Elevated‐temperature vacuum‐assisted resin transfer molding process for high performance aerospace composites

Vacuum‐assisted resin transfer molding (VARTM) is commonly used for general temperature applications (<150 °C) such as boat hulls and secondary aircraft structures. With growing demands for applications of composites in elevated temperature environments, significant cost savings can be achieved by employing the VARTM process. However, implementation of the VARTM process for fabricating elevated temperature composites presents unique challenges such as high porosity and low fiber volume contents. In the present work, a low cost and reliable VARTM process is developed to manufacture elevated temperature composites for aerospace applications. Modified single vacuum bagging infusion and double vacuum bagging infusion processes were evaluated. Details of the method to obtain high quality composite parts and the challenging issues related to the manufacturing process are presented. Density and fiber volume fraction testing of manufactured panels showed that high quality composite parts with void content less than 1% have been consistently manufactured. A property database of the resin system and the composites was developed. A three‐dimensional mathematical model has also been developed for flow simulation and implemented in the ABAQUS finite element package code to predict the resin flow front during the infusion process and to optimize the flow parameters. The results of the present study indicate that aircraft grade composite parts with high fiber volume fractions can be manufactured using the developed elevated temperature VARTM process. © 2013 Society of Chemical Industry     

Interlaminar fracture toughness behavior of electron‐beam cured carbon‐fiber reinforced epoxy–resin composites

The work describes the preparation and physical‐mechanical characterization of unidirectional CFRP panels manufactured by an electron beam curing technique. Delamination fracture toughness in Mode I and II is investigated in order to evaluate the influence of fiber–matrix adhesion strength, matrix toughness and matrix crosslinking density as determined by the radiation curing process. A matrix system comprising a DGEBA epoxy monomer and an initiator of cationic polymerization have been used, with one batch of resin mixed with a PES monomer in order to enhance matrix toughness. Curing was achieved with a pulsed 10 MeV Electron Beam accelerator. Thermally cured composite systems have also been manufactured and tested for comparison. Results from double cantilever beam and end notched flexure delamination tests have been analyzed and correlated with results from short beam shear, dynamic mechanical thermal analysis tests and SEM micrographs of delaminated surfaces. POLYM. COMPOS., 35:1529–1542, 2014. © 2013 Society of Plastics Engineers     

Three‐dimensionally braided carbon fiber–epoxy composites,a new type of materials for osteosynthesis devices. II. Influence of fiber surface treatment

Interfacial adhesion between carbon fiber and epoxy resin plays an important role in determining performance of carbon–epoxy composites. The objective of this research is to determine the effect of fiber surface treatment (oxidization in air) on the mechanical properties (flexural strength and modulus, shear and impact strengths) of three‐dimensionally (3D) braided carbon‐fiber‐reinforced epoxy (C_3D/EP) composites. Carbon fibers were air‐treated under various conditions to improve fiber–matrix adhesion. It is found that excessive oxidation will cause formation of micropits. These micropits are preferably formed in crevices of fiber surfaces. The micropits formed on fiber surfaces produce strengthened fiber–matrix bond, but cause great loss of fiber strength and is probably harmful to the overall performance of the corresponding composites. A trade‐off between the fiber–matrix bond and fiber strength loss should be considered. The effectiveness of fiber surface treatment on performance improvement of the C_3D/EP composites was compared with that of the unidirectional carbon fiber–epoxy composites. In addition, the effects of fiber volume fraction (V_f) and braiding angle on relative performance improvements were determined. Results reveal obvious effects of V_f and braiding angle. A mechanism was proposed to explain the experimental phenomena. © 2002 Wiley Periodicals, Inc. J Appl Polym Sci 85: 1040–1046, 2002     

Effect of compaction treatment on laminated CFRP composites fabricated by vacuum‐assisted resin‐transfer molding

Carbon fiber‐reinforced polymer (CFRP) composites were fabricated using ordinary and compaction setups (OS and CS, respectively) in the vacuum‐assisted resin‐transfer molding (VARTM) process. The mechanical properties and acoustic emission (AE) spectra of the CFRP composites were compared among fabricated samples. The CFRP plates with sequences of [+30/−30]₆ were sectioned to make specimens for Mode I interlaminar fracture tests and three‐point bending tests. The difference between the material properties and AE characteristics of the OS and CS specimens were statistically compared using one‐way analysis of variance. The OS specimens had a thicker resin layer, a higher resin fraction, larger average fracture toughness, and AE energy corresponding to the Mode I fracture, whereas the CS specimens had more macro‐scale voids and higher bending strength. AE analysis showed that frequency bands in the interlaminar fracture tests corresponding to matrix‐related fracture were dominant for the OS specimens, whereas those corresponding to the mixed fracture mode of the fiber and matrix fracture were dominant for the CS specimens. In the bending tests, mixed fiber‐matrix fractures were dominant for the OS specimens, and fiber‐related fractures were dominant for the CS specimens. In conclusion, the compaction treatment diminished interlaminar fracture toughness, due to the enhanced formation of macro‐scale voids around the fiber bundles during the resin impregnation stage. However, the bending strength improved with an increased fiber volume fraction. POLYM. COMPOS., 38:217–226, 2017. © 2015 Society of Plastics Engineers     

聚乙二醇/氯化锌条件下回收CFRP方法研究

以真空辅助成型工艺(VARI)制作的碳纤维增强复合材料(CFRP)平板件为降解试件,使用乙酸对其进行分层预处理,然后以聚乙二醇为溶剂,氯化锌为催化剂,采用控制变量法在不同的反应温度、反应时间,氯化锌浓度等工艺参数下对CFRP进行降解回收。利用扫描电子显微镜、X射线光电子能谱仪、动态接触角测量仪、纤维强度仪对回收碳纤维的表面形貌和元素、浸润性以及力学性能进行表征分析。结果表明,CFRP降解的理想工艺条件为:用乙酸于120℃下分层预处理30 min,然后在190℃下,使用浓度为0.6 mol/L氯化锌/聚乙二醇环境反应60 min。使用该方法回收的CFRP,树脂降解率能达到98%以上,碳纤维表面干净光滑无树脂残留,表面元素与原丝相比变化较小,碳纤维和水与乙二醇的浸润性相比原丝得到改善,碳纤维的弹性模量达到原丝的98%以上,拉伸强度达到原丝的97%以上。     

Chemical recycling of carbon fiber reinforced plastic using supercritical methanol

Advanced chemical recycling of carbon fiber reinforced plastic (CFRP) was developed using supercritical methanol. In this method, the thermosetting epoxy resin in CFRP was converted to a thermoplastic resin by the selective decomposition of the bridged structure by supercritical methanol at 270 °C and 8 MPa for 90 min and the resin dissolved in supercritical methanol. On the other hand, the carbon fiber was fully recovered from CFRP without the plastic component and it had no thermal damage. The bridged structure in the epoxy resin could be formed again by adding a cross-linker to the recovered thermoplastic resin and the thermosetting resin was reproduced. This was the first attempt on the recycling of thermosetting epoxy resin. However, in order to maintain the strength of the recycled epoxy resin to that of virgin epoxy resin, the proper ratio of the recovered thermoplastic resin to virgin epoxy resin was determined. The recovered carbon fiber from CFRP maintained the shape of the plain fabric and the reduction of the tensile strength was less than 9% compared with the virgin one. The recovered carbon fiber could be used to make a recycled CFRP with epoxy resin and cross-linker, the strength of which was close to that of virgin CFRP.     

碳纤维复合材料缠绕制品抗外压性能研究

研究了树脂基体模量、缠绕角和厚度对碳纤维复合材料缠绕制品抗外压性能的影响。实验结果表明:采用MNA共混PMDA固化环氧树脂并调整PMDA含量可以有效改变树脂模量,随着PMDA含量的增加,树脂模量提高。当PMDA含量仅为MNA的5%时,树脂模量从3.71 GPa增加到4.18 GPa,提高了13%;当PMDA含量为MNA的10%时,模量达到最大值,为4.61 GPa,提高了24%。随着基体模量增加,单向CFRP的压缩强度、剪切强度和环刚度均先增加后减少。当基体模量为4.18GPa时,CFRP的压缩强度和剪切强度均达到最大值,分别为655 MPa和71.6 MPa,提高了16%和12%。此时,缠绕管环刚度达到最大值,为277 k N/m~2,提高了87%;同时增加缠绕角和厚度能够提高缠绕管的抗失稳能力。     

Fabrication of C/C-SiC composites using high-char-yield resin

Carbon fiber reinforced ceramic matrix composites (C/C-SiC composites) were fabricated using a type of high-char-yield phenolic resin with the char yield of 81.17 wt.%. Firstly, the fabric prepreg was prepared by spreading the phenolic resin solution onto the two dimensional carbon fiber plain weave fabric and dried consequently. Afterward, the resin was cured and then the carbon fiber reinforced polymer (CFRP) was pyrolyzed to get amorphous carbon. Finally, C/C-SiC composites were obtained through liquid silicon infiltration (LSI) process. SEM micrographs showed that the Si/SiC area was homogeneously dispersed in the matrix, and during the siliconization process, a layer of SiC was formed along the surface of carbon fibers or carbon matrix. The fiber volume of CFRP was about 40 vol.%, which was much lower than other studies. XRD result indicated that only β-SiC type was formed. The result of X-ray computed tomography clearly showed the structure changes before and after the melt infiltration process. Mechanical property test showed that the composites had fracture strength of 186 ± 23 MPa, and a flexural modulus of 106 ± 8 GPa.     

Surface treatment of CFRP composites by Ar+ irradiation to improve bonding strength between aluminum and CFRP composites

The effect of surface treatment of carbon fiber reinforced plastic (CFRP) composites on the T-peel strength and the shear strength between CFRP and aluminum panels was studied. The surface of the composite panel was treated with Ar⁺ irradiation under oxygen environment. The optimal Ar⁺ ion dose was determined by measuring the changes of contact angle and surface energy as a function of ion dose. T-peel tests and SLS tests were performed using irradiated CFRP/aluminum specimens and unirradiated CFRP/aluminum specimens to determine the treatment effect by Ar⁺ irradiation under oxygen environment on the T-peel strength and shear strength of CFRP/aluminum composites. The results showed that contact angle on the surface of the composite panel was reduced from ∼80° to ∼8° and the surface energy increased from 31 ergs/cm² to 72.4 ergs/cm² with an ion dose of 10¹⁷ ions/cm². T-peel strength and shear strength are significantly affected by the surface treatment of composite panel. T-peel strength and shear strength improved 650% and 56%, respectively, when the treatment was made with an ion dose of 10¹⁶ ions/cm². SEM examination showed that the improvement of bonding strength was attributed to the uniform spread and fracture of epoxy adhesive.     

Properties of UHMWPE fiber-reinforced composites

Based on our previous work, a new thermosetting resin system, named PCH, has been developed to be used as the matrix of ultrahigh-molecular-weight polyethylene (UHMWPE) fiber composites in order to get improved interface bond and mechanical properties. In this work, UHMWPE fiber/PCH composites with different ratios of PCH/styrene were prepared and the impact resistance, dynamic mechanical properties, and dielectric properties of UHMWPE fiber/PCH composites were investigated. The interlaminar shear failure characteristic of composites was analyzed by introducing a series of energy indexes indicating the energy absorbed in interlaminar shear failure process, which show good correlation with interlaminar shear strength of samples. UHMWPE fiber/PCH composites have excellent impact property, and the impact strength can reach 140.8 kJ/m² as the ratio of PCH/styrene is 60/40. Dynamic mechanical analysis showed that UHMWPE fiber/PCH composites have high storage moduli (E′) and low dissipation factor (tan δ) and these properties are influenced by the interfacial adhesion. The dielectric property test demonstrated that UHMWPE fiber/PCH composites have low dielectric constant (2.20 < ε′ < 2.55) and dielectric loss tangent (1.50 × 10^?3 < tan δ < 1.81 × 10^?2) and show good stability in a large range of frequency and temperature.     

The Effect of Resin Matrix Composition on Mechanical Properties of E-glass Fiber-Reinforced Composite for Dental Use

The effects of resin matrix composition including bis-phenol-A-diglycidyl dimethacrylate (bis-GMA)-methyl methacrylate (MMA) based or urethane dimethacrylate (UEDMA)-triethylene glycol dimethacrylate (TEGDMA) based composition and storage conditions on the mechanical properties of E-glass fiber-reinforced composites (FRCs) were studied. Three experimental groups ('Exper 1', 'Exper 2', 'Exper 3') with differing UEDMA to TEGDMA ratio in the matrix together with a control group ('Control') based on bis-GMA–MMA resin matrix were prepared by light-curing. The storage conditions for each group were dry storage at room temperature for 24 h and 30- and 60-day immersion in deionized (DI) water at 37°C, which further divided each group into three subgroups. For all the four composition groups, mechanical properties including hardness, flexural strength and modulus in both three-point and four-point bendings were tested (n = 6), together with water sorption and solubility study (n = 6) and fracture site scanning with a scanning electron microscope (SEM). The experimental specimens were relatively strong and stiff in three-point bending compared to previous research. The same specimens in three-point bending had a lower flexural modulus and fractured at higher flexural stress than in four-point bending. According to the SEM images after fracture, some resin matrix was still bound to the fiber surface, showing cohesive–interfacial fracture type and relatively stable matrix–fiber adhesion. According to comprehensive analysis, the control group showed superior mechanical performance in most of the tests.     

Impact of nanoparticles on the process-induced distortions of carbon fiber reinforced plastics: An experimental and simulative approach

This article investigates the potential of aluminum oxide nanoparticles for the reduction of process-induced distortions of carbon fiber reinforced plastics (CFRP). Therefore the matrix properties, which affect the distortions, are experimentally and mechanistically analyzed in detail at various particle contents. The results clearly show an increasing impact of raised particle content on gelation, chemical and thermal shrinkage, on Young's modulus, as well as on Poisson's ratio. These alterations can be successfully transferred to reduce spring-in of L-shaped CFRP brackets, which are manufactured by infusion technology. However, it is found that particle contents higher than 5 wt % are needed to influence these parameters. For further understanding of the parameters controlling spring-in, a numerical sensitivity analysis is performed by the correlation of various matrix parameters and the induced distortions. The results from a structural simulation reveal that changes in thermal and chemical shrinkage as well as in gelation have a major impact on the distortions, but the modes of action of the particles also have to be taken into consideration. These mechanistical insights about nanoparticle impacts might be a valuable approach to lower or overcome distortions in composite materials in the future. © 2018 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2019 , 136, 47031.     

Use of an epoxidized oil‐based resin as matrix in vegetable fibers‐reinforced composites

Hemp fibers were used as natural reinforcement in composites of thermosetting vegetal oil based resin. Boards with fibers content from 0 to 65 vol % were produced by hot pressing. The mechanical properties were investigated with flexural testing. The effect of effect has been observed on both modulus and strength, indicating a good fiber–matrix interfacial adhesion, which was confirmed by means of scanning electron microscopy observations. Dynamic mechanical analysis also showed an important reinforcement effect in the polymer rubbery region, where at 180°C the storage modulus increased from 17 MPa for the neat resin to 850 MPa for 65 vol % fiber content composites. It also revealed an glass transition temperature decrease when fiber amount in the composite increased. Additional experiments based on differential scanning calorimetry show a weakly accelerated cure when fibers content increases, which usually lead to a lower T_g. But, this phenomenon alone cannot explain the observed T_g change. Contact angle on hemp evolution with time for the resin components show that anhydride is totally absorbed after a few seconds, whereas contact angle of epoxydized oil decreases slowly. This indicates probably a preferential anhydride absorption that leads to a lower amount of anhydride in the matrix and as a consequence to a reduced T_g. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 101: 4037–4043, 2006     

Improving the interlaminar shear strength and thermal conductivity of carbon fiber/epoxy laminates by utilizing the graphene-coated carbon fiber

The poor interlaminar properties restrict the application of carbon fiber reinforced polymer (CFRP) composites. In this work, a novel method for fabricating a graded interface structure is developed to improve the through-thickness thermal conductivity of CFRP composites. High-strength graphene nano-plates (GnP) and phenolic resin (PF) were selected to deposit on the surface of carbon fiber to design a novel CF/Epoxy laminates, where a simultaneous improvement of interlaminar shear strength (ILSS) and through-thickness thermal conductivity was observed. With addition of 1 wt % of GnP-PF in CF, 37.04% increase of the ILSS, and 16.67% enhancement of thermal conductivity compared to the original CFRP. The mechanism for improvement of both ILSS and thermal conductivity was studied by scanning electron microscopy and nano-indentation, where a better interface formed by GnP-PF has been clearly observed. © 2018 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2019 , 136, 47061.     

碳纤维树脂基复合板料的铺层方式对低速冲击性能的影响

为研究碳纤维增强树脂基复合材料(CFRP)板铺层方式对低速冲击性能的影响,设计了一系列CFRP板的冲击试验。对CFRP板的铺层方式、冲击能量的形式进行调节和改变,获取CFRP板在各种条件下的低速冲击行为;再通过冲击实验和超声波扫描的方法研究冲击过程中CFRP板的铺层方式和冲头质量对碳纤维树脂基复合材料板冲击性能的影响。结果表明,在15 J的低能量作用下冲击CFRP板时,冲头的质量越大,该板对能量的吸收率越大,损伤面积也越大;相同能量和相同冲头质量的冲击情况下,铺层方式为[0°/45°/90°/-45°]_2的抗冲击性能最好。CFRP板的冲击载荷、能量吸收和损伤形态与冲击能量的大小以及冲头动量密切相关。     

The permeability and compressibility of aligned and cross-plied carbon fiber beds during processing of composites

Two of the most important input parameters needed to simulate the processing of continuous fiber laminated composites are the fiber bed permeability and the portion of the autoclave load borne by the consolidating fiber network (compressibility). In this study we have experimentally examined how both these parameter change with resin volume fraction as pressure is applied and consolidation proceeds. For a unidirectional fiber bed, the Kozeny-Carman equation can be used to predict both the transverse (perpendicular to the laminate plies) permeability (Kozeny constant, K′_z = 11) and the axial (parallel to the fibers) permeability (Kozeny constant, K′_X = 0.57). The axial permeability was found to be dependent on the surface tension of the permeant. For a unidirectionally aligned fiber, the measured transverse permeabilities varied from 1.1 × 10^?10 cm² to 12. × 10^?9 cm² while the axial values varied from 2.1 × 10^?9 to 4.4 × 10^?8 cm² for a liquid volume fraction range of 0.25 to 0.5. Axial permeability measurements indicate that the permeability decreases with increasing off-axis angle × (measured from the laminate axial direction). The off-axis permeability behavior can be described by a modified Kozeny-Carman equation. The fiber network compressibility can be described with a logarithmic relation which has been found valid for a large number of consolidated soils.     

激光处理对CFRP与铝胶接性能的研究

碳纤维增强复合材料(CFRP)具有轻质高强的特点,被广泛应用于汽车、航空航天、建筑等领域。但CFRP表面惰性高,使得CFRP与其他异质材料复合时的胶接强度低,不能满足使用。采用激光(光纤激光器)对CFRP进行表面处理后,再与铝进行胶接测试。利用SEM、接触角测试和光学轮廓仪测试对不同脉宽的激光处理后的CFRP表面形貌、表面能、表面粗糙度进行研究。结果表明,随脉宽增加,处理后的CFRP表面树脂残留量减少,表面粗糙度增加,表面自由能也相应增加。对比激光处理与机械打磨两种方式与铝的胶接性能发现,激光处理的CFRP与铝的胶接强度比未处理提高了1.95倍,比打磨处理提高了1.02倍。对其胶接断面进行分析可知,激光处理试样的断裂模式主要为纤维撕裂破坏。     

GFRP填料塔的设计

以双酚A型不饱和聚酯，胶衣树脂为基体树脂，玻璃纤维表面毡，玻璃布，短玻璃纤维毡为增强材料，制备了玻璃纤维增强塑料（GFRP）填料塔。论述了基体树脂，增强材料的选择，GFRP塔的结构设计，强计计算和手糊成型，组装的工艺要求。应用结果表明，该GFRP填料完全可满足硫酸生产净化工艺的使用要求。     

Influence of the fiber surface properties on the mechanical strength of unidirectional fiber composites

The influence of the thermodynamic adhesion between fibers and matrix on the mechanical properties of a continuous fiber reinforced composite is studied for two systems: carbon fiber reinforced poly(ether ether ketone) and glass fiber reinforced poly(ether imide). The fibers are modified chemically and characterized by measuring the contact angle formed by molten resin on the fibers. Various fiber treatments yield a wide range of contact angles, which are determined optically. Unidirectional fiber reinforced laminates are manufactured and transverse flexural strength is measured with the values reported as a function of the specific work of adhesion. It is shown that adhesion at the fiber-resin interface correlates with both the composite strength and the void morphology within the laminate after consolidation.     

The Use of Dynamic Mechanical Methods to Study the Effect of Absorbed Water on Temperature-dependent Properties of an Epoxy Resin-Carbon Fibre Composite

Dynamic mechanical methods were used to study the effect of absorbed moisture on the properties of an epoxy resin matrix CFRP. The glass transition temperature (T_g)of the matrix resin, determined as the onset of the characteristic fall in dynamic modulus with increasing temperature, was found to decrease with increasing moisture content. Maximum shifts in T_g of 80 to 90°C, relative to the dry material, were observed for a resin moisture content of 5.2% by weight. The effects of sample geometry, fibre orientation, and frequency of oscillation, on the dynamic mechanical properties are discussed. Results are given of an analysis of the observed dependence of T_g on water content using two theoretical models.