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     

Influence of oxygen plasma treatment parameters on the properties of carbon fiber

This study is focused on the impact of oxygen plasma treatment on properties of carbon fibers and interfacial adhesion behavior between the carbon fibers and epoxy resin. The influences of the main parameters of plasma treatment process, including duration, power, and flow rate of oxygen gas were studied in detail using interlaminar shear strength (ILSS) of carbon fiber composites. The ILSS of composites made of carbon fibers treated by oxygen plasma for 1 min, at power of 125 W, and oxygen flow rate of 100 sccm presented a maximum increase of 28% compared to composites made of untreated carbon fibers. Furthermore, carbon fibers were characterized by scanning electron microscopy (SEM), tensile strength test, attenuated total reflectance Fourier transform infrared (ATR-FTIR), and Raman spectroscopy analyses. It was found that the concentration of reactive functional groups on the fiber surface was increased after the plasma modification, as well the surface roughness, which finally improved the interfacial adhesion between carbon fibers and epoxy resin. However, high power and long exposure times could partly damage the surface of carbon fibers and decrease the tensile strength of filaments and ILSS of treated fiber composites.     

Mechanical properties of surface‐modified ultra‐high molecular weight polyethylene fiber reinforced natural rubber composites

The mechanical properties of ultra‐high molecular weight polyethylene (UHMWPE) fibers reinforced natural rubber (NR) composites were determined, and the effects of fiber surface treatment and fiber mass fraction on the mechanical properties of the composites were investigated. Chromic acid was used to modify the UHMWPE fibers, and the results showed that the surface roughness and the oxygen‐containing groups on the surface of the fibers could be effectively increased. The NR matrix composites were prepared with as‐received and chromic acid treated UHMWPE fibers added 0–6 wt%. The treated UHMWPE fibers increased the elongation at break, tear strength, and hardness of the NR composites, especially the tensile stress at a given elongation, but reduced the tensile strength. The elongation at break increased markedly with increasing fiber mass fraction, attained maximum values at 3.0 wt%, and then decreased. The tear strength and hardness exhibited continuous increase with increasing the fiber content. Several microfibrillations between the fiber and NR matrix were observed from SEM images of the fractured surfaces of the treated UHMWPE fibers/NR composites, which meant that the interfacial adhesion strength was improved. POLYM. COMPOS., 38:1215–1220, 2017. © 2015 Society of Plastics Engineers     

An investigation of sound absorption coefficient on sisal fiber poly lactic acid bio‐composites

In this research, the mechanical, acoustical, thermal, morphological, and infrared spectral properties of untreated, heat and alkaline‐treated sisal fiber‐reinforced poly‐lactic‐acid bio‐composites were analyzed. The bio‐composite samples were fabricated using a hot press molding machine. The properties mentioned above were evaluated and compared with heat‐treated and alkaline‐treated sisal fibers. Composites with heat‐treated sisal fibers were found to exhibit the best mechanical properties. Thermo‐gravimetric analysis (TGA) was conducted to study the thermal degradation of the bio‐composite samples. It was discovered that the PLA‐sisal composites with optimal heat‐treated at 160°C and alkaline‐treated fibers possess good thermal stability as compared with untreated fiber. The results indicated that the composites prepared with 30wt % of sisal had the highest sound absorption as compared with other composites. Evidence of the successful reaction of sodium hydroxide and heat treatment of the sisal fibers was provided by the infrared spectrum and implied by decreased bands at certain wavenumbers. Observations based on scanning electron microscopy of the fracture surface of the composites showed the effect of alkaline and heat treatment on the fiber surface and improved fiber‐matrix adhesion. © 2015 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2015 , 132, 42470.     

Toughening vinyl ester networks with polypropylene meso-fibers: Interface modification and composite properties

Polymer-polymer composites comprised of vinyl ester matrices (VE) and polypropylene (PP) fiber meshes were fabricated and tested in this investigation. Results indicated that PP fibers greatly enhanced fracture toughness; however, strength of the VE was significantly reduced as voids were observed at the interface of the PP and VE. A two-step surface modification, oxygen plasma treatment followed by grafting vinyltrimethoxysilane (VTMS), was conducted on PP fibers in an effort to improve interfacial strength. Interfacial discontinuities of composites were improved after surface modification of PP. The oxygen plasma treatment added hydrophilic functional groups but caused surface roughness. Surface treatment of PP slightly increased fracture toughness of the PP-VE composite by enhancing energy absorption capacity at the interface. However, mechanical strength and modulus did not significantly increase for the composite using VTMS grafted PP fibers due to the weak fiber material. Small PP fibers with higher strength may attain the expected improvement in mechanical properties after surface treatment.     

Catalytic grafting: A new technique for polymer/fiber composites. II. Plasma treated UHMPE fibers/polyethylene composites

In this paper, the catalytic grafting technique for preparation of polymer/fiber composites is extended to plasma treated ultra-high modulus polyethylene (UHMPE) fiber/high density polyethylene (HDPE) system. The OH groups introduced on the UHMPE fiber surface by oxygen plasma treatment were used to chemically anchor Ziegler-Natta catalyst which then was followed by ethylene polymerization on the fiber surface. The morphology and interfacial behavior, as well as the mechanical properties, of the HDPE composites reinforced by catalytic grafted or ungrafted UHMPE fibers were investigated by SEM, DSC, polarized light optical microscopy, and tensile testing. The experimental results show that the polyethylene grafted on the fibers acted as a transition layer between the reinforcing UHMPE fibers and a commercial HDPE matrix. The interfacial adhesion was also significantly improved. Compared with the composite reinforced by ungrafted UHMPE fibers, the composite reinforced by catalytic grafted UHMPE fibers exhibits much better mechanical properties.     

Tribological behavior of short‐fiber‐reinforced polyimide composites under dry‐sliding and water‐lubricated conditions

Polyimide composites reinforced with short‐cut fibers such as carbon, glass, and quartz fibers were fabricated by the polymerization of monomer reactants process. The mechanical properties of the composites with different fiber contents were evaluated. The friction and wear properties of the polyimide and its composites were investigated under dry‐sliding and water‐lubricated conditions. The results indicated that the short‐carbon‐fiber‐reinforced polyimide composites had better tensile and flexural strengths and improved tribological properties in comparison with glass‐fiber‐ and quartz‐fiber‐reinforced polyimide composites. The incorporation of short carbon fibers into the polyimide contributed to decreases in the friction coefficient and wear rate under both dry and water‐lubricated conditions and especially under water lubrication because of the boundary lubrication effect of water. The polyimide and its composites were characterized by plastic deformation, microcracking, and spalling under both dry and water‐lubricated conditions, which were significantly abated under the water‐lubricated condition. The glass and quartz fibers were easily abraded and broken; the broken fibers transferred to the mating metal surface and increased the surface roughness of mating stainless steel, which led to the wear rate increasing for the glass‐fiber‐ and quartz‐fiber‐reinforced polyimide composites. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci 2008     

The effect of surface treatment on graphite nanoplatelets used in fiber reinforced composites

Atmospheric plasma treatment (APT) was used to surface‐activate graphite nanoplatelets (GnP) as well as highly graphitic P100 fibers used to manufacture composites. X‐ray photoelectron spectroscopy showed an increase in the O/C ratio of the treated surfaces when using either CO or O₂ as the active gas, whereas CO exhibited less damage to the treated reinforcement carbon material. APT of P100 fibers resulted in a 75% increase in composite tensile strength when compared to composites using untreated fibers. Surface treatment of GnPs also resulted in GnP/epoxy composites with significantly higher glass transition temperatures (Tg's) and 50% higher flexural strengths than those with no surface treatment because of stronger particle‐to‐resin coupling, which was also evidenced by the fracture surfaces. The effect of GnP loading concentration and plasma treatment duration was also evaluated on the tensile strength of fiber‐reinforced composites. The addition of untreated GnP filler resulted in a decrease in strength up to the 1% loading. However, higher loading conditions resulted in a 20% improvement because of GnP orientation effects. Fracture surfaces suggest that the fibers provided a mechanism for the GnPs to orient themselves parallel to the fiber axis, developing an oriented matrix microstructure that contributes to added crack deflection. Incorporating surface‐treated GnPs in these composites resulted in tensile strengths that were as high as 50% stronger than the untreated systems for all loading conditions. Increased GnP‐to‐matrix bonding as well as enhanced orientation of the GnPs resulted in multifunctional composites with improved mechanical performance. © 2013 Wiley Periodicals, Inc. J. Appl. Polym. Sci., 2014 , 131, 39994.     

Influence of surface treatment of carbon fibers on interfacial adhesion strength and mechanical properties of PLA‐based composites

In the present study C/PLA composites with different fiber surface conditions (untreated and with nitric acid oxidation for 4 h and 8 h) were prepared to determine the influence of surface treatment on the interfacial adhesion strength and mechanical properties of the composites. A chemical reaction at the fiber–matrix interfaces was confirmed by XPS studies. Nitric acid treatment was found to improve the amount of oxygen‐containing functional groups (particularly the carboxylic group, —COOH) on carbon fiber surfaces and to increase the surface roughness because of the formation of longitudinal crevices. The treated composites exhibited stronger interface adhesion and better mechanical properties in comparison to their untreated counterparts. There was a greater percentage of improvement in interfacial adhesion strength than in the mechanical properties. The strengthened interfaces and improved mechanical performance have been mainly attributed to the greater extent of the chemical reaction between the PLA matrix and the carbon fibers. The increased surface roughness also has had a slight contribution. © 2001 John Wiley & Sons, Inc. J Appl Polym Sci 80: 367–376, 2001     

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.     

The effect of silica (SiO2) nanoparticles and ammonia/ethylene plasma treatment on the interfacial and mechanical properties of carbon-fiber-reinforced epoxy composites

A nanoparticle dispersion is known to enhance the mechanical properties of a variety of polymers and resins. In this work, the effects of silica (SiO₂) nanoparticle loading (0–2 wt%) and ammonia/ethylene plasma-treated fibers on the interfacial and mechanical properties of carbon fiber–epoxy composites were characterized. Single fiber composite (SFC) tests were performed to determine the fiber/resin interfacial shear strength (IFSS). Tensile tests on pure epoxy resin specimens were also performed to quantify mechanical property changes with silica content. The results indicated that up to 2% SiO₂ nanoparticle loading had only a little effect on the mechanical properties. For untreated fibers, the IFSS was comparable for all epoxy resins. With ethylene/ammonia plasma treated fibers, specimens exhibited a substantial increase in IFSS by 2 to 3 times, independent of SiO₂ loading. The highest IFSS value obtained was 146 MPa for plasma-treated fibers. Interaction between the fiber sizing and plasma treatment may be a critical factor in this IFSS increase. The results suggest that the fiber/epoxy interface is not affected by the incorporation of up to 2% SiO₂ nanoparticles. Furthermore, the fiber surface modification through plasma treatment is an effective method to improve and control adhesion between fiber and resin.     

Structures and properties of HMPBO fibers treated by oxygen plasma/polyhedral oligomeric silsesquioxane

The surface of high modulus poly(p‐phenylene‐2,6‐benzobisoxazole) (HMPBO) fibers were treated by the combination method of oxygen plasma/polyhedral oligomeric silsesquioxane (POSS). The chemical compositions and surface morphologies of HMPBO fibers were characterized by Fourier transform infrared, X‐ray photoelectron spectroscopy, thermogravimetric analyzer, and scanning electron microscopy. The interfacial shearing strength (IFSS) of the HMPBO/cyanate ester (HMPBO/CE) micro‐composites was measured by single fiber pull out test. Results showed that the POSS was grafted on the surface of HMPBO fibers, and the grafting amount was about 0.82 wt%. After the treatment, the HMPBO fibers became coarser and the diameter was also increased. Compared with that of pure HMPBO/CE micro‐composites, the IFSS of treated HMPBO/CE micro‐composites was increased by 20.7%. POLYM. COMPOS., 34:2026–2030, 2013. © 2013 Society of Plastics Engineers     

Influence of plasma treatment on properties of ramie fiber and the reinforced composites

In this research, 9 series of ramie fibers were treated under low-temperature plasma with diverse output powers and treatment times. By analysis of the surface energy and adhesion power with epoxy resin, 3 groups as well as control group were chosen as reinforced fibers of composites. The influences of these parameters on the ramie fiber and its composites such as topography and mechanical properties were tested by scanning electron microscopy (SEM), atomic force microscopy (AFM), tensile property and fragmentation test of single-fiber composites. Contact angle and surface free energy results indicated that with the increased treatment times and output powers, surface energy and adhesion work with epoxy resin improved. Compared with the untreated fibers, surface energy and adhesion work with epoxy resin grew 124.5 and 59.1% after 3 min-200 w treatment. SEM and AFM showed low temperature plasma treatment etched the surface of ramie fiber to enhance the coherence between fiber and resin, consequently fiber was not easy to pull-out. After 3 min-200 w treatment, tensile strength of ramie fiber was 253.8 MPa, it had about 30.5% more than that of untreated fiber reinforced composite. Interface shear stress was complicated which was affected by properties of fiber, resin and interface. Fragmentation test showed biggest interface shear stress achieved 17.2 MPa, which represented a 54.0% increase over untreated fiber reinforced composites.     

Chemical interaction between carbon fibers and surface sizing

Functional groups on the surface of Polyacrylonitrile (PAN)‐based carbon fibers and in fiber surface sizing are likely to react during the curing process of composites, and these reactions could affect the infiltration and adhesion between the carbon fibers and resin. T300B‐3000‐40B fibers and fiber surface sizing were heat‐treated at different temperatures, and the structural changes of both the fiber surface sizing and extracted sizing after heat treatment were investigated by Fourier transform infrared spectroscopy. The results show that the concentration of epoxy groups in both the fiber surface sizing and extracted sizing decreased with increasing heat‐treatment temperature and decreased to zero after treatment at 200°C. The concentration of epoxy groups in the extracted sizing was lower than that of the fiber surface sizing after treatment under the same conditions; this indicated that the rate of reaction between the carbon fibers and fiber surface sizing was higher than the reaction rate of the fiber surface sizing system. X‐ray photoelectron spectroscopy analysis reveals that the content of C? O bonds and activated carbon atoms on the surface of the desized treated carbon fibers was the highest when the heat‐treatment temperature was 150°C; this proved the reaction between the carbon fibers and the fiber surface sizing. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2012     

Mechanical properties of carbon fiber composites modified with nano-SiO2 in the interphase

The performance of carbon fibers-reinforced composites is dependent to a great extent on the properties of fiber–matrix interface. To improve the interfacial properties in carbon fibers/epoxy composites, nano-SiO₂ particles were introduced to the surface of carbon fibers by sizing treatment. Atomic force microscope (AFM) results showed that nano-SiO₂ particles had been introduced on the surface of carbon fibers and increase the surface roughness of carbon fibers. X-ray photoelectron spectroscopy (XPS) showed that nano-SiO₂ particles increased the content of oxygen-containing groups on carbon fibers surface. Single fiber pull-out test (IFSS) and short-beam bending test (ILSS) results showed that the IFSS and ILSS of carbon fibers/epoxy composites could obtain 30.8 and 10.6% improvement compared with the composites without nano-SiO₂, respectively, when the nano-SiO₂ content was 1 wt % in sizing agents. Impact test of carbon fibers/epoxy composites treated by nano-SiO₂ containing sizing showed higher absorption energy than that of carbon fibers/epoxy composites treated by sizing agent without nano-SiO₂. Scanning electron microscopy (SEM) of impact fracture surface showed that the interfacial adhesion between fibers and matrix was improved after nano-SiO₂-modified sizing treatment. Dynamic mechanical thermal analysis (DMTA) showed that the introduction of nano-SiO₂ to carbon fibers surface effectively improved the storage modulus of carbon fibers/epoxy.     

等离子体射流载气流量大小对玻璃纤维改性效果影响的研究

通过大气压等离子体射流在玻璃纤维（GF）表面沉积氧化硅（SiOx）纳米颗粒的方法改善玻璃纤维增强聚丙烯（GFRP）复合材料的界面结合性能,利用扫描电子显微镜、原子力显微镜和X射线光电子能谱等表征分析了改性纤维的表面形貌、化学成分、润湿性能和复合材料的界面结合性能,并考察了等离子体射流载气流量大小对GF改性效果的影响。结果表明,当载气流量为40 mL/min时,GF的改性效果最好,且此时GF的表面能相比对照组提高了43.18%,GFRP复合材料的层间剪切强度提高了30.79%;经过等离子体处理后,GF的表面粗糙度增大,极性官能团增多,复合材料的界面结合性能提升。     

Effect of Fiber Acid Treatment on the Dynamic Mechanical Properties of Unsaturated Polyester/Carbon Fiber Unidirectional Composites

In this study, the surface modification of carbon fiber by sulfuric acid is investigated. Atomic Force Microscopy was employed to capture the corresponding changes in the surface roughness of the carbon fiber. Moreover, using treated and untreated fibers, unsaturated polyester unidirectional composite rods were prepared and their flexural properties were determined by three-point bending and dynamic mechanical thermal analysis.

The results indicated that the carbon fiber surface roughness increases in all samples. It is also found that treating the fiber decreases the magnitude of loss modulus. Besides, the flexural strength of composites made of the treated carbon fiber significantly increased.     

Mechanical properties of carbon fiber composites modified with graphene oxide in the interphase

The surface topographies of carbon fibers treated by sizing agents with different graphene oxide (GO) content were investigated by scanning electron microscopy. The surface elements compositions of carbon fibers were determined by X‐ray photoelectron spectrometer. The interfacial properties of composites were studied by interfacial shear strength. The thermo‐mechanical properties of two typical specimens (CF‐G0 and CF‐G1 composites) were investigated by dynamic mechanical thermal analysis. The results showed the introduction of GO sheets on carbon fibers surfaces effectively improved the mechanical properties of carbon fibers/epoxy composites. POLYM. COMPOS., 38:2425–2432, 2017. © 2016 Society of Plastics Engineers     

Characterization of three‐dimensional braided polyethylene fiber–PMMA composites and influence of fiber surface treatment

Three‐dimensional (3D) braided polyethylene (PE) fiber‐reinforced poly(methyl methacrylate) (PMMA), denoted as PE_3D/PMMA, composites were prepared. Mechanical properties including flexural and impact properties, and wear resistance were tested and compared with those of the corresponding unidirectional PE fiber–PMMA (abbreviated to PE_L/PMMA) composites. Both untreated and chromic acid‐treated PE fibers were used to fabricate the 3D composites in an attempt to assess the effect of chromic acid treatment on the mechanical properties of the composites. Relative changes of mechanical properties caused by fiber surface treatment were compared between the PE_3D/PMMA and PE_L/PMMA composites. The treated and untreated PE fibers were observed by scanning electron microscopy (SEM) and analyzed by X‐ray photoelectron spectroscope (XPS). SEM observations found that micro‐pits were created and that deeper and wider grooves were noted on the surfaces of the PE fibers. XPS analysis revealed that more hydroxyl (? OH) and carboxyl (? COOH) groups were formed after surface treatment. The physical and chemical changes on the surfaces of the PE fibers were responsible for the variations of the mechanical properties of the PE/PMMA composites. © 2005 Wiley Periodicals, Inc. J Appl Polym Sci 99: 949–956, 2006     

短切CF增强TPEE热塑性复合材料的注射成型及力学性能研究

以热塑性聚酯弹性体(TPEE)为基体材料,8 mm短切碳纤维(CF)为增强材料,制备CF/TPEE复合材料。材料通过双螺杆挤出系统混合塑化、挤出造粒后,再经过注塑成型制备成标准拉伸试样,通过力学性能测试及微观结构观察,系统研究了碳纤维含量和等离子表面处理对CF/TPEE复合材料拉伸性能的影响。结果表明,当碳纤维含量为20%时,CF/TPEE复合材料的拉伸强度最大,为39.08 MPa;相比于纯TPEE,其拉伸强度提高了217%;经过等离子表面处理后,拉伸强度进一步提高了5%。结合拉伸后断面的SEM图发现,注塑试样表层碳纤维取向度高,而近中区和中心层取向度相对较低,这是注射CF/TPEE复合材料拉伸性能提高效应不明显的主要原因。