CN101413209B - Method for carbon fiber surface modification of plasma coated with nano colloidal sols by plasma treatment - Google Patents
Method for carbon fiber surface modification of plasma coated with nano colloidal sols by plasma treatment Download PDFInfo
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- CN101413209B CN101413209B CN2008102026208A CN200810202620A CN101413209B CN 101413209 B CN101413209 B CN 101413209B CN 2008102026208 A CN2008102026208 A CN 2008102026208A CN 200810202620 A CN200810202620 A CN 200810202620A CN 101413209 B CN101413209 B CN 101413209B
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Abstract
The invention relates to a method for modifying the surface of carbon fiber coated with nano sol through plasma treatment, which comprises the following steps: firstly, nano particles are prepared into an organic solvent, a sol solution of water or a sol solution prepared by hybridization reaction of a precursor solution of organic-inorganic nano particles by the ultrasonic vibrating technology; secondly, the sol solution is coated on the surface of the carbon fiber, treated by means of spray coating and padding, and dried; and thirdly, the dried carbon fiber is placed on a special transport unit for plasma processing equipment and a plasma is sprayed on the surface of the carbon fiber to make the carbon fiber move in the plasma atmosphere, so as to generate surface modification, wherein the treating power is between 10 and , watts, and the treatment time is between 0.5 and 300 seconds. The method can effectively improve the performance of the fiber, improves the molded manufacturability and the overall properties of composite materials of the fiber, has simple technology, quick processing speed, good treatment effect and low cost, is convenient to operate and difficult to cause environmental pollution, can reduce energy consumption, and is suitable for industrial production.
Description
Technical field
The invention belongs to the preparation field of carbon fiber and composite thereof, particularly relate to the method for the carbon fiber surface modification of plasma coated with nano colloidal sols by plasma treatment.
Background technology
The axial strength of carbon fiber and modulus are high, no creep, and fatigue durability is good, and specific heat and electric conductivity are between nonmetal and metal, and thermal coefficient of expansion is little, and resistance to chemical reagents is good, and the density of fiber is low, and the X ray permeability is good.Shortcoming is that resistance to impact is relatively poor, easily damage; Oxidation takes place under hot strong acid effect, during with metal composite, metallic carbide, carburizing and electrochemical corrosion phenomenon can take place.Must comprise nickel plating etc. through surface treatment before compound for this reason.Carbon fiber has long filament, staple fibre, staple fiber etc., can be processed into fabric, felt, seat, band, paper and other materials, like metallized fiber.Long filament and fabric generally are processed into prepreg.In addition, also can produce preoxidized polyacrylonitrile silk and NACF without carbonization and graphitization.Carbon fiber is except that being used as heat-insulating material; Generally do not use separately; Normal resin, metal, pottery and the concrete etc. of adding; Constitute corresponding composite, be used to make health substitute materials such as high speed rotor, industrial robot, leaf springs of car and driving shaft that aircraft construction material, rocket envelope, universe machinery, golf club, racket, power ship, electric wave shielding remove electric material, TV set aerial, centrifugal separator, artificial ligament etc.
In normal carbon fiber process: surface treatment, carry out gas phase or liquid phase oxidation etc., give the fibre chemistry activity, to increase compatibility to resin.Starching is handled, and prevents fibre damage, improves the compatibility with resin matrix.
For the adhesion that improves carbon fiber and resin matrix etc., improve the surface treatment that the interlayer shear power of composite must be carried out.Purpose is polar group such as the functional groups such as carboxyl, carbonyl and lactone that increase carbon fiber, increases surface area, improves wettability and cohesive force with resin matrix.Surface preparation has five kinds: (1) liquid phase oxidation, oxidant are 1N Na2Cr2O7 or 6N HNO3 etc.; (2) plasma processing method makes plasma polymer be attached on the carbon fiber surface or a corrasion; (3) anode electrolysis or electrodeposition process method make the EVA anion of band carboxyl etc. under electric field action, be deposited on carbon fiber surface equably; (4) ozone treatment method; (5) vapour phase oxidation process adopts O2+Cl2 to carry out at about 1000 ℃.
Liquid-phase oxidation (USP3JlI13094), technology are comparatively complicated, and the processing time is long, can not be complementary with carbon fiber production line, are used for laboratory research mechanism or intermittently military surface treatment usually more.
What have industrial utility value mainly is electrolytic anodization and gas-phase oxidization process.
Electrolytic anodising process (spy opens clear 56~53275) processing time is short, and effect is remarkable, but the carbon fiber after electrolytic anodization is handled must be washed metal ion off through the hot water washing step earlier, again through drying process, could flood protection glue then.Technology is more numerous and diverse.
Vapour phase oxidation process: United States Patent (USP) (usP3723607) discloses the ozone oxidation carbon fiber surface treatment method; This method is after carrying out the dry decontamination dedusting of strictness with air or oxygen through cyclone separator, filter, drier etc.; Electrion annular space through ozone generator produces ozone; Handled earlier tens of seconds in the inert gas atmosphere of carbon fiber under 1200 degree high temperature, in ozone environment, handle then.Effect can but complex process.
Carbon fiber is used widely in high-performance composite materials as good composite reinforcing agent.But its high-temperature oxidation resistance is relatively poor, at the air more than 400 ℃ strong weightlessness and intensity reduction takes place promptly.In addition, the compatibility of carbon fiber and metallic matrix is poor, mainly shows: be prone to matrix harmful chemical reaction take place, undesirable with the interface wet ability of metallic matrix, thermal coefficient of expansion does not match.Can address this problem effectively the carbon fiber coating.Coating process is a lot, comprises technology such as PVD, CVD, plating, chemical plating and sol-gel.
The Low Temperature Plasma Treating technology is to carry out the maximum a kind of method of research in the carbon fiber surface modification technology at present.But traditional Low Temperature Plasma Treating technology is too slow in serialization speed, needs to keep the certain vacuum degree in the processing, and condition is relatively harsher, is not very desirable aspect suitability for industrialized production, is badly in need of a kind of new carbon fiber surface treatment method.Present existing plasma treatment carbon fiber surface modification technical patent does not relate to the nano material preparation colloidal sol technology of utilizing; More do not mention and utilize Nano sol technology coated carbon fibers, particularly the carbon fiber after Nano sol applies carries out the method for surface modification again through plasma technique.
Summary of the invention
Technical problem to be solved by this invention provides the method for the carbon fiber surface modification of plasma coated with nano colloidal sols by plasma treatment, changes the performance that method can effectively be improved fiber, and the moulding process property of its composite and whole synthesis performance are improved.
The method of the carbon fiber surface modification of plasma coated with nano colloidal sols by plasma treatment of the present invention comprises:
(1) utilizes the ultrasonic oscillation technology to be mixed with 0.01~15% sol solutions of organic solvent or water nano particle or the pioneer's liquid and the nano SiO 2 particle of organic-inorganic nano particle reacts through hydridization, make sol solutions;
(2) above-mentioned sol solutions is coated in carbon fiber surface, can uses spraying, method such as pad, then oven dry;
(3) carbon fiber with the coating nanometer powder of above-mentioned oven dry places on the dedicated transmissions device of apparatus for processing plasma shown in Figure 5; At atmospheric pressure, under the open environment, directly plasma jet is arrived carbon fiber and coating nanometer powder surface; The carbon fiber of coating nanometer powder is moved in plasma atmosphere; Processing power is 10W-15000W, and the time is 0.5-300s, produces carbon fiber and coating nanometer powder surface modification.
Said step (1) nano particle is one or more the mixing nano particle in iron oxide, zinc oxide, titanium oxide, aluminium oxide, silica, illiteracy holder soil, the CNT.
Said step (1) organic solvent is selected from hexane, isopentane, pentane, benzinum, hexane, cyclohexane, isooctane, trifluoroacetic acid, trimethylpentane, pentamethylene, heptane, butyl chloride; Butyl chloride, trichloro-ethylene; Acetylene trichloride, carbon tetrachloride, chlorotrifluoroethane, propyl ether; Propyl ether, toluene, paraxylene, chlorobenzene, o-dichlorohenzene, diethyl ether; Ether, benzene, isobutanol, carrene, ethylene dichloride, n-butanol, butyl acetate; Butyl acetate, propyl alcohol, methylisobutylketone, oxolane, ethyl acetate, isopropyl alcohol, chloroform, methyl ethyl ketone, dioxanes; Dioxane; Dioxane, pyridine, acetone, nitromethane, acetate, acetonitrile, aniline, dimethyl formamide; Methyl alcohol, ethylene glycol, n-octyl alcohol, n-hexyl alcohol, isobutanol, n-butanol, cyclohexanol, isopropyl alcohol; Normal propyl alcohol, methyl alcohol, ethylene glycol, DAA, methyl-sulfoxide DMSO, acetone, ethyl acetate, benzinum; Chloroform, oxolane, dioxane, DMF, carrene, carbon disulfide, oxolane; Three fluoro acetate, trichloroethanes, ethyl acetate, butanone, glycol dimethyl ether, glycol monomethyl ether, one or more in the butyl acetate.
Said step (1) organic nanometer granule is the ferroferric oxide particle that coats of oleic acid, with in acetic acid, the butyl titanate one or more.
Said step (1) inorganic nanoparticles is that nano level metal, nanosize metal oxide, nanoscale are nonmetal, one or more the mixture nano particle in the nanoscale nonmetal oxide.
The said nano level metal that mixes by different demands is silver, copper and composition thereof; Nanosize metal oxide is one or more the mixture in titanium, aluminium, zirconium, iron, tin, zinc, barium, the nickel oxide, and nonmetal and oxide nano particles is one or more a mixing compound nano particle of CNT, silica, imvite, phosphorous oxides.
The plasma producing apparatus of said step (3) is all kinds of plasma generators, and plasma atmosphere is produced by plasma generator, and is ejected into the plasma atmosphere that forms in normal temperature, normal pressure, the atmospheric environment via nozzle mechanism.
Said step (3) plasma is selected from one or more in helium, argon gas or the functional gas, and wherein helium, argon gas mol ratio are 50%-99.99%, and functional gas is 0.001~30%, and the plasma of flowing through simultaneously forms the district and forms plasma atmosphere.
Described functional gas is SO
2, ammonia, oxygen, hydrogen, nitrogen, carbon tetrafluoride, carbon dioxide, methane (CH
4), ethane (C
2H
6), propane (C
3H
8), butane (C
4H
10), pentane (C
5H
12), hexane (C
6H
14), heptane (C
7H
16), octane (C
8H
18), nonane (C
9H
20), decane (C
10H
22), hendecane (C
11H
24), dodecane (C
12H
26), tridecane (C
13H
28), ethene (C
2H
4), propylene (C
3H
6), butylene (C
4H
8), amylene (C
5H
10), hexene (C
6H
12), allene (C
3H
4), butadiene (C
4H
6), isoprene (C
5H
8), hexatriene (C
6H
8), acetylene (C
2H
2), propine (C
3H
4), butine (C
4H
6), pentyne (C
5H
8), hexin (C
6H
10), heptyne (C
7H
12), octyne (C
8H
14), n-heptylacetylene (C
9H
16), decine (C
10H
18), undecyne (C
11H
20), tetrafluoroethylene and silane, various siloxane gas, acrylic acid, the steam of methacrylic acid or their composition gas.
The carbon fiber that plasma modification is handled coats with nano particle colloidal sol earlier.
Concrete equipment is arranged and can be changed as required.
Referring to shown in Figure 5, with the gaily decorated basket cylindrical line immersion Nano sol of pending carbon fiber 1, pad processing along colloidal sol squeeze device 2, then carbon fiber is imported into drying unit 3, oven dry and collection solvent under specified temp.Then the carbon fiber plasma atmosphere district that is introduced into plasma nozzle 4 carries out plasma surface modification; An automatic winding machine 5 is arranged at the rear portion; Can the carbon fiber 1 after handling be carried out online rolling, regulate the Trace speed of carbon fiber through the rotating speed of regulating Scroll.According to the needs of different processing technologys, carbon fiber is through the distance of plasma nozzle, and speed is adjusted accordingly.
Following physicochemical change takes place carbon fiber surface after plasma treatment: the part chemical bond of the nano-material surface of (1) carbon fiber surface and surface applied breaks off, and forms the high free radical of chemism; (2) free radical that exists with plasmoid rapidly and the combined with radical of the nano-material surface of carbon fiber surface and surface applied, forms new chemical bond; (3) nano-material surface of carbon fiber surface and surface applied is bombarded and etching, and microstructure helps the infiltration of organic basis material such as resin by smooth roughening.
Use plasma that fiber and coating are carried out surface modification treatment; The carbon fiber surface performance is improved; Improve with the infiltration speed of matrix resin, the infiltration amount increases, and effect of impregnation may is improved; Simultaneously under the effect of plasma reinforcing fiber be coated with combining of interlayer, make the fiber bodies performance obtain optimization to a certain degree.The carbon fiber of handling through the method for the invention has obtained improving greatly with the composite performance between the organic basis material.Its technological advantage is with the Nano sol coating unit, and composition continuous devices such as plasma jet separately or be mounted on the surface treatment of carbon fibers production line.Form to import the coated with nano colloidal sols carbon fiber continuously and then handle the coated with nano colloidal sols carbon fiber surface and form carbon fiber surface modification with jet plasma.Present device is simple in structure.Technological process is short.Easy to operate and can match obvious processing effect with carbon fiber production line.According to the requirement of different systems, the convenient treatment process that changes satisfies different application requirements.
Beneficial effect
(1) carbon fiber of handling through the method for the invention has obtained improving greatly with the composite performance between the organic basis material;
(2) technology is simple, easy to operate, process velocity is fast, treatment effect good, cost is low, be difficult for causing environmental pollution, and can cut down the consumption of energy, and is fit to suitability for industrialized production;
(3) according to the requirement of different systems, the convenient treatment process that changes satisfies different application requirements.
Description of drawings
5000 times of electromicroscopic photographs of Fig. 1;
Fig. 2 infared spectrum;
5000 times of electromicroscopic photographs of Fig. 3;
Fig. 4 infared spectrum;
The process chart of Fig. 5 SURFACE TREATMENT OF CARBON FIBER method.
The specific embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in the restriction scope of the present invention.Should be understood that in addition those skilled in the art can do various changes or modification to the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Instance 1
Helium plasma treatment Nano sol coated carbon fibers
Referring to shown in Figure 5, with the gaily decorated basket cylindrical line immersion Nano sol (0.05%) of pending carbon fiber 1, pad processing along colloidal sol squeeze device 2, then carbon fiber is imported into drying unit 3, oven dry and collection solvent under specified temp.Then the carbon fiber plasma atmosphere district that is introduced into plasma nozzle 4 carries out plasma surface modification (the fibre bundle upper surface is apart from nozzle distance 5MM; The fibre bundle lower surface is apart from nozzle < 20MM; Obtain under 40 watts of power and 2 second time handling); An automatic winding machine 5 is arranged at the rear portion, can the carbon fiber 1 after handling be carried out online rolling, regulate the Trace speed of carbon fiber through the rotating speed of regulating Scroll.According to the needs of different processing technologys, carbon fiber is through the distance of plasma nozzle, and speed is adjusted accordingly.Surface treatment of carbon fibers effect: 5000 times of electromicroscopic photographs such as Fig. 1, infared spectrum such as Fig. 2.
Instance 2
Oxygen plasma treatment Nano sol coated carbon fibers
Referring to shown in Figure 5, with the gaily decorated basket cylindrical line immersion Nano sol (0.05%) of pending carbon fiber 1, pad processing along colloidal sol squeeze device 2, then carbon fiber is imported into drying unit 3, oven dry and collection solvent under specified temp.Then the carbon fiber plasma atmosphere district that is introduced into plasma nozzle 4 carries out plasma surface modification (the fibre bundle upper surface is apart from nozzle distance 5MM; The fibre bundle lower surface is apart from nozzle < 20MM; Obtain under 40 watts of power and 2 second time handling); An automatic winding machine 5 is arranged at the rear portion, can the carbon fiber 1 after handling be carried out online rolling, regulate the Trace speed of carbon fiber through the rotating speed of regulating Scroll.According to the needs of different processing technologys, carbon fiber is through the distance of plasma nozzle, and speed is adjusted accordingly.Surface treatment of carbon fibers effect: 5000 times of electromicroscopic photographs such as Fig. 3, infared spectrum such as Fig. 4.
Claims (5)
1. the method for the carbon fiber surface modification of plasma coated with nano colloidal sols by plasma treatment comprises:
(1) utilize the ultrasonic oscillation technology to be mixed with 0.01~15% sol solutions of organic solvent or water nano particle; Wherein nano particle is one or more the mixing nano particle in iron oxide, zinc oxide, titanium oxide, aluminium oxide, illiteracy holder soil, the CNT;
(2) above-mentioned sol solutions is coated in carbon fiber surface, uses spraying or pad method, oven dry then;
(3) carbon fiber with the coating nanometer powder of above-mentioned oven dry places on the dedicated transmissions device of apparatus for processing plasma; At atmospheric pressure, under the open environment, directly plasma jet is arrived carbon fiber coating nanometer powder surface; The carbon fiber of coating nanometer powder is moved in plasma atmosphere; Plasma treatment power is 10W-15000W, and the time is 0.5-300s, produces carbon fiber coating nanometer powder surface modification.
2. the method for the carbon fiber surface modification of plasma coated with nano colloidal sols by plasma treatment according to claim 1; It is characterized in that: the organic solvent in the said step (1) is selected from hexane, isopentane, pentane, cyclohexane, isooctane, trifluoroacetic acid, trimethylpentane, pentamethylene, heptane, butyl chloride, butyl chloride, trichloro-ethylene, carbon tetrachloride, chlorotrifluoroethane, toluene, paraxylene, chlorobenzene, o-dichlorohenzene, benzene, carrene, ethylene dichloride, isobutanol, n-butanol, butyl acetate, propyl alcohol, methylisobutylketone, oxolane, ethyl acetate, chloroform, methyl ethyl ketone, dioxanes, pyridine, acetone, nitromethane, acetate, acetonitrile, aniline, dimethyl formamide, methyl alcohol, ethylene glycol, n-octyl alcohol, one or more in n-hexyl alcohol, cyclohexanol, DAA, methyl-sulfoxide, carbon disulfide, trichloroethanes, butanone, the ether.
3. the method for the carbon fiber surface modification of plasma coated with nano colloidal sols by plasma treatment according to claim 2; It is characterized in that: described ether is benzinum, propyl ether, diethyl ether, glycol dimethyl ether or glycol monomethyl ether, and described propyl alcohol is isopropyl alcohol or normal propyl alcohol.
4. the method for the carbon fiber surface modification of plasma coated with nano colloidal sols by plasma treatment according to claim 1; It is characterized in that: the plasma producing apparatus of the apparatus for processing plasma of said step (3) is all kinds of plasma generators; Plasma atmosphere is produced by plasma generator, and is ejected into the plasma atmosphere that forms in normal temperature, normal pressure, the atmospheric environment via nozzle mechanism.
5. the method for the carbon fiber surface modification of plasma coated with nano colloidal sols by plasma treatment according to claim 1 is characterized in that: concrete equipment is arranged and can be changed as required.
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