CN108625151A - A kind of surface treatment method of high-strength carbon fiber - Google Patents
A kind of surface treatment method of high-strength carbon fiber Download PDFInfo
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- D06M10/00—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements
- D06M10/02—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements ultrasonic or sonic; Corona discharge
- D06M10/025—Corona discharge or low temperature plasma
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
- C08J5/06—Reinforcing macromolecular compounds with loose or coherent fibrous material using pretreated fibrous materials
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- D06M10/00—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements
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- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/50—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with hydrogen peroxide or peroxides of metals; with persulfuric, permanganic, pernitric, percarbonic acids or their salts
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- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/58—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with nitrogen or compounds thereof, e.g. with nitrides
- D06M11/59—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with nitrogen or compounds thereof, e.g. with nitrides with ammonia; with complexes of organic amines with inorganic substances
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- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
- D06M13/12—Aldehydes; Ketones
- D06M13/127—Mono-aldehydes, e.g. formaldehyde; Monoketones
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
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- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/40—Fibres of carbon
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Abstract
The invention discloses a kind of surface treatment methods of high-strength carbon fiber, include the following steps：S1, carbon fiber is subjected to low temperature plasma bombardment processing；S2, step S1 treated carbon fiber Wesys acetone soln is subjected to immersion treatment 30s~120s, is then rinsed well with deionized water；S3, step S2 treated carbon fibers are subjected to surface modification using liquid phase oxidation；S4, by step S3, treated that carbon fiber is rinsed well with deionized water, and liquid film is formed in carbon fiber surface；S5, by step S4, treated that carbon fiber enters that electrolytic cell carries out anodized；S6, by step S5, treated that carbon fiber impregnates 1 10 seconds continuously across ammonia spirit, and carbon fiber is made in drying, starching, winding.Compared with traditional technology, this method surface treatment speed is fast, and efficient, carbon fiber surface surface damage is small；Device is simple and practicable, easy to operate, is suitble to industrial large-scale production.
Description
Technical field
The invention belongs to the technical field of surface of carbon fiber, more specifically more particularly to a kind of high intensity carbon fiber
The surface treatment method of dimension.
Background technology
Carbon fiber has excellent mechanical property (especially tensile property), therefore through the enhancing frequently as composite material
Phase, especially carbon fiber enhancement resin base composite material have obtained more and more extensive attention and application.The mechanics of composite material
Performance additionally depends on the transmission situation of interfacial stress other than depending on the mechanical property of reinforced phase and matrix.The table of carbon fiber
Face is in chemical inertness, and surface energy is low, is lyophobicity, causes its imperfect bonding with matrix, therefore carbon fiber will before use
By surface treatment.Currently, surface treatment of carbon fibers is mainly the desire to the chemical mobility of the surface of enhancing carbon fiber, enhance carbon fiber
Interface binding intensity between matrix, to enhance the performance of composite material.
Carbon fiber is a kind of high-performance special fiber, and for carbon content 90% or more, the oxygen-containing nitrogen-containing group in surface is few, must
It must be surface-treated, by enhancing its interface adhesion with matrix resin, the excellent properties of carbon fiber could be multiple
It is not fully exerted in condensation material.
Invention content
The purpose of the present invention is to solve disadvantages existing in the prior art, and a kind of high-strength carbon fiber proposed
Surface treatment method.
To achieve the above object, the present invention provides the following technical solutions：
A kind of surface treatment method of high-strength carbon fiber, includes the following steps：
S1, carbon fiber is subjected to low temperature plasma bombardment processing；
S2, step S1 treated carbon fiber Wesys acetone soln is subjected to immersion treatment 30s~120s, then uses deionization
Water is rinsed well, and fiber surface slurry is removed；
S3, step S2 treated carbon fibers are subjected to surface modification, the oxidant that surface is modified using liquid phase oxidation
For potassium permanganate, the additive amount of potassium permanganate is 6-15%owf, and surface treatment temperature is 60-100 DEG C, and the surface treatment time is
2-6 hours；
S4, by step S3, treated that carbon fiber is rinsed well with deionized water, and liquid film is formed in carbon fiber surface；
S5, by step S4, treated that carbon fiber enters that electrolytic cell carries out anodized；
S6, step S5 treated carbon fibers are impregnated 1-10 second continuously across ammonia spirit, drying, starching wind and make
Obtain carbon fiber.
Preferably, the mass fraction of ammonium hydroxide is 15-30% in the step S6.
Preferably, deionized water purging method is carried out using spray, spraying or dipping to carbon fiber in the step S4.
Preferably, treatment temperature is 20~40 DEG C in the step S5, and control applies 0.1~10mA/cm2 of current density,
Handle 60~220s.
Preferably, the step S5 Anodic Oxidations processing refers to using carbon fiber as anode, is the moon with graphite, stainless steel material
Pole carries out electrochemical anodic oxidation by electrolyte of alkalescent electrolyte, and temperature is 20-60 DEG C.
The technique effect and advantage of the present invention：A kind of surface treatment method of high-strength carbon fiber provided by the invention, with
Traditional technology is compared, and this method surface treatment speed is fast, and efficient, carbon fiber surface surface damage is small；Device is simple and practicable, operation side
Just, it is suitble to industrial large-scale production.
The present invention should remove carbon fiber surface sizing agent (or using no starching carbon fiber) before surface treatment, by third
It is impregnated in ketone solution, dissolve and removes carbon fiber surface sizing agent.
After surface treatment, the interfacial adhesion of carbon fiber and resin matrix is enhanced, carbon fibre composite is improved
Interlaminar shear strength, while to its body tensile strength damage very little.
It is acted on by potassium permanganate oxidation, in carbon fiber surface generation-COOH ,-OH isopolarities group to improve carbon fiber
The chemism in dimension table face reduces its contact angle with liquid.
Carbon fiber needs, by processing such as cleaning-dryings, the residual of carbon fiber surface to be eliminated with cleaning after surface treatment
Object avoids residual chemicals from continuing to react with carbon fiber, causes the damage of carbon fiber, reduce its mechanical property.
Specific implementation mode
In order to make the purpose , technical scheme and advantage of the present invention be clearer, below in conjunction with specific embodiment, to this
Invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, not
For limiting the present invention.Based on the embodiments of the present invention, those of ordinary skill in the art are not before making creative work
The every other embodiment obtained is put, shall fall within the protection scope of the present invention.
Embodiment 1
A kind of surface treatment method of high-strength carbon fiber, includes the following steps：
S1, carbon fiber is subjected to low temperature plasma bombardment processing：Low temperature plasma bombardment process be：It will experience height
Carbon fiber after temperature carbonization continues through low temperature plasma emitter with 150m/h speed, makes carbon fiber apart from plasma
Emission source 50mm, plasma emission power are 900W/ beams, and treatment temperature is 80 DEG C.；
S2, measurement mass fraction are 30% aqueous acetone solution, by step S1 treated carbon fiber Wesy aqueous acetone solutions into
Row immersion treatment 60s, is then rinsed well with deionized water, removes fiber surface slurry；
S3, step S2 treated carbon fibers are subjected to surface modification, the oxidant that surface is modified using liquid phase oxidation
Additive amount for potassium permanganate, potassium permanganate is 6%owf, and surface treatment temperature is 60 DEG C, and the surface treatment time is 2 hours；
S4, by step S3, treated that carbon fiber is rinsed well with deionized water, and liquid film is formed in carbon fiber surface；
S5, by step S4, treated that carbon fiber enters that electrolytic cell carries out anodized；
S6, step S5 treated carbon fibers are impregnated 5 seconds continuously across ammonia spirit, drying, starching, the obtained carbon of winding
Fiber.
Specifically, the mass fraction of ammonium hydroxide is 20% in the step S6.
Specifically, carrying out deionized water purging method using spray, spraying or dipping to carbon fiber in the step S4.
Specifically, treatment temperature is 20 DEG C in the step S5, control applies current density 5mA/cm2, handles 60s.
Specifically, the step S5 Anodic Oxidations processing refers to using carbon fiber as anode, it is the moon with graphite, stainless steel material
Pole carries out electrochemical anodic oxidation by electrolyte of alkalescent electrolyte, and temperature is 30 DEG C.Electrochemical anodic oxidation processing is not only
It can be good at generating coordinated effect with the processed carbon fiber of aqueous acetone solution, and Gao Meng be used alone before avoiding
The damage for the carbon fiber ontology that sour potassium is brought as oxidant.
Embodiment 2
A kind of surface treatment method of high-strength carbon fiber, includes the following steps：
S1, carbon fiber is subjected to low temperature plasma bombardment processing：Low temperature plasma bombardment process be：It will experience height
Carbon fiber after temperature carbonization continues through low temperature plasma emitter with 100m/h speed, makes carbon fiber apart from plasma
Emission source 20mm, plasma emission power are 100W/ beams, and treatment temperature is 50 DEG C.
When carbon fiber is by low-temperature plasma processing equipment, the electronics in low temperature plasma obtains energy from electric field
As free high energy electron, the excitation molecule, atom, ion and the free radical that thus generate have higher chemical reactivity,
The weak floor structure of carbon fiber surface can be removed, morphology is improved, reduces the loss of carbon fiber tensile strength；Meanwhile
The energy of the high energy electron is less than high-energy ray, pertains only to material surface, does not influence the performance of matrix；
S2, measurement mass fraction are 35% aqueous acetone solution, by step S1 treated carbon fiber Wesy aqueous acetone solutions into
Row immersion treatment 120s, is then rinsed well with deionized water, removes fiber surface slurry；
S3, step S2 treated carbon fibers are subjected to surface modification, the oxidant that surface is modified using liquid phase oxidation
Additive amount for potassium permanganate, potassium permanganate is 15%owf, and surface treatment temperature is 100 DEG C, and the surface treatment time is 6 hours；
S4, by step S3, treated that carbon fiber is rinsed well with deionized water, and liquid film is formed in carbon fiber surface；
S5, by step S4, treated that carbon fiber enters that electrolytic cell carries out anodized；
S6, step S5 treated carbon fibers are impregnated 10 seconds continuously across ammonia spirit, drying, starching, winding are obtained
Carbon fiber.
Specifically, the mass fraction of ammonium hydroxide is 30% in the step S6.
Specifically, carrying out deionized water purging method using spray, spraying or dipping to carbon fiber in the step S4.
Specifically, treatment temperature is 40 DEG C in the step S5, control applies current density 10mA/cm2, handles 220s.
Specifically, the step S5 Anodic Oxidations processing refers to using carbon fiber as anode, it is the moon with graphite, stainless steel material
Pole carries out electrochemical anodic oxidation by electrolyte of alkalescent electrolyte, and temperature is 40 DEG C.Electrochemical anodic oxidation processing is not only
It can be good at generating coordinated effect with the processed carbon fiber of aqueous acetone solution, and Gao Meng be used alone before avoiding
The damage for the carbon fiber ontology that sour potassium is brought as oxidant.
In summary：A kind of surface treatment method of high-strength carbon fiber provided by the invention should compared with traditional technology
Method surface treatment speed is fast, and efficient, carbon fiber surface surface damage is small；Device is simple and practicable, easy to operate, is suitble to industrial big
Large-scale production.
The present invention should remove carbon fiber surface sizing agent (or using no starching carbon fiber) before surface treatment, by third
It is impregnated in ketone solution, dissolve and removes carbon fiber surface sizing agent.
After surface treatment, the interfacial adhesion of carbon fiber and resin matrix is enhanced, carbon fibre composite is improved
Interlaminar shear strength, while to its body tensile strength damage very little.
It is acted on by potassium permanganate oxidation, in carbon fiber surface generation-COOH ,-OH isopolarities group to improve carbon fiber
The chemism in dimension table face reduces its contact angle with liquid.
Carbon fiber needs, by processing such as cleaning-dryings, the residual of carbon fiber surface to be eliminated with cleaning after surface treatment
Object avoids residual chemicals from continuing to react with carbon fiber, causes the damage of carbon fiber, reduce its mechanical property.
Finally it should be noted that：The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention,
Although the present invention is described in detail referring to the foregoing embodiments, for those skilled in the art, still may be used
With technical scheme described in the above embodiments is modified or equivalent replacement of some of the technical features,
All within the spirits and principles of the present invention, any modification, equivalent replacement, improvement and so on should be included in the present invention's
Within protection domain.
Claims (5)
1. a kind of surface treatment method of high-strength carbon fiber, it is characterised in that：Include the following steps：
S1, carbon fiber is subjected to low temperature plasma bombardment processing；
S2, step S1 treated carbon fiber Wesys acetone soln is subjected to immersion treatment 30s~120s, is then rushed with deionized water
Wash clean removes fiber surface slurry；
S3, step S2 treated carbon fibers are subjected to surface modification using liquid phase oxidation, the oxidant that surface is modified is height
The additive amount of potassium manganate, potassium permanganate is 6-15%owf, and surface treatment temperature is 60-100 DEG C, and the surface treatment time is that 2-6 is small
When；
S4, by step S3, treated that carbon fiber is rinsed well with deionized water, and liquid film is formed in carbon fiber surface；
S5, by step S4, treated that carbon fiber enters that electrolytic cell carries out anodized；
S6, step S5 treated carbon fibers are impregnated 1-10 second continuously across ammonia spirit, drying, starching wind obtained carbon
Fiber.
2. a kind of surface treatment method of high-strength carbon fiber described in claim 1, it is characterised in that：Ammonia in the step S6
The mass fraction of water is 15-30%.
3. a kind of surface treatment method of high-strength carbon fiber described in claim 1, it is characterised in that：It is right in the step S4
Carbon fiber carries out deionized water purging method using spray, spraying or dipping.
4. a kind of surface treatment method of high-strength carbon fiber described in claim 1, it is characterised in that：In the step S5
It is 20~40 DEG C to manage temperature, and control applies 0.1~10mA/cm2 of current density, handles 60~220s.
5. a kind of surface treatment method of high-strength carbon fiber described in claim 1, it is characterised in that：The step S5 middle-jiao yang, function of the spleen and stomach
Pole oxidation processes refer to using carbon fiber as anode, using graphite, stainless steel material as cathode, are carried out by electrolyte of alkalescent electrolyte
Electrochemical anodic oxidation, temperature are 20-60 DEG C.
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Cited By (5)
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| CN110029485A (en) * | 2019-04-29 | 2019-07-19 | 安徽巨创化纤科技有限公司 | A kind of preprocess method of filter cloth spraying |
| CN110396814A (en) * | 2019-08-13 | 2019-11-01 | 北京理工大学 | The method and device of the anodized carbon fiber of plasma enhancing |
| CN110528277A (en) * | 2019-08-21 | 2019-12-03 | 大同新成新材料股份有限公司 | A kind of surface treatment method of carbon fiber |
| CN110592927A (en) * | 2019-08-28 | 2019-12-20 | 大同新成新材料股份有限公司 | Surface treatment method of carbon fiber |
| CN111074525A (en) * | 2020-01-02 | 2020-04-28 | 广州黑希复合材料科技有限公司 | Carbon fiber cloth surface treatment process |
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| CN111074525A (en) * | 2020-01-02 | 2020-04-28 | 广州黑希复合材料科技有限公司 | Carbon fiber cloth surface treatment process |
| CN111074525B (en) * | 2020-01-02 | 2021-10-01 | 广州黑希复合材料科技有限公司 | Carbon fiber cloth surface treatment process |
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