CN106436274A - Method for treating carbon fiber anodic oxidation surfaces - Google Patents
Method for treating carbon fiber anodic oxidation surfaces Download PDFInfo
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- CN106436274A CN106436274A CN201610824727.0A CN201610824727A CN106436274A CN 106436274 A CN106436274 A CN 106436274A CN 201610824727 A CN201610824727 A CN 201610824727A CN 106436274 A CN106436274 A CN 106436274A
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- carbon fiber
- anodic oxidation
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- 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
- D06M10/04—Physical treatment combined with treatment with chemical compounds or elements
- D06M10/06—Inorganic compounds or elements
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- 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
- D06M11/64—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 nitrogen oxides; with oxyacids of nitrogen or their salts
- D06M11/65—Salts of oxyacids of nitrogen
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- 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
- D06M11/73—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 carbon or compounds thereof
- D06M11/76—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 carbon or compounds thereof with carbon oxides or carbonates
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- 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
- D06M13/184—Carboxylic acids; Anhydrides, halides or salts thereof
- D06M13/192—Polycarboxylic acids; Anhydrides, halides or salts thereof
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- 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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- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
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- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
- Inorganic Fibers (AREA)
Abstract
The invention provides a method for treating carbon fiber anodic oxidation surfaces. The method includes the steps: 1) soaking carbon fibers by diluted nitric acid solution for 6h-12h under the conditions that ultrasonic power ranges from 100W to 1500W, ultrasonic frequency ranges from 20kHz to 100kHz, and bath temperature ranges from 20 DEG C to 60 DEG C, and flushing by deionized water; 2) performing anodic treatment for flushed carbon fibers in the step 1) in an applied magnetic field with intensity ranging from 2mT-15 mT, taking a graphite plate, a stainless steel plate or a nickel plate as a cathode, performing electrochemical oxidation treatment by ammonium salt electrolyte solution for 15-200s at the temperature ranging from 0 DEG C to 50 DEG C under applied current density ranging from 0.2-8mA/cm<2>, washing, drying, starching, and winding to obtain the carbon fiber anodic oxidation surfaces. According to the treating method, performance of the fibers is effectively improved, tensile strength and shearing strength of the carbon fibers can be improved, and the tensile strength of the carbon fibers cannot be damaged.
Description
Technical field
The invention belongs to carbon fiber processing technology field and in particular to a kind of carbon fiber anodic oxidation surface treatment side
Method.
Background technology
Carbon fiber refers to that the fibrous material more than more than 85% for the phosphorus content, including carbon fibre and graphite through high temperature cabonization
Fiber.Carbon fibre is that after organic fiber is processed through 1000~2300 DEG C, phosphorus content is 85%~95% fiber;Graphite fibre
It is that organic fiber is processed through more than 2300 DEG C, fiber more than 98% for the phosphorus content.Carbon fiber as a kind of high-performance fiber, because
There is the characteristics such as specific strength is high, specific modulus is high, thermal coefficient of expansion is little, coefficient of friction is low, resistance to low temperature is good and become in recent years
Carry out the most important reinforcing material of polymer matrix composites, be widely used in Aero-Space component and sports goods.Carbon fiber
Surface is inert, and specific surface area is little, and edge active carbon atom is few, and surface energy is low and resin wellability and two-phase interface caking property
Difference, composite interlayer shear strength (Interlaminar Shearing Strength, ILSS) is low, thus affecting composite wood
The performance of material combination property, the further genralrlization constraining carbon fiber in advanced field of compound material is applied.Fine in order to improve carbon
The performance of dimension reinforced resin based composites, must be modified to carbon fiber surface, to improve the viscous of carbon fiber and other materials
Knot ability.
In various surface treatment methods, electrochemical oxidation method can continuously produce because it has, simple to operation, process
The features such as mild condition is easily controllable, is industrially used widely, but its equally exist intrinsic anti-to damage carbon fiber
The drawbacks of Zhang Qiangdu improves Properties of Carbon Fiber Surface for cost.The reduction of carbon fiber tensile strength is mostly derived from surface treatment process
Middle deep oxidation corrasion introduces new defect in carbon fiber surface.These defects come from the orderly crystal layer of outer layer and peel off
The weak spot that the inside disordered structure exposing afterwards increases in fiber bodies.For surface treatment of carbon fibers process tensile strength fall
The low origin cause of formation, we are modified to carbon fiber surface defect by appropriate corrasion;And by suitable electrochemical treatments
Grain refining effect is produced on carbon fiber, reduces crystallite dimension, produce newborn crystal boundary in a large number, stop the extension of crackle;Reach same
The intrinsic tensile strength of Shi Tigao carbon fiber and the purpose of interlaminar shear strength.
To improve for the purpose of carbon fiber surface structure improves tensile strength, research is few at present, more rarely has with electrochemical oxidation
Method improves the intrinsic tensile strength of carbon fiber and its report of composite interlayer shear strength simultaneously.
Content of the invention
The present invention proposes a kind of method of carbon fiber anodic oxidation surface treatment, and this processing method is effectively improved the property of fiber
Can, tensile strength and the shear strength of carbon fiber can not only be improved, and the tensile strength of carbon fiber body will not be damaged.
The technical scheme is that and be achieved in that:
A kind of method of carbon fiber anodic oxidation surface treatment, comprises the following steps:
1) in ultrasonic power 100W~1500W, ultrasonic frequency 20kHz~100kHz, 20 DEG C~60 DEG C of bath temperature
Under conditions of, carbon fiber is carried out immersion treatment 6h~12h with dilute nitric acid solution, then deionized water is rinsed well;
2) by step 1) rinse well after carbon fiber carry out anodization, the intensity of externally-applied magnetic field in externally-applied magnetic field
For 2~15mT, using graphite cake, corrosion resistant plate, copper coin or nickel plate as negative electrode, carry out electrochemistry oxygen with ammonium salt class electrolyte solution
Change is processed, and treatment temperature is 0~50 DEG C, controls and applies electric current density 0.2~8mA/cm2, process 15~200s, subsequently wash,
Drying, starching, winding are obtained.
Further, the concentration of described dilute nitric acid solution is 10~15wt%.
Further, described ammonium salt class electrolyte solution is sal volatile, ammonium nitrate solution or ammonium oxalate solution.
Further, the concentration of described ammonium salt class electrolyte solution is 0.02~0.8mol/L.
Further, step 2) applying electric current density be 1~4mA/cm2.
Further, described step 2) the electrochemicial oxidation time be 60~120s.
Further, carbon fiber is polyacrylonitrile-based carbon fibre or asphalt base carbon fiber..
Beneficial effects of the present invention:
1st, with dust technology, pretreatment is carried out to carbon fiber under ultrasound condition of the present invention, has activated the group of carbon fiber surface,
Improve the wellability of carbon fiber simultaneously, improve the caking property between carbon fiber and resin matrix, make carbon fiber and other materials
In conjunction with interface performance be improved.
2nd, during electrochemicial oxidation under additional magnetic strips part, with ammonium salt as electrolyte solution, accelerate carbon fiber surface
Face processing speed, is conducive to improving tensile strength and the shear strength of carbon fiber simultaneously.
Specific embodiment
All using carbon containing mass ratio > 90%, tensile strength 3.25Gpa, interlaminar shear strength is 73.0Mpa to following example
Polyacrylonitrile carbon fiber be unmodified carbon fiber.But the present invention is not limited to this carbon fiber.
Comparing embodiment 1
By carbon fiber by filling 30 DEG C, the electrochemical processing cell of 0.5mol/l oxalic acid aqueous ammonium, by the time be
100s, does not apply electric current, subsequently cleans at room temperature, 100 DEG C of dryings, gluing, collects product.
Embodiment 1
A kind of method of carbon fiber anodic oxidation surface treatment, comprises the following steps:
1) under conditions of ultrasonic power 100W, ultrasonic frequency 20kHz, 20 DEG C of bath temperature, carbon fiber is used
10wt% dilute nitric acid solution carries out immersion treatment 6h, and then deionized water is rinsed well;
2) by step 1) rinse well after carbon fiber carry out anodization, the intensity of externally-applied magnetic field in externally-applied magnetic field
For 2mT, using copper coin as negative electrode, carry out electrochemicial oxidation with 0.02mol/L ammonium carbonate electrolyte solution, treatment temperature is
0 DEG C, control and apply electric current density 0.2mA/cm2, process 150s, subsequently washing, drying, starching, winding is obtained.
Embodiment 2
A kind of method of carbon fiber anodic oxidation surface treatment, comprises the following steps:
1) under conditions of ultrasonic power 500W, ultrasonic frequency 40kHz, 30 DEG C of bath temperature, carbon fiber is used
12wt% dilute nitric acid solution carries out immersion treatment 8h, and then deionized water is rinsed well;
2) by step 1) rinse well after carbon fiber carry out anodization, the intensity of externally-applied magnetic field in externally-applied magnetic field
For 6mT, using graphite cake as negative electrode, carry out electrochemicial oxidation, treatment temperature with 0.4mol/L ammonium nitrate electrolyte solution
For 20 DEG C, control and apply electric current density 3mA/cm2, process 30s, subsequently washing, drying, starching, winding is obtained.
Embodiment 3
A kind of method of carbon fiber anodic oxidation surface treatment, comprises the following steps:
1) under conditions of ultrasonic power 1000W, ultrasonic frequency 60kHz, 50 DEG C of bath temperature, carbon fiber is used
14wt% dilute nitric acid solution carries out immersion treatment 10h, and then deionized water is rinsed well;
2) by step 1) rinse well after carbon fiber carry out anodization, the intensity of externally-applied magnetic field in externally-applied magnetic field
For 10mT, using nickel plate as negative electrode, carry out electrochemicial oxidation with 0.6mol/L ammonium oxalate electrolyte solution, treatment temperature is
40 DEG C, control and apply electric current density 6mA/cm2, process 60s, subsequently washing, drying, starching, winding is obtained.
Embodiment 4
A kind of method of carbon fiber anodic oxidation surface treatment, comprises the following steps:
1) under conditions of ultrasonic power 1500W, ultrasonic frequency 100kHz, 60 DEG C of bath temperature, carbon fiber is used
15wt% dilute nitric acid solution carries out immersion treatment 12h, and then deionized water is rinsed well;
2) by step 1) rinse well after carbon fiber carry out anodization, the intensity of externally-applied magnetic field in externally-applied magnetic field
For 15mT, using graphite cake as negative electrode, carry out electrochemicial oxidation, treatment temperature with 0.8mol/L ammonium oxalate electrolyte solution
For 50 DEG C, control and apply electric current density 8mA/cm2, process 100s, subsequently washing, drying, starching, winding is obtained.
Embodiment 5
The carbon fiber modified to embodiment 1, embodiment 1-5 is tested carbon fiber body tension according to GB3362-2005
Intensity, tests carbon fiber and composite interlayer shear strength according to GB3357-82, and result is as follows:
The tensile strength of comparative example 1 is 3.23GPa, and interlaminar shear strength is 74.8MPa;
The tensile strength of embodiment 1 is 4.36GPa, and interlaminar shear strength is 86.4MPa;
The tensile strength of embodiment 2 is 4.57GPa, and interlaminar shear strength is 87.2MPa;
The tensile strength of embodiment 3 is 4.75GPa, and interlaminar shear strength is 91.2MPa;
The tensile strength of embodiment 4 is 4.87GPa, and interlaminar shear strength is 92.4MPa.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all essences in the present invention
Within god and principle, any modification, equivalent substitution and improvement made etc., should be included within the scope of the present invention.
Claims (7)
1. a kind of method of carbon fiber anodic oxidation surface treatment is it is characterised in that comprise the following steps:
1) ultrasonic power 100W~1500W, ultrasonic frequency 20kHz~100kHz, 20 DEG C~60 DEG C of bath temperature bar
Under part, carbon fiber is carried out immersion treatment 6h~12h with dilute nitric acid solution, then deionized water is rinsed well;
2) by step 1) rinse well after carbon fiber carry out anodization in externally-applied magnetic field, the intensity of externally-applied magnetic field is 2
~15mT, using graphite cake, corrosion resistant plate, copper coin or nickel plate as negative electrode, carries out electrochemical oxidation with ammonium salt class electrolyte solution
Process, treatment temperature is 0~50 DEG C, control and apply electric current density 0.2~8mA/cm2, process 15~200s, subsequently wash, do
Dry, starching, winding are obtained.
2. the method for carbon fiber anodic oxidation surface treatment according to claim 1 is it is characterised in that described dust technology is molten
The concentration of liquid is 10~15wt%.
3. the method for carbon fiber anodic oxidation surface treatment according to claim 1 is it is characterised in that described ammonium salt class is electric
Electrolyte solution is sal volatile, ammonium nitrate solution or ammonium oxalate solution.
4. the method for carbon fiber anodic oxidation surface treatment according to claim 3 is it is characterised in that described ammonium salt class is electric
The concentration of electrolyte solution is 0.02~0.8mol/L.
5. the method for carbon fiber anodic oxidation according to claim 1 and 2 surface treatment is it is characterised in that step 2) apply
Powering up current density is 1~4mA/cm2.
6. the method for carbon fiber anodic oxidation according to claim 1 and 2 surface treatment is it is characterised in that described step
2) the electrochemicial oxidation time is 60~120s.
7. the method for carbon fiber anodic oxidation surface treatment according to claim 1 is it is characterised in that carbon fiber is poly- third
Alkene itrile group carbon fiber or asphalt base carbon fiber.
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Cited By (10)
Publication number | Priority date | Publication date | Assignee | Title |
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CN107385896A (en) * | 2017-07-05 | 2017-11-24 | 北京航空航天大学 | A kind of organic matter immersion and the method for electrochemicial oxidation carbon fiber |
CN108625151A (en) * | 2018-05-29 | 2018-10-09 | 安徽睿知信信息科技有限公司 | A kind of surface treatment method of high-strength carbon fiber |
CN111286773A (en) * | 2020-02-21 | 2020-06-16 | 石河子大学 | Preparation method for enhancing adsorption performance of graphite felt material by electrochemical anodic oxidation |
CN111793857A (en) * | 2020-06-30 | 2020-10-20 | 镇江市高等专科学校 | Carbon fiber surface treatment method |
CN112941965A (en) * | 2021-01-26 | 2021-06-11 | 中国建筑材料科学研究总院有限公司 | Carbon fiber filter paper and preparation method thereof |
CN113502662A (en) * | 2021-08-09 | 2021-10-15 | 陕西天策新材料科技有限公司 | Surface treatment method of asphalt-based graphite carbon fiber |
CN113502656A (en) * | 2021-08-03 | 2021-10-15 | 长春工业大学 | Preparation method of high-specific-surface carbon fiber suitable for carbon paper |
CN113924933A (en) * | 2021-11-12 | 2022-01-14 | 安徽和美生态农业科技有限公司 | Planting method of sweet potatoes rich in SOD |
CN115959870A (en) * | 2022-12-30 | 2023-04-14 | 中建商品混凝土有限公司 | Anti-cracking low-carbon high-performance concrete and preparation method thereof |
CN116122038A (en) * | 2022-12-30 | 2023-05-16 | 中国人民解放军军事科学院系统工程研究院 | Carbon fiber sizing agent removing method |
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CN103321036A (en) * | 2013-06-29 | 2013-09-25 | 西北工业大学 | Method for electrochemically modifying surface of ultrasonic-enhanced carbon fiber |
CN104562631A (en) * | 2013-10-21 | 2015-04-29 | 大连市沙河口区中小微企业服务中心 | Anodic oxidation surface treatment method of carbon fibers |
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CN101660185A (en) * | 2009-09-25 | 2010-03-03 | 北京化工大学 | Method of strong effect carbon fiber anodic oxidation surface treatment |
CN102628212A (en) * | 2012-04-06 | 2012-08-08 | 武汉理工大学 | Carbon fiber surface treatment method based on ultrasonic strengthening |
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Cited By (12)
Publication number | Priority date | Publication date | Assignee | Title |
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CN107385896A (en) * | 2017-07-05 | 2017-11-24 | 北京航空航天大学 | A kind of organic matter immersion and the method for electrochemicial oxidation carbon fiber |
CN107385896B (en) * | 2017-07-05 | 2019-07-23 | 北京航空航天大学 | A kind of method of organic matter immersion and electrochemicial oxidation carbon fiber |
CN108625151A (en) * | 2018-05-29 | 2018-10-09 | 安徽睿知信信息科技有限公司 | A kind of surface treatment method of high-strength carbon fiber |
CN111286773A (en) * | 2020-02-21 | 2020-06-16 | 石河子大学 | Preparation method for enhancing adsorption performance of graphite felt material by electrochemical anodic oxidation |
CN111793857A (en) * | 2020-06-30 | 2020-10-20 | 镇江市高等专科学校 | Carbon fiber surface treatment method |
CN112941965A (en) * | 2021-01-26 | 2021-06-11 | 中国建筑材料科学研究总院有限公司 | Carbon fiber filter paper and preparation method thereof |
CN113502656A (en) * | 2021-08-03 | 2021-10-15 | 长春工业大学 | Preparation method of high-specific-surface carbon fiber suitable for carbon paper |
CN113502662A (en) * | 2021-08-09 | 2021-10-15 | 陕西天策新材料科技有限公司 | Surface treatment method of asphalt-based graphite carbon fiber |
CN113924933A (en) * | 2021-11-12 | 2022-01-14 | 安徽和美生态农业科技有限公司 | Planting method of sweet potatoes rich in SOD |
CN115959870A (en) * | 2022-12-30 | 2023-04-14 | 中建商品混凝土有限公司 | Anti-cracking low-carbon high-performance concrete and preparation method thereof |
CN116122038A (en) * | 2022-12-30 | 2023-05-16 | 中国人民解放军军事科学院系统工程研究院 | Carbon fiber sizing agent removing method |
CN116122038B (en) * | 2022-12-30 | 2024-02-27 | 中国人民解放军军事科学院系统工程研究院 | Carbon fiber sizing agent removing method |
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