1. Introduction

2. Role and Characterization of Sizing Agent Used for the Modification of Carbon Fibers:

2.1. Role of Sizing Agent in Enhancing the Interfacial Strength of CFRP’s:

Sizing process is defined as a potential chemical method of modifying the surface of the carbon fibers. As a result of sizing the surface of carbon fibers becomes polar enriched with heteroatom (oxygen/nitrogen/sulphur) containing function groups. As a result of sizing process, CF becomes chemically more reactive with the resin matrix facilitating stronger interface formation in the CFRPs. Sizing process has commercial significance and so, much of the knowledge of sizing process, sizing agents used, sizing composition are often a subject of intellectual property [6,7,8] and only limited details are available in open literature [9,10,11,12]. Among several types of sizing agents, namely, epoxy resin, unsaturated resin and thermoplastic resin, the epoxy resins (for example, E44 , E51) are most widely used. Chemical structures of epoxy sizing agents E51, dimer of DGEBA (diglycedyl ether of bisphenol A), and E44, hydroxy propyl derivative of DGEBA, are shown in Figure 1 [3,13]. The carbon and proton nuclei in different chemical environments are numbered and alphabeted respectively. The choice and selection of the sizing agent for modifying the CF surface is largely based on the application dictated by the polymer resin matrix used in the preparation of carbon fiber reinforced plastics (CFRPs) [3].

The structure of strongly polar unsaturated resin, N-(4′4-diaminodiphenyl methane)-2 hydroxypropyl methacrylate (DMHM), that was used as sizing agent for CF (polyacryl nitrile based) is shown in Figure 2. A two fold enhancement in IFSS is observed upon using DMHM as sizing agent instead of the epoxy type sizing agent, E44 [3].

Thermoplastic resins are another class of sizing agents. Thermoplastics are different from thermosetting plastics. Typical examples of thermoplastics include, polyethylene (PE), polypropylene (PP), acrylonitrile butadiene styrene (ABS), polyamide (PA), polycarbonate (PC), polyether ether ketone (PEEK), polyetherimide (PEI), and polyether sulfone (PES). Typical advantages of thermoplastics being a choice of sizing compound/resin matrix is that they do not require curing stage, less hazardous chemical composition, improved recycling convenience and large scale production capability [2,14].

CF play crucial role as load bearing component in CFRPs. Owing to the merits of CF, CFRPs are used as a replacement to metal components in high tech fields like aerospace, automotive, wind energy, marine turbine blades. A comparison of the thermo-physical properties of CF with graphite fiber and Al metal shows the superiority of CFs with lower density value (ρ, g/cm³), modest heat capacity (J/g/K) and thermal conductivity (W/mK) values (where g, cm, J, m and K refers to gram, centimeter, Joule, meter and Kelvi) as shown in Table 1 [15].

Use of CFRPs is particularly advantageous over metals in space vehicles (like rocket motors, and satellites) as the amount of fuel needed to put a small weight into space is reduced considerably. Other metal replacements include helicopter blades, air craft structural components, air craft containers and chemical and ship building industries. In fact, the first ever carbon fibers were made by a group at Royal air craft establishment (RAE) with good tensile properties for high performance reinforcement applications [16]. As early as 1971, Jeffries has correctly assessed the potential of CFs and their unique properties making them ideal candidates for diverse application. Any engineering device involving rotating component will obviously be improved in its performance if manufactured from CFRP. This is because the centrifugal forces in the rotating part are dependent on the weight of the part. The structure of carbon fibers is similar to graphite. The carbon atoms are in layers or planes which are arranged almost parallel to each other. In true graphite, the atoms in each plane are arranged in a regular manner with respect to those in the adjacent planes. On the contrary, in CF, there is no such regular arrangement and the structure is described as turbostratic [16].

Typical demerits of CFs namely, the smooth, non-polar, chemically inert surface with poor wettability and adhesion to resin (polymer) matrix, can be surmounted by the process of sizing [17]. Sizing process reduces the surface defects caused during fiber production process and thereby leads to improved adhesion with the resin matrix and results in enhanced mechanical properties [18]. Sizing agent performs multiple roles, namely, protecting the CF during processing, providing active functional groups on the surface of CF and improving the wettability of CF surface and the compatibility between CF and resin matrix. Solution and emulsion are the two types of sizing agents usually employed. Solution type sizing agent requires large amount of organic solvent while emulsion type comprise of organic resin dispersed in water with the help of an emulsifier. Emulsion type sizing agents are environmentally friendly and are safe to handle and so predominantly used compared to the solution type sizing agents [12]. The pH value of the sizing agent affects the IFSS of the CFRP as shown in Figure 3. Emulsion type sizing agent with dispersed reduced graphene oxide (rGO) was used to size the CF’s with a concentration of 2 %. The sizing agent with acidic or neutral pH value has a minor influence on the improvement of IFSS of CF-epoxy composite. Optimum value of IFSS (92.3 MPa) was observed when the pH value of the sizing agent is 10.5. Beyond a pH value of 10.5, the IFSS value varied only slightly. When the pH value of the sizing agent increased to 12, the sizing agent became unstable due to deemulsification. ~ 20.3 % improvement in IFSS of the CF-epoxy (E51) composite is achieved when the pH of the sizing agent is increased from 4.2 to 10.5 [12]. Increasing the mechanical properties of CFRPs is a challenge and a requirement from the high technology sector like missile applications [19].

Typical example of the measurement of the vital property of the CFRP, namely, IFSS is depicted in Figure 4. The IFSS between the single carbon fiber (SYT49) (sized with rGO modified epoxy based emulsion type sizing agent) and the resin microdroplets (E51) is determined by micro de-bonding test carried out on a interfacial evaluation equipment. The carbon fiber single filament is taped on the iron frame work. Resin microdroplets (E51) are wetted on the surface of the fiber. The resin microdroplets formed on the single fiber taped to the sample holder were cured by placing the sample in air oven at the curing conditions of 80 °C for 3 h, 140 °C for 1 h and 150 °C for 1 h. The temperature programming of the curing process is dependent on the resin matrix used in the CF-epoxy composite preparation. Two metal blades were clamped near a particular resin droplet and the sample holder is moved (in the direction of V) at a speed of 5 mm/min during the IFSS measurement. The metal blades were fixed during the test. The embedded length of the measured microdroplet of the resin (l_m; μm) is approximately 40-60 μm. The parameter measured during this test is the maximum force (F_max) required to de-bond a particular resin microdroplet from the single carbon fiber. The IFSS value of the composite is deduced by substituting the value of F_max in the following equation (1) [12,20]:

$$\mathit{I}\mathit{F}\mathit{S}\mathit{S} \left(\mathit{M}\mathit{P}\mathit{a}\right)=\frac{{\mathit{F}}_{\mathit{m}\mathit{a}\mathit{x}}}{\pi {\mathit{d}}_{\mathit{f}}{\mathit{l}}_{\mathit{m}}}$$

(1)

where F_max is the maximum load force (μN)

d_f is the fiber diameter (μm)

l_m is the embedded length of the microdroplet (μm)

Figure 4. Schematic representation of the single carbon fiber resin microdroplet debonding test. V indicates the direction of the movement of the iron framework (sample holder). Adapted from reference 12 with permission from John Wiley and Sons.

Figure 4. Schematic representation of the single carbon fiber resin microdroplet debonding test. V indicates the direction of the movement of the iron framework (sample holder). Adapted from reference 12 with permission from John Wiley and Sons.

Analogous to IFSS, ILSS is another vital mechanical property of the composites influenced by the sizing agent of the CFs. ILSS of the composites is deduced from the following equation (2) [21]:

$$\mathit{I}\mathit{L}\mathit{S}\mathit{S} \left(\mathit{M}\mathit{P}\mathit{a}\right)=\frac{\mathbf{3}{\mathit{P}}_{\mathit{b}}}{\mathbf{4}\mathit{d}\mathit{h}}$$

(2)

where P_b - breaking load at fracture (N)

h - width of the specimen (mm)

d - thickness of the specimen (mm)

Recent advances in the design of sizing agents for the surface modification of CFs and the corresponding enhancement in the mechanical properties of the CFRPs are summarized in Table 2.

Sizing plays an important role in improving the interfacial properties of CFRPs. The sizing layer on the CF act as additional compatibilizing phase where in some physical properties (for instance, stiffness modulus) of the composite have gradients, facilitating stress transfer from the polymer matrix to the CFs. In addition, sizing leads to formation of active functional groups on the CF surface enhancing the compatibility of CFs with polymer matrix. Particle size of the sizing agent and its distribution (PSD) is a crucial parameter determining the adhesion, stability, maximum solid content, drying time, rheological and optical properties of the sizing composition. The work of Yuan et al., on the surface modification of CFs with sizing agent (polyacrylate) and engineering the interface of sized CFs and polymer resin matrix (E44, DGEBA) has significantly improved the understanding of the region of interface that is critical for mechanical properties of the CFRPs with applicability in high technology sectors [24,35]. Sizing emulsions (water borne polyacrylate sizing agent) with five different particle size distributions, PSD, (P1, P2, P3, P4 and P5) with a respective mean particle diameters of 12.32 nm, 95.35 nm, 110.35 nm, 594.28 nm and 1.67 μm were prepared by controlling the PSD by physical filtration through differently sized filter screens (Figure 5). Irrespective of the PSD, all the sizing compositions have a zeta potential (ζ) value of ~ 40 mV with a low value of polydispersity coefficient (0.198-0.217). Usually, ζ value of more than 30 mV imply stability of the emulsion particles due to high electrostatic repulsion. Thus all the sizing emulsions (P1-P5, water borne polyacrylate sizing agents with varying particle size distributions) are thermostable. The aim of the study was to know the effect of PSD of the sizing composition on the adhesion strength of the polymer (epoxy resin) with the CF, and to find the optimal value of the PSD that can fill up the surface defects and interstitial sites on the CF surface and there by enhance the mechanical locking between fiber and the matrix. The authors have judiciously employed various physico-chemical interface characterization techniques like AFM and XPS to study the interface formed by the sizing compound at the interface of the CF and epoxy resin matrix.

Load and stress transition role of interfacial phase (formed by sizing layer) due to the polarity matching between polymer matrix and sized CF was analyzed by force modulation mode of AFM [35,36,37]. The stiffness of various phases, namely, the CF reinforcement, the sizing layer (poly acrylate, P5, P3, and P1) on the CF surface and the polymer resin matrix (epoxy E44) as well as the thickness of the interface (formed by the sizing layer that bridges the CFs and the resin matrix) is examined by imaging the phase of the sizing layer at the interface using force modulation microscopy. The change in the stiffness modulus at the interface is a qualitative measure to know the crosslinking density between the fiber and the matrix as well as to understand the transition area between the fiber and the matrix formed by the sizing layer. Using the oscillating cantilever tip that probes the CFRP surface, the stiffness of various phases in the unidirectional CF-epoxy composite is examined. The force modulus images obtained from the cross-section of the composites reinforced by differently sized carbon fibers, namely, with sizing agents P5, P3 and P1 are shown in Figure 6 a-c respectively. It should be noted that the relative stiffness image of CF’s is brighter than the surrounding epoxy matrix (E44). The corresponding relative stiffness modulus value variation [the gradation of the voltage generated from the cantilever deflection of the AFM as the tip moves from right (CF phase) to left (epoxy matrix) along the white line (through the interfacial phase of the sizing layer) in the images Figure 6 a-c] at the interface of the sizing layers formed by P5, P3 and P1 (along the white line in the images 6 a-c respectively) is shown in Figure 6. d-f, respectively.

The stiffness image, wherein P5 sizing is employed for the CFs in the CFRP, a clear distinction between the CFs and the surrounding epoxy matrix is observed (Figure 6 a). On the contrary, the boundary between the CF and the epoxy matrix becomes blurrier and a light brown interfacial phase is observed in P3 and P1 sized composites (Figure 6 b and c respectively), signifying the role of optimal particle size distribution (P3 with mean particle diameter of ~ 110 nm) in forming an effective interface between CFs and epoxy matrix. In P5 sized CFRPs (Figure 6d), the magnitude of stiffness modulus drops suddenly (as reflected in the magnitude of current measured in nA and plotted on the Y-axis of Figure 6 d-f), along the white line from right to left. The thickness of the sizing phase at the interface is 0.33 μm which is lower than the thickness of interface formed with sizing agents P3 (0.39 μm) and P5 (0.38 μm). These parameters illustrate that large particle size (P5 - 1.67 μm) of the sizing emulsion plays a negative role in the surface modification (wettability and roughness) and adhesion ability of CF surface with the epoxy resin matrix. In contrast, the stiffness modulus at the interface of CFRPs sized with P3 and P1 sizing agents decrease gradually (from right to left, from CF surface to the matrix along the white line in the images Figure 6 e-f respectively) indicating the gradient sizing distribution in the interface layer forming thicker interface (~ 0.39 μm). Thus relatively small size (~ 110 nm, P3) sizing droplets particles of the polyacrylate spread out on the CF surface uniformly healing the penetrating into the surface defects and interstitial sites facilitating the stress transfer efficiency. These observations were further confirmed by the evaluation of IFSS values of CFRPs without sizing agent (81.2 MPa) and CFRPs sized with P1-P5 sizing compounds (88.3-92.5 MPa). The CFRPs sized with P3 showed a 13.9 % enhancement compared to unsized CFRPs (with no sizing agent) and 4.7 % enhancement compared to P5 sized CFRP’s [10].

The geometry and location of sizing agent/compound and the mechanism of interlocking of CF and resin matrix through sizing agent (poly acrylate) at the interface with optimal PSD was demonstrated by Yuan et al., in the typical example of CF-epoxy (E44) composite [35].

Sizing agent with optimal multimodal PSD fit into the defects and interstices on CF surface and increase the packing efficiency and uniformity of surface distribution. The surface groves and defects of CFs are reduced and rectified. Relatively small particle size of sizing agent (~110 nm as in the above example) results in the formation of interface of moderate thickness and even distribution of sizing compound permeating through the bundles of CFs. As a result, surface defects are reduced, chemically active surface is formed leading to strong interfacial adhesion and effective stress transfer from polymer matrix to CF and thereby the load bearing ability with high tensile strength of CFs is utilized in various applications as metal replacement [35]. The chemical interlocking (by covalent and hydrogen bonding interactions) of the CF surface and epoxy matrix is facilitated by the increase in oxygen functional groups at the interface due to sizing by polyacrylate emulsion particles of optimum PSD (~ 110 nm) as deduced from XPS analysis [35].

Conclusion:

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179. Liu, X. G. , Cui, X. J., Zhang, C. X., Zhang, X. D., Wu, G. S., Effects of different silanization followed via the sol-gel growing of silica nanoparticles onto carbon fiber on interfacial strength of silicone resin composites. Chemical physics letters, 707, 2018, 1-7.
180. Cui, H. Z. , Jin, Z. Y., Zheng, D. P., Tang, W. C., Li, Y. B., Yan, Y. C., Lo, T. Y., Xing, F., Effect of carbon fibers grafted with carbon nanotubes on mechanical properties of cement-based composites. Construction and building materials, 181, 2018, 713-720.
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182. Yadav, A. K. , Benerjee, S., Kumar, R., Kar, K. K., Ramkumar, J., Dasgupta, K., Mechanical analysis of nickel particle-coated carbon fiber – reinforced epoxy composites for advanced structural applications. ACS applied nano materials, 1 (8), 2018, 4332-4339.
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184. Chen, B. B. , Li, X. F., Li, X., Jia, Y. H., Yang, J., Li, C. S., Hierarchial carbon fiber-SiO2 hybrid/polyimide composites with enhanced thermal, mechanical and tribological properties. Polymer composites, 39, 2018, E1626-E1634.
185. Xie, F. , Hu, W. J., Ning, D. D., Zhuo, L. H., Deng, J. B., Lu, Z. Q., ZnO nanowires decoration on carbon fiber via hydrothermal synthesis for paper based friction materials with improved friction and wear properties. Ceramics International, 44 (4), 2018, 4204-4210.
186. Senthilkumar, N. , Kumar, G. G., Manthiram, A., 3D hierarchical core-shell nanostructured arrays on carbon fibers as catalysts for direct urea fuel cells. Adv Energy Mater, 8, 2018, 1-11.
187. Yu, P, Ma, J. C, Zhang, R., Zhang, J. Z., Botte, G. G., Novel Pd-Co electrocatalyst supported on carbon fibers with enhanced electrocatalytic activity for coal electrolysis to produce hydrogen. ACS Applied Energy Materials, 1 (2), 2018, 267-272.
188. Xie, J. G. , Song, M. M., Fu, H. Q., Synthesis and properties of electrical conductive and antibacterial siloxane-modified carbon fiber-silver-acrylate nanocomposites. International Journal of Polymeric materials and polymeric biomaterials. 67 (16), 2018, 951-960.
189. Awan, F. S. , Fakhar, M. A., Khan, L. A., Zaheer, U., Khan, A. P., Subhani, T., Interfacial mechanical properties of carbon nanotube-deposited carbon fiber epoxy matrix hierarchical composites. Composite Interfaces, 25 (8), 2018, 681-699.
190. Zabihi, O. , Ahmadi, M., Li, Q.,, Shafei, S.,, Huson, M. G., Naebe, M., Carbon fiber surface modification using functionalized nanoclay: A hierarchical interphase for fiber-reinforced polymer composites. Composites Science and Technology, 148, 2017, 49-58.
191. Fang, J. , Xie, Z. G., Wallace, G., Wang, X. G., Co-deposition of carbon dots and reduced graphene oxide nanosheets on carbon –fiber micro electrode surface for selective detection of dopamine. Applied surface science, 412, 2017, 131-137.
192. Zhou, W. , Long, L., Xiao, P., Li, Y., Luo, H., Hu, W. D., Yin, R. M., Silicon carbide nano-fibers in-situ grown on carbon fibers for enhanced microwave absorption properties. Ceramics International, 43 (7), 2017, 5628-5634.
193. Gao, B. , Zhang, R. L., He, M. S., Sun, L. C., Wang, C. G., Liu, L., Zhao, L. F., Cui, H. Z., Cao, A. P., Effect of a multiscale reinforcement by carbon fiber surface treatment with graphene oxide/carbon nanotubes on the mechanical properties of reinforced carbon/carbon composites. Composites Part A – Applied Science and manufacturing, 90, 2016, 433-440.
194. Mei, H. , Zhang, S. M., Chen, H., Zhou, H. S., Zhai, X. Y., Chen, L. F., Interfacial modification and enhancement of toughening mechanisms in epoxy composites with CNT’s grafted as carbon fibers. Composites Science and Technology, 134, 2016, 89-95.
195. Zhang, R. L. , Gao, B.,, Ma, Q. H., Zhang, J., Cui, H. Z., Liu, L., Directly grafting graphene oxide onto carbon fiber and the effect on the mechanical properties of carbon fiber composites. Materials and Design, 93, 2016, 364-369.
196. Hoshi, K. , Maramatsu, K., Sumi, H., Nishioka, Graphene coated carbon fiber cloth for electrodes of glucose fuel cells. Japanese Journal of Applied Physics, 55 (2), 2016.
197. Jiang, J. J. , Yao, X. M., Xu, C. M., Su, Y., Deng, C., Liu, F., Wu, J. J., Preparation of graphene oxide coatings onto carbon fibers by electrophoretic deposition for enhancing interfacial strength in carbon fiber composites. Journal of Electrochemical Society, 163 (5), 2016, D133-D139.
198. Wu, G. S. , Ma, L. C., Wang, Y. W., Lie, L., Huang, Y. D., Interfacial properties and thermos-oxidative stability of carbon fiber reinforced methyl phenyl silicone resin composites modified with polyhedral oligomeric silsesquioxanes in the interphase. RSC Advances, 6 (6), 2016, 5032-5039.
199. Wang, C. F. , Li, J., Sun, S. F., Li, X. Y., Wu, G. S., Wang, Y. W., Xie, F., Huang, Y., Controlled growth of silver nanoparticles on carbon fibers for reinforcement of both tensile and interfacial strength. RSC Advances, 6 (17), 2016, 14016-14026.
200. Potschke, L. , Huber, P., Schriever, S., Rizzotto, V., Gries, T., Blank, L. M., Rosenbaum, M. A., Rational selection of carbon fiber properties for high-performance textile electrodes in bioelectrochemical systems. Frontiers in energy research, 7, 2019, 1-15.
201. Ding, Y. , Gou, L., Li, Y., Modifying nano carbon fiber surface comprises e.g. subjecting nano carbon fiber to low temperature plasma treatment, coating the nano carbon fiber with polydopamine, coupling modification on the nano carbon fiber with coupling agent. CN110130102, 16 Aug 2019.
202. Lv, X. , Wang, F., Mixed solution formulation for surface modification of conductive fibers, comprises nitric acid, lead nitrate, binder, and rest is pure water, adhesive is sodium silicate or starch with high purity, placing formulated mixed solution. CN110085825-A, 2 Aug 2019.
203. Du, B. , Qian, J., He, C., Wang, X., Shui, A., Preparing carbon fiber having multi-scale silicon carbide-silicon oxide carbides ceramic coating on surface involves adding transition metal compound to water and mixing uniformly to obtain mixed solution and soaking carbon fiber. CN110042653, 23 Jul 2019.
204. Qin, W. , He, J., Zhu, F., Meng, J., Method for surface modification of carbon fiber surface functionalization, involves soaking carbon fiber raw material with acetone, and preparing dopamine hydrochloride solution, and placing washed carbon fiber in dry box. CN1100168007-A, 16 Jul 2019.
205. Ikeda, T. , Nishina, Y., Kano, S., Aoyagi, Y., Fujiwara, T., Mori, M., Surface modification method for carbon fiber of carbon nanostructure e.g. carbon nanotube involves cutting the C-C coupling of the carbon fiber by the ultraviolet rays which generate on the light emission process of gas. JP2019099989-A, 24 Jun 2019.
206. Tao, F. , Preparing high thermal conductive polymer involves carrying out surface modification on carbon nanofibers and composite structure aluminum particles, and then mixing with filler and PVDF resin. CN109593305-A, 9 Apr 2019.
207. Li, G. , Xu, P., Lin, J., Xiang, Z., Yu, Y., Yang, X., Modifying carbon fiber surface by aromatic condensed ring molecular assembly comprises carrying out imidization reaction, immersing carbon fiber and combining. CN109338730-A, 15 Feb 2019.
208. Guo, P. , Preparing high-strength carbon fiber involves pretreating carbon fiber surface by first immersing carbon fiber in sulphuric acid solution, continuously stirring, filtering fiber out, and then using deionized water, until it is neutral. CN109371662-A, 22 Feb 2019.
209. Guan, M. , Surface modification method of polymer fiber by soaking untreated carbon fiber in sulphuric acid solution, cleaning residual sulfuric acid in carbon fiber surface, oven drying and fixing carbon fiber filament ribbon on PTFE oriented frame. CN109265921-A, 25 Jan 2019.
210. Ma, S. , Zhang, S., Jiao, Z., Sun, Z., Preparing modified carbon fiber comprises mixing carbon fiber in nitric acid solution and carrying out oxidation process, adding carbon oxide fiber into ethanol solution of the silane coupling agent and carryingout surface modification. CN108997719-A, 14 Dec 2018.
211. Xu, H. , Chen, X., Yan, C., Liu, D., Zhu, Y., Thermoplastic sizing agent useful for surface modification of carbon fiber comprises cyclic phenyl sulfide mixture composed of cyclic phenyl sulfide. CM108951173-A, 7 Dec 2018.
212. Park, S. W. , Jung, H. K., Shin, Y. J., Song, S. H., Surface modifying carbon fiber useful for reinforced plastic comprises dissizing the carbon fibers, surface modifying the surface of the desized carbon fiber, and sizing the plasma treated carbon fibers. KR2018128578-A; KR1968646-B1, 4 Dec 2018.
213. Jin, Y. , Zheng, X., Fang, Y., Chen, J., He, G., Huang, C., Shi, B., Modifying of spiral nano carbon fibers involves mixing graphitized spiral nano carbon fiber with ethanol and ball milling to obtain spiral nano carbon fiber, and acidifying ball-milled spiral nanocarbon fiber. CN108864773-A, 23 Nov 2018.
214. Li, M. , Improved power generation efficiency of a wind power generator and reducing noise, comprises choosing carbon fiber blade of wind power generator, subjecting the activation treatment, surface modification, and applying a performance coating. CN108864457-A, 23 Nov 2018.
215. Park, Y. B. , Kim, B. J., Cha, S. H., Method for forming zinc oxide nanostructure of carbon fiber using plasma process, involves reforming surface of woven carbon fiber (WCF) using atmospheric pressure plasma and growing nanostructure on surface-modified surface. KR1919496-B1, 16 Nov 2018.
216. Lv, Y. , Yao, L., Zhang, W., Zhang, J., Guo, Y., Method for surface modification of carbon fibers involves subjecting carbon fiber coated with thermostetting resin sizing agent to low-temperature heat treatment. CN108642882-A, CN108642882-B, 12 Oct 2018.
217. He, Y. , Li, S., Zhang, Z., Xue, L., Miao, S., Wang, C., Carbon nanotube modified carbon fiber surface large-scale production equipment include anode insulating bracket, clamping hopper, anode discharge wire, electric push rod, oven, and electronic portion including pulse high-voltage generator. CN108442101-A, 24 Aug 2018.
218. Wang, J. , Jiang, Y., Preparing high strength carbon fiber sizing agent comprises e.g. reacting acetic anhydride ammonium persulfate, sulfuric acid solution, polycarbonate, tetrahydrofuran, emulsifier, heating, agitating and ultrasonically dispersing. CN108360252-A, 3 Aug 2018.
219. Wang, Z. Y. , Replacement method of oil agent of surface of carbon fiber, involves performing pasting step that covers second type oil agent to carbon fiber, after plasma surface treatment to provide plasma gas flow and making it act on carbon fiber. JP2018115396-A, 26 Jul 2018; JP6393348-B2, 19 Sep 2018.
220. Joo, S. W. , Dillip, G. R., Kim, C. S., Carbon fiber/metal oxide complex composite used in electrode for ultrahigh capacity capacitor, comprises carbon fiber, and at least one metal oxide bonded to the carbon fiber. KR2018082799-A, ; KR1960154-B1, 4 Jul 2019. 19 July.
221. Zhu, B. , Yuan, X., Qiao, K., Yu, J., Zhao, S., Preparing oxidized graphene modified carbon fiber by silane coupling agent assisted electrophoretic deposition comprise e.g. placing carbon fiber after desulfurization in aqueous solution containing amino propyl triethoxy-silane and ethanol. CN108286187-A, 17 Jul 2018.
222. Jin, Y. , Chen, J., Wang, L., Jiang, C., Zhou, X., Li, B., Modification of nanosilica particles on spiral nano carbon fiber, condensing and refluxing liquids, suction filtering obtained mixture and drying filter residue. CN108219194-A, 29 Jun 2018; CN108219194-B, 17 Dec 2019.
223. Tian, Y. , Zhang, X., Yang, Y., Surface-modification of carbon fiber involves carrying out electrochemical treatment using composite electrolyte containing mixture of water, glycol, oxalic acid and acetonitrile as solvent, and nitrogen containing compound. CN108193482-A, 22 Jun 2018.
224. Song, G. , Ma, L., Tang, L., Li, J., Zhao, T., Grafting branched molecular tannic acid on carbon fiber surface by adding tannic acid into ethyl acetate, adding p-toluene sulfonic acid, stirring, obtaining reaction liquid, and adding dried acryl chloride carbon fiber into reaction liquid. CN107761375-A, 6 Mar 2018.
225. Xue, Z. , Wenqi, C., Xiaoming, C., Hebin, H., Preparation of carbon fiber reinforced epoxy resin matrix composite by modified double-sizing agent involves dissolving silane coupling agent into ethanol solution, stirring, and introducing modified carbon. CN107629224-A, 26 Jan 2018.
226. Chen, F. , Anti-static high-rigidity linear low density polyethylene composition for film comprises linear low-density polyethylene having certain density and certain value of melt flow rate, and surface modified carbon nanofibers modified surface. CN107365443-A, 21 Nov 2017.
227. Lee, Y. S. , Jung, M. J., Park, M. S., Lee, S., Jo, H., Surface modification of carbon fiber by irradiation with acid involves supporting carbon fiber in acid solution, irradiating carbon fiber supported on acid solution, and then washing and drying carbon fiber, where radiation is electron rays. IR1789205-B1, 24 Oct 2017.
228. Yang, H. , Feng, J., Yan, W., Modification of carbon fiber surface by in-situ polymerization of pyrrole comprises soaking carbon fiber in poly pyrrole aqueous dispersion, and reacting mixture with oxidizing agent to polymerize in situ on carbon fiber surface. CN107083680-A, 22 Aug 2017.
229. Wang, L. , Chang, Z., Wei, Q., Hu, Y., Chen, W., Wang, J., Modifying immobilized enzyme vector by using microwave assisted method comprises e.g. pretreatment of enzyme vector, using organic reagents for carbon fiber surface treatment and drying, stirring and washing. CN107058280-A, 18 Aug 2017.
230. Gao, S. , Chen, K., Xu, Z., Li, H., Hu, C.,, Luo, Y., Yang, H., Surface modification of carbon fiber used in e.g. biomedical material involves degelling carbon fiber, oxidising carbon fiber, reducing oxidized carbon fiber, cleaning, and drying. CN107034662-A, Aug 2017.
231. He, Y. , Bai, Y., Li, S., Jing, C.,, Zhu, Y., Device for surface modification of carbon fibers by rapid attachment of double-phase carbon nanotubes, has power source which is comprised with high voltage module, positive connection line and negative connection line. CN106906642-A, 30 Jun 2017.
232. Wang, R. , Lin, W., Jiao, W., Preparation of acylamide-based graft-modified carbon fiber involves dissolving modified in volatile organic solvent, heating, carrying out surface modification of carbon fiber with modifier solution and drying. CN106835695-A, 13 Jun 2017; CN106835695-B, 14 May.
233. Ren, L. , Sang, L., Ding, F., Liu, X., Zhao, Q., Li, Y., Preparation of cathode used for oxygen dissolved seawater battery, involves forming surface active layer by subjecting poly acrylonitrile carbon fiber material surface matrix core to surface modification treatment and heat-treating surface. CN106654163, 10 May.
234. Qian, X. , Ren, Q., She, Z., Song, Y., Yuan, H., Zhang, L., Zhao, C., Preparation method of bioactive carbon fiber used in sewage treatment, involves pre-oxidizing poly acrylonitrile fibers, carbonizing fibers, and performing activation treatment for modification of carbon fiber surface. CN106567158-A, 19 Apr 2017.
235. Yin, R. , Zhou, W.,, Preparing carbon fiber sialon ceramics composite material comprises subjecting carbon fiber to surface treatment to obtain modified carbon fiber having silicon carbide coating on its surface, chopping, ball milling, drying and molding. CN106518124-A, 24 Mar 2017; CN106518124-B, 27 Aug 2019.
236. Chu, Y. , Liu, S., Song, W., Wang, H., Wang, J., Producing surface modified layer of carbon fiber-titanium carbide – titanium diboride for ship involves utilizing friction agitation processing and forming S-shaped groove on upper surface of substrate and small holes in periphery of groove. CN106480451-A, 8 Mar 2017; CN106480451-B, 21 Aug 2018.
237. Li, Y. , Method for surface modification of carbon fiber material involves putting carbon fiber material into extraction device, extracting in acetone solution, removing surface coating of carbon fiber material, and wetting with deionized water. CN106436273-A, 22 Feb 2017.
238. Jiang, J. , Guo, Q., Zhou, L., Su, Y., Xu, C., Deng, G., Surface modification of carbon fiber involves graphene solution on carbon fiber surface, placing dried carbon fiber in plasma device and spraying plasma on surface of carbon fiber coated with nano graphene of graphene solution. CN106283601-A, 4 Jan 2017.
239. Jiang, J. , Guo, Q., Zhou, L., Su, Y., Xu, C., Chen, X., Surface modification of carbon fiber by extracting carbon fiber material with acetone by boiling, cleaning in deionized water, putting into vacuum drying box, with mixed acid, magnetically stirring, washing and vacuum drying. CN106245319-A, 21 Dec 2016.
240. Li, Y. , Carbon fiber coating modification process comprises e.g. adding tetra butyl titanate to ethanol solution, then adding alcohol solution of hydrochloric acid, stirring to obtain titanium dioxide sol, and post-processing. CN106245318-A, 21 Dc 2016.
241. Li, Y. , Surface modification of carbon fiber involves dispersing material (CF-3) formed by processing carbon fiber in diethyl ether and lithium borohydride, to silane coupling agent hydrolysate, ultrasonically processing filters and drying. CN106192407-A, 7 Dec 2016.
242. Gao, X. , Guo, S., Ding, C., Surface modification of carbon fiber comprising using titanic acid ester as coupling agent for carrying out surface treatment to the carbon fiber, then carrying out high-temperature air oxidation to the processed carbo n fiber. CN106032410-A, 19 Oct 2016.
243. Gao, Z. , Tan, Y., Yang, H., Zhang, B., Wang, M., Preparation of atomic layer deposition modified confinement catalyst used for preparation of heterogeneous solid catalyst, involves dispersing dried carbon nanofibers in alcohol, depositing platinum nanoparticles and aluminum oxide. CN105771972-A, 20 Jul 2016; CN105771972-B, 20 Jul 2018.
244. Liu, D. , Lv, F., Li, G., Li, S., Yi, W., Zhang, F., Zhou, Y., Li, C., Zhang, X., Li, N., Chen, Y., Preparing filter screen filler involves heating the carbon fiber, treating carbon fiber with concentrated nitric acid for surface modification and then dissolving fluorinated organosilane solution in dimethyl sulfoxide solutions. CN105350287-A, 24 Feb 2016; CN105350287-B, 18 Jul 2017.
245. Ma, J. , Zhai, C., Zhang, Q., Preparing carbon fiber enhanced polyimide coated complex and short carbon fiber and subjecting to surface modification and increasing carbon fiber. CN105295373-A, 03 Feb 2016.
246. Han, W. , Hong, C., Hu, P., Zhao, C., Zhang, X., Cheng, Y., An, J., Du, H., Zhou, S., Chemically grafting graphene oxide on carbon fiber surface comprises using modified Hummer’s method for preparing graphene oxide, oxidizing carbon fiber, carrying out carbon fiber surface modification and amination process and grafting. CN105239357-A, 13 Jan 2016.
247. Zeininger, H. , Eder, F., Maleika, M., Modified carbon fiber used for preparing composite plastic, comprises silicone-containing coating laser having thickness less than preset value. WO2015197299-A1, 30 Dec 2015; DE102014212241-A1, 31 Dec 2015; EP3129543-A1, 15 Feb 2017; US2017130393-A1, ; JP2017524835-W, 31 Aug 2017. 11 May.
248. Feng, R. , Sun, M., Sun, H., Yang, H., Nickel-graphite-poly (methyl meth acrylate) nano-composite wave-absorbing material useful e.g. in preparation of high temperature plastic, comprises e.g. modified sub-miron nickel plated carbon fiber and modified nano-nickel graphite. CN104592461-A, 6 May.
249. Liu, J. , Production of polypyrrole/carbon fiber composite electromagnetic wave absorbing material, involves dispersing surface-modified carbon fiber in valine, adding pyrrole monomer and ammonium persulfate solution, reacting, washing and drying. CN104592514-A, ; CN104592514-B, 31 Aug 2016. 6 May.
250. Qin, H. , Anodized carbon fiber surface treatment method involves carrying out anode oxidation treatment of carbon fiber beam, washing with distilled water, carrying out acetone extraction, rinsing with distilled water, and drying. CN104562631-A, 29 Apr 2015.
251. Han, W. , Xue, Z., Wang, P., Zhao, G., Zhang, X., Cheng, Y., Surface modification of carbon fiber comprises e.g. carrying out surface halogenation and azidation of nano silicon dioxide, carrying out alkynylation of carbon fiber, and grafting nano silicon dioxide on surface of carbon fiber. CN104499270-A, 8 Apr 2015; CN104499270-B, 6 Jul 2016.
252. Polycarbonate modified rubber, e.g. used in vehicle and electric industries comprises polycarbonate surface modified, organic montmorillonite, compatibilizer, light stabilizer, composite antioxidant and lubricant. (Inventor name not available in the Web of Science), CN104419181-A, 18 Mar 2015.
253. He, J. , Li, J., Liu, C., Wei, F., Wang, Z., Carbon fiber surface modification method comprise extracting carbon fiber with acetone in a soxhlet extractor, drying, carrying out oxidation and acylation, then grafting with bis (3-aminophenyl) phenyl phosphine oxide. CN104195824-A, 10 Dec 2014; CN104195824-B, 27 Apr 2016.
254. Guo, Z. , Huang, H., Pan, M., Surface modification method for carbon fiber powder used in e.g. aviation involves air preprocessing powder, heating in muffle furnace and immersing into oxidizing liquid for surface modification using strong oxidizing agent/sulfuric acid. CN104088132-A, 8 Oct 2014; CN10404088132-B, 16 Nov 2016.
255. Sun, H. , Yao, C., Method for modifying carbon fiber that is utilized in anode material of vanadium redox flow battery, involves preprocessing carbon fiber fabric, depositing beta-lead oxide particles, and scanning fiber fabric for multiple times. CN104064781-A, 24 Sep 2014; CN104064781-B, 4 Jan 2017.
256. Wang, B. , Duan, Y., Wang, H., Li, J., Chemically modifying microwave ultrasonic handled carbon fiber surface involves immersing carbon fiber in solvent among sonication carbon fibers, adding acid solution while ultrasonic dispersion and microwave radiation, adding initiator. CN104032565-A, 10 Sep 2014; CN104032565-B, 17 Aug 2016.
257. Wang, C. , Pan, H., Zhang, X., Zheng, X., Jiao, S., Continuous surface modification of carbon fibers involves purifying by immersing carbon fiber in acetone solution while continuously stirring, cleaning using ultra-pure water to surface of carbon fibers, oxidizing, dispersing and drying. CN104018340-A, 3 Sep 2014; CN104018340-B, 9 Dec 2015.
258. Xu, H. , Lu, Y., Oxygen and nitrogen co-doped poly acrylonitrile-based carbon fiber is prepared by electro chemical modification of raw material of poly acrylonitrile-based carbon fiber. WO2014127501-A1, 28 Aug 2014; CN104838051-A, 12 Aug, 2015; JP2016510367-W, 07 Apr 2016; CN104838051-B; JP6106766-B2, 05 Apr 2017; US9683314-B2, 20 Jun 2017; EP2960361-B1, 30 May.
259. Cai, T. , Chen, D., Huang, X., Lie, Z., Song, W., Yi, M., Xie, H., Emulsion used for preparing modified carbon fiber for polyamide composite material, comprises specified amount of surface modifier containing hydroxyl group-containing compound, polyamide, emulsifier, organic solvent and water. CN103993484-A, 20 Aug 2014; CN103993484-B, 23 Dec 2015.
260. Huang, Y. , Mengi, L., Ma, L., Pan, L., Wang,, Y., Qi, M., Yu, J., Modification of carbon fiber surface involves performing primary soxhlet-extraction in carbon fiber beam with acrylic ketone, removing impurity, leaching in supercritical acetone-water system, and removing carbon fiber epoxy coating. CN103966843-A, 6 Aug 2014; CN103966843-B, 2 Dec 2015.
261. Xu, Z. , Wang, J., Huang, H., Hao, Y., Surface modification of carbon fiber comprises layering an industrial crbon fiber felt and an active metal in an inert material lining container, reacting under inert gas atmosphere, cooling, washing with water and the air-drying. CN103966837-A, 6 Aug 2014.
262. Fan, X. , Liu, D., Xu, H., Yan, C., Zhang, X., Surface modification of carbon fiber used for interface modification composite material, involves preparing surface grafted polyphophazene carbon fiber, reacting with graphite, and obtaining surface grafted graphene carbon fiber. CN103850123-A, 11 Jun 2014; CN103850123-B, 3 Feb 2016.
263. Xu, F. , Liu, B., Qiu, Y., Hu, Q., Zhang, Y., Carbon fiber interface modification comprises carrying out cryogenic treatment of carbon fiber with liquid nitrogen in cryogenic medium, and heating. CN103590233-A, 19 Feb 2014; CN103590233-B, 28 Oct 2015.
264. Chen, S. , Feng, J., Surface modification of carbon fibers comprises a material containing catechol structure as surface modifying agent on a carbon fiber surface under polymerization condition. CN103572591-A, 12 Feb 2014.
265. Cai, T. , Huang, X., Ma, L., Song, W., Xin, W., Zeng, X., Yi, M., Chen, D., Modifying carbon fiber surface, useful e.g. in aerospace, comprises e.g. performing electrolytic oxidation with strong alkaline electrolyte to electrochemically modify and performing electrolytic oxidation with week alkaline electrolyte. CN103541212-A, 20 Jan 2014; CN103541212-B, 18 May, 2016.
266. Zhang, C. , Ma, L., Zhou, H., Meng, L., Qi, M., Yu, J., Modification method of surface-modified carbon fibers involves extracting carbon fiber into soxhlet extractor, cleaning acetone as extraction agent, removing surface impurities from carbon fibers, purifying soaking and washing. CN103450501-A, 18 Dec 2013; CN103450501-B, 26 Nov 2014.
267. Xu, S. , Modification of poly acrylo nitrile-based carbon fiber surface involves plasma treating poly acrylonitrile based carbon fiber plasma under inert gas atmosphere and atomizing with grafting liquid. CN103361768-A, 23 Oct 2013.
268. Huang, S. , Lv, C., Wu, G., Method for modifying carbon fiber surface, involves dissolving graphene oxide in water followed by obtaining graphene oxide water solution, and carrying out thermal treatment with coated carbon fiber on furnace to obtain finished product. CN103243544-A, 14 Aug 2013; CN103243844-B, 2 Sep 2015.
269. Li, J. , Huang, Y., Song, Y., Hu, Z., Liu, L., Preparation of carbon fiber surface modification coating used for, e.g. aviation, by reacting monomer phenolic and aldehyde compounds with catalyst, diffusing in slurry to obtain phenolic resin pre polymer, drying and carbonizing. CN103061111-A, 24 Apr 2013.
270. Tu, L. , Meng, J., yang, M., Li, L., Environment friendly carbon fiber surface modification for, e.g. lake water, by soaking carbon fiber precursor in acetone solution, drying, soaking in nitric acid, drying to obtain modified carbon fiber wire, and placing in gas atmosphere. CN103058356-A, 24 Apr 2013; CN103058365-B, 18 Jun 2014.
271. Li, J. , Song, Y., Huang, Y., Hu, Z., Liu, L., Etching surface of controllable fiber e.g. carbon fiber, comprises passing continuous fibers to irradiation furnace, controlling twisting degree of fibers, reducing fibers from furnace, and washing fiber tow layers away by solvent. CN103046308-A, 17 Apr 2013; CN103046308-B, 27 Aug 2014.
272. Meng, L. , Qi, M., Lin, Y., Zhang, C., Yu, J., Fan, D., Surface modification method of carbon fiber used in chemical industry, involves pre-processing carbon fiber bundle surface, carrying out surface oxidation treatment of obtained surface-treated carbon fiber bundle, washing and drying. CN102888750-A, 23 Jan 2013; CN102888750-B, 12 Mar 2014.
273. Fang, L. , Deng, C., Jiang, J., Shi, J., Method of ultrasonic enhanced carbon fiber surface comprises surface preprocessing, washing and drying. CN102851940-A, 2 Jan 2013.
274. Shi, J. , Deng, C., Jiang, J., Fang, L., Surface modification of carbon fiber used for composite material, involves coating sol solution of nano graphene and water on carbon fiber surface, drying and spraying plasma to surface of coated carbon fiber under specified conditions. CN102839534-A, 26 Dec 2012; CN102839534-B, 11 Jun 2014.
275. Liu, J. , Liang, J., Wang, C., Electrochemical surface modification of carbon fiber involves preparing electrolyte solution, processing composite electrolyte system, providing carbon fiber, pouring into electrolyte cell, washing and drying. CN102660866-A, 12 Sep 2012.
276. An, F. , Guo, J., Li, D., Lv, C., Wu, G., Electrochemical surface – modification of carbon fiber, involves carrying out electrochemical reaction using electrolyte containing modified carbon nanotubes, carbon fibers as anode, and conductive metal or graphite material as cathode. CN102505449-A, 20 Jun 2012.
277. Fan, X. , Li, X., Ruan, C., Yu, L., Zhang, X., Yan, C.,, Zhu, Y., Modification of carbon fiber surface used for carbon fiber/polycaprolactam composite material, by reacting carbon fiber with hexa chloro cyclo triphosphazene, and reacting modified carbon fiber surface with caprolactam monomer. CN102493184-A, 13 Jun 2012; CN102493184, 26 Mar 2014.
278. Li, J. , Luo, R., Xu, N., Modification of poly acrylonitrile-base carbon fiber by carbon nanotube, involves loading prefabricating component of carbon fiber pricking felt in catalyst precursor, calcining, deoxidizing, cooling, and thermally treating. CN101671951-A, 17 Mar 2010; CN10167951-B, 15 Feb 2012.
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