The effect of hyperbranched polyester and zirconium slag nanoparticles on the impact resistance of epoxy resin thermosets

A hyperbranched polyester (HBP) was synthesized through a polymerization of AB₂ approach with succinic anhydride and diethanolamine. The effect of HBP and Zirconium slag nanoparticle (ZSN, a kind of solid waste in Zirconium industry) content on the toughness enhancement and morphology of diglycidyl ether of bisphenol A epoxy resin (DGEBA) thermosets was studied. The results indicated that HBP can greatly improve the impact strength (IS) of epoxy thermosets, but the flexural strength (FS) was decreased with increasing the HBP content. The IS of epoxy thermosets modified with ZSN was also improved, and the FS decreases as increase of ZSN. The thermosets modified with both HBP and ZSN showed excellent IS and FS. The toughening enhancement mechanism was also discussed.     

Studies on blends of epoxy-functionalized hyperbranched polymer and epoxy resin

An epoxy-functionalized hyperbranched polymer (HBP) was used to toughen a conventional epoxy resin, diglycidyl ether of bisphenol A (DGEBA) cured with diethyltoluene-2,6-diamine (DETDA). There was little change in gel time as a result of addition of HBP, even though the HBP reacts at a slower rate with amine hardeners compared to DGEBA alone. Phase separation was investigated for various HBP contents and as a function of cure conditions as well. The thermal and dynamic viscoelastic behavior of the modified matrices have been examined and compared to the DGEBA epoxy matrix. It appears that the HBP which phase separates does not react as fully as when it is reacted with the amine alone. Nonetheless, good improvement in impact strength as a result of incorporation of HBP were observed and explained in terms of morphological behavior for a DGEBA matrix modified with various amounts of HBP.     

The influence of nanoadhesives on the tensile properties and Mode-I fracture toughness of bonded joints

Nanoadhesives of epoxy resin are synthesized and evaluated. They are organically modified by multiwalled carbon nanotubes (MWCNT) (1% by weight) as reinforcement. Tensile tests are conducted on multiple identical unnotched and notched specimens to evaluate the overloading and fracture behavior of the nanoadhesives and are compared with the neat epoxy resin. In comparison with the neat epoxy, it is found that the 1% MWCNT reinforcement increased the ultimate and residual strength by about 29% and 56%, respectively. In comparison with the neat resin, there is a 265% increase in the fracture toughness of the MWCNT adhesive. Fracture surface analysis revealed the various mechanisms by which the MWCNT adhesives acquire their superior strength and toughness in comparison with the neat resin.     

Characterization of epoxy functionalized graphite nanoparticles and the physical properties of epoxy matrix nanocomposites

This work presents a novel approach to the functionalization of graphite nanoparticles. The technique provides a mechanism for covalent bonding between the filler and matrix, with minimal disruption to the sp² hybridization of the pristine graphene sheet. Functionalization proceeded by covalently bonding an epoxy monomer to the surface of expanded graphite, via a coupling agent, such that the epoxy concentration was measured as approximately 4 wt.%. The impact of dispersing this material into an epoxy resin was evaluated with respect to the mechanical properties and electrical conductivity of the graphite–epoxy nanocomposite. At a loading as low as 0.5 wt.%, the electrical conductivity was increased by five orders of magnitude relative to the base resin. The material yield strength was increased by 30% and Young’s modulus by 50%. These results were realized without compromise to the resin toughness.     

Evaluation of the mechanical behavior of epoxy composite reinforced with Kevlar plain fabric and glass/Kevlar hybrid fabric

In this study, composite plates were manufactured by hand lay-up process with epoxy matrix (DGEBA) reinforced with Kevlar fiber plain fabric and Kevlar/glass hybrid fabric, using to an innovative architecture. Results of the mechanical properties of composites were obtained by tensile, bending and impact tests. These tests were performed in the parallel direction or fill directions of the warp and in a 90° direction. FTIR was used in order to verify the minimum curing time of the resin to perform the mechanical tests, and scanning electron microscopy was used to observe reinforcement and matrix fractures. Composites with Kevlar/glass hybrid structure in the reinforcing fabric showed the better results with respect to specific mechanical strength, as well as bending and impact energy.     

Flexural fatigue behavior of synthesized graphene/carbon-nanofiber/epoxy hybrid nanocomposites

In the present research, effects of adding a combination of synthesized graphene nanosheets and carbon nanofibers (CNFs) on the flexural fatigue behavior of epoxy polymer have been investigated. Graphene nanosheets are synthesized based on a changing magnetic field. The flexural bending fatigue life of 0.5 wt.% of graphene/CNF/epoxy hybrid nanocomposites has been considered at room temperature. The samples were subjected to different displacement amplitudes fatigue loadings. Due to the addition of hybrid nanoparticles, a remarkable improvement in fatigue life of epoxy resin was observed in comparison with results obtained by adding 0.25 wt.% graphene or 0.25 wt.% CNF into the resin. Experimental observations show that at a strength ratio equal to 43% by using 0.5 wt.% of hybrid nanoparticles; 37.3-fold improvement in flexural bending fatigue life of the neat epoxy was observed. While, enhancement of adding only graphene or CNF was 27.4 and 24-fold, respectively.     

热塑性塑料对环氧树脂热膨胀系数的影响研究

环氧树脂基体的热膨胀系数(CTE)对碳纤维增强环氧树脂层状材料的性能影响巨大,如何降低环氧树脂基体的CTE是提高碳纤维增强环氧树脂复合材料低温使用性能的关键。本研究采用聚对苯二甲酸丁二醇酯(PBT)、聚碳酸酯(PC)和聚醚酰亚胺(PEI)3种热塑性塑料改性环氧树脂,研究了这3种热塑性塑料对环氧树脂基体CTE的影响。结果表明:这3种热塑性塑料分子链中的羰基在环氧树脂固化过程中可与环氧分子侧链上的羟基形成氢键作用,从而加强了热塑性塑料与环氧树脂的界面作用;采用这3种热塑性塑料改性环氧树脂均可提高环氧树脂基体的玻璃化转变温度;相对于纯环氧树脂,PBT、PEI和PC改性的环氧树脂在玻璃化转变温度下的CTE分别降低了14.99%、17.44%和23.96%,但在玻璃化转变温度上的CTE均高于纯环氧树脂。     

Improving the flexural and thermomechanical properties of amino-functionalized carbon nanotube/epoxy composites by using a pre-curing treatment

A prior thermal (pre-curing) treatment of mixtures of epoxy monomer and amino-functionalized carbon nanotubes (CNTs) was used to promote a chemical reaction between the matrix and the reinforcement, favouring the formation of a strong interface. Samples of epoxy resin and different weight percentages of amino-functionalized multi-walled CNTs were prepared with and without the pre-curing treatment (150 °C, 1 h). The degree of dispersion of the nanofiller was better when this pre-curing treatment was used. This allowed a higher CNT content while keeping a high sample homogeneity. Without the pre-curing step, the addition of CNTs increases both the flexural strength and strain to failure by 45%. Moreover, with the pre-curing step, the nanocomposite with 0.25 wt.% CNTs presents an increase of flexural strength by 58% and strain to failure by 68% regard to neat epoxy resin.     

Cyclic fatigue crack propagation of nanoparticle modified epoxy

An experimental study on the fatigue performance of nanoparticle modified epoxy was conducted. Seven material systems were examined which were: neat epoxy (E), 6 and 12 weight percent (wt.%) silica nanoparticle modified epoxy (S6, S12), 6 and 12 wt.% rubber nanoparticle modified epoxy (R6, R12), 3 wt.% each of silica and rubber nanoparticle modified epoxy (S3R3) and 6 wt.% each of silica and rubber nanoparticle modified epoxy (S6R6). Effects of those nanoparticles on the fatigue threshold (ΔG_th and ΔK_th) and fatigue crack propagation rates (da/dN) were studied. It was found that, compared to neat epoxy (E), nanosilica (S6, S12) increased ΔG_th (and ΔK_th) but nanorubber (R6 and R12) did not. However, a synergistic effect was observed on the fatigue threshold when both silica and rubber nanoparticles were added into epoxy. All these nanoparticles, individually or conjointly, decreased da/dN with silica the most effective. Morphology of the fracture surface was examined to understand the role of nanoparticles on toughening mechanisms under cyclic loading, which depended on the applied ΔG levels.     

Size reduction of WO3 nanoparticles by ultrasound irradiation and its applications in structural nanocomposites

The porous WO₃ (pore size 2–5 nm) nanoparticles were synthesized using a high intensity ultrasound irradiation of commercially available WO₃ nanoparticles (80 nm) in ethanol. The high resolution transmission electron microscopic (HRTEM) and X-ray studies indicated that the 2–5 nm uniform pores have been created in commercially available WO₃ nanoparticles without much changing the initial WO₃ nanoparticles (80 nm) sizes. The nanocomposites of WO₃/SC-15 epoxy were prepared by infusion of 1 wt.%, 2 wt.% and 3 wt.% of porous WO₃ nanoparticles into SC-15 epoxy resin by using a non-contact (Thinky) mixing technique. Finally the neat epoxy and nanocomposites were cured at room temperature for about 24 h in a plastic rectangular mold. The cured epoxy samples were removed and precisely cut into required dimensions and tested for their thermal and mechanical properties. The HRTEM and SEM studies indicated that the sonochemically modified porous WO₃ nanoparticles dispersed more uniformly over the entire volume of the epoxy (without any settlement or agglomeration) as compared to the unmodified WO₃/epoxy nanocomposites.     

Multiscale fiber reinforced composites based on a carbon nanofiber/epoxy nanophased polymer matrix: Synthesis, mechanical, and thermomechanical behavior

Vacuum assisted resin infusion molding (VARIM) was used to produce multiscale fiber reinforced composites (M-FRCs) based on carbon nanofibers dispersed in an epoxy resin. Flexural, interlaminar shear strength (ILSS) and thermomechanical tests are presented for the 0.1 wt% and 1 wt% M-FRCs and compared with the neat fiber reinforced composites (FRCs). Flexural strength and modulus increased (16–20%) and (23–26%), respectively for the 0.1 wt% and 1 wt% M-FRCs when compared to the neat FRCs. ILSS properties increased (6% and 25%) for the 0.1 wt% and 1 wt% M-FRCs, respectively when compared to neat FRCs. The glass transition temperatures (T_g) of both M-FRC samples were 25 °C higher than the neat FRC. Coefficients of thermal expansion (CTE) of the M-FRC samples improved compared to the neat FRC. The improved T_g and CTE properties in the M-FRC samples are attributed to synergistic interactions between the CNF/PNC matrix and glass fibers.     

Improvement of tensile properties and toughness of an epoxy resin by nanozirconium-dioxide reinforcement

Zirconium dioxide (ZrO₂) nanoparticles were systematically added as reinforcement to a diglycidyl ether of bisphenol A (DGEBA)-based epoxy resin. A series of composites with varying amounts of nanoparticles was prepared and their morphology and mechanical properties were studied. The obtained nanocomposites were characterized by tensile tests, dynamic mechanical thermal analysis, and fracture toughness (K_IC) investigations; by standardized methods, to define the influence of the nanoparticle content on their mechanical and thermal properties. The morphological analysis of the composites shows that nanoparticles form small clusters, which are uniformly distributed into the matrix bulk. The tensile modulus (E) and the K_IC of the epoxy matrix increase at rising zirconia content. Improvements of more than 37% on modulus and 100% on K_IC were reached by the nanocomposite containing 10 vol.-% ZrO₂ with respect to the neat epoxy (E_o = 3.1 GPa, K_ICo = 0.74 MPam^0.5). The presence of nanoparticles produces also an increment on glass transition temperature (T _g). The epoxy resin added with 8 vol.-% ZrO₂ records a T _g approximately 8% higher than the unmodified matrix (T _go = 100.3 °C).     

CF/EP composite laminates with carbon black and copper chloride for improved electrical conductivity and interlaminar fracture toughness

An experimental study was conducted to improve the electrical conductivity of continuous carbon fibre/epoxy (CF/EP) composite laminate, with simultaneous improvement in mechanical performance, by incorporating nano-scale carbon black (CB) particles and copper chloride (CC) electrolyte into the epoxy matrix. CF/EP laminates of 65 vol.% of carbon fibres were manufactured using a vacuum-assisted resin infusion (VARI) technique. The effects of CB and the synergy of CB/CC on electrical resistivity, tensile strength and elastic modulus and fracture toughness (K_IC) of the epoxy matrix were experimentally characterised, as well as the transverse tensile modulus and strength, Mode I and Mode II interlaminar fracture toughness of the CF/EP laminates. The results showed that the addition of up to 3.0 wt.% CB in the epoxy matrix, with the assistance of CC, noticeably improved the electrical conductivity of the epoxy and the CF/EP laminates, with mechanical performance also enhanced to a certain extent.     

碳纤维/TiO2改性树脂复合材料的制备及力学性能

针对环氧树脂脆性大、与碳纤维形成的界面性能较差等问题,本文选用纳米TiO₂对5284环氧树脂进行改性,并以角联锁机织物为增强体制备了碳纤维/环氧树脂复合材料。使用FT-IR、旋转流变仪、表面张力仪等设备对TiO₂/环氧树脂进行表征,并研究了树脂改性对复合材料压缩与层间剪切性能的影响。研究表明：TiO₂的羟基与环氧树脂的环氧基和羟基发生了反应;经1wt.%TiO₂改性的树脂复数黏度为0.066 Pa·s,纤维与树脂间接触角为28.85°,浸润效果较好;相较于未改性复合材料,树脂改性的复合材料纵向压缩强度与模量分别提高了7.46%和11.03%,横向压缩强度与模量分别提高了6.99%和4.96%,纵向、横向的剪切强度分别提高了6.88%和4.65%。TiO₂改性环氧树脂提高了复合材料的承载能力,改善了界面结合强度。     

Novel nanocomposites based on epoxy resin/epoxy-functionalized polydimethylsiloxane reinforced with POSS

The purpose of the present study is to develop novel nanocomposites based on diglycidylether of bisphenol A (DGEBA) combined with diglycidylether-terminated polydimethylsiloxane (DG-PDMS), reinforced with 10 wt.% (mono-/octa) epoxy POSS nanocages (MEP or OEP-POSS). DG-PDMS and POSS compounds were covalently incorporated into DGEBA resin via copolymerization of epoxy groups. The effect of both DG-PDMS and POSS nanoparticles on the curing reaction, glass transition temperature (T_g), thermal stability, hardness and morphology of DGEBA/DG-PDMS ± POSS nanocomposites were studied by DSC, FTIR, DMA, TGA, SEM/EDX, AFM and contact angle measurements. SEM/EDX and AFM results prove that OEP-POSS is well dispersed within DGEBA/DG-PDMS polymer matrix, while MEP-POSS forms large POSS aggregates. The thermo-mechanical properties of POSS based nanocomposites are also in good correlation with morphology features. MEP-POSS based nanocomposite with heterogeneous dispersion of POSS aggregates exhibits lower T_g value and thermal stability in comparison with OEP-POSS nanocomposite which exhibits a nanoscale dispersion of the POSS cages. The obtained T_g of OEP-POSS based nanocomposite increases with 31 °C in comparison with the unreinforced matrix. Moreover, this nanocomposite shows the highest storage modulus (E′) and hardness.     

Effect of particle size and weight fraction on the flexural strength and failure mode of TiO2 particles reinforced epoxy

Effect of inclusions size and weight fraction on flexural strength and failure mode of composite containing SC-15 epoxy resin and TiO₂ particles has been studied in this investigation. The sizes of particles varied from macro (0.02 mm) to nano (5 nm) scale, and these particles were infused into the part-A of SC-15 through sonic cavitations and then mixed with part-B of SC-15 by using a high speed mechanical agitator. Three-point bending tests were performed on unfilled, 0.5 wt.%, 1.0 wt.% and 1.5 wt.% particles filled SC-15 epoxy to identify the loading effect on mechanical properties of the composites. Results show that 1.0 wt.% nanoparticles reinforced epoxy exhibit the highest mechanical performance. Higher than 1.0%, strength of composite decreased because of poor dispersion. Experimental results also shown that micro-sized particles have little effect on strength of epoxy at such low loading, and strength of composite increased as the size of particles decreased to nano scale. However, degradation in strength was found in 5 nm TiO₂/epoxy system due to agglomeration.     

Mechanical and barrier properties of epoxy polymer filled with nanolayered silicate clay particles

The diglycidyl ether of bisphenol A (DGEBA) epoxy resin system filled with organo clay (OC) and unmodified clay (UC) were processed separately by two different curing agents. Triethylene tetramine (TETA) and Diaminodiphenyl methane (DDM) hardeners were used as curing agents. The nanocomposites were processed by shear mixing at different clay concentrations (1, 2, 3,5 and 10 wt%). The OC and UC were characterized by x-ray diffraction (XRD) technique. The morphology of the nanocomposites was obtained by XRD and Transmission Electron Microscopy (TEM). Bending and Impact tests conducted on these materials revealed that the organo clay filled epoxy resin showed good improvement in property over unmodified clay filled epoxy composites. The mass uptake of the nanocomposites was studied in the acid, base and water mediums. It is observed that the mass uptake in the acid medium is higher than in other mediums. The equilibrium mass uptake in all the mediums for nanocomposites was found to be lower compared to neat epoxy polymer system.     

The tensile fatigue behaviour of a silica nanoparticle-modified glass fibre reinforced epoxy composite

An anhydride-cured thermosetting epoxy polymer was modified by incorporating 10 wt.% of well-dispersed silica nanoparticles. The stress-controlled tensile fatigue behaviour at a stress ratio of R = 0.1 was investigated for bulk specimens of the neat and the nanoparticle-modified epoxy. The addition of the silica nanoparticles increased the fatigue life by about three to four times. The neat and the nanoparticle-modified epoxy resins were used to fabricate glass fibre reinforced plastic (GFRP) composite laminates by resin infusion under flexible tooling (RIFT) technique. Tensile fatigue tests were performed on these composites, during which the matrix cracking and stiffness degradation was monitored. The fatigue life of the GFRP composite was increased by about three to four times due to the silica nanoparticles. Suppressed matrix cracking and reduced crack propagation rate in the nanoparticle-modified matrix were observed to contribute towards the enhanced fatigue life of the GFRP composite employing silica nanoparticle-modified epoxy matrix.     

New development of self-damping MWCNT composites

Epoxy resin modified with nanofillers cannot be used alone for high performance structural applications due to their low-mechanical properties. Therefore, the objective of this work is to hybridize unidirectional and quasi-isotropic glass fiber composite laminates with 1.0 wt% multi-walled carbon nanotubes (MWCNTs). Results from flexural and damping characterizations showed that the flexural strength and modulus, storage modulus, and damping ratio of MWCNT/E nanocomposite are improved by about 7% ± 1.5% compared to neat epoxy. The enhancement in the flexural strength of quasi-isotropic laminate (20.7%) is about ten times higher than that for unidirectional laminate (2.1%). The flexural moduli of the nano-hybridized laminates are reduced by about 7.5–10.8%. Accordingly, the ultimate failure strain and damping properties are evidently improved. The improvement in damping ratio in some cases is about 100%. The high correlation coefficient (0.9995) between flexural and storage moduli suggests using the dynamic nondestructive tests for evaluation the elastic properties of composites.     

Grafting of nano-TiO2 onto flax fibers and the enhancement of the mechanical properties of the flax fiber and flax fiber/epoxy composite

In this article, a flax fiber yarn was grafted with nanometer sized TiO₂, and the effects on the tensile and bonding properties of the single fibers and unidirectional fiber reinforced epoxy plates were studied. The flax fiber yarn was grafted with nanometer sized TiO₂ through immersion in nano-TiO₂/KH560 suspensions under sonification. The measured grafting content of the nano-TiO₂ ranged from 0.89 wt.% to 7.14 wt.%, dependent on the suspension concentration. With the optimized nano-TiO₂ grafting content (∼2.34 wt.%), the tensile strength of the flax fibers and the interfacial shear strength to an epoxy resin were enhanced by 23.1% and 40.5%, respectively. The formation of Si–O–Ti and C–O–Si bonds and the presence of the nano-TiO₂ particles on the fiber surfaces contributed to the property enhancements. Unidirectional flax fiber reinforced epoxy composite (V_f = 35.4%) plates prepared manually showed significantly enhanced flexural properties with the grafting of nano-TiO₂.