CN103835117A - Carbon fiber surface treatment method - Google Patents
Carbon fiber surface treatment method Download PDFInfo
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- CN103835117A CN103835117A CN201210481067.2A CN201210481067A CN103835117A CN 103835117 A CN103835117 A CN 103835117A CN 201210481067 A CN201210481067 A CN 201210481067A CN 103835117 A CN103835117 A CN 103835117A
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Abstract
The invention provides a carbon fiber surface treatment method. Carbon fibers are placed in a solution of a treatment agent and undergo ultrasonic treatment, and the treatment agent includes a solvent, an alkaline compound, silicone oil and/or modified silicone oil, and a chemical treatment agent. Compared with the steam or chemical modification treatment of the carbon fibers in the prior art, the method adopting ultrasonic waves to carry out the surface treatment of the carbon fibers has the following advantages: 1, the propagation of ultrasonic waves in a liquid enables the intensification and the bursting of energy to be generated, and the instant impact force is utilized to smash the carbon fibers, so the openability of the carbon fibers is improved, and the fibers are in a single fiber state, thereby the netting uniformity and the thermodynamic stability of a carbon fiber heat field material are improved; and 2, the instant impact force can also smash surface impurities or weaken the adsorption effect between the impurities and an object, so the separation of the impurities from the object is accelerated, thereby the obtained treated carbon fibers have a good flexibility and a good antistatic property, and the fragility of the carbon fibers is improved.
Description
Technical field
The invention belongs to material modification technical field, relate in particular to a kind of method of surface treatment of carbon fibers.
Background technology
Carbon fiber is the fibrous carbon material that phosphorus content is greater than 90%, it has the premium properties such as high-tensile strength, high stretch modulus, low-density, high temperature resistant, anti-ablation, anticorrosive, high conduction and thermal conductance, low-thermal-expansion self-lubricating and good biocompatibility, is desirable resistance to ablation, 26S Proteasome Structure and Function composite constituent element.At present, carbon fiber and composite thereof are mainly used in the aspects such as the manufacture of the hard-core technology industry such as aerospace, aviation, atomic energy and sports equipment.
As a kind of novel high-performance fiber, the prefabricated component that the net tire that carbon fiber superimposed fiber is made and carbon cloth form through acupuncture all has special high-temperature mechanics and thermal property, both all have the characteristics such as excellent elevated temperature strength, wear-resistant and high temperature resistant ablation, are therefore widely used in high temperature thermal field material.But due to easily crisp, easily broken, the feature such as rigidity is large, elastic modelling quantity is little of carbon fiber self, between fiber, collude with powerful poorly, cause later stage production and processing inconvenience, therefore must carry out surface treatment to its carbon fiber and improve its surface-activity.
Application number is that 201010547718.4 Chinese patent discloses a kind of carbon fiber composite pricking prefabricated body and preparation method, wherein the method for carbon fiber modifying is: the short silk of the carbon fiber that is 40 ~ 50mm by length sprays moisture, make the humidity of staple fibre remain on 5% left and right, be heated to afterwards 30 ℃, insulation 25h.Adopt the short silk of the method carbon fiber after treatment owing to not passing through water-bath or chemical treatment modification, just spray certain moisture at carbon fiber surface, therefore, carbon fiber surface after treatment still contains a large amount of colloids and is sticked together, dispersed and flexibility is not all well improved, after impact, road becomes net and acupuncture effect, and then affects the total quality of net tire.
Application number is that 02138191.7 Chinese patent discloses a kind of non-woven needle-punched fabric and quasi three-dimensional prefab, it adopts fibre length is the polyacrylonitrile-based carbon fibre of 50 ~ 100mm, and it is 40 ~ 120g/m that surface density is made in, combing loose through steam or chemical modification processing, machinery, acupuncture
2thin layer net tire.The carbon fiber obtaining by steam or chemical modification processing method, between fiber, poor, the easy adhesion of discreteness becomes piece, affects rear road shredding, carding effect, and then affects the uniformity of net tire, brings very large hidden danger to properties of product.
Summary of the invention
In view of this, the technical problem to be solved in the present invention is to provide a kind of method of surface treatment of carbon fibers, and the carbon fiber of the method processing is better dispersed.
The invention provides a kind of method of surface treatment of carbon fibers, carry out ultrasonic wave processing after carbon fiber is placed in to finishing agent solution, described finishing agent comprises solvent, strongly alkaline compound, silicone oil and/or modified silicon oil and chemical treatments.
Preferably, the length of described carbon fiber is 40 ~ 80mm.
Preferably, the frequency of described ultrasonic wave processing is 28 ~ 60KHz.
Preferably, the temperature of described ultrasonic wave processing is 20 ~ 80 ℃, and the time is 10 ~ 60min.
Preferably, described solvent is selected from one or more in water, acetone and ethanol.
Preferably, described strongly alkaline compound is NaOH or potassium hydroxide.
Preferably, described chemical treatments is antistatic finishing agent or softener.
Preferably, the mass ratio of described carbon fiber and finishing agent solution is (1:50) ~ (1: 100).
Preferably, the mass ratio of described solvent, strongly alkaline compound, silicone oil and/or modified silicon oil and chemical treatments is (1 ~ 4): 1:1:1.
Preferably, the quality of described finishing agent is 1% ~ 8% of finishing agent solution quality.
The invention provides a kind of method of surface treatment of carbon fibers, carry out ultrasonic wave processing after carbon fiber is placed in to finishing agent solution, described finishing agent comprises solvent, strongly alkaline compound, silicone oil and/or modified silicon oil and chemical treatments.Compared with available technology adopting steam or chemical modification Treatment of Carbon, the present invention adopts ultrasonic wave to carry out surface treatment to carbon fiber, first, ultrasonic wave is propagated and can energy-producingly be intensified and happen suddenly in liquid, utilize instant impact can smash carbon fiber, that has improved carbon fiber can opening character, easily makes to be between fiber single fiber state, and then has improved the thermodynamic stability that becomes net uniformity and carbon fiber thermal field material; Secondly, moment impulse force also can smash surface impurity or weaken the suction-operated between impurity and object, impel between impurity and object and accelerate to depart from, make carbon fiber after treatment there is good flexibility and antistatic behaviour, and improved easy the to be crisp characteristic of carbon fiber.
Experimental result shows, the carbon fiber shredding rate after treatment that the present invention obtains can reach more than 90%.
The specific embodiment
The invention provides a kind of method of surface treatment of carbon fibers, the method is: after carbon fiber is placed in to finishing agent solution, carry out ultrasonic wave processing, described finishing agent comprises solvent, strongly alkaline compound, silicone oil and/or modified silicon oil and chemical treatments.
Wherein, the specification that the specification of described carbon fiber is carbon fiber well known to those skilled in the art, there is no special restriction, is preferably 3K, 6K, 12K, 24K or 48K in the present invention.
The length of described carbon fiber is 40 ~ 80mm, is preferably 40 ~ 70mm, more preferably 40 ~ 60mm.The source of described carbon fiber can be commercial, also can be commercial continuous carbon fibre long filament is carried out to chopping processing, obtains the carbon fiber that in the present invention, length is 40 ~ 80mm.
In described finishing agent, the mass ratio of solvent, strong basicity chemicals, silicone oil and/or modified silicon oil and chemical treatments is (1 ~ 4): 1:1:1, is preferably (1.5 ~ 3.5): 1:1:1.
Described solvent is solvent well known to those skilled in the art, there is no special restriction.Solvent described in the present invention is preferably one or more in water, acetone and ethanol, more preferably acetone or alcohol, and described water is preferably deionized water, can reduce electrolyte and the impact of impurity on carbon fiber in water.
Described strongly alkaline compound is preferably potassium hydroxide or NaOH, makes finishing agent keep an alkaline environment.
Described chemical treatments is chemical treatments well known to those skilled in the art, there is no special restriction, in the present invention, be preferably antistatic treatment agent or softener, more preferably antistatic treatment agent, then be preferably aliphatic amine polyoxyethylene ether (AC1200) class finishing agent.
In described finishing agent solution, the mass content of finishing agent is 1% ~ 8%, be preferably 3% ~ 8%, more preferably 4% ~ 8%, solvent in described finishing agent solution is solvent well known to those skilled in the art, be preferably one or more in water, acetone and ethanol, more preferably water or ethanol, described water is preferably deionized water, can reduce electrolyte and the impact of impurity on carbon fiber in water.
In the present invention, preferably finishing agent solution is first heated to 25 ~ 80 ℃, is preferably 30 ~ 80 ℃, more preferably 40 ~ 80 ℃, then add described carbon fiber.
The reagent adopting in the present invention is nontoxic, for environmentally friendly reagent, and at high temperature volatile, can not bring impurity to carbon fiber, and then bring ash content and impurity can to final carbon/carbon composite, guarantee the purity of photovoltaic thermal field material crystals growth.
Mass ratio according to carbon fiber of the present invention and finishing agent solution is 1:50 ~ 1:100, is preferably 1:50 ~ 1:80.
The frequency of described ultrasonic wave processing is 28 ~ 60KHz, is preferably 30 ~ 50KHz.
The temperature of described ultrasonic wave processing is 20 ~ 80 ℃, is preferably 30 ~ 80 ℃, more preferably 45 ~ 80 ℃; The time of described ultrasonic wave processing is 10 ~ 60min, is preferably 20 ~ 55min.
When high-intensity ultrasonic wave is propagated in liquid, i.e. " cavitation effect " can energy-producingly intensify and happen suddenly, can discharge huge energy, produce up to a hundreds of atmospheric local instantaneous pressure, form shock wave, make the surface of solids and liquid medium receive great impulsive force and machinery " destruction ", this energy is enough to interrupt very strong chemical bonds, therefore, adopt ultrasonic wave Treatment of Carbon, not only can utilize instant impact to smash carbon fiber bundle, also can smash surface impurity or weaken the suction-operated between impurity and object, impel between impurity and object and accelerate to depart from, make carbon fiber after treatment there is good dispersiveness, be difficult for adhesion, easily shredding, and then the thermodynamic stability of the one-tenth net uniformity in use procedure and carbon fiber thermal field material after can improving, extend the service life of carbon/carbon composite, also make carbon fiber after treatment there is good flexibility and antistatic behaviour, improved easy the to be crisp characteristic of carbon fiber simultaneously.
Carbon fiber after treatment makes the production of net tire more even, be convenient to produce, use Z-direction fiber content and the interlaminar shear strength of the carbon fiber needling preform that carbon fiber after treatment makes to be all improved, and needling preform also have good resin wettability and thermal field uniformity.
According to the present invention, in the time of the nonaqueous solvents such as be acetone or alcohol of the solvent in solvent in finishing agent and finishing agent solution, preferably also carbon fiber after treatment to be washed, the number of times of washing is preferably 1 ~ 3 time.
In the present invention, preferably that carbon fiber after treatment ultrasonic wave is dry.Described being dried preferably carried out in atmospheric air, and described dry temperature is preferably 30 ~ 50 ℃, heats up gradually, and the described dry time is preferably 1 ~ 8h, more preferably 4 ~ 8h.
According to dried carbon fiber of the present invention preferably its moisture content be 1% ~ 8%, more preferably 5% ~ 8%.
In order to further illustrate the present invention, below in conjunction with embodiment, the method for a kind of surface treatment of carbon fibers provided by the invention is described in detail.
In following examples, agents useful for same is commercially available.
Embodiment 1
1.1 by continuous 6K carbon fiber filament chopping, obtains the carbon fiber that length is 50mm.
1.2 by ethanol, NaOH, silicone oil and AC1200 in mass ratio the ratio of 2:1:1:1 mix, obtain finishing agent, finishing agent and deionized water are mixed with to the finishing agent aqueous solution, the quality of finishing agent is 5% of finishing agent aqueous solution quality.
The 1.2 finishing agent aqueous solution that obtain put into by the carbon fiber obtaining in 1.1 by 1.3, the mass ratio of carbon fiber and the finishing agent aqueous solution is 1:50, be 40KHz by hyperacoustic frequency setting, be heated to 60 ℃, carbon fiber in the finishing agent aqueous solution is processed to 30min, with filter screen taking-up, be squeezed to no longer and drip gently.Carbon fiber after treatment is put into baking oven, be warming up to gradually 40 ℃, dry 4h.
Utilize microscope to detect the carbon fiber after treatment obtaining in 1.3, known carbon fiber after treatment is dispersity, and shredding rate reaches more than 90%, and soft surface is smooth.
The carbon fiber after treatment obtaining in 1.3 is made to net tire, and disconnected fine, useless fine rate obviously reduces, and known carbon fiber toughness after treatment and flexibility are improved.
Embodiment 2
2.1 by continuous 12K carbon fiber filament chopping, obtains the carbon fiber that length is 50mm.
2.2 by ethanol, NaOH, silicone oil and AC1200 3:1:1 in mass ratio: 1 ratio is mixed, and obtains finishing agent, and finishing agent and deionized water are mixed with to the finishing agent aqueous solution, and the quality of finishing agent is 8% of finishing agent aqueous solution quality.
The 2.2 finishing agent aqueous solution that obtain put into by the carbon fiber obtaining in 2.1 by 2.3, the mass ratio of carbon fiber and the finishing agent aqueous solution is 1:50, be 28KHz by hyperacoustic frequency setting, be heated to 50 ℃, carbon fiber in the finishing agent aqueous solution is processed to 50min, with filter screen taking-up, be squeezed to no longer and drip gently.Carbon fiber after treatment is put into baking oven, be warming up to gradually 40 ℃, dry 7h.
Utilize microscope to detect the carbon fiber after treatment obtaining in 2.3, known carbon fiber after treatment is dispersity, and shredding rate reaches 95%, and soft surface is smooth.
The carbon fiber after treatment obtaining in 2.3 is made to net tire, and disconnected fine, useless fine rate obviously reduces, and known carbon fiber toughness after treatment and flexibility are improved.
Embodiment 3
3.1 by continuous 12K carbon fiber filament chopping, obtains the carbon fiber that length is 50mm.
3.2 by ethanol, NaOH, silicone oil and AC1200 3:1:1 in mass ratio: 1 ratio is mixed, and obtains finishing agent, and finishing agent and deionized water are mixed with to the finishing agent aqueous solution, and the quality of finishing agent is 8% of finishing agent aqueous solution quality.
The 3.2 finishing agent aqueous solution that obtain put into by the carbon fiber obtaining in 3.1 by 3.3, the mass ratio of carbon fiber and the finishing agent aqueous solution is 1:100, be 40KHz by hyperacoustic frequency setting, be heated to 60 ℃, carbon fiber in the finishing agent aqueous solution is processed to 30min, with filter screen taking-up, be squeezed to no longer and drip gently.Carbon fiber after treatment is put into baking oven, be warming up to gradually 40 ℃, dry 8h.
Utilize microscope to detect the carbon fiber after treatment obtaining in 3.3, known carbon fiber after treatment is dispersity, and shredding rate reaches 95%, and soft surface is smooth.
The carbon fiber after treatment obtaining in 3.3 is made to net tire, and disconnected fine, useless fine rate obviously reduces, and known carbon fiber toughness after treatment and flexibility are improved.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (10)
1. a method for surface treatment of carbon fibers, is characterized in that, carries out ultrasonic wave processing after carbon fiber is placed in to finishing agent solution, and described finishing agent comprises solvent, strongly alkaline compound, silicone oil and/or modified silicon oil and chemical treatments.
2. processing method according to claim 1, is characterized in that, the length of described carbon fiber is 40 ~ 80mm.
3. processing method according to claim 1, is characterized in that, the frequency of described ultrasonic wave processing is 28 ~ 60KHz.
4. processing method according to claim 1, is characterized in that, the temperature of described ultrasonic wave processing is 20 ~ 80 ℃, and the time is 10 ~ 60min.
5. processing method according to claim 1, is characterized in that, described solvent is selected from one or more in water, acetone and ethanol.
6. processing method according to claim 1, is characterized in that, described strongly alkaline compound is NaOH or potassium hydroxide.
7. processing method according to claim 1, is characterized in that, described chemical treatments is antistatic finishing agent or softener.
8. processing method according to claim 1, is characterized in that, the mass ratio of described carbon fiber and finishing agent solution is (1:50) ~ (1:100).
9. processing method according to claim 1, is characterized in that, the mass ratio of described solvent, strongly alkaline compound, silicone oil and/or modified silicon oil and chemical treatments is (1 ~ 4): 1:1:1.
10. processing method according to claim 1, is characterized in that, the quality of described finishing agent is 1% ~ 8% of finishing agent solution quality.
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| CN201210481067.2A CN103835117A (en) | 2012-11-22 | 2012-11-22 | Carbon fiber surface treatment method |
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| CN201210481067.2A CN103835117A (en) | 2012-11-22 | 2012-11-22 | Carbon fiber surface treatment method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104163474A (en) * | 2014-08-19 | 2014-11-26 | 中山大学 | Activation method of graphite felt applied to cathode of Electro-Fenton system |
| CN105421078A (en) * | 2015-12-04 | 2016-03-23 | 镇江奥立特机械制造有限公司 | Method for treating surfaces of novel carbon fibers |
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| JPH0291226A (en) * | 1988-09-27 | 1990-03-30 | Toray Ind Inc | Production of raw material yarn for carbon yarn |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104163474A (en) * | 2014-08-19 | 2014-11-26 | 中山大学 | Activation method of graphite felt applied to cathode of Electro-Fenton system |
| CN105421078A (en) * | 2015-12-04 | 2016-03-23 | 镇江奥立特机械制造有限公司 | Method for treating surfaces of novel carbon fibers |
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Application publication date: 20140604 |