A study of the effect of oxygen plasma treatment on the interfacial properties of carbon fiber/epoxy composites

In this work, effects of the interface modification on the carbon fiber‐reinforced epoxy composites were studied. For this purpose, the surface of carbon fibers were modified by oxygen plasma treatment. The surface characteristics of carbon fibers were studied by X‐ray photoelectron spectroscopy (XPS), atomic force microscopy (AFM), dynamic contact angle analysis (DCAA), and dynamic mechanical thermal analysis (DMTA), respectively. The interlaminar shear strength (ILSS) was also measured. XPS and AFM analyses indicated that the oxygen plasma treatment successfully increased some oxygen‐containing functional groups concentration on the carbon fiber surfaces, the surface roughness of carbon fibers was enhanced by plasma etching and oxidative reactions. DCAA and DMTA analyses show that the surface energy of carbon fibers increased 44.9% after plasma treatment for 3 min and the interfacial bonding intensities A and α also reached minimum and maximum value respectively. The composites exhibited the highest value of ILSS after oxgen plasma treated for 3 min. © 2010 Wiley Periodicals, Inc. J Appl Polym Sci, 2010     

Effect of MWCNTs irradiation grafting treatment on the surface properties of PBO fiber

The aim of this article is improved the surface properties of Poly[p‐phenylenebenzobisoxazole] (PBO) fiber with epichlorohydrin hybridized carboxylic multi walled carbon nanotubes (MWCNTs‐Ecp) grafting by using γ‐ray irradiation technology. The surface chemical properties, the surface morphology, the amount of the grafted MWCNTs on PBO fiber and the surface free energy of PBO fibers have been analyzed. The results show that MWCNTs‐Ecp have been grafted on the surface of PBO fiber by γ‐ray irradiation treatment. The surface chemical inertness and the surface smoothness of PBO fiber are significantly improved by grafting MWCNTs‐Ecp chains, the amount of the grafted MWCNTs on PBO fiber is about 11.9%, and the surface free energy of PBO fiber has an increase of 42.6% by generating some active groups such as ? COOH, ? OH, and ? C? Cl on the surface of PBO fiber. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2011     

Comparative study on electrical properties of orientated carbon nanotubes/epoxy composites

The percolation threshold of carbon nanotubes (CNTs)/epoxy resin composites was simulated in the Bruggeman' Effective‐Medium Theory based on experiment. Both distinct percolation effect and low percolation threshold in the aligned CNTs/epoxy composites were predicted. With the CNTs loading larger than the percolation threshold, the critical exponent of CNTs/epoxy composites rises rapidly with the increase of aspect ratio of CNTs. It is shown that the electrical conductivity of composites presents distinct aeolotropism, the percolation threshold is sensitive relative to the tiny change of the orientation factor, the aspect ratio, and the structure of CNTs in the composites matrix. The simulated results are consistent with the experimental results basically, and the discrepancy between simulated results and experimental results has been interpreted reasonably. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2012     

Study on the interfacial properties of two‐dimensionally arranged glass fiber/epoxy resin model composites

The effect of interfiber distance on the interfacial properties in two dimensional multi‐E‐glass fiber/epoxy resin composites has been investigated using fragmentation test. In addition, the effect of the fiber surface treatment on the interfacial properties has been studied. We found that the interfacial shear strength decreased with the decreasing interfiber distance at the range of <50 μm and the extent of the decreasing was more serious as the increasing of the number of adjacent fiber. This is probably that the interface between the fiber and the resin was damaged by the breaking of adjacent fibers and the damage increased with minimizing the interfiber spacing and the number of adjacent fibers. We can guess that interfacial shear strength in real composites is much smaller than that of multifiber fragmentation sample with touched fiber. When the interfiber distance was >50 μm, the interfacial shear strengths were saturated regardless of fiber surface treatment and were in close agreement with those of the single fiber fragmentation test. Finally, the interfacial shear strength evaluated using two dimensional fragmentation tests are shown as real values in‐site regardless of fiber surface treatment, interfiber distance, and existing matrix cracks. © 2005 Wiley Periodicals, Inc. J Appl Polym Sci 99: 1541–1551, 2006     

Study on the interfacial properties of three‐dimensionally arranged glass fiber/epoxy resin model composites

The effect of interfiber distance on the interfacial properties in three‐dimensional multi‐E‐glass fiber/epoxy resin composites has been investigated using fragmentation test. In additions, the effect of the fiber surface treatment on the interfacial properties has been studied. The interfacial shear strength decreased with the decreasing the interfiber distance at the range of under 50 μm and the extent of the decreasing was more serious as the increasing of the number of adjacent fiber. This is probably due to the fact that the interface between the fiber and the resin was damaged by the adjacent fiber breaks and the damage increased with closing the interfiber spacing and the number of adjacent fiber. It was found that the interfacial shear strengths saturated when the interfiber distance was over 50 μm, the ones were saturated regardless of fiber surface treatment and the ones were in close agreement with those of the single fiber fragmentation test. Finally, the interfacial shear strength evaluated using three‐dimensional fragmentation tests are shown as real values in‐site regardless of fiber surface treatment, interfiber distance and existing of matrix cracks. © 2010 Wiley Periodicals, Inc. J Appl Polym Sci, 2010     

Effects of fiber surface grafting by functionalized carbon nanotubes on the interfacial durability during cryogenic testing and conditioning of CFRP composites

Carbon fiber reinforced epoxy (CE) composite is ideal for a cryogenic fuel storage tank in space applications due to its unmatched specific strength and modulus. In this article, inter-laminar shear strength (ILSS) of carbon fiber/epoxy (CE) composite is shown to be considerably improved by engineering the interface with carboxyl functionalized multi-walled carbon nanotube (FCNT) using electrophoretic deposition technique. FCNT deposited fibers from different bath concentrations (0.3, 0.5, and 1.0 g/L) were used to fabricate the laminates, which were then tested at room (30°C) and in-situ liquid nitrogen (LN) (−196°C) temperature as well as conditioning for different time durations (0.25, 0.5, 1, 6, and 12 h) followed by immediate RT testing to study the applicability of these engineered materials at the cryogenic environment. A maximum increment in ILSS was noticed at bath concentration of 0.5 g/L, which was ~21% and ~ 17% higher than neat composite at 30°C and − 196°C, respectively. Short-term LN conditioning was found to be detrimental due to developed cryogenic shock, which was further found to be compensated by cryogenic interfacial clamping upon long-term exposure.     

多壁碳纳米管／环氧树脂复合材料性能研究

采用物理机械方法与化学方法相结合的手段,制备了多壁碳纳米管（MWNTS）／环氧树脂（Epoxy）复合材料。通过力学拉伸试验测试了MWNTs/Epoxy复合材料拉伸强度和拉伸模量与MWNTS添加量的关系,利用扫描电镜（SEM）分析了MWNTS／Epoxy复合材料的拉伸断面,并用表面电阻测试仪对所制备的碳纳米管复合材料进行了电学性能测试。结果表明：经过化学酸化的方法处理后的MWNTS在复合材料中的分散得到了改善,力学性能也得到了明显的提高,但酸处理后的复合材料的电学性能明显低于未处理的复合材料。     

微脱黏法在碳纤维/环氧树脂界面性能评价中的应用

利用微脱黏法测定碳纤维/环氧树脂复合材料的界面剪切强度,并分析了造成测试结果分散的影响因素.结果表明:在脱黏过程中,最大脱黏力随碳纤维埋人环氧树脂内长度的增加而线性递增,当埋人长度超过一定值后最大脱黏力趋于稳定:碳纤维与环氧树脂间的接触角对复合材料界面剪切强度有一定影响,接触角越大,界面剪切强度越高;测试结果的分散性与树脂微球的半月板区域、钳口区等因素有关;未经表面处理的碳纤维增强环氧树脂复合材料的界面剪切强度仪为39.4 MPa,低于处理后的复合材料(60.6 MPa).     

Increasing the interfacial strength in carbon fiber/epoxy composites by controlling the orientation and length of carbon nanotubes grown on the fibers

Multi-walled carbon nanotubes (MWCNTs) were grafted onto carbon fibers (CFs) using an injection chemical vapor deposition method. The orientation and length (16.6–108.6 μm) of the MWCNTs were controlled by the surface treatment of the CFs and the growth time, respectively. The interface between the MWCNTs and the CFs indicated the grafted CNTs were immobilized by embedding catalyst on CFs. Two orders of magnitude increase in the specific surface areas of CFs was obtained by grafting the MWCNT. MWCNT–CF hybrids exhibited good wettability with the epoxy resin due to the surface roughness and capillary action. Single-fiber composite fragmentation tests revealed an remarkable improvement of interfacial shear strength (IFSS) controlled by the orientation and length of MWCNTs. MWCNTs with an perpendicular alignment and long length showed a high IFSS in epoxy composites due to better wettability and a large contact interface between the hybrids and the resin. Hybrids with an optimum length (47.2 μm) of aligned MWCNTs showed a dramatic improvement of IFSS up to 175% compared to that of pristine CFs.     

Influence of fiber modification on interfacial adhesion and mechanical properties of pineapple leaf fiber‐epoxy composites

Three kinds of surface treatment, that is, the alkalization (5% w/v NaOH aqueous solution), the deposition of diglycidyl ether of bisphenol A (DGEBA) from toluene solution (1% w/v DGEBA), and the alkalization combined with the deposition of DGEBA (5% w/v NaOH/1% w/v DGEBA) were applied to modify interfacial bonding and to enhance mechanical properties of pineapple leaf fiber (PALF) reinforced epoxy composites. The fiber strength and strain were measured by single fiber test and the fiber strength variation was assessed using Weibull modulus. Furthermore, a fragmentation test was used to quantify the interfacial adhesion of PALF‐epoxy composite. It was verified that the interfacial shear strength of modified PALFs was substantially higher than that of untreated PALF by almost 2–2.7 times because of the greater interaction between the PALFs and epoxy resin matrix. The strongest interfacial adhesion was obtained from the fibers that had been received the alkalization combined with DGEBA deposition. Moreover, the flexural and impact properties of unidirectional PALF‐epoxy composites were greatly enhanced when reinforced with the modified PALFs due to an improvement in interfacial adhesion, particularly in the synergetic use of 5% NaOH and 5% NaOH/1% DGEBA. © 2008 Wiley Periodicals, Inc. J Appl Polym Sci, 2008     

Dispersion, interfacial interaction and re-agglomeration of functionalized carbon nanotubes in epoxy composites

The surface, interfacial and dispersion properties of carbon nanotubes (CNTs), and the mechanical properties of the CNT/epoxy composites affected by CNT functionalization are investigated. It is demonstrated that there exists strong correlations between amino-functionalization, dispersion, wettability, interfacial interaction and re-agglomeration behaviour of CNTs and the corresponding mechanical and thermo-mechanical properties of CNT/epoxy composites. The amino-functionalized CNTs exhibit higher surface energy and much better wettability with epoxy resin than the pristine CNTs, and the attached amine molecules arising from the functionalization effectively inhibit the re-agglomeration of CNTs during the curing of resin. These ameliorating effects along with improved interfacial adhesion between the matrix and functionalized CNTs through covalent bonds result in improved flexural and thermo-mechanical properties compared with those without functionalization.     

Preparation and properties of multi‐walled carbon nanotubes/carbon fiber/epoxy composites

Multi‐walled carbon nanotubes/carbon fiber (MWCNTs/CF) hybrid fillers are employed to prepare MWCNTs/CF/epoxy composites. Results reveal that a great improvement of the thermal conductivities of the epoxy composites with the addition of MWCNTs/CF hybrid fillers, and the thermal conductivity of the MWCNTs/CF/epoxy composites is 1.426 W/mK with 8 vol% treated MWCNTs/CF hybrid fillers (5 vol% MWCNTs + 3 vol% CF). Both the flexural and impact strength of the MWCNTs/CF/epoxy composites are increased firstly, but decreased with the excessive addition of MWCNTs. The flexural and impact strength of the MWCNTs/epoxy composites are optimal with 2 vol% MWCNTs. For a given MWCNTs/CF hybrid fillers loading, the surface treatment of MWCNTs/CF hybrid fillers can further increase the thermal conductivities and mechanical properties of the MWCNTs/CF/epoxy composites. POLYM. COMPOS., 35:2150–2153, 2014. © 2014 Society of Plastics Engineers     

Synergetic effects on the mechanical and fracture properties of epoxy composites with multiscale reinforcements: Carbon nanotubes and short carbon fibers

The ball‐milling/liquid‐phase oxidation (BMLPO) method was used to fabricate surface‐modified short carbon fibers (SCFs). Multiscale epoxy composites reinforced with a combination of SCFs and multiwalled carbon nanotubes (MWNTs) were prepared. Atomic force microscopy observations and contact angle measurement were used to investigate the modification effect of the BMLPO method. Mechanical tests and scanning electron microscopy observations were used to study the effects of the SCFs, MWNTs, and their combination on tensile properties, impact strength, and fracture toughness of the epoxy composites. The results show that the surface roughness of the SCFs after BMLPO treatment increased, and the wettability of the SCFs was improved as well. The combined use of the SCFs and MWNTs had a synergetic effect on the tensile strength, fracture toughness, and impact strength of the epoxy composites. The addition of MWNTs promoted the plastic deformation of the epoxy matrix and decreased the stress‐concentration level near the SCF/matrix interface; these were considered the main causes of the synergetic effect. © 2016 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2016 , 133, 43500.     

A comparative study on the properties of the different amino‐functionalized multiwall carbon nanotubes reinforced epoxy resin composites

Multiwall carbon nanotubes (MWCNTs) were amino‐functionalized by 1,2‐ethylenediamine (EDA)' triethylenetetramine (TETA), and dodecylamine (DDA), and investigated by fourier transform infrared spectroscopy (FTIR), Raman spectroscopy, and thermogravimetric analysis (TGA). The dispersion of the DDA functionalized MWCNT in DMF is better than that of the MWCNT functionalized by the EDA and the TETA. Carbon nanotubes reinforced epoxy resin composites were prepared, and the effect of the amino‐functionalization on the properties of the composites was investigated by differential scanning calorimetry (DSC), dynamical mechanical analysis (DMA), and TGA. The composites reinforced by the MWCNTs demonstrate improvement in various mechanical properties. The increase of T_g of the composites with the addition of amino‐functionalized MWCNT compared to the T_g of the composites with the addition of unfunctionalized MWCNT was due to the chemical combination and the physical entanglements between amino group from modified MWNTs and epoxy group from the epoxy resin. The interfacial bonding between the epoxy and the amino group of the EDA and the TETA‐modified MWCNT is more important than the well dispersion of DDA‐modified MWCNT in the composites for the improvement of the mechanical properties. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2012     

Dielectric properties of epoxy composites with modified multiwalled carbon nanotubes

We report here a high dielectric percolative polymer nanocomposite, fabricated by a combination of triethylene-tetramine (TETA) modified multiwalled carbon nanotube (named as TETA-MWNT) within epoxy resin matrix. In this composite system, with various TETA-MWNT volume fractions, the dielectric constant (K) is well fitted by the scaling law of the percolation theory with the percolation threshold f _c is 0.042 and the critical exponent p is 0.786. At 1,000 Hz of room temperature, the value of the dielectric constant is as high as 421 with the TETA-MWNT content of 4.14vol%, which is almost 60 times higher than that of epoxy resin. In contrast, a simple blend of pristine MWNT in epoxy composite shows evident lower dielectric constant and much higher loss with the same volume fraction.     

The effect of carbon nanotubes on the damage development in carbon fiber/epoxy composites

The aim of this study is to investigate the effect of carbon nanotubes (CNTs) on the initiation and development of damage in a woven carbon fiber/epoxy composite under quasi-static tensile loading. The composite is produced using resin transfer moulding and contains 0.25 wt.% of CNTs in the matrix. The results in the fiber direction report no improvement of the Young’s modulus and a slight improvement of the strength and strain-to-failure. The most important result of the study is a notion that CNTs have a hindering effect on the formation of transverse cracks. The conclusion is drawn from a combined analysis of the acoustic emission measurements (reporting a pronounced shift of all damage development thresholds towards higher strains by more than 30%) and X-ray/SEM observations (revealing a lower crack density in the CNT modified composite). The same analysis also indicates that the mechanism of energy dissipation through transverse microcracking is partially replaced by another mechanism that promotes (distributed) damage through fiber debonding.     

Improved interfacial adhesion in carbon fiber/epoxy composites through a waterborne epoxy resin sizing agent

A series of self‐emulsified waterborne epoxy resin (WEP) emulsions were used as surface sizing for carbon fibers (CFs) to improve the interfacial adhesion between the CF and epoxy matrix. In this work, the hydrogenated bisphenol‐A epoxy resin (HBPAE) was modified by polyethylene glycol (PEG) with molecular weights of 400, 800, 1000, 1500, 2000, 4000, and 6000 g/mol. The properties of the WEP emulsion were examined by Fourier transform infrared spectroscopy, dynamic light scattering, and transmission electron microscopy. The surface characteristics of sized CFs were evaluated using scanning electron microscopy, atomic force microscopy, and X‐ray photoelectron spectroscopy. Afterwards, CF/EP composites were prepared and their fracture surface and interlaminar shear strength (ILSS) were examined. The results indicated that PEG2000 modified HBPAE sizing had the optimum emulsion stability and film‐forming ability. Meanwhile, the results also demonstrated that a continuous and uniform sizing layer was formed on the surface of CFs and the surface sizing was excellent in improving the chemical activity of CFs. Compared with unsized CFs, the O1s/C1s composition ratio was observed to increase from 11.51% to 33.17% and the ILSS of CF/EP composites increased from 81.2 to 89.7 MPa, exhibiting better mechanical property than that of commercial Takemoto S64 sized CFs. © 2017 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2017 , 134, 44757.     

Carbon fiber-reinforced composites: Effect of fiber surface on polymer properties

Dynamic mechanical measurements in a torsional (shear) mode have been used to characterize an unfilled epoxy (Epon 828/m-phenylene diamine) and A series of uniaxial graphite fiber (Hercules types A and HM) composites. In unfilled resins containing an excess of the epoxy component, M_c—the average molecular weight between crosslinks—decreases with increasing temperature and duration of cure, suggesting a temperature-dependent side reaction. In fiber-reinforced composites, the dynamic mechanical response is sensitive to fiber type and curing schedule; elevation of T_g by as much as 45°C has been observed. Comparison of the dynamic data with properties predicted by micromechanical models shows only a fair agreement at room temperature, which rapidly worsens at higher temperatures. Surface treatment of type A fibers gives enhanced interlaminar shear strength (ILSS), both at ambient conditions and after hydrothermal aging. Dynamic data for surface-treated systems during hydrothermal aging show a sharper drop in G′ and increase in tan δ. The dynamic data and ILSS results are interpreted in terms of a balance of polymer-fiber interactions, a weak but widespread preferential adsorption of epoxy oligomers on the graphite basal planes at the fiber surface, and a low concentration of covalent bonds between polymer and fiber-surface-functional groups.     

The ultrasound‐based interfacial treatment of aramid fiber/epoxy composites

The quality of interfacial adhesion of aramid/epoxy composites affects the mechanical performance of the material, and thus there is a need to improve the condition by using the ultrasound‐based interfacial treatment. To do so, an ultrasonic transducer has been developed and evaluated under various operational conditions when it is installed in the winding system. It has demonstrated several key characteristics such as low power, high amplitude (more than 80 μm), and continuous working (more than 8 h) without water‐cooling. Subsequently, experiments were carried out to determine the mechanical performance of the polymer material with and without ultrasound treatment, showing that the ultrasonic treatment has improved the interfacial performance up to 10%, compared with those without any ultrasound‐treatment. © 2009 Wiley Periodicals, Inc. J Appl Polym Sci, 2009