Effect of colloidal silica on the strength and energy absorption of glass fiber/epoxy interphases

Prior research has demonstrated that fiber-sizings can be designed to yield composite materials that simultaneously possess high energy absorption and structural properties. The improved mechanical properties resulted from control of the fiber surface chemistry and nano-scale topological features within the fiber–matrix interphase. The present study further explains the role of sizing chemistry and surface roughness on composite material performance. Model and commercial glass fiber epoxy specimens were fabricated using these fiber sizing systems resulting in interphase regions with varied surface topology and chemical functionality. Micromechanical measurements were performed using the microdroplet adhesion test method to quantify the fiber–matrix interfacial properties. Improvement in energy absorption and interfacial shear strength due to the presence of the nano-scale silica were quantified. Inspection of the failure modes revealed that the existence of colloidal silica promotes crack propagation along a more tortuous path within the interphase that results in progressive failure and contributes to increased energy dissipation.     

氧化石墨烯改性玄武岩纤维及其增强环氧树脂复合材料性能

为了改善玄武岩纤维/环氧树脂复合材料的界面性能,通过偶联剂对氧化石墨烯进行改性,并将改性后的氧化石墨烯引入到上浆剂中对玄武岩纤维进行表面涂覆改性,同时制备了氧化石墨烯-玄武岩纤维/环氧树脂复合材料.采用FTIR表征了氧化石墨烯的改性效果;运用SEM分析了改性上浆剂处理对玄武岩纤维表面及复合材料断口形貌的影响和作用机制.结果表明:偶联剂成功接枝到氧化石墨烯表面;玄武岩纤维经氧化石墨烯改性的上浆剂处理后,表面粗糙度及活性官能团含量增加,氧化石墨烯-玄武岩纤维/环氧树脂界面处的机械齿合作用及化学键合作用增强,界面黏结强度得到改善,玄武岩纤维的断裂强力提高了30.8%,氧化石墨烯-玄武岩纤维/环氧树脂复合材料的层间剪切强度提高了10.6%.     

上浆剂对国产T700级碳纤维复合材料界面性能的影响

采用扫描电镜(SEM)、原子力显微镜(AFM)、X射线光电子能谱(XPS)等测试方法表征了上浆/未上浆国产T700级(MT700)碳纤维的表面特性,并通过单丝断裂实验测试了单丝复合体系微观界面剪切强度(IFSS),在此基础上研究了碳纤维表面特性对单丝复合体系微观界面性能及其耐湿热性能的影响.研究表明:MT700碳纤维表面上浆剂改善了纤维/基体微观界面强度及其耐湿热性能;湿热环境对复合材料的微观界面性能影响显著,尤其是造成纤维/基体间的化学键合作用破坏,去湿后部分界面性能可恢复.     

Inorganic–organic fiber sizings for enhanced energy absorption in glass fiber-reinforced composites intended for structural applications

Achieving high impact energy absorption without loss of structural performance in a glass fiber-reinforced composite can be obtained through a “materials by design” approach of the fiber matrix interphase through modification of current commercially formulated silane-based fiber sizing packages. In this paper, we document our attempt to balance the structural and impact performance of glass-reinforced composites produced using a fiber-sizing package composed of mixed silane coupling agents to vary the reactivity of the fiber with the matrix phase. Additionally, enhancement of post-failure energy absorption through increased frictional dissipation during fiber–matrix pull-out was explored through control of the surface roughness of the glass fibers. A unique inorganic–organic hybrid fiber sizing formulation was successfully applied at a commercial E-glass manufacturing facility to produce rovings as well as woven fabric reinforcements. Composite materials were manufactured using these specialized fabrics and the preliminary structural and impact energy responses of these materials have been measured.     

水性上浆剂对碳纤维表面及碳纤维/环氧树脂复合材料界面性能的影响

以4,4'-亚甲基双(异氰酸苯酯)(MDI)为扩链剂, 将Triton X-100(TX-100)引入到双酚A二缩水甘油醚(DGEBA) 中, 设计合成水性碳纤维上浆剂(DGEBA-MDI-TX-100), 并利用合成的水性上浆剂对碳纤维表面进行改性。在此基础上, 以环氧树脂为基体, 制备碳纤维/环氧树脂复合材料, 研究了水性上浆剂改性碳纤维对碳纤维表面性能及其复合材料界面性能的影响。结果表明:与未经处理的碳纤维相比, 经过上浆剂改性后的碳纤维润湿性能得到了较大的提高, 与环氧树脂的接触角下降了 9.1%;与环氧树脂复合后制备的复合材料的界面剪切强度提高了64.7%。      

Enhanced mechanical properties of multiscale carbon fiber/epoxy composites by fiber surface treatment with graphene oxide/polyhedral oligomeric silsesquioxane

Graphene oxide (GO) and polyhedral oligomeric silsesquioxane (POSS) grafted carbon fiber (CF) was demonstrated to reinforce the mechanical properties of fiber composites. Such a fiber composite was prepared by grafting POSS onto the CF surface using GO as the linkage. The presence of GO linkage and POSS could significantly enhance both the area and wettability of fiber surface, leading to an increase in the interfacial strength between fibers and resin. Compared with the desized CF composites, the grafted CF composites fabricated by compression molding method exhibited 53.05% enhancement in the interlaminar shear strength. The changed surface morphology, surface composition and surface energy were supposed to be related with the interfacial performance of unidirectional composites, as revealed by scanning electron microscopy, atomic force microscope, dynamic contact angle test and X-ray photoelectron microscopy charaterizations.     

Toughening of carbon fiber-reinforced epoxy polymer composites utilizing fiber surface treatment and sizing

Toughening of fiber-reinforced epoxy composites while maintaining other mechanical properties represents a significant challenge. This paper presents an approach of enhancing the toughness of a DGEBA/mPDA-based carbon fiber-reinforced epoxy composite, without significantly reducing the static-mechanical properties such as flexural properties and glass transition temperature. The impact of combining an UV-ozone fiber surface treatment with an aromatic and aliphatic epoxy fiber sizing on composite toughness is investigated. Carbon fiber-epoxy adhesion was increased as measured by the single fiber interfacial shear test. The Mode I composite fracture toughness was enhanced by 23% for the UV-ozone fiber surface treatment alone. With the addition of an aromatic and aliphatic fiber sizing, the composite fracture toughness was further increased to 50% and 84% respectively over the as-received, unsized fiber. The increased fiber/matrix adhesion also improved the transverse flexural strength.     

Interfacial shear strength of a glass fiber/epoxy bonding in composites modified with carbon nanotubes

In recent years, carbon nanotubes (CNTs) grown on fibers have attracted a lot of interest as an additional reinforcing component in conventional fiber-reinforced composites to improve the properties of the fiber/matrix interface. Due to harsh growth conditions, the CNT-grafted fibers often exhibit degraded tensile properties. In the current study we explore an alternative approach to deliver CNTs to the fiber surface by dispersing CNTs in the fiber sizing formulation. This route takes advantage of the developed techniques for CNT dispersion in resins and introduces no damage to the fibers. We focus on unidirectional glass fiber/epoxy macro-composites where CNTs are introduced in three ways: (1) in the fiber sizing, (2) in the matrix and (3) in the fiber sizing and matrix simultaneously. Interfacial shear strength (IFSS) is investigated using single-fiber push-out microindentation. The results of the test reveal an increase of IFSS in all three cases. The maximum gain (over 90%) is achieved in the composite where CNTs are introduced solely in the fiber sizing.     

单丝断裂能量法研究温度对碳纤维/环氧界面性能的影响

针对两种不同上浆剂碳纤维/高温固化环氧树脂体系, 采用基于WND(Wagner-Nairn-Detassis)能量模型的单丝断裂法, 测试分析了从室温到130 ℃范围内单丝复合体系界面断裂能的变化规律, 研究了碳纤维上浆剂对界面耐热性能的影响, 并结合复合材料层板的短梁剪切性能, 分析了微观和宏观界面性能的关联性。结果表明: 在测试温度范围内, 碳纤维/环氧体系的界面断裂能随温度升高呈先下降而后基本不变的趋势, 去除上浆剂后界面断裂能及其随温度的变化程度与未去除上浆剂的情况存在差异, 说明上浆剂对界面耐热性有重要作用。碳纤维/环氧树脂层板层间剪切强度随温度升高线性下降, 与界面断裂能的变化规律不一致, 这与两种测试方法的原理及界面破坏位置的不同有关。      

不同湿热条件下碳纤维/环氧复合材料湿热性能实验研究

对比研究了环氧5228A树脂及碳纤维/环氧5228A树脂复合材料层合板在3种湿热环境(水煮、70℃水浸,70℃85%相对湿度)下的湿热性能,考察了湿热条件对复合材料层间剪切性能的影响规律,并从吸湿特性、物理化学特性、树脂力学性能、湿应力等方面分析了不同湿热环境下复合材料性能衰减的机制。研究表明,碳纤维/高温固化环氧树脂复合材料层间剪切性能主要是由吸湿率决定,相同吸湿率不同湿热条件下性能的下降幅度基本相同;3种湿热条件下该树脂及其复合材料未发生化学反应、微裂纹等不可逆变化,复合材料层合板湿热老化机制主要是吸入水分后基体增塑和树脂、纤维湿应变不一致导致的湿应力对复合材料性能的负面作用。     

Effects of interphase properties in unidirectional fiber reinforced composite materials

A micromechanical study has been performed to investigate the mechanical properties of unidirectional fiber reinforced composite materials under transverse tensile loading. In particular, the effects of different properties of interphase within the representative volume element (RVE) on both the transverse effective properties and damage behavior of the composites have been studied. In order to evaluate the effects of interphase properties on the mechanical behaviors of unidirectional fiber reinforced composites considering random distribution of fibers, the interphase is represented by pre-inserted cohesive element layer between matrix and fiber with tension and shear softening constitutive laws. Results indicate a strong dependence of the RVE transverse effective properties on the interphase properties. Furthermore, both the damage initiation and its evolution are also clearly influenced by the interphase properties.     

Control of strength anisotropy of metal matrix fiber composites

Summary This paper examines theoretically the stress distribution around fiber breaks in a unidirectional reinforced metal matrix composite, subjected to axial loading when plastic yielding of the matrix is allowed to occur. The composites considered have a ductile interphase, bonding the matrix to the fiber. The likelihood of failure of a fiber adjacent to the existing broken fiber is considered. Detailed and systematic results are given for composites with a wide range of fiber volume fractions, Young's modulus of the fibers and the matrix, interphase properties and Weibull modulus for the strength of the fibers. The objective is the optimization of these material and geometric variables to ensure global load sharing among the fibers in the longitudinal direction, which will give the composite good longitudinal strength. Calculations are carried out for transverse loading of the composite to determine the effect of the ductile interphase on the yield strength. Characteristics of the ductile interphase are determined that will provide good longitudinal strength through global load sharing and a relatively high yield strength in the direction transverse to the fibers. This, in turn, will allow control of the strength anisotropy of uniaxially reinforced metal matrix composites.     

甲基丙烯酰氧基倍半硅氧烷改性碳纤维/聚芳基乙炔复合材料界面性能

利用微脱粘法、三点弯曲法、扫描电镜（SEM）、力调制模式原子力显微镜（AFM）和动态力学热分析（DMTA）研究了甲基丙烯酰氧基倍半硅氧烷（Methacryl-POSS）涂层改性前后的碳纤维增强的聚芳基乙炔（PAA）复合材料的界面性能。用Wilhelmy法研究了处理前后的碳纤维与PAA树脂的浸润性。结果表明: POSS涂层处理后的碳纤维表面粗糙度增大,与PAA树脂的浸润性提高;复合材料的界面剪切强度提高了36%,层间剪切强度提高了50%。DMTA图谱表明, POSS涂层改性后,复合材料的玻璃化转变温度提高了12℃,损耗因子降低了53%,表明复合材料的界面粘接性能得到大幅度的改善。      

上浆剂对炭纤维表面和环氧树脂复合材料的影响

采用两种上浆剂对聚丙烯腈(PAN)基炭纤维进行表面上浆,利用扫描电子显微镜(SEM)、原子力显微镜(AFM)、X射线元素分析(XPS)和反向气相色谱(IGC)研究了未上浆、上浆炭纤维的表面形貌、化学组成及纤维表面能,测试了未上浆和上浆炭纤维所制备复合材料的层间剪切强度(ILSS)并用SEM观察其断面形貌。结果表明,上浆后炭纤维表面变平滑,纤维表面n(O)/n(C)明显提高,含氧官能团(羟基、羧基)增加,炭纤维表面能降低。上浆后,复合材料的ILLS有所提高。     

Investigation on adhesion, interphases, and failure behaviour of cyclic butylene terephthalate (CBT)/glass fiber composites

Interphases exist in hybrid materials and significantly influence their mechanical performance. To find a bridge between the microscopic and macroscopic mechanical properties, this work investigates the microscopic nature of glass fiber surfaces and glass/CBT interphases in terms of topography, fractography, and adhesion properties. The variations in glass fiber surface properties result from the different sizings. Using the single fiber pull-out test, AFM, and ζ potential tests, it is shown that the interfacial bond strengths in CBT resin composites can vary depending on the kind of sizing formulation and properties. The greatest adhesion strength is achieved by aminosilane sizings with epoxy resin film former. The surface roughness of the fibers can be varied by sizings with different content and ζ potential values, which has no significant contribution to interphase adhesion strength from ‘mechanical interlocking’. For the systems with film formers, cohesive failure occurs and similar values of both interfacial adhesion strength, τ_d, and fracture energy release rate, G_ic, are obtained, in which τ_d approaches the shear yield strength of CBT matrix. A further enhancement of interfacial adhesion is limited by the mechanical properties and the non-homogeneous microstructure of CBT resin due to the less-than-perfect CBT polymerization.     

超高分子量聚乙烯(UHMWPE)纤维表面处理对UHMWPE/环氧树脂复合材料界面性能的影响机制

从工程化应用角度研究了常压空气等离子体改性对超高分子量聚乙烯（UHMWPE）纤维/环氧树脂复合材料界面性能的调节机制,主要分析了不同处理时间对UHMWPE纤维表面状态变化的影响,及其对UHMWPE/环氧树脂复合材料界面黏结性能的影响规律。采用SEM及纤维吸水测试研究了等离子体处理对UHMWPE纤维表面物理形貌及纤维表面浸润性能的影响,分别以拉伸和弯曲的方式,通过纤维表面脱黏力及层合板层间剪切强度对UHMWPE/环氧树脂复合材料的界面黏结性能进行表征。结果表明,仅经过4 s的空气等离子体处理之后,UHMWPE纤维表面脱黏力的提高幅度为84.0%,UHMWPE/环氧树脂复合材料层合板的层间剪切强度由未处理的7.01 MPa提高至15.81 MPa,增幅高达125.5%。研究发现,通过常压空气等离子体处理改变了UHMWPE纤维的表面状态,可以显著高效地调节UHMWPE/环氧树脂复合材料的界面性能,为扩大该材料的后续工程化应用提供了理论基础。      

Improving the interfacial property of carbon fiber/vinyl ester resin composite by grafting modification of sizing agent on carbon fiber surface

The poor interfacial adhesion between carbon fibers (CFs) and vinyl ester resin (VE) has seriously hampered the application of CFs/VE composites. In this work, the interfacial adhesion was efficiently enhanced by grafting acrylamide with epoxy sizing agent on CFs surface. The grafting reaction was feasible according to the thermodynamic calculation. The optimal grafting condition was 80 °C for 10 min based on the kinetic investigation by differential scanning calorimeter. Surface morphology and surface composition of modified carbon fibers (MCFs) were characterized, which indicated that acrylamide was grafted successfully on CFs surface and the surface roughness was increased slightly. After grafting, the interface shear strength of MCFs/VE composites was significantly improved by 86.96% and the interlaminar shear strength was enhanced by 55.61% due to the covalent bonds in interphase and the toughening effect of sizing gent. Moreover, the static and dynamic mechanical properties of composites with different interfacial adhesion were measured, which further confirmed the effect of the grafting modification.     

聚乙烯醇交联改性对天然纤维增强聚丙烯复合材料性能的影响

采用聚乙烯醇(PVA)交联对洋麻(KF)增强聚丙烯(PP)、棕榈(PF)增强聚丙烯(PP)复合材料进行改性,通过模压成型工艺制备KF/PP和PF/PP复合材料。研究不同交联方法对复合材料的结构和性能的影响,采用SEM、DMA等技术研究了改性对复合材料的界面结合及力学性能影响。结果表明:PVA协同偶联剂交联改性对天然纤维/PP复合材料的综合改性效果最好,当用5%PVA+3%偶联剂对KF/PP改性时,KF/PP复合材料的弯曲强度提升25.2%,弯曲模量提升35.49%,剪切强度提升28%,分别达到了50.90 MPa、5.76 GPa、5.4MPa。当用5%PVA+2%偶联剂对PF/PP改性时,PF/PP复合材料的弯曲强度提升31.46%,弯曲模量提升27.07%,剪切强度提升21.75%,分别达到44.33MPa、2.32GPa、5.18MPa。改性后KF/PP、PF/PP复合材料的含水率分别下降了46.89%、10.63%,吸水率分别下降了8.57%、6.12%。KF/PP改性后储能模量提高20.93%,PF/PP改性后Tg值由90.1℃上升到113.8℃。SEM表明:PVA协同偶联剂交联改性有效改善了纤维与PP间的粘结,纤维与PP间的界面结合得到改善。     

Characterization of the interfacial bond between old concrete substrate and ultra high performance fiber concrete repair composite

The interfacial bond characteristics between normal concrete substrate as old concrete and ultra high performance fiber concrete as repair material have been investigated. Normal concrete substrates were first subjected to different surface preparation methods prior to bonding the ultra high performance fiber concrete to form repair composites. The interfacial mechanical bond of the composites was assessed using slant shear and tensile splitting strength tests. In addition, rapid chloride permeability test was performed to ascertain the potential chloride resistance of the composites. The microstructure of the transition zone between the normal concrete and ultra high performance fiber concrete was also studied using scanning electron microscope. The results generally indicate that surface preparation of the substrate is very much required to obtain superior mechanical bond of the composites; whereby the composites with the sand-blasted substrate providing the most superior mechanical bond. The excellent bond of the composite is also evident through the rapid chloride permeability test, as well as confirms by the scanning electron microscope image of the interface. Hence, the ultra high performance fiber concrete exhibits significant potential as an excellent material for repair and rehabilitation of concrete structures.     

Interphase study in cyanate/glass fibre composites using thermomechanical analysis and micro-thermal analysis

Fibre/matrix interphase has a dramatic influence on the composite performances. For the best understanding of interfacial phenomena, sizing has been characterized “in situ” by dynamic mechanical analysis, and sizing extract part, by different techniques. To know sizing impact on interphase nature and properties in the composite, four types of samples have been realized: three composites, which have been elaborated according to the technique of vacuum molding and differed by sizing state, and neat resin samples. The dynamic mechanical analysis (DMA) has allowed us to study both these composites and their interphases. Moreover, micro-thermal analysis has been a good technique for interphase investigation in our composites.