Flame retardant effect of polyhedral oligomeric silsesquioxane and triglycidyl isocyanurate on glass fibre‐reinforced epoxy composites

Polyhedral oligomeric silsesquioxane (POSS) and triglycidyl isocyanurate (TGIC) were added to an aerospace grade epoxy resin (EP) individually or in combinations at low concentrations. The EP samples containing additives were cast into resin laminates and also used to produce glass fibre‐reinforced composite laminates. The flammability of the two types of laminates was studied by limiting oxygen index, UL‐94 and cone calorimetry. The cone results indicated that the use of POSS (10 wt%) in EP can significantly decrease resin/composite's peak heat release rate, total heat release, and CO production. The mechanical performance in flexural modes of the fibre‐reinforced composite laminates was not adversely affected by the addition of POSS and TGIC in the resin. POSS containing samples had better retention of mechanical properties after exposure to radiant heat in a cone calorimeter compared with other samples. The results of thermogravimetry (TG), TG‐FTIR, and dynamic FTIR indicated that the thermal degradation behavior of the EP is significantly changed by the addition of POSS. POSS can get grafted on the EP's main chain during earlier stages of decomposition and form a stable char layer to protect the underlying material from further decomposition. POLYM. COMPOS., 2011. © 2010 Society of Plastics Engineers     

Investigations into lightweight solutions for epoxy composite fire property improvement

Abstract

The aim is to study methods to improve the fire properties of carbon fibre reinforced epoxy composites with interlayers without compromising structural performance, i.e. using a carbon fibre veil with expandable graphite, an intrinsically flame retardant thermoplastic film or a carbon fibre reinforced thermoplastic (CFTP) layer. The CFTP layer seems the most promising, with a significant improvement in fire properties as determined with cone calorimetry, while the mechanical performance of the modified composite appears unaffected.     

电抗器用玻纤纱/环氧树脂复合材料最优含胶量的研究

玻璃纤维纱增强环氧树脂是玻璃钢的一种,由于其良好的电气绝缘性能及机械性能,所以在干式空心电抗器包封绝缘层中被广泛使用。主要研究了玻纤/环氧树脂复合材料中玻璃纤维纱与环氧树脂的最佳比例,因环氧树脂固化物本身具有良好的电气绝缘性,故只针对其力学性能进行测试和评估,最终确定出二者的最优比例,同时确立一个行业的标准。     

Influence of carbon fibre orientation on reaction‐to‐fire properties of polymer matrix composites

The influence of the orientation of carbon fibres on the reaction‐to‐fire characteristics of a layered composite has been investigated in detail. 8552/IM7 prepregs were laid up to give unidirectional and quasi‐isotropic laminates. Specimen thickness (0.25 to 8.0 mm) and heat flux (15 to 80 kW/m²) were varied for irradiation. Fundamental reaction‐to‐fire properties of this composite are interpreted on the basis of the matrix components: epoxy resin and polyethersulfone. Cone calorimetry and temperature distributions through the laminate showed that the velocity and degree of combustion are dominated by fibre orientation for a given resin. In general, a quasi‐isotropic fibre orientation leads to faster ignition, because of preferred delaminations, but retards combustion processes more effectively than a unidirectional lay‐up. Migration velocities of the pyrolysis zone were measured. Copyright © 2011 John Wiley & Sons, Ltd.     

Fire-hazard assessment of extended-chain polyethylene and aramid composites by cone calorimetry

A cone calorimeter is used to determine the fire performance of polymer composite materials containing combustible reinforcing fibres in addition to combustible matrix resins. Extended-chain polyethylene and aramid fibre-reinforced composites containing epoxy, vinylester and phenolic matrix resins are examined at various cone irradiances. Values for time to ignition, rate of heat release, effective heat of combustion, smoke density and evolved carbon monoxide and carbon dioxide are reported for the reinforcements, matrix resins and composites. The reinforcements have a significant effect on the fire-hazard properties of the composite materials. For the epoxy and vinylester composites, times to ignition reflect those of the component of higher ignitability. This was not the case for the aramid-reinforced phenolic composite, in which the resin surface layer hinders combustion of the fabric reinforcement. Resin and reinforcement contributions to the composite rate of heat release behaviour as a function of time are generally discernible.     

一种中温固化高强度耐烧蚀环氧结构胶的特性

介绍了一种中温固化、粘接强度高、氧-乙炔烧蚀性能好的环氧胶粘剂,讨论了树脂和填料等对组分性能和工艺的影响。满足了小型固体火箭发动机中金属和玻璃钢之间的粘接及其耐烧蚀性能的要求。     

Interaction between the reinforcement and matrix in carbon-fiber-reinforced composite: Effect of forming the thin layer of polyimide resin on carbon fiber by in situ polymerization

For the purpose of enhancing the reinforcement–matrix interaction in carbon-fiber-reinforced polymer composite, mechanical and spectroscopic studies were made on the epoxy resin composite reinforced with the carbon fiber coated with thin Layer of polyimide resin. On the loss modulus and loss tangent vs. temperature curves, a subtransition appears at a temperature above the primary transition. The T-peel strength of a laminated specimen and the fiber efficiency factors for modulus and strength are larger than those of the composite reinforced with nonpolyimide treated fiber. These results show the increased interaction between the epoxy resin and the carbon fiber coated with polyimide resin. The occurrence of specific interaction between an epoxy resin and the polyimide resin are recognized on fourier transform infrared spectra.     

T700碳纤维复合材料耐湿热老化研究

选用TDE-85和E-51作为主体树脂,制备了一种T700碳纤维复合材料,并对这种复合材料进行耐湿热老化研究,分别测定其抗剪切强度、抗拉伸强度及模量和玻璃化转变温度随老化时间的变化值。结果表明,该T700碳纤维复合材料耐湿热老化性能较好,其力学性能在2 000 h的老化过程中变化不太大,但是其玻璃化转变温度值降低很多。     

The dynamic mechanical analysis of epoxy–copper powder composites using azole compounds as coupling agents

The dynamic mechanical properties of cured epoxy resin have been studied in which copper powder treated or untreated with azole compounds was used as fillers. The untreated fillers do not shift the glass transition temperature of the matrix polymer of the composites, whereas the storage modulus rises with increasing content of fillers. The application of azole compounds as coupling agents, which could react with both copper and epoxy resin, extended the polymer–filler interactions. The composite filled with copper powder treated with benzotriazole shows a strong reinforcement effect and high resistance to moisture.     

高低温老化对碳纤维复合材料芯棒结构性能的影响

采用拉挤工艺制备了碳纤维增强环氧树脂基复合材料芯棒,并对其进行高低温人工加速老化试验,以及对老化前后碳纤维复合材料芯棒的横截面、外观颜色和密度进行了测试和分析。结果表明,高低温老化使芯棒颜色加深,主要对芯棒的外层产生一定的影响,内部结构没有明显变化;老化后芯棒的密度比老化前减小约2.5%,并且不同老化周期对芯棒的密度基本不变。     

Mechanical properties of hybrid structural composites reinforced with nanosilica

Epoxy‐based hybrid structural composites reinforced with 14 nm spherical silica particles were investigated for mechanical properties as a function of nanosilica loading fractions. Composites were fabricated using continuous glass or carbon fiber of unidirectional architecture and nanosilica dispersed epoxy, through resin film infusion process. Uniform dispersion of nanoparticles in resin matrix was ensured by an optimized ultrasound‐assisted process. Although resin viscosity marginally reduces in the presence of nanosilica enabling a better control in composite manufacturing process, glass transition temperature of epoxy remained unaffected at low weight fractions. Compressive strength of hybrid glass or carbon fiber/epoxy composites showed more than 30–35% increase with nanosilica at a concentration as low as 0.2 wt%. Tensile and compressive properties of hybrid composites in transverse direction to the reinforcement remained unaffected. POLYM. COMPOS. 37:1216–1222, 2016. © 2014 Society of Plastics Engineers     

Improvement of Hardness and Wear Resistance of Glass Fiber-Reinforced Epoxy Composites by the Incorporation of Silica/Carbon Hybrid Nanofillers

The tribological performance of hybrid composite (epoxy reinforced with woven, nonwoven tissue glass fibers, silica and carbon black nanoparticles) was investigated. Two methods were used to ensure good dispersion of nanoparticles in epoxy resin which were ultrasonic processor and magnetic stirrer. The effect of silica and/or carbon black nanoparticle content on microindentation hardness and wear properties of the neat glass fiber-reinforced epoxy composites was investigated. The results from the wear test indicated that, under all applied loads, incorporation of silica and carbon black nanoparticles either single or combined significantly improved the wear resistance of neat glass fiber reinforced epoxy. A significant increase in hardness of the hybrid nanocomposite laminates was achieved. Analysis of variance was developed to study the optimal wear testing parameters on composite samples. The most significant parameter is the time, followed by nanoparticle (silica and carbon black) content.     

A Study of the Interphase Region in Carbon Fibre/Epoxy Composites using Dynamic Mechanical Thermal Analysis

We have examined the effect of fibre addition on the glass transition temperature (T_g) of two epoxy resin systems (an amine cured and an anhydride cured epoxy system) using dynamic mechanical thermal analysis (DMTA) and differential scanning calorimetry (DSC). The presence of fibres changes the glass transition temperature (T_g) of an anhydride cured epoxy resin but does not affect that of an amine cured epoxy. The data suggest that two counteracting mechanisms are responsible for these changes: firstly, the presence of fibres causes a restriction of the molecular motion in the resin system, and secondly, the presence of carboxyi and keto-enol groups on the fibre surface inhibit curing of the resin close to the fibre, i.e. in the interphase region. The former increases the T_g and is a long range effect whereas the latter decreases the T_g and is a localised phenomenon. Changes in the dynamic properties of the interphase region are only detected when the samples are loaded in the longitudinal direction and not in the transverse direction where bulk matrix properties dominate. Sizing the fibres before their incorporation into the epoxy resin eliminates the variation in interfacial properties arising from differences in fibre surface chemistry.     

深潜壳体用高模量树脂基体的研究——基体模量对复合材料抗压抗剪性能的影响

制备了高模量树脂基单向复合材料，测试了单向复合材料的纵向压缩性能和平面剪切性能。研究了基体模量对单向复合材料抗压强度及复合材料平面剪切性能的影响，结果表明：单向复合材料的抗压强度与基体模量成线性比例关系，随基体模量的提高而提高，复合材料的平面剪切性能与基体模量基本上呈线性关系，平面剪切强度亦随基体模量的提高而提高。以模量达５．３６ＧＰａ的环氧树脂作为复合材料的树脂基体制备的，单向玻璃纤维增强复合材料其抗压强度高达１．２９５ＧＰａ，碳纤维增强的复合材料抗压强度高达１．３７２ＧＰａ，与普通环氧树脂的单向复合材料相比，分别提高了５５％和４５．８％；复合材料的平面剪切强度达６４．５ＭＰａ，比普通环氧树脂复合材料的平面剪切强度提高了４４．３％，满足了深潜壳体对复合材料抗压强度的要求。     

Pseudoreinforcement effect of multiwalled carbon nanotubes in epoxy matrix composites

The carbon nanotube possesses outstanding physical properties. Theoretically, adding carbon nanotubes into a polymer matrix can remarkably improve the mechanical properties of the polymer matrix. In the present work, a series of composites was prepared by incorporating multiwalled carbon nanotubes (MWNTs) into an epoxy resin. The influences of MWNT content and curing temperature on the flexural properties of the epoxy resin were investigated. The results showed that a very low MWNT content should be used to ensure homogeneous dispersion of MWNTs in the epoxy matrix. A higher MWNT content may lead to deteriorated mechanical properties of the composites because of the aggregation of MWNTs. A decline in the flexural properties of the neat epoxy resin with increasing curing temperature was found. However, under the same curing conditions, improvement in flexural properties was observed for the composite with the low MWNT content and a mild curing temperature. The improvement was far beyond the predictions of the traditional short‐fiber composite theory. In fact, this improvement should be attributed to the retarding effect of MWNTs on the curing reaction of epoxy matrix. Therefore, the improvement in the flexural properties was only a pseudoreinforcement effect, not a nano‐reinforcement effect of the MWNTs on the epoxy resin. Perhaps, it is better for MWNTs to be used as functional fillers, such as electrical or thermal conductive fillers, than as reinforcements. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 102: 3664–3672, 2006     

Experimental and numerical investigations on the thermal response of multilayer glass fibre/unsaturated polyester/organoclay composite

Organoclay glass fibre reinforced polymer (GFRP) nanocomposites are fabricated using the vacuum assisted resin transfer moulding. The unsaturated polyester resin is prepared with and without organoclay involving mechanical mixing, sonication, dilution solvent and heat treatment. Three levels of organophilic clay content are added, and its influences on the fire performance of composite samples are investigated. A novel numerical procedure combining pyrolysis analysis of the organoclay‐composites and the fire dynamic simulation of the combustion process are developed to validate the thermal responses obtained from the cone calorimetry experiments. Kinetic parameters obtained from the TGA tests and pyrolysis analyses are used as inputs for the models measuring the fire growth index and total heat release. To account for multilayer composite structure and organoclay distribution, three numerical models are proposed including composite (CPS), component (CPN) and CPN‐layer models. While CPS model assumes the homogeneity of the composite, later models consider multilayer effects with uniform (CPN model) or concentrated (CPN‐layer model) distribution of organoclay. Numerical results are compared with experimental ones in terms of total heat release, fire growth index. Finally, the fire resistance and total smoke release of the polyester/glass composites with the addition of organoclay will be evaluated taking into account influences of the fabrication processes.     

预固化环氧树脂基复合材料自粘结性能研究

通过拉丝法测定了5228A环氧树脂在不同温度下的凝胶时间,选择了特定的预固化温度;在预固化温度下制备了不同预固化度的碳纤维增强环氧树脂基复合材料,采用DMA测试了预固化复合材料层板的玻璃化转变温度;采用自制粘接模具制备了复合材料自粘结接头,测试了复合材料接头的搭接剪切性能;采用光学显微镜观测了自粘结搭接结构和剪切断口形貌,分析了搭接结构对剪切强度的影响。结果表明:复合材料层板的预固化度<αgel时,接头的搭接剪切强度变化不大,当预固化度>αgel时,接头的搭接剪切强度降低幅度较大;剪切性能受搭接结构的完整性影响较大。     

A Study of the Interphase Region in Carbon Fibre/Epoxy Composites using Dynamic Mechanical Thermal Analysis

We have examined the effect of fibre addition on the glass transition temperature (T _g ) of two epoxy resin systems (an amine cured and an anhydride cured epoxy system) using dynamic mechanical thermal analysis (DMTA) and differential scanning calorimetry (DSC). The presence of fibres changes the glass transition temperature (T _g ) of an anhydride cured epoxy resin but does not affect that of an amine cured epoxy. The data suggest that two counteracting mechanisms are responsible for these changes: firstly, the presence of fibres causes a restriction of the molecular motion in the resin system, and secondly, the presence of carboxyi and keto-enol groups on the fibre surface inhibit curing of the resin close to the fibre, i.e. in the interphase region. The former increases the T _g and is a long range effect whereas the latter decreases the T _g and is a localised phenomenon. Changes in the dynamic properties of the interphase region are only detected when the samples are loaded in the longitudinal direction and not in the transverse direction where bulk matrix properties dominate. Sizing the fibres before their incorporation into the epoxy resin eliminates the variation in interfacial properties arising from differences in fibre surface chemistry.     

环氧树脂,酚醛树脂及其复合材料的动态力学表征

用动态力学方法对酚醛树脂和环氧树脂的固化行为进行了表征，讨论了纤维取向对碳纤维增强环氧树脂粘弹行为的影响。     

Processing and characterization of epoxy nanocomposites reinforced by cup-stacked carbon nanotubes

The effect of the dispersion, ozone treatment and concentration of cup-stacked carbon nanotubes on mechanical, electrical and thermal properties of the epoxy/CSCNT nanocomposites were investigated. Ozone treatment of carbon fibers was found to increase the surface oxygen concentration, thereby causing the contact angle between water, epoxy resin and carbon fiber to be decreased. Thus, the tensile strength, modulus and the coefficient friction of carbon fiber reinforced epoxy resin were improved. Moreover, the dispersion of fibers in polymer was increased and the electrical resistivity was decreased with the addition of filler content. The dynamic mechanical behavior of the nanocomposite sheets was studied. The storage modulus of the polymer was increased by the incorporation of CSCNTs. But the glass transition temperature decreased with increasing fiber loading for the ozone treated fiber composites. The ozone treatment did affect the morphology, mechanical and physical properties of the CSCNT.