CN1844481A - Metallization treatment method for short carbon fiber - Google Patents
Metallization treatment method for short carbon fiber Download PDFInfo
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- CN1844481A CN1844481A CN 200610024510 CN200610024510A CN1844481A CN 1844481 A CN1844481 A CN 1844481A CN 200610024510 CN200610024510 CN 200610024510 CN 200610024510 A CN200610024510 A CN 200610024510A CN 1844481 A CN1844481 A CN 1844481A
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Abstract
This invention relates to a short-carbon fiber metal processing method, firstly adding suitable short-carbon fiber in the plating liquid, and adding some surface active agent to make the fiber disperse uniformly, and then choosing the current density and electroplating time according to the plating layer thickness, disturbing slightly to make the short-carbon fiber gather on the cathode surface and wrap mutually during electroplating, finally forming the loose sediment with uniform plating layer. Then after the sediment is peeled off from cathode, it processed through washing, drying, dispersing and other simply disposals to obtain the single short-carbon fiber covered with metal. If plating with copper, it must do hydrogh reduction to remove oxide. This invention can be applied in electromagnetic shielding material, anti-static material, wave--absorbing material, structure material and so on.
Description
Technical field
The present invention relates to a kind of metallization treating method of short carbon fiber, belong to technical field of surface.
Background technology
Carbon fiber has a series of advantages such as high specific strength, high ratio modulus, high temperature resistant, corrosion-resistant, conduction, heat conduction and low-expansion coefficient, is a kind of important composite material reinforcement body.The raising of the cost of carbon fiber decline in recent years and performance is for condition has been created in the application of matrix material.Ideal carbon-fibre composite (metal matrix, resin base etc.) not only has good mechanical property, and have favorable conductive, heat conduction, dimensional stabilizing, high temperature resistant, aging-resistant characteristic, in fields such as Aeronautics and Astronautics, the energy, electronics, automobiles very application prospects is arranged.Present general carbon fiber surface coating technology, promptly can increase the material of wetting property and blocking harmful surface reaction at carbon fiber surface coating one deck, as sputtering method, ion plating method, metal powder painting, electroless plating and plating etc., wherein electroplating technology and other technology relatively have outstanding advantages such as technology is simple, equipment requirements is low, service temperature is low.Carbon fiber after the metallization, as: plating Ni carbon fiber, plating Cu carbon fiber or the double-deck carbon fiber of plating Ni/Cu etc. all are well to strengthen copper base, matrix material such as aluminium base, utilize its excellent conducting performance, can and make various functional components and parts etc. with the electromagnetic shielding of small-sized large value capacitor, magneticthin film, electronics.
Compare with long carbon fiber, that short carbon fiber has is cheap, the simple and performance isotropy of the technology of preparation matrix material, in functional materialss such as electromagnetic shielding, suction ripple, electrode materials, use short carbon fiber to have advantages such as easy-formation processing, so short carbon fiber more have application prospect simultaneously.But the metallization process of short carbon fiber generally is an employing carbon fiber electroless plating at present, plating is cut short afterwards and get or directly adopt the short carbon fiber electroless plating, as Xu Jincheng etc. at " Lanzhou University's journal (natural science edition) " (Vol.40, No.4, Aug.2004) " preparation of Properties of Cu and the research of performance thereof " delivered, the method that adopts is to carry out long carbon fiber electroless plating 1h earlier, electroplate the copper coating of 2h and handle, the better carbon fiber of plating is cut into the staple fibre of 1～2mm.This method technology is more loaded down with trivial details, cost is higher, and the coating uniformity of plating gained is bad.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art, propose a kind of metallization treating method of short carbon fiber, simple for process, with low cost, can prepare the metallic short fiberous of coating homogeneous and controllable.
For realizing this purpose, the present invention adopts directly short carbon fiber is carried out galvanized mode, utilizes the electroconductibility of short carbon fiber that it is assembled near negative electrode, electroplates the back and forms the loose uniformly shape settling of a coating.At first in plating bath, add an amount of short carbon fiber, and add an amount of tensio-active agent and make it to be uniformly dispersed, select current density and electroplating time according to the requirement of thickness of coating then, apply gentle agitation in the electroplating process and short carbon fiber is accumulated on the cathode surface and entangled to each other, finally form the loose uniformly shape settling of coating.The settling of gained after cathodic disbonding, is obtained the short carbon fiber of one metal lining after simple subsequent disposal such as washing, drying, dispersion, promptly obtain metallized short carbon fiber.
Concrete steps of the present invention are as follows:
1, by the monometallic of required metal plating preparation routine or the plating bath of alloy, in plating bath, adds short carbon fiber, dispersion agent etc., and the short carbon fiber in the plating bath is uniformly dispersed.Wherein, the short carbon fiber length range is 0.5mm～5cm, and the content of short carbon fiber is 0.05～2g/L in the plating bath, and dispersant is 0.01～2g/L.
Dispersion agent of the present invention can be selected anionic dispersing agents, as sodium polyacrylate, sodium lauryl sulphate etc.; Cation dispersing agent is as cetyl trimethylammonium bromide, Xylo-Mucine etc.; And non-ionic dispersing agent, as polyethylene glycol type, fluorine carbon type etc.
2, select current density and time according to the requirement of thickness of coating, be about 0.5A/dm respectively
2～5.0A/dm
2, about 10～120 minutes.Connect power supply, the part short carbon fiber is deposited on the negative electrode when electroplating beginning, applies slight stirring in the process, makes in the plating bath short carbon fiber assemble and becomes entangled in cathode surface mutually.Along with the prolongation of electroplating time, finally form the more loose shape settling of coating.
3, with the settling of gained after cathodic disbonding, washing is also dry in baking oven, obtains the short carbon fiber of metal lining again through dispersing technology.If wherein during copper facing, also need hydrogen reducing to remove oxide compound.
Dispersing technology is selected suitable method according to the thickness of coating of desired short carbon fiber, length etc., and High-Pressure Water or gas percussion, shearing, ball milling etc. are arranged.When requiring greater than 500 μ m less than 50 μ m, mean length, can adopt High-Pressure Water or gas percussion as the coating mean thickness of short carbon fiber; During less than 500 μ m, can adopt methods such as shearing, ball milling greater than 50 μ m, mean length as the coating mean thickness.
Thickness of coating can wait by adjusting current density and electroplating time and control, and the short carbon fiber thickness of coating after the metallization is in 1 μ m～100 mu m ranges.
By selecting different electroplating bath solutions and technology can obtain the coating of different compositions.The inventive method is applicable to the plating of present various metal ingredients, and coating can be monometallics such as nickel, copper, iron, also can be various binary, ternary alloy etc.
The present invention proposes to utilize the electroconductibility of short carbon fiber and the mutual entanglement between them and the electric field shielding effect that produces first, prepares the even metal short carbon fiber.This technology can make the uniform short carbon fiber of coating, its reason is: the short carbon fiber near negative electrode is deposited on the negative electrode earlier, and metal on the plating, and on the fiber of the short carbon fiber after leaning on before being wrapped in gradually deposition go up metal, and the short carbon fiber after leaning on has big electric field shielding effect to forward, and therefore whole sedimental metal deposition rates is all near equating.The equipment that the present invention adopts is simple, only needs common plating tank to get final product, and is simultaneously simple for process similar to the common electrical depositing process.The present invention can effectively control thickness of coating, staple length and metal ingredient, can make the metallized short carbon fiber of thickness coating in 1 μ m～100 mu m ranges, and the length of short carbon fiber also can be in 50 μ m～10cm scope inner control.The composition of coating is various, almost is all existing monometallics that plate or alloy etc.The prepared metallized short carbon fiber of the present invention is expected electromagnetic shielding material, antistatic material, absorbing material, medium being applied of structured material (as metal matrix, polymer matrix composites).
Embodiment
Below by several specific embodiments technical scheme of the present invention is further described.
Embodiment 1:
Thickness of coating is the preparation of the nickel plating short carbon fiber about 1 micron:
With reference to common nickel-plating liquid prescription, as the sulfamate plating bath: nickel sulfamic acid 400g/L, nickelous chloride 5g/L, boric acid 40g/L prepares and is placed in the plating tank, and about heating in water bath to 50 ℃.(about 0.5～1mm) 0.05g/L of length, polyoxyethylene glycol is made dispersion agent 0.01g/L, pours in the groove after ultra-sonic oscillation and stirs to get short carbon fiber.As anode, copper sheet is made negative electrode with the pure nickel plate.The plating bath pH regulator is about 4.0.Adopt the magnetic stirring apparatus gentle agitation.Current density is 0.5A/dm
2, the time was controlled at 120 minutes.After electroplating beginning, short carbon fiber is accumulating on the cathode surface successively, and tangles mutually.Along with the prolongation of time, settling is constantly grown up, the continuous thickening of coating.After time arrives, stop to electroplate, settling is taken off.After the cleaning, settling is put into High-Pressure Water impact, settling is separated obtaining required nickel plating short carbon fiber at last, thickness of coating is about 2 μ m.
Embodiment 2:
Thickness of coating is the nickel plating short carbon fiber about 20 microns
Electroplate liquid formulation is: nickel sulfamic acid 400g/L, and nickelous chloride 5g/L, boric acid 40g/L prepares and is placed in the plating tank, and about heating in water bath to 50 ℃.(1～2mm) 0.5g/L, sodium lauryl sulphate is made dispersion agent 0.5g/L, pours in the groove after ultra-sonic oscillation and stirs to get short carbon fiber.As anode, copper sheet is made negative electrode with the pure nickel plate.The plating bath pH regulator is about 4.0.Adopt the magnetic stirring apparatus gentle agitation.Current density is 2.0A/dm
2, the time was controlled at 80 minutes.After electroplating time arrives, stop to electroplate, the settling that accumulates in negative electrode is taken off.After settling cleaned, it was broken to put into high pressure gas, settling was separated obtaining required nickel plating short carbon fiber at last, and thickness of coating is about 20 μ m.
Embodiment 3:
Thickness of coating is the copper facing short carbon fiber about 100 microns
By common electro-coppering formulated plating bath, wherein copper sulfate 200g/L, sulfuric acid 70g/L.Plating is in room temperature (25 ℃) operation down.(5～6mm) content are 0.5g/L to short carbon fiber, dispersion agent cetyl trimethylammonium bromide 1.5g/L.Short carbon fiber and dispersant before using are poured in the groove after ultra-sonic oscillation and are stirred.As anode, copper sheet adopts the magnetic stirring apparatus gentle agitation as negative electrode with phosphorus copper plate.Current density is 5.0A/dm
2, the time was controlled at 40 minutes.After electroplating time arrives, stop to electroplate, the settling that accumulates in negative electrode is taken off.After settling cleaned, it was broken to put into high pressure gas, afterwards separation was obtained the 400 ℃ of reduction down in hydrogen furnace of copper facing short carbon fiber, obtained required copper facing short carbon fiber at last, and thickness of coating is about 100 μ m.
Embodiment 4:
Thickness of coating is the nickel plating-cobalt-base alloy short carbon fiber about 2 microns
The prescription of this plating bath is: nickel sulfamic acid 600g/L, and thionamic acid cobalt 1.25g/L, nickelous chloride 10g/L, boric acid 35g/L prepares and is placed in the beaker, and temperature is controlled at about 60 ℃.(10～11mm) content are 0.5g/L to short carbon fiber, dispersion agent Xylo-Mucine 0.5g/L.Short carbon fiber and dispersant before using are poured in the groove after ultra-sonic oscillation and are stirred.Anode is the pure nickel plate, the negative electrode stainless steel plate, and current density is controlled at 3.0A/dm
2, the time is 25 minutes.Electroplating time takes off settling after arriving, and promptly gets the short carbon fiber of required nickel plating-cobalt-base alloy after the High-Pressure Water fragmentation, and thickness of coating is about 2 μ m.
Embodiment 5:
Thickness of coating is the copper facing-tin alloy short carbon fiber about 2 microns
Electroplate liquid formulation is: potassium pyrophosphate 250g/L, cupric pyrophosphate 15g/L, the inferior tin 2.0g/L of potassium pyrophosphate, Sodium phosphate dibasic 40g/L, Trisodium Citrate 7.5g/L, nitrilotriacetic acid(NTA) 35g/L, and pH is about 8.5, and temperature is 30 ℃.The soluble anode of anode for casting in proportion with copper and tin, negative electrode is a stainless steel plate.Plating bath needs gentle agitation, and current density is 1.5A/dm
2, the time is 23 minutes.Electroplating time takes off settling after arriving, and promptly gets the short carbon fiber of required copper facing-tin alloy after the High-Pressure Water fragmentation, and thickness of coating is about 2 μ m.
Claims (4)
1, a kind of metallization treating method of short carbon fiber is characterized in that comprising the steps:
1) according to required metal plating preparation plating bath, add short carbon fiber and dispersion agent in plating bath, the short carbon fiber length range is 0.5mm～5cm, and content is 0.05～2g/L, and dispersant is 0.1～2g/L, and the short carbon fiber in the plating bath is uniformly dispersed;
2) selecting current density according to the requirement of thickness of coating is 0.5A/dm
2～5.0A/dm
2, electroplating time is 10～120 minutes, connects power supply and electroplates, and the part short carbon fiber is deposited on the negative electrode, applies in the electroplating process to stir short carbon fiber to be assembled become entangled in cathode surface, finally form the loose uniformly shape settling of coating;
3) with the settling of gained after cathodic disbonding, washing is also dry in baking oven, obtains the short carbon fiber of metal lining again through dispersing technology.
2, according to the metallization treating method of the short carbon fiber of claim 1, it is characterized in that described dispersing technology for adopting High-Pressure Water or gas percussion, perhaps adopt shear, ball milling.
3, according to the metallization treating method of the short carbon fiber of claim 1, it is characterized in that described dispersion agent is anionic dispersing agents, cation dispersing agent and non-ionic dispersing agent.
4, according to the metallization treating method of the short carbon fiber of claim 1, when it is characterized in that described metalized is copper facing, the short carbon fiber after handling is carried out hydrogen reducing to remove oxide compound.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101886330A (en) * | 2010-06-10 | 2010-11-17 | 天津大学 | Fe-Co magnetic alloy plated carbon fiber, preparation method and application thereof |
| CN101463494B (en) * | 2007-12-19 | 2011-05-11 | 富葵精密组件(深圳)有限公司 | Electroplating method |
| CN102409386A (en) * | 2011-11-02 | 2012-04-11 | 上海交通大学 | Method for preparing novel ball-rod-shaped short carbon fiber compound reinforcing body |
| CN105460916A (en) * | 2015-11-20 | 2016-04-06 | 安徽工业大学 | Preparation method of hollow carbon nanospheres-assembled mesoporous carbon fiber material |
| CN108203794A (en) * | 2018-01-04 | 2018-06-26 | 中南大学 | A kind of short carbon fiber aluminum matrix composite and preparation method thereof |
| CN109020591A (en) * | 2018-08-22 | 2018-12-18 | 至玥腾风科技投资集团有限公司 | A kind of preparation method and tesla's turbine disk of tesla's turbine disk |
-
2006
- 2006-03-09 CN CN 200610024510 patent/CN1844481A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101463494B (en) * | 2007-12-19 | 2011-05-11 | 富葵精密组件(深圳)有限公司 | Electroplating method |
| CN101886330A (en) * | 2010-06-10 | 2010-11-17 | 天津大学 | Fe-Co magnetic alloy plated carbon fiber, preparation method and application thereof |
| CN101886330B (en) * | 2010-06-10 | 2012-07-11 | 天津大学 | Fe-Co magnetic alloy plated carbon fiber, preparation method and application thereof |
| CN102409386A (en) * | 2011-11-02 | 2012-04-11 | 上海交通大学 | Method for preparing novel ball-rod-shaped short carbon fiber compound reinforcing body |
| CN105460916A (en) * | 2015-11-20 | 2016-04-06 | 安徽工业大学 | Preparation method of hollow carbon nanospheres-assembled mesoporous carbon fiber material |
| CN105460916B (en) * | 2015-11-20 | 2017-07-14 | 安徽工业大学 | A kind of preparation method of the assembly mesoporous carbon fibre material of hollow Nano carbon ball |
| CN108203794A (en) * | 2018-01-04 | 2018-06-26 | 中南大学 | A kind of short carbon fiber aluminum matrix composite and preparation method thereof |
| CN109020591A (en) * | 2018-08-22 | 2018-12-18 | 至玥腾风科技投资集团有限公司 | A kind of preparation method and tesla's turbine disk of tesla's turbine disk |
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