Investigation of the microwave curing of the PR500 epoxy resin system

Microwave heating has been used to cure a resin system, PR500 (3M). The same resin has been cured using a conventional oven. The cured resins have been compared using a number of techniques including modulated differential scanning calorimetry (MDSC), dynamic thermal analysis, infrared spectroscopy (IR) and solid-state NMR spectroscopy. The reaction path appears to be slightly different depending upon the nature of the heating. The epoxy-amine reaction occurs to a greater extent than the epoxy-hydroxyl reaction in the microwave cured resin compared to the thermally cured resin. The dielectric properties for the thermally and microwave cured materials were measured for degrees of cure greater than 75% and over this range are similar for materials cured by the two techniques and thus not sensitive to this change. Broadening of the glass transition for microwave-cured epoxy resins was observed. Since the IR and solid-state NMR results show small differences as does the DMA behaviour of materials cured using the two routes the broadening is attributed to a difference in network structure.     

Electrical properties of carbon-containing epoxy compositions under shape memory effect realization

The behavior of electrical resistance R of compression-deformed samples of the epoxy polymer-thermoexpanded graphite (EP-TEG) and EP-TEG-kaolin compositions has been investigated in the shape recovery temperature range. It is shown that the process of shape recovery is accompanied by a jump-like increase of R related to the sample length change. The addition of kaolin decreases the absolute value of electrical resistivity of the deformed polymer compositions and increases the value of R jump. The revealed changes in R are explained with the attraction of data on differential scanning calorimetry (DSC) measurements, results of investigations of composite microstructure and percolation model representations.     

快速固化环氧树脂及其碳纤维/环氧复合材料性能

采用双酚A型环氧树脂（DGEBA）、改性咪唑（MIM）及改性脂肪胺（MAA）研制快速固化树脂体系。分别利用DSC和流变仪测试了树脂体系的固化特性与流变行为,优选了树脂配方。采用真空辅助树脂灌注工艺（VARIM）制备了快速成型的碳纤维/环氧复合材料层板,考察了层板的成型质量和力学性能,并与常规固化的层板性能进行了对比。结果表明：采用优选的树脂配方,120 ℃下树脂在5 min内固化度达95%,碳纤维/环氧复合材料层板成型固化时间可控制在13 min以内,固化度达95%以上,并且没有明显缺陷;与常规固化相比（固化时间大于2 h）,快速固化碳纤维/环氧复合材料层板的弯曲性能和耐热性能降低幅度较小。     

Mechanical and morphological properties of fly ash/epoxy composites using conventional thermal and microwave curing methods

Conventional thermal and microwave curing methods were utilized to cure fly ash/epoxy composites, and the mechanical and morphological properties of the composites were evaluated. The conventional thermal curing was performed at 70 °C for 80 min while microwave curing was carried out at 240 W for 18 min in order to achieve the optimum cure of the composites, determined using Differential Scanning Calorimeter. The results suggested that the tensile and flexural moduli of the composites increased with increasing fly ash content while the effect became opposite for tensile, flexural and impact strengths, and tensile strain at break. Improved mechanical properties of the composite could be obtained by addition of N-2(aminoethyl)-3-aminopropyltrimethoxysilane coupling agent, the contents of 0.5 wt% being recommended for the optimum mechanical properties. Beyond these recommended contents, the mechanical properties greatly reduced, except for the flexural modulus. The comparative results indicated that the composites by the microwave cure consumed shorter cure time and had higher ultimate strengths (especially impact strength), and strain at break than those by the conventional thermal cure. The composites with higher tensile and flexural moduli could be obtained by the conventional thermal cure.     

Combinatory model of curing process in epoxy composite

A combinatory model of curing process in a mixture of multifunctional active components was developed. The model was tested with an analysis of curing kinetics in epoxy resin based on Bisphenol A with amine hardener. The experimental kinetics data obtained with FTIR and Raman spectroscopy, chromatography and viscosimetry methods were applied. The theoretical results show good agreement with experiment. The model can predict a concentration of middle products during curing reaction. The model is developed for calculation of the curing kinetics in free space environment.     

环氧树脂/聚酰胺体系固化工艺分析

利用差热分析仪对环氧树脂E51/聚酰胺650体系的固化反应过程进行测试。分析了固化剂添加量、改性剂种类及粉煤灰微珠对体系固化反应的影响。结果表明,固化促进剂和粉煤灰微珠会降低反应起始温度,促进反应进行;固化剂添加量和稀释剂等对固化温度影响较小。根据实验结果确定预固化温度为80℃,制备固化试样并进行DTA测试,由测试结果确定后固化温度为120℃。结合预固化温度和后固化温度制备不同的固化试样测试其红外谱线,并利用内标法计算环氧基面积表征固化度,最终确定最优固化制度为预固化温度80℃(120 min),后固化温度120℃(30 min)。     

室温固化柔性环氧树脂固化剂的制备与性能研究

通过聚醚多元醇和甲基丙烯酸甲酯进行酯交换反应,然后利用多元胺与烯双键的加成改性,将多乙烯多胺与甲基丙烯酸酯反应,合成了含甲基丙烯酸聚醚多元醇酯柔性基目的新型环氧树脂室温固化剂.通过IR等方法对产物进行了征,探讨优化了各种反应条件,并考察了其对环氧树脂性能的影响.     

Water-based epoxy materials: properties of curing agents and film-forming properties

The structural changes of polyamino-amide and polyamino-imidazoline, used as curing agents for water-based epoxy materials (WBEM), have been examined under various conditions of storage. Additionally, epoxy emulsion stabilization and film-forming in WBEM needed special research to set the limits of material utility. Infrared analysis, potentiometric titration and viscometric data obtained for some curing agents for WBEM, commercial polyamino-amide and the derived polyamino-imidazoline compounds, prove that during prolonged storage (from 1 to 140 days) these products can hydrolyse to yield free amines and carboxyl groups. The reaction mechanisms are suggested. The results include considerations for further development of epoxy compositions and a study of film-forming properties.     

Effects of compound curing agent on the thermo-mechanical properties and structure of epoxy asphalt

Epoxy asphalt curing system was prepared by sebacic acid compound with methyl-tetrahydrophthalic anhydride (MeTHPA) or Tung oil anhydride (TOA). Tensile strength, penetration, differential scanning calorimetry, dynamic mechanical thermal analysis, torn section microscopy photographs and scanning electron microscope analysis were utilised to investigate the mechanical properties, thermodynamic behaviour and micro-structure of epoxy asphalt curing systems under different curing agents. The results showed that in the presence of compound curing agent, the tensile strength and surface hardness of the epoxy asphalt curing system effectively improved, the induction period of the curing reaction decreased, the curing reaction mechanism turned to one-step reaction from two-step reaction, the Tg of asphalt phase and epoxy phase could simultaneously increase, and high-temperature damping performance also improved, but the particle size of asphalt dispersed in epoxy resin becomes uneven, while the curing system becomes semi-brittle from toughness. Compared to TOA, the effects of MeTHPA on such performance were more obvious.     

单向碳化硅纤维/环氧树脂复合材料吸波性能的研究

采用真空袋工艺制备了纤维体积分数为10%~40%的单向碳化硅纤维/环氧树脂复合材料,研究其力学性能和介电性能,计算其吸波性能和反射率。结果表明,在10%~25%范围内,随着碳化硅纤维体积分数的提高,复合材料的介电损耗实部、虚部及损耗角正切值均增大,反射率减少,即吸波能力增大;而在高于25%之后,就吸波能力而言,存在着最优纤维体积分数值;在纤维体积分数固定之后,就吸波能力而言,也存在着最佳的材料厚度;当复合材料的SiC纤维体积分数为25%、厚度为3 mm时,其在X波段内的反射率均低于-5dB,最低为-9.9dB,平均值为-7.8dB。     

乳化型水性环氧树脂固化剂的合成与性能研究

在三乙烯四胺(TETA)的分子链段上引入醇羟基、环氧基团,使其改性为亲水亲油的两亲性化合物,即乳化型的水性环氧树脂固化剂,兼具乳化和固化功能.采用封端剂调节亲水亲油平衡值(HLB)使乳化固化性能最佳.激光粒度分析仪的测试乳化环氧树脂粒径在200nm左右.涂料涂膜后的性能测试:表干时间2h左右;涂膜后4天其硬度即达到稳定...     

Non-stoichiometric curing effect on fracture toughness of nanosilica particulate-reinforced epoxy composites

Non-stoichiometric curing effects on the fracture toughness behaviors of nanosilica particulate-reinforced epoxy composites were experimentally investigated in this study by comparing them with bending strengths to take into consideration the effect of interaction between nanoparticles and network structures in matrix resins. The matrixes were prepared by curing them with an excess mixture of diglycidyl ether of bisphenol A-type epoxy resin as the curing agent for the stoichiometric condition. The volume fractions of the silica particles with a median diameter of 240 nm were constantly 0.2 for all composites. The neat epoxy resins and the composites were cured non-stoichiometrically to change the crosslinking densities of the neat epoxy resins and the matrix resins of the composites within 2740–490 mol/m³. The fracture toughnesses and bending strengths of the composites and the neat epoxy resins strongly depended on the crosslinking densities in the resins. Although the fracture toughness decreased monotonously from that of the stoichiometrically cured resins as the crosslinking density decreased, the fracture toughnesses of composites were largest at a slightly lower crosslinking density of approximately 2490 mol/m³ from the stoichiometric condition of 2740 mol/m³. The fracture toughness and the bending strength were improved for crosslinking densities higher than 2000 mol/m³ by adding particles. At crosslinking density lower than 2000 mol/m³, the particles worked against the mechanical properties as defects in matrix resins.     

自乳化型非离子水性环氧树脂固化剂的合成与性能研究

在三乙烯四胺(TETA)的分子链段上通过两步扩链法接入环氧基团,将亲水性多乙烯多胺改性成为亲水亲油的两亲性化合物,即自乳化非离子水性环氧树脂固化剂,兼具乳化和固化功能.激光粒度分析仪测试乳化环氧树脂平均粒径在1μm左右,对该水性环氧涂料涂膜后的性能测试表明:表干时间1.5h左右,涂膜6d后硬度达到稳定值,硬度为4H,涂膜附着力达到1级,涂膜的透明性及耐腐蚀性都较好.     

Effect of rapid curing process on the properties of carbon fiber/epoxy composite fabricated using vacuum assisted resin infusion molding

Long processing cycle makes vacuum assisted resin infusion molding (VARIM) only suitable for low and medium volumes of production, and shortening of curing time is critical to improving the processing efficiency of automotive composite parts. In this paper, unidirectional carbon fiber reinforced composite laminates were fabricated by VARIM. Three different processes (namely quick, quick-post and preheating) were employed, in which a kind of rapid curing epoxy resin is used. The preheating of mold and fiber was conducted to shorten the filling time compared with that of quick process. Quick-post process with a post cure stage was investigated to verify the composite properties fabricated by quick process. The cycle time was 16 min for preheating process, about 30% shorter than that of quick process, simultaneously, flexural strength and interlaminar shear strength (ILSS) were respectively improved by 29% and 7% compared with those of quick process. The non-uniformity of mechanical properties at different positions along resin flow direction under preheating process was found, but the processing quality of composite was good. The preheating process is confirmed to be suitable for the improvement of processing efficiency of VARIM with good mechanical properties. In addition, the composite fabricated by quick-post process has better mechanical properties, which is attributed to the alleviation of residual stress during post curing process.     

Investigation of the microwave absorbing properties on polymer sheets

Journal of Materials Science: Materials in Electronics - Electromagnetic (EM) absorbers are becoming an important tool in the recent advanced technologies as well as for environments to minimize...     

Study on the curing process for carbon/epoxy composites to reduce thermal residual stress

In this work, a cure monitoring system using dielectrometry and a fiber Bragg grating (FBG) sensor, was devised to measure the dissipation factor and thermal residual stress of carbon fiber-reinforced epoxy composite materials. Three rapid-cooling points, which were based on the cure initiation point, were chosen as test variables to investigate the effect of cure cycle on process-induced internal strain. The internal strains generated in the composite specimens were measured using embedded FBG sensors. Three-point bending tests were conducted to investigate the effect of thermal residual stress on the flexural strength of the composite specimens.     

Effect of filler content and size to properties of composite resins on microwave curing

The effect of filler content and size to property of composite resin using high purity spherical silica particles on microwave curing was examined by mechanical means and electron microscope observation to develop microwave-curing composite resin inlay. Increasing filler content in three kinds of filler particles (0.45, 0.96 and 1.46 m) resulted in increasing compressive strength, diametral tensile strength and knoop hardness and indicated the highest values at the operative mixing limit. The effect of particle size was that the mechanical property of the 0.96 m filled resin was highest, followed by 1.46 m and 0.45 m on the same filler content. The 0.96 m filled resin had about the same knoop hardness on both surfaces of the cured sample, which means that uniform polymerization occurred in the cured sample.With electron microscope observation, the bubbles of about 1.0 m and the cracks between the fillers and the matrix were observed in each cured resin. This is caused by the excessive absorption of microwave energy in fillers and surface treatment materials of fillers. Therefore, improvement of the composition of filler and surface treatment material of filler are needed, which makes it harder to absorb the microwave energy. ©©1999©Kluwer Academic Publishers