Influence of addition of silica particles on reaction-induced phase separation and properties of epoxy/PEI blends

Polyether imides (PEI)/silica nanocomposites, prepared by sol–gel process, were used to modify the epoxy resin (ER), and the effect of silica particles on reaction-induced phase separation and mechanical properties of these systems were investigated. SEM images of the fracture surface of ER/PEI/silica composites showed an interesting morphology transformation with the increase of silica particle content. SEM–EDX results indicated that silica particles once formed in the PEI gradually migrated and concentrated in epoxy-rich region during the phase separation because of the better affinity between silica particles and epoxy resin. FTIR measurement and rheological test confirmed that the silica particles make the polymerization reaction of epoxy faster and the dynamic DSC results demonstrated that the activation energy of these systems decreased with the increase of the silica particles. Mechanical measurements approved that the introducing of PEI/silica nanocomposites into the epoxy could lead to great improvement of the impact strength and storage module.     

Preparation and characterization of epoxy-silica hybrid materials by the sol-gel process

A transparent organic-inorganic epoxy/silica hybrid material was prepared by epoxy resin, functionalized-epoxy resin, which was partially functionalized by 3-aminopropyl triethoxylsilane(APTES), and highly reactive polysilcic acid (PSA), which was prepared through hydrolysis and condensation of metasilicate salt. The properties of hybrid materials such as impact strength, tensile strength, glass transition temperature (T_g), thermogravimetric temperature (TGA), and thermal effect of the hybrid materials were studied. The size of PSA particles in THF measured by dynamic light scattering technique, ranged from 10–28 nm. The results of experiment indicated that modified epoxy resin possed better roughness than that of the pure epoxy resin. The structure of the hybrid materials was characterized by FT-IR spectroscopy and 29SiNMR spectroscopy.     

Tribological properties of surface modified nano-alumina/epoxy composites

Nano-sized Al₂O₃ particles grafted with polystyrene or polyarcrylamide were employed as fillers for fabricating epoxy based composites. Curing habit, mechanical properties and tribological performance revealed by sliding wear tests of the composites were investigated. The experimental results indicated that the nanoparticles accelerate curing of epoxy, increase composites' impact strength and decrease wear rate and frictional coefficient of the composites. The surface modification by means of grafting polymerization can further enhance the properties improvement of epoxy due to the increased filler/matrix interfacial interaction. Compared to frictional coefficient, wear rate of epoxy can be decreased more remarkably by the addition of nano-alumina when rubbing against steel. The wear mode changes from severe peeling off of unfilled epoxy to mild micro-ploughing in the case of nano-alumina filled composites.     

Study on thermal and mechanical properties of nano-calcium carbonate/epoxy composites

A study on evaluating the effect of nano-CaCO₃ particles on thermal and mechanical properties of epoxy resin cast was performed by TGA and mechanical tests. A silane coupling agent KH550 as an interfacial modifier was introduced into nanocomposites through preparing KH550/nano-CaCO₃ master batch. It is revealed that epoxy resin cast filled with nano-CaCO₃ particles represents higher thermal stability and mechanical strength. The improvement of thermal and mechanical properties is attributed to the surface modification of nano-particles, which can enhance the interfacial properties between nano-CaCO₃ fillers and epoxy resin. The mechanical properties of nano-CaCO₃/epoxy/carbon fibres composites based on the modified epoxy matrix are also enhanced.     

SiO2/环氧树脂基纳米复合材料的室温和低温力学性能

利用溶胶-凝胶法制备了SiO₂/环氧树脂基复合材料,研究了材料的室温与低温(77 K)下的力学性能。结果表明,适量SiO₂的引入提高了室温与低温下材料的拉伸强度、断裂伸长率和冲击强度,即SiO₂含量在2%时可同时起到增强、增韧作用。采用扫描电镜(SEM)和透射电镜 (TEM)分别对复合材料的断口形貌和高温焚烧后残留物纳米颗粒进行了观察。还利用动态力学分析(DMA)研究了二氧化硅的引入对复合材料的影响。      

Improvement in properties of epoxy-based electrophoretic coating by silica/polyurethane nanocomposites

Silica/polyurethane (SiO₂/PU) nanocomposites, prepared by in situ formation of silica from tetraethoxysilane (TEOS) in cationic polyurethane microreactor, are used to modify epoxy resin-based electrophoretic coating. The co-electrophoresis property of silica/PU nanocomposites with epoxy particles is verified by X-ray photoelectronic spectroscopy (XPS) analysis of the electrophoretically prepared membrane. The particle sizes and size distribution in the aqueous paint show a considerable reduction as demonstrated by dynamic light scattering. The surface morphology is investigated by scanning electron microscope. The properties of SiO₂/PU-modified electrophoretically prepared membrane have a significant improvement compared to those of unmodified and PU-modified membranes. It is noteworthy that both strength and toughness of the electrophoretically prepared membrane increase considerably due to incorporation of rigid silica encapsulated by tough PU.     

Preparation and characterization of EP/SiO<Subscript>2</Subscript> hybrid materials containing PEG flexible chain

EP/SiO₂ hybrid materials, which contained flexible chain, were prepared by epoxy resin (EP) and polyethylene glycol (PEG)-grafted polysilicic acid (PSA), which was obtained by endcapping polyethylene glycol-1000 with toluene 2,4-diisocyanate (TDI), followed by a reaction with polysilicic acid. The formation of hybrid materials was confirmed by a wide-angle X-ray diffraction (WAXD) and atomic force microscopy (AFM) analysis. Results showed that the EP/SiO₂ hybrid particles were nanosized and the average size was about 20–50 nm. The mechanical properties, dynamic mechanical properties, and thermal properties were evaluated and compared with the corresponding matrix. The improvement in impact properties in hybrid materials was explained in terms of the impact fracture surface analysis by scanning electron microscope (SEM).     

Wear and mechanical properties of epoxy/SiO<Subscript>2</Subscript>-TiO<Subscript>2</Subscript> composites

Preparation of epoxy/SiO₂-TiO₂ composites is investigated in this paper. The products are characterized by FT-IR spectroscopy. Results of FT-IR spectroscopy and atom force microscope (AFM) demonstrated that epoxy chains have been covalently bonded to the surface of the SiO₂-TiO₂ particles. The particles sized of SiO₂-TiO₂ are about 20–50 nm, which characterized by AFM. The properties of composites such as impact strength, flexural strength, tensile strength and ring-on-block wear are also investigated. Dry sliding wear tests showed that the SiO₂-TiO₂ particles could improve the wear resistance of the epoxy matrix even though the content of the SiO₂-TiO₂ particles was at a relatively low level (1.95–2.65 wt%). This makes it possible to develop novel type of epoxy-based materials with improved wear resistance for various applications. The worn surface was observed by scanning electron microscopy (SEM), and mechanisms for the improvement are discussed in this paper     

Studies on mechanical properties of epoxy composites filled with the grafted particles PGMA/Al2O3

In the present work, the epoxy resin composites filled with the particulates of PGMA/Al₂O₃ which were prepared by grafting poly-glycidyl methacrylate (PGMA) onto the Al₂O₃, were obtained by incorporating and curing the resin containing the particulates. The mechanical properties of the resulting resin composites epoxy/PGMA/Al₂O₃ were evaluated and compared with epoxy/Al₂O₃. The morphologies of the fracture surfaces of the filled epoxy resin composites were analyzed by means of scanning electron microscopy (SEM). The results indicate that after grafting polymers onto Al₂O₃ particles, the interfacial combination of epoxy resin with PGMA/Al₂O₃ can be significantly increased due to the higher bonding strength and bonding modulus between them, therefore, the properties of the composites are improved largely. And the higher grafting degree of PGMA, the greater the impact strength and yield strength of the resin composites are, which primarily depends on the structure-properties relationship of the composites. In addition, the additive amount of PGMA/Al₂O₃ particles and the curing agents are also important factors that influence the properties of composites.     

接枝微粒PGMA/Al2O3对环氧树脂电子灌封材料的增强增韧作用

采用甲基丙烯酸缩水甘油酯对Al2O3颗粒进行接枝改性,制备了接枝微粒,考察了PGMA/Al2O3对环氧电子灌封材料力学性能的影响,并利用扫描电镜观察了环氧灌封材料经PGMA/Al2O3填充前后的冲击断面的形貌变化。研究结果表明,经接枝改性后,接枝微粒PGMA/Al2O3对环氧灌封材料的力学性能起到了明显的改善作用:PGMA/Al2O3对环氧灌封料的增韧效果明显优于未改性的Al2O3,且随PGMA/Al2O3填充量的增大,冲击韧性先增大后减小,在填充量较小(0.7%)时,冲击韧性最大;屈服强度也随PGMA/Al2O3的加入出现一最佳值;并随接枝微粒PGMA/Al2O3的接枝率的增加,其冲击韧性和屈服强度明显增大。     

Preparation and characterization of water-borne epoxy shape memory composites containing silica

Shape memory silica/epoxy composites were successfully prepared by hydrolysis of tetraethoxysilane (TEOS) within the epoxy matrix via latex, freeze-drying, and hot-press molding method. The silane coupling agent 3-triethoxysilylpropylamine (KH550) was introduced to improve the interfacial properties between the in-situ generated silica particle and epoxy matrix. The morphology structure and the effect of the content of the in-situ formed silica on the mechanical and shape memory properties of the silica/epoxy composites were studied. The experimental results indicated that the silica particles were homogenously dispersed and well incorporated into the epoxy matrix. Significant improvements were achieved in the mechanical property of the organic–inorganic hybrid materials. The silica/epoxy composites exhibited high shape recovery and fixity ratio approximately 100% even after 10 thermo-mechanical cycles.     

Effect of the particle size of nanosilica on the performance of epoxy/silica composite coatings

Four kinds of colloidal silica particles with different size (27, 58, 79 and 173 nm, respectively) were synthesized by sol-gel process and modified with 3-glycidoxypropyltrimethoxysilicane, then homogenously dispersed into the epoxy resin and cured with alicyclic amine on aluminum alloy substrates. The results showed that the Si-O-Al bond was formed at nanocomposite coat/substrate interface, introducing nanosilica significantly enhanced the adhesive strength, scratch resistance, abrasion resistance and corrosion resistance of coats, but different particle sizes of nanosilica had various impact on these properties, which seemed to be related to the structure of the silica surface.     

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.     

Effect of hybridization of liquid rubber and nanosilica particles on the morphology, mechanical properties, and fracture toughness of epoxy composites

A liquid carboxyl-terminated butadiene–acrylonitrile copolymer (CTBN) and SiO₂ particles in nanosize were used to modify epoxy, and binary CTBN/epoxy composites and ternary CTBN/SiO₂/epoxy composites were prepared using piperidine as curing agent. The morphologies of the composites were observed by scanning electron microscope (SEM) and transmission electron microscope (TEM), and it is indicated that the size of CTBN particles increases with CTBN content in the binary composites, however, the CTBN particle size decreases with the content of nanosilica in the ternary composites. The effects of CTBN and nanosilica particles on the mechanical and fracture toughness of the composites were also investigated, it is shown that the tensile mechanical properties of the binary CTBN-modified epoxy composites can be further improved by addition of nanosilica particles, moreover, obvious improvement in fracture toughness of epoxy can be achieved by hybridization of liquid CTBN rubber and nanosilica particles. The morphologies of the fractured surface of the composites in compact tension tests were explored attentively by field emission SEM (FE-SEM), it is found that different zones (pre-crack, stable crack propagation, and fast crack zones) on the fractured surface can be obviously discriminated, and the toughening mechanism is mainly related to the stable crack propagation zone. The cavitation of the rubber particles and subsequent void growth by matrix shear deformation are the main toughening mechanisms in both binary and ternary composites.     

Preparation and characterization of an epoxy nanocomposite toughened by a combination of thermoplastic,layered and particulate nano-fillers

This paper reports the development of an epoxy-based nanocomposite toughened by the combination of thermoplastic, layered and particulate nano-fillers. The main objective of this work is to incorporate poly(acrylonitrile-co-butadiene-co-styrene) (ABS), clay (layered nano-filler) and nano-TiO₂ (particulate nano-filler) into epoxy matrix with the aim of obtaining the quaternary nanocomposite with higher impact strength and lower cost without attenuating the other desired mechanical properties such as tensile strength. Taguchi methodology was applied for the optimization and statistical determination of the significant factors influencing the mechanical properties of the quaternary nanocomposite. Impact and tensile strengths of the quaternary nanocomposite with optimum composition increased by 168% and 64% compared to neat epoxy, respectively. Furthermore, synergistic effect was observed with the addition of three type modifiers. It was found that ABS content has the most significant effect on mechanical properties of the obtained quaternary nanocomposite. Also correlation between morphological and mechanical properties of the nanocomposite was investigated. A dispersion of nano-size ABS and TiO₂ particles along with exfoliated clay nano-platelets in epoxy matrix was achieved as main morphological property of the quaternary nanocomposite. A new morphology was obtained for ABS phase in epoxy rich matrix.     

Mechanical properties of epoxy composites reinforced with a low volume fraction of nanosilica fillers

In this paper we focus on the preparation and mechanical properties of the nanosilica-reinforced, epoxy resin Epikote 828LVEL. Epoxy composites containing two sizes of spherical silica nanoparticles, 130 nm and 30 nm, were prepared at a fixed volume fraction (V_P = 0.5%). To prevent agglomeration, the silica fillers were initially pre-treated with diglycidyl ether of bisphenol A (BADGE). Due to the low content of silica fillers, their inclusion in the matrix was confirmed by the increased roughness of a fracture surface compared to the smooth surface of the neat epoxy. Raman spectroscopy was employed to obtain additional information about the crack-propagation path. The mechanical properties, characterized by a three-point bending test, revealed a 10–20% increase in the composite's modulus of elasticity with 30-nm and 130-nm silica-filler inclusions. Elongation at break, on the other hand, decreased for 5–10% in both composites compared to neat epoxy, suggesting brittle fracture behavior in silica/epoxy composites. The fracture toughness results showed a 25–30% improved toughening for both composites compared to the pure epoxy. The composite's resistance to failure in terms of the impact energy was, however, strongly dependent on the size of the silica: we observed a 30% increase for the 130-nm, and a 60% increase for the 30-nm, silica/epoxy composites, compared to the pure epoxy.     

Characterization of SiO2/Ag composite particles synthesized by in situ reduction and its application in electrically conductive adhesives

In the study, SiO₂/Ag composite particles with silver coating onto the surface of silica have been successfully prepared via a novel and facile approach (Oxidation–Reduction Method). In this approach, the SiO₂ particles were first modified with 3-ammoniatriethoxysilane (APTES) and glyoxalic acid (GA) through two-step reaction, the aldehyde group (CHO) were anchored onto the surfaces of silica spheres via electrostatic attraction, these [Ag(TEA)₂]⁺ ions in the solution were then reduced by the CHO and coated onto the surface of silica to obtain SiO₂/Ag composite particles. The effects of the reaction conditions on silver content and synthetic mechanism had also been discussed. The structure, morphology and optical properties of the SiO₂/Ag composite particles were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), and UV–vis spectroscopy. The results showed the surface of SiO₂ was surrounded by pure silver nanoparticles, and the silver nanoparticles had face-centered-cubic structure, the SiO₂/Ag composite particles with core–shell morphology and special optical properties. And the small content SiO₂/Ag composite particles applied in electrically conductive adhesives (ECAs) improved the electrical bulk resistivity and tensile shear strength.     

微纳米SiO2/PP复合材料增强增韧的实验研究

为了研究无机刚性颗粒对通用塑料聚丙烯 (PP) 的力学性能的影响, 采用熔融共混方法制备了经硅烷偶联剂A-151处理的SiO₂/PP 复合材料, 并通过其缺口冲击、 拉伸、 弯曲试验和冲击断面的形貌观察, 分析研究了微纳米SiO₂颗粒大小、 填充量、 表面改性以及不同颗粒大小SiO₂混合物对PP复合材料增韧、 增强效果的影响。实验结果表明: 纳米SiO₂的加入可以同时改善其韧性、 刚性和强度; 填充量相同, 颗粒越细, SiO₂/PP复合材料的力学性能越好。SiO₂经改性后填充到PP基体中, 明显改善了颗粒在基体中的分散性及基体与颗粒之间界面结合性能, 使复合材料的综合力学性能得到提高。不同颗粒大小的SiO₂混合后填充到PP基体中, 混合SiO₂的协同效应使复合材料拉伸、 弯曲性能进一步提高, 对PP基体具有更好的增强效果, 但其冲击性能下降。      

Effects of emulsion sizing with nano-SiO<Subscript>2</Subscript> on interfacial properties of carbon fibers/epoxy composites

Nano-SiO₂ particles were used to modify epoxy emulsion sizing of carbon fibers to improve the interfacial properties of carbon fibers reinforced epoxy composites. The mechanical interfacial strength between fibers and matrix was investigated by the single fiber fragmentation test and the 3-point short beam shear test, respectively. Dynamic contact angle analysis (DCAA), X-ray photoelectron spectrometry (XPS) and atomic force microscopy (AFM) were performed on the carbon fibers with unmodified sizing and nano-SiO₂ modified sizing. The results indicated that modified sizing with nano-SiO₂ slightly increased the surface energy, the hydroxyl functional group and the surface roughness of carbon fibers compared to unmodified sizing, so that the interfacial shear strength (IFSS) of the single fiber composites and the interlaminar shear strength (ILSS) of composites were enhanced. SEM images of fracture sections of composites proved powerfully that the interfacial adhesion between fibers and matrix was improved after nano-SiO₂ modified emulsion sizing treatment.     

不同结构聚合物核壳粒子对环氧树脂的增韧改性

传统环氧树脂的增韧改性方法往往达不到理想的效果。核壳粒子与环氧树脂混合,能减小内应力,获得显著的增韧效果,且不改变热变形温度。文中采用微皂核壳乳液的聚合方法合成了不同的核壳粒子,并对这些核壳粒子增韧环氧树脂体系的力学性能进行试验研究、理论分析和数值计算。用力学强度、动态力学分析等表征手段对核壳粒子的结构和改性环氧树脂体系的增韧机理进行了探讨。结果发现,改善核、壳之间或者核壳粒子壳层同环氧树脂之间的相容性和界面粘合力,核层能更好地将能量充分耗散,改性体系的冲击强度得以进一步提高。