CN105063994A - Surface treatment method for carbon fibers - Google Patents
Surface treatment method for carbon fibers Download PDFInfo
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- CN105063994A CN105063994A CN201510514103.4A CN201510514103A CN105063994A CN 105063994 A CN105063994 A CN 105063994A CN 201510514103 A CN201510514103 A CN 201510514103A CN 105063994 A CN105063994 A CN 105063994A
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Abstract
The invention discloses a surface treatment method for carbon fibers. The method is characterized in that when electrochemical anode oxidation treatment is carried out on the carbon fibers, a carbon fiber bundle is moistened with deionized water firstly and then enters an electrolytic cell to carry out anodic oxidation treatment. Thus, the uniformity of the surface treatment effect of the carbon fibers can be improved, and the adhesive property of the carbon fibers and a resin matrix is better.
Description
Technical field
The present invention relates to a kind of method for surface treatment of carbon fibers, belong to electrochemistry and fibrous material field.
Background technology
Carbon fiber is a kind of reinforcing material grown up after the 1950's, it has high specific strength, high ratio modulus, high temperature resistant, corrosion-resistant, conduction and a series of excellent properties such as thermal coefficient of expansion is little, is therefore widely used in the field such as Aero-Space, sports equipment.Carbon fiber uses mainly as the reinforcement of composite, and its surface-activity directly affects composite material interface adhesive property.Carbon fiber is after high temperature cabonization or graphitization heat treatment, and smooth surface, active site is few, and chemical reactivity is poor, needs to introduce active oxygen-containing functional group by surface oxidation treatment technique at fiber surface, improves the adhesive strength of itself and resin matrix.On Industry of Carbon Fiber, widely used surface treatment method is electrochemistry anodic oxidation, and its oxidation reaction relaxes, and is easy to control, obvious processing effect.But due to the strong hydrophobicity of carbon fiber surface, when the tow of drying enters electrolytic cell, can not be soaked equably by electrolyte fast, cause the uneven of electrochemicial oxidation, carbon fiber and resin matrix compound tense interfacial adhesion is caused to exist discrete, improve the uniformity of surface treatment of carbon fibers, the safe handling of carbon fiber is had great importance.
Summary of the invention
The object of the invention is to solve the problems of the prior art, a kind of surface treatment method of carbon fiber is provided, the method increases the uniformity of whole bundle carbon fiber surface oxidation processes.
For achieving the above object, technical scheme of the present invention is as follows:
A surface treatment method for carbon fiber, is characterized in that, before carbon fiber carries out anodized, is first soaked by carbon fibre tow ionized water, forms liquid film, and then enter electrolytic cell and carry out anodized at carbon fiber surface.
The carbon fiber that described carbon fiber is take polyacrylonitrile as raw material, finished heat treatment temperature obtains within the scope of 1300-3000 DEG C.
The humidity method of carbon fibre tow adopts spray, spraying or dipping.
Wetting carbon fibre tow water content control is in mass ratio 0.5-10%.
Anodized refers to take carbon fiber as anode, and with graphite, stainless steel material for negative electrode, with ammonium salt, alkali or aqueous acid for electrolyte carries out electrochemical anodic oxidation, the current density of applying is 0.5--10mA/cm
2, temperature is room temperature-60 DEG C.
The method of the wetting carbon fibre tow used in the present invention, the method that can adopt spraying, spray or flood, from the angle of minimizing Carbon Fiber Damage, the method for spraying or spray is better.Wetting carbon fibre tow water content control is in mass ratio 0.5-10% scope, and moisture is less than 0.5%, DeGrain, and moisture is greater than 10%, then can cause the significantly change of cell bath concentration, be unfavorable for the raising of surface treatment uniformity.
What the present invention proposed makes carbon fiber surface be formed after moisture film, then enters the method that electrolytic cell carries out anodized, can greatly improve surface-treated uniformity.Its reason is mainly from two aspects:
One is that the moisture film of carbon fiber surface makes its hydrophily improve, and is more easily infiltrated rapidly by electrolyte, uniform electrochemical oxidation reactions occurs; In addition, wetting carbon fibre tow and the contact resistance of anode diminish, and the voltage differences between tow inside and surperficial single fiber is reduced, improves the uniformity of whole bundle carbon fiber surface oxidation processes.
Detailed description of the invention
Below by embodiment, the present invention will be further described:
embodiment 1
3K, PAN base carbon fibre that 1300 DEG C of heat treatment obtains from carbide furnace out after, first adopt the method for spray that carbon fiber is soaked by deionized water, moisture is 2%, then enter electrolytic cell and carry out anodized, the ammonium bicarbonate aqueous solution adopting mass ratio 5% is electrolyte, and current density is 0.2mA/cm
2, temperature 30 DEG C, spends deionized water, 120--260 DEG C temperature range drying, last starching, drying, receipts silk after surface oxidation treatment.Sizing agent is bisphenol A type epoxy resin aqueous emulsion, and starching amount is 1.2%.
Carbon fiber after surface treatment carries out interlaminar shear strength test, and by carbon fiber and bisphenol A type epoxy resin 6101 compound, the volume ratio of fiber and resin is 6:4, curing agent is triethylene tetramine, solidification temperature 80 DEG C, 2 hours hardening times, obtains testing sample.Test result is as follows:
Interlaminar shear strength: 81.5MPa
Coefficient of dispersion: 1.2%.
embodiment 2
3K, PAN base carbon fibre that 2600 DEG C of heat treatment obtains from graphitizing furnace out after, adopt the method for spray that carbon fiber is soaked by deionized water, moisture is 5%, then enter electrolytic cell and carry out anodized, the ammonium bicarbonate aqueous solution adopting mass ratio 5% is electrolyte, and current density is 1.0mA/cm
2, temperature 50 C, other condition is identical with embodiment 1.Test result is as follows:
Interlaminar shear strength: 61.5MPa
Coefficient of dispersion: 0.8%.
comparative example 1
In embodiment 1, carbon fiber from carbide furnace out after, directly enter electrolytic cell and carry out anodized, other is identical with embodiment 1.Test result is as follows:
Interlaminar shear strength: 80.7MPa
Coefficient of dispersion: 4.7%.
comparative example 2
In embodiment 2, carbon fiber from graphitizing furnace out after, directly enter electrolytic cell and carry out anodized, other is identical with embodiment 2.Test result is as follows:
Interlaminar shear strength: 61.0MPa
Coefficient of dispersion: 3.5%.
Effect of the present invention is by the interlaminar shear strength of unidirectional composite laminate of carbon fiber and epoxy resin and the coefficient of dispersion evaluation of interlaminar shear strength, and the evaluation method of interlaminar shear strength is measured by GB GB3357-82 method.Resin matrix adopts epoxy 6101, and curing agent is triethylene tetramine.The coefficient of dispersion Cv of interlaminar shear strength is calculated as follows:
Cv(%)=(S/X)*100%
Wherein, X is the mean value of interlaminar shear strength; S is the standard error often organizing sample, is calculated as follows:
Comparing us and can find by embodiment 1,2 and comparative example 1,2, the coefficient of dispersion having carried out the carbon fibre tow of wettability treatment before anodic oxidation significantly reduces, and the carbon fibre tow anodic oxidation rear surface uniformity namely through wettability treatment is improved.
It is emphasized that: be only preferred embodiment of the present invention above, not any pro forma restriction is done to the present invention, every above embodiment is done according to technical spirit of the present invention any simple modification, equivalent variations and modification, all belong in the scope of technical solution of the present invention.
Claims (5)
1. a surface treatment method for carbon fiber, is characterized in that, before carbon fiber carries out anodized, is first soaked by carbon fibre tow ionized water, forms liquid film, and then enter electrolytic cell and carry out anodized at carbon fiber surface.
2. the surface treatment method of a kind of carbon fiber as claimed in claim 1, is characterized in that, the carbon fiber that described carbon fiber is take polyacrylonitrile as raw material, finished heat treatment temperature obtains within the scope of 1300-3000 DEG C.
3. the surface treatment method of a kind of carbon fiber as claimed in claim 1, is characterized in that, the humidity method of carbon fibre tow adopts spray, spraying or dipping.
4. the surface treatment method of a kind of carbon fiber as claimed in claim 3, is characterized in that, wetting carbon fibre tow water content control is in mass ratio 0.5-10%.
5. the surface treatment method of a kind of carbon fiber as claimed in claim 1, it is characterized in that, described anodized refers to take carbon fiber as anode, with graphite, stainless steel material for negative electrode, with ammonium salt, alkali or aqueous acid for electrolyte carries out electrochemical anodic oxidation, the current density of applying is 0.5--10mA/cm
2, temperature is room temperature-60 DEG C.
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Cited By (8)
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| CN105699377A (en) * | 2016-01-21 | 2016-06-22 | 中国科学院宁波材料技术与工程研究所 | Method for characterizing radial structure of carbon fiber |
| CN106436273A (en) * | 2016-09-14 | 2017-02-22 | 郑州峰泰纳米材料有限公司 | Carbon fiber material surface modification method |
| CN106808715A (en) * | 2016-12-29 | 2017-06-09 | 盐城赛福汽车零部件有限公司 | A kind of preparation method of carbon fibre composite auto parts and components |
| CN108193482A (en) * | 2017-12-22 | 2018-06-22 | 北京化工大学 | A kind of processing method for carbon fiber surface modification |
| CN108486692A (en) * | 2018-04-16 | 2018-09-04 | 中国科学院宁波材料技术与工程研究所 | A kind of processing method and system of high-strength high-modules carbon fibre |
| CN108659651A (en) * | 2018-03-08 | 2018-10-16 | 河北晨阳工贸集团有限公司 | Natural gas heating outer wall pipeline environment-protective water paint 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 |
| CN113622185A (en) * | 2021-08-30 | 2021-11-09 | 陕西天策新材料科技有限公司 | Method for improving surface activity of asphalt-based graphite carbon fiber |
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| CN105699377A (en) * | 2016-01-21 | 2016-06-22 | 中国科学院宁波材料技术与工程研究所 | Method for characterizing radial structure of carbon fiber |
| CN106436273A (en) * | 2016-09-14 | 2017-02-22 | 郑州峰泰纳米材料有限公司 | Carbon fiber material surface modification method |
| CN106808715A (en) * | 2016-12-29 | 2017-06-09 | 盐城赛福汽车零部件有限公司 | A kind of preparation method of carbon fibre composite auto parts and components |
| CN106808715B (en) * | 2016-12-29 | 2018-12-14 | 盐城赛福汽车零部件有限公司 | A kind of preparation method of carbon fibre composite auto parts and components |
| CN108193482A (en) * | 2017-12-22 | 2018-06-22 | 北京化工大学 | A kind of processing method for carbon fiber surface modification |
| CN108659651A (en) * | 2018-03-08 | 2018-10-16 | 河北晨阳工贸集团有限公司 | Natural gas heating outer wall pipeline environment-protective water paint and preparation method thereof |
| CN108486692A (en) * | 2018-04-16 | 2018-09-04 | 中国科学院宁波材料技术与工程研究所 | A kind of processing method and system of high-strength high-modules carbon fibre |
| CN108486692B (en) * | 2018-04-16 | 2024-01-02 | 中国科学院宁波材料技术与工程研究所 | High-strength high-modulus carbon fiber processing method and system |
| 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 |
| CN113622185A (en) * | 2021-08-30 | 2021-11-09 | 陕西天策新材料科技有限公司 | Method for improving surface activity of asphalt-based graphite carbon fiber |
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