CN103484842A - Copper plating process for surface of carbon fiber - Google Patents
Copper plating process for surface of carbon fiber Download PDFInfo
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- CN103484842A CN103484842A CN201310410798.2A CN201310410798A CN103484842A CN 103484842 A CN103484842 A CN 103484842A CN 201310410798 A CN201310410798 A CN 201310410798A CN 103484842 A CN103484842 A CN 103484842A
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Abstract
The invention relates to a copper plating process for a surface of a carbon fiber. The process comprises the following steps: (1) carrying out modified pretreatment on the carbon fiber, namely modifying the carbon fiber by adopting a chemical method or a water vapor activation method, so as to overcome the characteristics that the carbon fiber surface is not suitable for copper plating due to smoothness, hydrophobicity and surface inertia; (2) chemical copper plating, namely adding the carbon fiber which is subjected to surface pretreatment to a plating solution and continuously stirring, detecting the pH value of the plating solution by precise pH test paper, observing the color change of the carbon fiber, wherein the carbon fiber gradually becomes red, and air bubbles emit; taking out the carbon fiber after the air bubbles in the plating solution gradually reduce and disappear, cleaning and drying. The copper plating process has the beneficial effects that the frequently happening problem of 'black heart' of carbon cellulose when the carbon fiber is plated by copper is effectively solved; the copper plated carbon fiber is tightly combined with a clad layer; the diameter of the carbon fiber is increased; the resistance is reduced; the electrical conductivity is increased. The copper plated carbon fiber is even to coat and good in glossiness; the electrical resistivity is obviously reduced; the electrical conductivity of the copper plated carbon fiber is significantly improved when compared with that of the carbon fiber which is not plated by copper.
Description
Technical field
The invention belongs to the textile dyeing and finishing technical field, be specifically related to a kind of carbon fiber surface copper-plating technique.
Background technology
Metal-based carbon fiber composite material has the premium propertiess such as high specific strength, high ratio modulus and good toughness, in Aeronautics and Astronautics, biomaterial and civilian industry field, is with a wide range of applications.Make filler with the carbon fiber of surface metalation, prepared shielding material has good shield effectiveness, can be used as the absorbing material of aircraft; Metal coated carbon fiber is woven into fabric by certain way, can make the three-dimensional bait body of emulation, for counterradar reconnaissance and the counter of high-tech war, leads.The capability of electromagnetic shielding of material depends primarily on its electroconductibility, the electro-magnetic screen function that the material of good conductivity has had usually.
Copper is because the characteristics that its conductivity is strong, price is suitable are used to carbon fiber surface is carried out to modification.Electroless plating is a kind of surface modifying method commonly used, is in the situation that do not have extrinsic current to pass through, and utilizes reductive agent by the reduction of the metal ion in solution, forms a kind of coating technology of metal plating at the body surface that is catalytic activity.The carbon fiber electroless copper has worked out a lot of processing methodes, but still there are many problems in the copper facing result of these processing methodes.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of carbon fiber surface copper-plating technique, to obtain the copper carbon fiber that glossiness is good, binding force of cladding material is strong, conductivity is high.
A kind of carbon fiber surface copper-plating technique, comprise the steps:
(1) carbon fiber modifying pre-treatment: adopt chemical method or vapor activation to carry out modification to carbon fiber;
(2) electroless copper: will add through the carbon fiber of surface preparation in plating solution and constantly and stir, detect bath pH value with accurate pH test paper, observe the carbon fiber colour-change, carbon fiber reddens gradually, and there is bubble to emerge, after bubble in plating solution is decreased to disappearance gradually, takes out carbon fiber and clean and dry.
Further, the chemical method in described step (1) is:
(a) remove photoresist: adopt air calcination method, carbon fiber bundle is put into to the baking oven calcination, 400 ℃ of calcination temperatures, calcination time is 60min, to slough the outer field protection glue of carbon fiber;
(b) alligatoring: get 20g ammonium persulphate and 100ml H
2o is made into coarsening solution and carries out etching at carbon fiber surface, makes its surface present channel form, and makes carbon fiber surface become wetting ability by hydrophobicity;
(c) neutralization: will put into 10% NaOH solution with the carbon fiber after the ammonium persulphate alligatoring and soak, neutralization remains in the ammonium persulphate of carbon fiber surface, then cleans to neutral;
(d) sensitization: with 2.5g SnCl
2, 27ml HCl (37%), 23ml H
2o is mixed with sensitizing solution, and sensitization time is 5 minutes, then carbon fiber is taken out and cleans, and makes carbon fiber surface absorption one deck reducing substances, and when activation, activator is reduced and stays carbon fiber surface and forms the catalysis nucleus, and the reaction formula of this process is as follows:
2SnCl
2+3H
2O→Sn
2(OH)
3C1+3HCl；
(e) activation: use 5g/L AgNO
3solution, 8mL ammoniacal liquor, the carbon fiber of putting into after sensitization soaks 5 minutes, and then washing is clean, makes carbon fiber surface form the layer of precious metal that one deck has catalytic activity;
(f) reduction: the 20g/L ortho phosphorous acid sodium solution of take is reduced liquid, in 25 ℃ of water-baths, is incubated, and then adds the carbon fiber after activation treatment, after 1 minute, takes out and cleans, and will remain in the AgCl reduction of carbon fiber surface;
Further, the vapor activation in described step (1) is:
(a) carbon fiber is put into to activation furnace and heat, then pass into nitrogen protection, while reaching 700 ℃～800 ℃, to carbon fiber water spray steam, make its surface etch pore-forming, then cooling rear taking-up under nitrogen atmosphere, complete steam-activation treatment;
(b) sensitization: with 2.5g SnCl
2, 27ml HCl (37%), 23ml H
2o is mixed with sensitizing solution, and sensitization time is 5 minutes, then carbon fiber is taken out and cleans, and makes carbon fiber surface absorption one deck reducing substances, and when activation, activator is reduced and stays carbon fiber surface and forms the catalysis nucleus, and the reaction formula of this process is as follows:
2SnCl
2+3H
2O→Sn
2(OH)
3C1+3HCl；
(c) activation: use 5g/L AgNO
3solution, 8mL ammoniacal liquor, the carbon fiber of putting into after sensitization soaks 5 minutes, and then washing is clean, makes carbon fiber surface form the layer of precious metal that one deck has catalytic activity;
(d) reduction: the 20g/L ortho phosphorous acid sodium solution of take is reduced liquid, in 25 ℃ of water-baths, is incubated for some time, then adds the carbon fiber after activation treatment, after 1 minute, takes out and cleans, and will remain in the AgCl reduction of carbon fiber surface;
Further, consisting of of the middle plating solution of described step (2): CuSO
45H
2o 10g/L, NaOH 20g/L, Seignette salt 50g/L, formaldehyde 10ml/L,
The electroless copper reaction formula is as follows:
Cu
2+complex compound+2HCHO+4OH
-=Cu ↓+2HCOO
-+ H
2↑+2H
2the O+ complex compound.
The beneficial effect that the present invention has is: recurrent carbon cellulose " evil mind " problem when this technique has effectively solved Copper Plating of Carbon Fiber, after copper facing, carbon fiber and coating combination is very tight, and the carbon fiber diameter increases, and resistance reduces, electroconductibility increases, and brute force obviously increases.The copper carbon fiber plating is even, and glossiness is good, and binding force of cladding material is strong, and resistivity obviously descends, and electroconductibility has had and significantly improved than copper carbon fiber not.
Embodiment
In order further to understand advantage of the present invention, below by specific embodiment, effect of the present invention is described.
Embodiment mono-:
A kind of carbon fiber surface copper-plating technique, comprise the steps:
(1) carbon fiber modifying pre-treatment: adopt chemical method to carry out modification to carbon fiber, to overcome, carbon fiber surface is smooth, hydrophobicity and surface inertness etc. are not suitable for copper-plated characteristics;
(2) electroless copper: will add through the carbon fiber of surface preparation in plating solution and constantly and stir, detect bath pH value with accurate pH test paper, observe the carbon fiber colour-change, carbon fiber reddens gradually, and there is bubble to emerge, after bubble in plating solution is decreased to disappearance gradually, takes out carbon fiber and clean and dry.
Described chemical method is specially:
(a) remove photoresist: adopt air calcination method, carbon fiber bundle is put into to the baking oven calcination, 400 ℃ of calcination temperatures, calcination time is 60min, to slough the outer field protection glue of carbon fiber, improves the bonding force of copper facing and carbon fiber;
(b) alligatoring: get 20g ammonium persulphate and 100ml H
2o is made into coarsening solution and carries out etching at carbon fiber surface, makes its surface present channel form, and makes carbon fiber surface become wetting ability by hydrophobicity, is convenient to subsequent disposal;
(c) neutralization: will put into 10% NaOH solution with the carbon fiber after the ammonium persulphate alligatoring and soak for some time, neutralization remains in the ammonium persulphate of carbon fiber surface, then with cleaning to neutral;
(d) sensitization: with 2.5g SnCl
2, 27ml HCl (37%), 23ml H
2o is mixed with sensitizing solution, and sensitization time is 5 minutes, then carbon fiber is taken out and cleans, and makes carbon fiber surface absorption one deck reducing substances, and when activation, activator is reduced and stays carbon fiber surface and forms the catalysis nucleus, and the reaction formula of this process is as follows:
2SnCl
2+3H
2O→Sn
2(OH)
3C1+3HCl
(e) activation: use 5g/L AgNO
3solution, 8mL ammoniacal liquor, the carbon fiber of putting into after sensitization soaks 5 minutes, and then washing is clean, makes carbon fiber surface form the layer of precious metal that one deck has catalytic activity;
(f) reduction: the 20g/L ortho phosphorous acid sodium solution of take is reduced liquid, be incubated for some time in 25 ℃ of water-baths, then add the carbon fiber after activation treatment, after 1 minute, take out and clean, will remain in the AgCl reduction of carbon fiber surface, prevent that it from bringing plating solution into plating solution is produced to detrimentally affect;
Consisting of of the middle plating solution of described step (2): CuSO
45H
2o 10g/L, NaOH 20g/L, Seignette salt 50g/L, formaldehyde 10ml/L,
The electroless copper reaction formula is as follows:
Cu
2+complex compound+2HCHO+4OH
-=Cu ↓+2HCOO
-+ H
2↑+2H
2the O+ complex compound.
Embodiment bis-:
A kind of carbon fiber surface copper-plating technique, comprise the steps:
(1) carbon fiber modifying pre-treatment: adopt vapor activation to carry out modification to carbon fiber, to overcome, carbon fiber surface is smooth, hydrophobicity and surface inertness etc. are not suitable for copper-plated characteristics;
(2) electroless copper: will add through the carbon fiber of surface preparation in plating solution and constantly and stir, detect bath pH value with accurate pH test paper, observe the carbon fiber colour-change, carbon fiber reddens gradually, and there is bubble to emerge, after bubble in plating solution is decreased to disappearance gradually, takes out carbon fiber and clean and dry.
Vapor activation in described step (1) is specially:
(a) carbon fiber is put into to activation furnace and heat, when certain temperature, pass into nitrogen protection, while reaching 700 ℃～800 ℃, to carbon fiber water spray steam, make its surface etch pore-forming, then cooling rear taking-up under nitrogen atmosphere, completed steam-activation treatment;
(b) sensitization: with 2.5g SnCl
2, 27ml HCl (37%), 23ml H
2o is mixed with sensitizing solution, and sensitization time is 5 minutes, then carbon fiber is taken out and cleans, and makes carbon fiber surface absorption one deck reducing substances, and when activation, activator is reduced and stays carbon fiber surface and forms the catalysis nucleus, and the reaction formula of this process is as follows:
2SnCl
2+3H
2O→Sn
2(OH)
3C1+3HCl
(c) activation: use 5g/L AgNO
3solution, 8mL ammoniacal liquor, the carbon fiber of putting into after sensitization soaks 5 minutes, and then washing is clean, makes carbon fiber surface form the layer of precious metal that one deck has catalytic activity;
(d) reduction: the 20g/L ortho phosphorous acid sodium solution of take is reduced liquid, be incubated for some time in 25 ℃ of water-baths, then add the carbon fiber after activation treatment, after 1 minute, take out and clean, will remain in the AgCl reduction of carbon fiber surface, prevent that it from bringing plating solution into plating solution is produced to detrimentally affect;
Consisting of of the middle plating solution of described step (2): CuSO
45H
2o 10g/L, NaOH 20g/L, Seignette salt 50g/L, formaldehyde 10ml/L,
The electroless copper reaction formula is as follows:
Cu
2+complex compound+2HCHO+4OH
-=Cu ↓+2HCOO
-+ H
2↑+2H
2the O+ complex compound.
In sum, above embodiment is only in order to illustrate the present invention and unrestricted technical scheme described in the invention; Therefore, although this specification sheets has been described in detail the present invention with reference to each above-mentioned embodiment,, those of ordinary skill in the art should be appreciated that still and can modify or be equal to replacement the present invention; And all do not break away from technical scheme and the improvement thereof of the spirit and scope of the present invention, it all should be encompassed in claim scope of the present invention.
Claims (4)
1. a carbon fiber surface copper-plating technique, is characterized in that, comprises the steps:
(1) carbon fiber modifying pre-treatment: adopt chemical method or vapor activation to carry out modification to carbon fiber;
(2) electroless copper: will add through the carbon fiber of surface preparation in plating solution and constantly and stir, detect bath pH value with accurate pH test paper, observe the carbon fiber colour-change, carbon fiber reddens gradually, and there is bubble to emerge, after bubble in plating solution is decreased to disappearance gradually, takes out carbon fiber and clean and dry.
2. carbon fiber surface copper-plating technique according to claim 1, is characterized in that, the chemical method in described step (1) is:
(a) remove photoresist: adopt air calcination method, carbon fiber bundle is put into to the baking oven calcination, 400 ℃ of calcination temperatures, calcination time is 60min, to slough the outer field protection glue of carbon fiber;
(b) alligatoring: get 20g ammonium persulphate and 100ml H
2o is made into coarsening solution and carries out etching at carbon fiber surface, makes its surface present channel form, and makes carbon fiber surface become wetting ability by hydrophobicity;
(c) neutralization: will put into 10% NaOH solution with the carbon fiber after the ammonium persulphate alligatoring and soak, neutralization remains in the ammonium persulphate of carbon fiber surface, then cleans to neutral;
(d) sensitization: with 2.5g SnCl
2, 27ml HCl (37%), 23ml H
2o is mixed with sensitizing solution, and sensitization time is 5 minutes, then carbon fiber is taken out and cleans, and makes carbon fiber surface absorption one deck reducing substances;
(e) activation: use 5g/L AgNO
3solution, 8mL ammoniacal liquor, the carbon fiber of putting into after sensitization soaks 5 minutes, and then washing is clean, makes carbon fiber surface form the layer of precious metal that one deck has catalytic activity;
(f) reduction: the 20g/L ortho phosphorous acid sodium solution of take is reduced liquid, in 25 ℃ of water-baths, is incubated, and then adds the carbon fiber after activation treatment, after 1 minute, takes out and cleans, and will remain in the AgCl reduction of carbon fiber surface.
3. carbon fiber surface copper-plating technique according to claim 1, is characterized in that, the vapor activation in described step (1) is:
(a) carbon fiber is put into to activation furnace and heat, then pass into nitrogen protection, while reaching 700 ℃～800 ℃, to carbon fiber water spray steam, make its surface etch pore-forming, then cooling rear taking-up under nitrogen atmosphere, complete steam-activation treatment;
(b) sensitization: with 2.5g SnCl
2, 27ml HCl (37%), 23ml H
2o is mixed with sensitizing solution, and sensitization time is 5 minutes, then carbon fiber is taken out and cleans, and makes carbon fiber surface absorption one deck reducing substances;
(c) activation: use 5g/L AgNO
3solution, 8mL ammoniacal liquor, the carbon fiber of putting into after sensitization soaks 5 minutes, and then washing is clean, makes carbon fiber surface form the layer of precious metal that one deck has catalytic activity;
(d) reduction: the 20g/L ortho phosphorous acid sodium solution of take is reduced liquid, in 25 ℃ of water-baths, is incubated for some time, then adds the carbon fiber after activation treatment, after 1 minute, takes out and cleans, and will remain in the AgCl reduction of carbon fiber surface.
4. carbon fiber surface copper-plating technique according to claim 1, is characterized in that, the consisting of of plating solution in described step (2): CuSO45H2O 10g/L, NaOH 20g/L, Seignette salt 50g/L, formaldehyde 10ml/L.
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|---|---|---|---|
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104190922A (en) * | 2014-09-12 | 2014-12-10 | 四川理工学院 | Composite copper plating process for graphite particles |
| CN104233421A (en) * | 2014-09-12 | 2014-12-24 | 西安理工大学 | Method for covering surface of carbon or carbon fibers with metal chromium |
| CN104226986A (en) * | 2014-09-12 | 2014-12-24 | 华东理工大学 | Metallic copper coated calcium sulfate whisker preparation method |
| CN104975278A (en) * | 2015-07-02 | 2015-10-14 | 甘肃郝氏炭纤维有限公司 | Heat-reduction metallization copper plating process for carbon fiber surface |
| CN105185440A (en) * | 2015-08-27 | 2015-12-23 | 江苏通鼎光电科技有限公司 | Light-weight and fatigue-resistant flexible cable of braided shielding transponder |
| CN105256349A (en) * | 2015-10-29 | 2016-01-20 | 无锡桥阳机械制造有限公司 | Preparation technology for composite material |
| CN105670570A (en) * | 2016-02-24 | 2016-06-15 | 武汉理工大学 | Preparation method of sizing composite heat storage material for moderate-high temperature |
| CN106602036A (en) * | 2017-01-19 | 2017-04-26 | 华南理工大学 | Carbon core/copper oxide housing composite electrode for lithium ion battery and preparation method thereof |
| CN109207970A (en) * | 2018-10-31 | 2019-01-15 | 华南理工大学 | A kind of carbon cloth-Nanometer Copper composite material and preparation method and application |
| CN112301736A (en) * | 2020-11-18 | 2021-02-02 | 沈阳工业大学 | Preparation method of copper-tin composite coating on surface of short carbon fiber |
| CN114808521A (en) * | 2022-04-20 | 2022-07-29 | 江南大学 | Method for preparing electrode precursor by using copper-plated carbon fiber papermaking |
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Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104233421A (en) * | 2014-09-12 | 2014-12-24 | 西安理工大学 | Method for covering surface of carbon or carbon fibers with metal chromium |
| CN104226986A (en) * | 2014-09-12 | 2014-12-24 | 华东理工大学 | Metallic copper coated calcium sulfate whisker preparation method |
| CN104190922B (en) * | 2014-09-12 | 2016-04-13 | 四川理工学院 | Graphite granule Composite Coatings process for copper |
| CN104190922A (en) * | 2014-09-12 | 2014-12-10 | 四川理工学院 | Composite copper plating process for graphite particles |
| CN104975278A (en) * | 2015-07-02 | 2015-10-14 | 甘肃郝氏炭纤维有限公司 | Heat-reduction metallization copper plating process for carbon fiber surface |
| CN104975278B (en) * | 2015-07-02 | 2017-08-25 | 甘肃郝氏炭纤维有限公司 | Carbon fiber surface thermal reduction metallization copper-plating technique |
| CN105185440A (en) * | 2015-08-27 | 2015-12-23 | 江苏通鼎光电科技有限公司 | Light-weight and fatigue-resistant flexible cable of braided shielding transponder |
| CN105256349A (en) * | 2015-10-29 | 2016-01-20 | 无锡桥阳机械制造有限公司 | Preparation technology for composite material |
| CN105670570B (en) * | 2016-02-24 | 2019-05-24 | 武汉理工大学 | A kind of preparation method for high temperature composite heat storage material of being formed |
| CN105670570A (en) * | 2016-02-24 | 2016-06-15 | 武汉理工大学 | Preparation method of sizing composite heat storage material for moderate-high temperature |
| CN106602036A (en) * | 2017-01-19 | 2017-04-26 | 华南理工大学 | Carbon core/copper oxide housing composite electrode for lithium ion battery and preparation method thereof |
| CN106602036B (en) * | 2017-01-19 | 2023-11-21 | 华南理工大学 | Carbon core/copper oxide shell composite electrode for lithium ion battery and preparation method thereof |
| CN109207970A (en) * | 2018-10-31 | 2019-01-15 | 华南理工大学 | A kind of carbon cloth-Nanometer Copper composite material and preparation method and application |
| CN112301736A (en) * | 2020-11-18 | 2021-02-02 | 沈阳工业大学 | Preparation method of copper-tin composite coating on surface of short carbon fiber |
| CN112301736B (en) * | 2020-11-18 | 2022-06-07 | 沈阳工业大学 | Preparation method of copper-tin composite coating on surface of short carbon fiber |
| CN114808521A (en) * | 2022-04-20 | 2022-07-29 | 江南大学 | Method for preparing electrode precursor by using copper-plated carbon fiber papermaking |
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