocompatibility

Modified nano‐fumed silica (mn‐silica)/poly(glycerol‐sebacate‐citrate), in which mn‐silica loadings varied from 0 to 20 phr, were prepared by in situ polymerization and surface modification. The influence of mn‐silica loadings on the structure and properties of the composites was studied. Scanning electron microscope (SEM) and transmission electron microscope (TEM) photos showed that the mn‐silica dispersed well as nano‐scale network in the matrix, and exhibited good interfacial bonding with the matrix. The mn‐silica filled composites exhibited excellent comprehensive properties relative to the unfilled elastomers. Specially, the tensile strength improved from 0.9 MPa to 5.3 MPa. Results of the in vitro degradation test suggested that mn‐silica loading could adjust the degradation rate of the composites in simulated body fluid solution. The MTT colorimetry with L929 cells substantiated that the introduction of mn‐silica weakened the cytotoxicity of elastomers and made the composites accepted as qualified biomedical materials. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2012     

Effect of single‐mineral filler and hybrid‐mineral filler additives on the properties of polypropylene composites

The present study was carried out to determine the filler characteristics and to investigate the effects of three types of mineral fillers (CaCO₃, silica, and mica) and filler loadings (10–40 wt%) on the properties of polypropylene (PP) composites. The characteristics of the particulate fillers, such as mean particle size, particle size distribution, aspect ratio, shape, and degree of crystallinity were identified. In terms of mechanical properties, for all of the filled PP composites, Young's modulus increased, whereas tensile strength and strain at break decreased as the filler loading increased. However, 10 wt% of mica in a PP composite showed a tensile strength comparable with that of unfilled PP. Greater tensile strength of mica/PP composites compared to that of the other composites was observed because of lower percentages of voids and a higher aspect ratio of the filler. Mica/PP also exhibited a lower coefficient of thermal expansion (CTE) compared to that of the other composites. This difference was due to a lower degree of crystallinity of the filler and the CTE value of the mica filler. Scanning electron microscopy was used to examine the structure of fracture surfaces, and there was a gradual change in tensile fracture behavior from ductile to brittle as the filler loading increased. The nucleating ability of the fillers was studied with differential scanning calorimetry, and a drop in crystallinity of the composites was observed with the addition of mineral filler. Studies on the hybridization effect of different (silica and mica) filler ratios on the properties of PP hybrid composites showed that the addition of mica to silica‐PP composites enhanced their tensile strength and modulus. J. VINYL ADDIT. TECHNOL., 2009. © 2009 Society of Plastics Engineers     

Mechanical properties and morphologies of polypropylene/single‐filler or hybrid‐filler calcium carbonate composites

Three types of polypropylene (PP) with different intrinsic toughness were used to study the mechanical properties and morphologies of the PP composites filled with single‐filler and hybrid‐filler of calcium carbonate particles. The calcium carbonate particles used were with average particle sizes of 25 μm (CC25), and 0.07 μm (CC0.07), respectively. A hybrid‐filler CaCO₃ named CC25/CC0.07 was used as a mixture of CC25 and CC0.07 (CC25/CC0.07 weight ratio = 1:1). It was found that the type of PP and the particle size of inorganic filler were the two important factors for the determination of mechanical properties of the composites. And the general mechanical properties of the composites filled with hybrid‐filler CaCO₃ were better than those of the composites filled with single‐filler CaCO₃, but the synergistic hybridization effect of the hybrid‐filler CaCO₃ did not exist. The major toughening mechanism of the PP/CC25 composites was the cavitation of the matrix caused by CC25, and the major toughening mechanism of the PP/CC0.07 composites was the pinning effect introduced by CC0.07. For the PP/CC25/CC0.07 composites, the cavitation of the matrix caused by CC25 and the pinning effect introduced by CC0.07 existed simultaneously. And when the intrinsic toughness of the matrix was large enough, the major factor to toughen PP was the pinning effect introduced by CC0.07, otherwise the major factor to toughen PP was the cavitation of the matrix caused by CC25. POLYM. ENG. SCI., 47:95–102, 2007. © 2007 Society of Plastics Engineers     

Simultaneous effects of silanized coal fly ash and nano/micro glass fiber on fracture toughness and mechanical properties of carbon fiber‐reinforced vinyl ester resin composites

In this study, the simultaneous effects of both silanized coal fly ash (S‐CFA) and nano/micro glass fiber (nGF) on fracture toughness and mechanical properties of vinyl ester (VE) resin filled with carbon fiber‐based composite materials were investigated. The CFA was treated with (3‐trimethoxysilyl) propyl methacrylate to introduce the methacryloxy groups into the surface of CFA, and was confirmed by using FTIR technique. The nGF and S‐CFA with different weight ratios were well mixed with VE resin by using of high‐speed mechanical stirrer, and ultrasonic technique before using as matrices for fabrication of carbon fiber‐based composite materials via sheet molding compound (SMC) method and hot curing processing. Many characteristics of both cured VE resin composites and carbon fiber‐based composite were examined such as mechanical properties, fracture toughness, and morphology. The results showed that by adding of both 0.1 wt% nGF and 1 wt% S‐CFA into VE resin the tensile strength, tensile modulus, flexural strength, K_IC, impact strength as well as the Mode I interlaminar fracture toughness (G_IC) of VE composites and carbon fiber based composites get optimum values and increased about 61.39%; 39.83%; 36.21%; 103.1%; 81.79%; 48.61%, respectively when compared with pristine materials. POLYM. ENG. SCI., 59:584–591, 2019. © 2018 Society of Plastics Engineers     

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     

Fracture behavior of glass bead-filled poly(oxymethylene) injection moldings

The mechanical properties of glass bead filled poly(oxymethylene) were investigated as a function of glass bead content and glass bead diameter using injection molded test pieces. Fracture toughness measurements were made using single edge-notched tension and single edge-notched bend specimens. The effect of notch orientation with respect to the mold fill direction on fracture toughness was studied using single gate and double gate moldings. Tensile strength and flexural modulus were measured using standard test pieces. It was found that; (i) fracture toughness of the filled and unfilled polymer was relatively independent of notch orientation, (ii) the presence of weldlines in the molded test pieces did not affect the fracture toughness of unfilled polymer or its composites, (iii) fracture toughness of filled polymer was always considerably lower than that of the unfilled polymer; fracture toughness decreased sharply with increasing bead concentration, (iv) fracture toughness was not a sensitive function of glass bead diameter; it decreased slightly as bead diameter increased, (v) strain energy release rate as measured under impact decreased with increasing bead concentration, (vi) tensile strength decreased linearly with increasing glass bead concentration and was inversely proportional to the square root of the bead diameter, (vii) weldlines did not affect the tensile strength of the polymer or its composities, (viii) flexural modulus increased linearly with increasing glass bead concentration according to the Einstein equation.     

The influence of silane treatment on nylon 6/nano‐SiO2 in situ polymerization

Silane treatment has been applied to the preparation of nylon 6/nano‐SiO₂ composites through in situ polymerization. The influence of such treatment on the reactivity of silica, polymerization of nylon 6, and the mechanical properties of the achieved composites has been studied. Fourier transform infrared (FTIR) spectroscopy and thermal gravimetric analysis (TGA) of silicas isolated from the composites have shown that the conversion of surface silanol groups to amino and epoxy groups did not cause a significant change in the reactivity of silica and that the percentage of silica surface grafting was around 15% for all treated and untreated silicas. End group analysis has shown that the presence of silica (pretreated or not) in the composite system resulted in the decrease of the average molecular weight of the polymer matrix. However, dynamic mechanical analysis and mechanical tests revealed that treating silica with silane improved the strength and toughness of the composite materials, while untreated silica improved their strength at the expense of toughness. This can be attributed to the existence of the flexible interlayer introduced by silane treatment. © 2002 John Wiley & Sons, Inc. J Appl Polym Sci 84: 827–834, 2002; DOI 10.1002/app.10349     

Morphology and mechanical properties of dual‐curable epoxyacrylate hybrid composites

A dual‐curable epoxyacrylate (EA) oligomer with one epoxide group and one vinyl group at each end was synthesized for the application as adhesive sealant in the liquid crystal display panels. However, after UV and thermal cure, the EA resin was brittle with a poor resistance to crack initiation and propagation. Liquid rubbers with different functional end groups were thus tried as toughening agents for the EA resin. Among all the rubber‐toughened EAs, the EA‐V5A5 added with vinyl‐terminated and amino‐terminated butadiene‐acrylonitrile copolymers (VTBN and ATBN) each at 5 phr had the highest fracture toughness, tensile strength, and elongation at break but a lower initial modulus. To raise the modulus, submicron‐sized silica particles (∼170 nm) with surface vinyl functional groups were further added to the EA‐V5A5 to prepare the hybrid composites. Because of interfacial chemical bonding provided by the surface vinyl functional groups, both modulus and fracture toughness were increased by adding silica particles, without any appreciable decrease in extensibility. For the hybrid composite at 20 phr silica particles, the initial modulus, fracture toughness, and fracture energy were raised by 10.3, 100, and 267%, respectively, when compared to the neat epoxyacrylate. Owing to their strong interfacial bonding, the increase of fracture toughness was mainly due to the crack deflection and bifurcation on silica particles, in addition to the rubber particle bridging and tearing as evidenced by SEM pictures on the fracture surface. © 2014 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2015 , 132, 41820.     

Wood-fiber reinforcement of styrene–maleic anhydride copolymers

Styrene–maleic anhydride (SMA) copolymers containing either 7 or 14% maleic anhydride were filled with either pine flour or dry-process aspen fiber from a medium density fiberboard (MDF) plant. Material properties of the filled and unfilled SMA plastics were compared with those of aspen-fiber-filled and unfilled polystyrene (PS). The fiber-filled SMA composites were equivalent or superior to unfilled SMA in strength, stiffness, and notched Izod impact strength. Filled PS composites outperformed or matched the performance of filled SMA composites in the parameters tested. Unnotched Izod impact strength of filled polymers was generally inferior to that of the unfilled polymers. Water absorption from a 90% relative humidity exposure, a 24-h soak, and a 2-h boil showed mixed results when compared to the unfilled polymers. Dynamic mechanical analysis showed no change in glass transition temperature (T_g) after the addition of filler for either SMA or PS composites. The presence of the anhydride functionality on the polymer backbone did not appear to improve the strength of the composite. No evidence was found for chemical bond formation between the SMA and wood fiber. © 1998 John Wiley & Sons, Inc. J Appl Polym Sci 68: 1567–1573, 1998     

Fracture toughness of poly(lactic acid)/ ethylene acrylate copolymer/wood‐flour composite ternary blends

A fracture mechanics analysis based on the J‐integral method was adopted to determine the resistance of composites with various concentrations of wood‐flour and ethylene acrylate copolymer (EAC) to crack initiation (J_in) and complete fracture (J_f). The J_in and J_f energies of unmodified poly(lactic acid) (PLA)/wood‐flour composites showed the deleterious effect of incorporating wood fibers into the plastic matrix by significantly decreasing the fracture toughness of PLA as the wood‐flour content increased. The reduced fracture toughness of the matrix induced by adding brittle wood‐flour into PLA was well recovered by impact modification of the composites with EAC. Microscopic morphological studies revealed that the major mechanisms of toughening were through the EAC existing as separate domains in the bulk matrix of the composites which tended to act as stress concentrators that initiated local yielding of the matrix around crack tips and enhanced the toughness of the composites. © 2012 Society of Chemical Industry     

Preparation and properties of an oxide fiber‐reinforced silica matrix composite

Oxide (Nextel? 440) fiber‐reinforced silica composites, with the density and porosity of 1.97 g/cm³ and 21.8%, were prepared through sol‐gel. Their average flexure strength, elastic modulus, shear strength, and fracture toughness at room temperature were 119.7 MPa, 25.6 GPa, 10.8 MPa, and 4.0 MPa·m^1/2, respectively. The composites showed typical toughened fracture behavior, and distinct pullout fibers were observed at the fracture surface. Their mechanical properties were performant up to 1000°C, with the maximum flexural strength of 132.2 MPa at 900°C. Moreover, the composites showed good thermal stability, even after thermal aging and thermal shock at elevated temperatures.     

Mode II interlaminar fracture behavior of carbon bead‐filled epoxy/glass fiber hybrid composite

To investigate the effect of including carbon beads on the mechanical properties of epoxy resin, the fracture toughness of carbon bead‐filled epoxy was earlier evaluated using a CT (compact tension) specimens and Mode I fracture toughness was observed. Based on those results, in this study, the Mode II interlaminar fracture toughness of carbon bead filled epoxy/glass fiber hybrid composites was evaluated using end notch flexure (ENF) specimens. The hybrid composites showed increased Mode II interlaminar fracture toughness. The optimal bead volume fraction was around 15%.     

Fracture toughness of polyamide 6/maleated ethylene–propylene–diene terpolymer rubber/nano calcium carbonate ternary composites according to essential work of fracture analysis

Polyamide 6 (PA6)/maleated ethylene–propylene–diene terpolymer rubber/nano calcium carbonate ternary composites were prepared. The effect of the compounding route on the morphology, toughness, and fracture behavior of the ternary composites were investigated by scanning electron microscopy, Charpy impact testing, and essential work of fracture (EWF) testing. The construction of sandbag microstructure particles in PA6 matrix was crucial to the toughness of the ternary composites. The Charpy impact strength and the specific essential work of fracture (w_e) of the ternary composites with a sandbag microstructure were 137.9 and 71.4% higher, respectively, than those of the ordinary ternary composites with a separated dispersion microstructure. The observation of the fracture surface after EWF testing indicated that the improvement of w_e was attributed to the sandbag microstructure particles; this structure was more effective for resisting the growth of cracks; meanwhile, the influence of the amount of fibrillation on the nonspecific essential work of fracture, including the nonspecific essential work of fracture before yielding and that in the necking–tearing stage, was insignificant. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2011     

Effect of graphite content on properties of B4C‐W2B5 ceramic composites by in situ reaction of B‐Gr‐WC

Strip‐shaped W₂B₅ reinforced B₄C ceramic composites were prepared via in situ reaction of boron(B)‐graphite(Gr)‐WC system by powder metallurgy (P/M). In order to study the effect of the graphite content on the properties of the as‐fabricated ceramic composites, the powder mixture of B‐Gr‐WC with various amounts of Gr powder were blended and consolidated by spark plasma sintering (SPS). The sintering parameters were shown as following: sintering pressure was set as 30 MPa; The three‐step sintering temperature was 1100‐1550‐1700°C and the duration time was set as 5‐5‐6 minutes, respectively. In situ formed strip‐shaped W₂B₅ particles were dispersed homogeneously in B₄C matrix, which resulted in a remarkable improvement on the fracture toughness and mechanical properties. Appropriate 5vol% residual Gr in the composite shows positive effect on the mechanical properties which achieved an optimal counter‐balance of fracture toughness and hardness, the relative density was 99.8%, the Vickers hardness can reach 30.2 GPa, and the fracture toughness was 11.9 MPa·m^1/2 when the sintering temperature was set at 1700°C.     

Mechanical properties and fracture behaviors of epoxy composites with phase‐separation formed liquid rubber and preformed powdered rubber nanoparticles: A comparative study

Epoxy composites filled with phase‐separation formed submicron liquid rubber (LR) and preformed nanoscale powdered rubber (PR) particles were prepared at different filler loading levels. The effect of filler loading and type on the rheological properties of liquid epoxy resin suspensions and the thermal and mechanical properties of the cured composites as well as the relative fracture behaviors are systematically investigated. Almost unchanged tensile yield strength of the cured epoxy/PR composites is observed in the tensile test compared with that of the neat epoxy; while the strength of the cured epoxy/LR composites shows a maximum value at ∼4.5 wt% and significantly decreases with increasing LR content. The glass transition temperature (T_g) of the cured PR/epoxy has shifted to the higher temperature in the dynamic mechanical thermal analysis compared with that of the cured pure epoxy and epoxy/LR composites. Furthermore, the presence of LR results in highly improved critical stress intensity factor (K_IC) of epoxy resin compared with the corresponding PR nanoparticles. In particular, the PR and LR particles at 9.2 wt% loading produce about 69 and 118% improvement in K_IC of the epoxy composites, respectively. The fracture surface and damage zone analysis demonstrate that these two types of rubber particles induce different degrees of local plastic deformation of matrix initiated by their debonding/cavitation, which was also quantified and correlated with the fracture toughness of the two epoxy/rubber systems. POLYM. COMPOS., 36:785–799, 2015. © 2014 Society of Plastics Engineers