CN102644069A - Method for chemically plating nickel on surface of carbon fiber - Google Patents
Method for chemically plating nickel on surface of carbon fiber Download PDFInfo
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- CN102644069A CN102644069A CN2012101602324A CN201210160232A CN102644069A CN 102644069 A CN102644069 A CN 102644069A CN 2012101602324 A CN2012101602324 A CN 2012101602324A CN 201210160232 A CN201210160232 A CN 201210160232A CN 102644069 A CN102644069 A CN 102644069A
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Abstract
The invention relates to a method for chemically plating nickel on the surface of carbon fiber. The invention aims to solve the problem that the existing method for chemically plating the nickel on the surface of the carbon fiber causes environment pollution, is unstable in activation fluid, complex in operation, and low in plating layer bonding intensity. The method comprises the following steps of: 1, firstly, removing glue and oil from the surface of the carbon fiber; 2, soaking in concentrated nitric acid for coarsening, then washing by distilled water under the help of ultrasound, and finally drying into constant weight, so that the cleaned and coarsened carbon fiber can be obtained; 3, firstly, soaking the obtained product in the activation fluid, then washing by distilled water and soaking in sodium borohydride solution to be reduced, and finally rewashing by distilled water, so that the activated carbon fiber can be obtained; and 4, soaking into chemical nickel-plating liquid, withdrawing, and washing by distilled water, and then drying into constant weight, so that the nickel can be chemically plated on the surface of the carbon fiber. The method for is mainly used for chemically plating the nickel on the surface of the carbon fiber.
Description
Technical field
The present invention relates to a kind of method of carbon fiber surface nickel plating.
Background technology
Thomel is a kind of novel anisotropy strongthener, have high specific strength (3～7GPa), high ratio modulus (200～650GPa), light weight (1.7g/cm
3～2.0g/cm
3), coefficient of thermal expansion is little by (0～-1.1 * 10
6K
-1), mechanical property good (polymkeric substance is had certain strengthening action), antifatigue, carbon peel off many premium propertiess such as few, in field of compound material, be widely used.But owing to be connected with nonpolar covalent linkage between the carbon fiber surface carbon carbon; The turbostratic that is parallel graphite microcrystal between crystal boundary; Cause its wellability relatively poor; Not good with the consistency of metal, be difficult for forming firm interfacial adhesion, so thomel has received restriction to a certain degree in the matrix material Application Areas.
In order to enlarge the use range of thomel, adopt the method for coating surface metal level that thomel is carried out surface-treated with premium properties.The thomel of surface metalation has been opened up the Application Areas of carbon-fibre composite, makes it at the electromagnetic shielding film of military aircraft, small-sized large value capacitor, magneticthin film, electronics and make aspects such as various functional components and parts and be used widely.(author: Yi Pei etc.) the discovery nickel-coated carbon fibers can be adjusted the electromagnetic parameter of absorbing material in " pre-test of metallizing wave absorbing carbon fiber coating additive "; Wavelength band at 9.5～13GHz; The extinction curve that adds the sample of NiCF has an attenuation absorption peak highly significant and that have suitable width; Have good absorbing property, can be used as good electromagnetic protection microwave absorbing coating.Relevant research shows that when the volume content of thomel in the matrix material reached 20%～30%, the volume specific resistance of this material can drop to 10 Ω cm, and therefore, carbon fiber surface nickel plating is best electromagnetic interference shielding weighting material.
The method of carbon current fiber nickel plating has a lot, like plating method, electroless plating method, ion sputtering method, vacuum vapour deposition etc.Wherein, advantage such as it is high that chemically coated nickel method coating has hardness and wear resistance, and corrosion stability, covering power and controllability are good, and the pin hole rate is low, fine and close, glossiness is good is simple, easy to operate, the respond well method of a kind of equipment requirements.The activating treatment process that chemical nickel plating is commonly used has sensitization-activation method, colloidal palladium activation method and ionic palladium activation method.Domestic carbon fiber surface chemical plating Mi-P alloy generally adopts sensitization-activation method.(author: adopt sensitization-activation method Shu Weiguo etc.) before the plating, though this activation method technical maturity, preparation of raw material are simple and easy, but coating is very coarse at " chemical nickel plating of thomel "; Complicated operation; Work-ing life is short, is not suitable for automatic production, and this method is eliminated gradually." research of thomel nickel chemical plating technology " (author: adopt the colloidal palladium activation method in carbon fiber surface nickel plating Wu Yong etc.),, safeguard easy to usely, save operation though colloidal pd activation solution is more stable, the preparation trouble, the acid mist of generation is harmful to healthy and equipment.Ionic state palladium activation solution does not contain stannous ion, and preparation is simple, can keep stable over a long time, but carbon fiber surface makes the sticking power of coating low to the no chemically bonded effect of ionic state palladium absorption, comes off easily." carbon fiber surface does not have the performance analysis of palladium Electroless Plating of Ni-P Alloy coating " (author: adopt NiSO Luo Xiaoping etc.) before the plating
4Solution and KBH
4The solution soaking thomel is implemented electroless plating then in acidic bath, though obtained chemical plating, have the nickel dam obscission in earlier stage at plating.
Existing in sum carbon fiber surface chemical nickel plating method exists environmental pollution, activation solution instability, complicated operation, problem that coat binding strength is low; Cause the carbon fiber surface quality of coating not good enough, influence carbon-fibre composite performance and the life-span in use.
Summary of the invention
The objective of the invention is to solve existing carbon fiber surface chemical nickel plating activation method and have environmental pollution, activation solution instability, complicated operation and the low problem of gained coat binding strength, and a kind of method of carbon fiber surface chemical nickel plating is provided.
A kind of method of carbon fiber surface chemical nickel plating; Specifically accomplish according to the following steps: one, surface treatment: 1. remove glue: with acetone is solvent; Adopting soxhlet extraction is condensing reflux 12h～48h under 70 ℃～80 ℃ water bath condition with thomel in temperature, obtains except that the thomel behind the glue; 2. oil removing: will place concentration except that the thomel behind the glue is the sodium hydroxide solution of 0.8mol/L～1.2mol/L; Low whipping speed is to boil 10min～20min under 40 commentaries on classics/min～130 commentaries on classics/min then; It is in 0.8mol/L～1.2mol/L hydrochloric acid soln that taking-up is placed on concentration; Low whipping speed is to boil 10min～20min under 40 commentaries on classics/min～130 commentaries on classics/min then, obtains the thomel behind the surface degreasing after the taking-up; Two, roughening treatment: thomel behind the surface degreasing is immersed in the concentrated nitric acid, and sealing, under 80 ℃～100 ℃ water bath condition, flood 20min～40min then; Obtain thomel after the alligatoring after the taking-up; Be the ultrasonic down auxiliary of 30kHz～50kHz in frequency then, thomel after the acidifying of employing distilled water wash, the liquid to washing is till the neutrality; Be to be dried to constant weight under 70 ℃～90 ℃ in temperature again, promptly obtain thomel after the clean alligatoring; Three, activation treatment: thomel after the alligatoring is immersed in the activation solution; Infiltrating time is 4min～14min; Taking-up drains the back and adopts zero(ppm) water I washing 1s～5s, immerses and carries out reduction reaction in the sodium borohydride solution, and the recovery time is 8min～12min; Adopt zero(ppm) water II washing 1s～5s after taking-up drains once more, promptly obtain thomel after the activation; Four, nickel plating: thomel after the activation is immersed in the chemical nickel-plating plating solution; And be that chemical nickel plating is 20min～30min under 65 ℃～75 ℃ water bath condition in temperature; Take out the back and adopt distilled water wash; Till the liquid clarification, be to be dried to constant weight under 50 ℃～70 ℃ in temperature again after washing to the washing that obtains, promptly accomplish the carbon fiber surface chemical nickel plating; The fine quality of carbon is 1g with the ratio of activation solution volume after the alligatoring described in the step 3: (200mL～500mL); The volume ratio of activation solution described in the step 3 and zero(ppm) water I is (4～16): 10; The fine quality of carbon is 1g with the ratio of sodium borohydride solution volume after the alligatoring described in the step 3: (50mL～100mL); The volume ratio of sodium borohydride solution described in the step 3 and zero(ppm) water II is (20～30): 10; The thomel quality is 1g with the ratio of chemical nickel-plating plating solution volume after the activation described in the step 4: (1000mL～2000mL).
Advantage of the present invention: one, the present invention is solvent with acetone, takes soxhlet extraction to remove the epoxy resin of carbon fiber surface effectively; Two, the present invention puts into sodium hydroxide solution with thomel and hydrochloric acid soln boils successively, promptly reaches the carbon fiber surface oil removing, and further improves the wetting ability of thomel; Three, the present invention adopts concentrated nitric acid to change for the alligatoring agent makes carbon fiber surface functional group state; A large amount of carboxyls, hydroxyl etc. contain the water base group of oxygen affinity and generate; Adopt activation solution absorption and sodium borohydride reduction two-step approach activated carbon fibre then, make carbon fiber surface form nickel autocatalysis activation site, for electroless plating provides a large amount of Wasserstoffatoms attachment sites; Guarantee carrying out continually and steadily of chemical nickel plating, finally obtained even, dense carbon fiber coating; Four, the present invention does not have the introducing of palladium salt, reactivation process nickel ion and carbon fiber surface carboxyl bonding, and the activation solution that adopts is identical with the chemical nickel-plating plating solution composition; Can stable existence several weeks; Therefore, both alleviate traditional palladium system activation heavy metal palladium and polluted, overcome problems such as activation solution instability, complicated operation, coat binding strength are low; Having simplified electroless plating activation act flow process again, is a kind of chemical nickel plating activating process of practicality and high efficiency.
Description of drawings
Fig. 1 is the schematic flow sheet of embodiment one step 2 to step 4; Fig. 2 is the 10000 times of apparent patterns of thomel amplification after this testing sequence one obtains surface degreasing; Fig. 3 is that thomel amplified 5000 times of apparent patterns after this testing sequence three obtained activation; Fig. 4 is 5000 times of apparent patterns of thomel amplification that this test obtains accomplishing the carbon fiber surface chemical nickel plating; Fig. 5 is 1000 times of apparent patterns of thomel amplification that this test obtains accomplishing the carbon fiber surface chemical nickel plating; Fig. 6 is an XRD figure, and a among Fig. 6 representes that this testing sequence one obtains the XRD figure of the thomel behind the surface degreasing, and a among Fig. 6 representes that this test obtains accomplishing the XRD figure of the thomel of carbon fiber surface chemical nickel plating.
Embodiment
Embodiment one: this embodiment is a kind of method of carbon fiber surface chemical nickel plating, specifically accomplishes according to the following steps:
One, surface treatment: 1. remove glue: with acetone is solvent, and adopting soxhlet extraction is condensing reflux 12h～48h under 70 ℃～80 ℃ water bath condition with thomel in temperature, obtains except that the thomel behind the glue; 2. oil removing: will place concentration except that the thomel behind the glue is the sodium hydroxide solution of 0.8mol/L～1.2mol/L; Low whipping speed is to boil 10min～20min under 40 commentaries on classics/min～130 commentaries on classics/min then; It is in 0.8mol/L～1.2mol/L hydrochloric acid soln that taking-up is placed on concentration; Low whipping speed is to boil 10min～20min under 40 commentaries on classics/min～130 commentaries on classics/min then, obtains the thomel behind the surface degreasing after the taking-up; Two, roughening treatment: thomel behind the surface degreasing is immersed in the concentrated nitric acid, and sealing, under 80 ℃～100 ℃ water bath condition, flood 20min～40min then; Obtain thomel after the alligatoring after the taking-up; Be the ultrasonic down auxiliary of 30kHz～50kHz in frequency then, thomel after the acidifying of employing distilled water wash, the liquid to washing is till the neutrality; Be to be dried to constant weight under 70 ℃～90 ℃ in temperature again, promptly obtain thomel after the clean alligatoring; Three, activation treatment: thomel after the alligatoring is immersed in the activation solution; Infiltrating time is 4min～14min; Taking-up drains the back and adopts zero(ppm) water I washing 1s～5s, immerses and carries out reduction reaction in the sodium borohydride solution, and the recovery time is 8min～12min; Adopt zero(ppm) water II washing 1s～5s after taking-up drains once more, promptly obtain thomel after the activation; Four, nickel plating: thomel after the activation is immersed in the chemical nickel-plating plating solution; And be that chemical nickel plating is 20min～30min under 65 ℃～75 ℃ water bath condition in temperature; Take out the back and adopt distilled water wash; Till the liquid clarification, be to be dried to constant weight under 50 ℃～70 ℃ in temperature again after washing to the washing that obtains, promptly accomplish the carbon fiber surface chemical nickel plating.
The fine quality of carbon is 1g with the ratio of activation solution volume after the alligatoring described in this embodiment step 3: (200mL～500mL); The volume ratio of activation solution described in this embodiment step 3 and zero(ppm) water I is (4～16): 10; The fine quality of carbon is 1g with the ratio of sodium borohydride solution volume after the alligatoring described in this embodiment step 3: (50mL～100mL); The volume ratio of sodium borohydride solution described in this embodiment step 3 and zero(ppm) water II is (20～30): 10.
The thomel quality is 1g with the ratio of chemical nickel-plating plating solution volume after the activation described in this embodiment step 4: (1000mL～2000mL).
Thomel be a kind of be raw material with polyacrylonitrile fibre, pitch fibers, viscose fiber etc.; Make through preheating oxidation, carbonization, graphitization technique; It is the glued membrane of epoxy resin that commercially available carbon fiber surface all has one deck staple; It directly influences the bonding strength of metal plating and carbon fiber surface, need to remove with improve its surfaceness, wettability and with the conjugation of metal.
The schematic flow sheet of this embodiment step 2 to step 4 is as shown in Figure 1, and A representes the thomel after step 1 obtains surface degreasing among the figure, 1. representes the vitriol oil among the figure; B representes that step 2 obtains thomel after the clean alligatoring among the figure; 2. represent activation solution among the figure, C representes to adopt the thomel after zero(ppm) water I cleans in the step 3 among the figure, 3. representes sodium borohydride solution among the figure; D representes thomel after the activation that step 3 obtains among the figure; D among the figure on the D representes nickel catalytic activity site, 4. representes chemical nickel-plating plating solution among the figure, and E representes the nickel-coated carbon fibers that this embodiment obtains among the figure.
This embodiment is solvent with acetone, takes soxhlet extraction to remove the epoxy resin of carbon fiber surface effectively.
Thomel is put into sodium hydroxide solution to this embodiment successively and hydrochloric acid soln boils, and promptly reaches the carbon fiber surface oil removing, and further improve the wetting ability of thomel.
This embodiment adopts concentrated nitric acid to change for the alligatoring agent makes carbon fiber surface functional group state; A large amount of carboxyls, hydroxyl etc. contain the water base group of oxygen affinity and generate; Adopt activation solution absorption and sodium borohydride reduction two-step approach activated carbon fibre then, make carbon fiber surface form nickel autocatalysis activation site, for electroless plating provides a large amount of Wasserstoffatoms attachment sites; Guarantee carrying out continually and steadily of chemical nickel plating, finally obtained even, dense carbon fiber coating.
This embodiment does not have palladium salt to be introduced; Reactivation process nickel ion and carbon fiber surface carboxyl bonding, and the activation solution that adopts is identical with the chemical nickel-plating plating solution composition, can stable existence several weeks; Therefore; Both alleviate traditional palladium system activation heavy metal palladium and polluted, overcome problems such as activation solution instability, complicated operation, coat binding strength are low, simplified electroless plating activation act flow process again; Be a kind of chemical nickel plating activating process of practicality and high efficiency, and prepared thomel nickel plating matrix material can be widely used in industries such as electronics, computingmachine, petrochemical complex, automotive industry and military project.
Embodiment two: this embodiment with the difference of embodiment one is: the activation solution described in the step 3 is mixed by single nickel salt, sodium-acetate, ammonium chloride, inferior sodium phosphate, lactic acid, thiocarbamide, ammoniacal liquor and deionized water; And the concentration of single nickel salt is 25g/L～35g/L in the described activation solution; The concentration of sodium-acetate is 15g/L～25g/L, and the concentration of ammonium chloride is 20g/L～30g/L, and the concentration of inferior sodium phosphate is 25g/L～35g/L; Concentration of lactic acid is 15g/L～20g/L, and the concentration of thiocarbamide is 1.5 * 10
-3G/L～2.5 * 10
-3G/L, the concentration of ammoniacal liquor is 45g/L～55g/L; And the pH of described activation solution is 8.0～9.0.Other are identical with embodiment one.
Embodiment three: this embodiment with one of embodiment one or two difference is: the sodium borohydride solution described in the step 3 is mixed by Peng Qinghuana, sodium hydroxide and deionized water; And the concentration of Peng Qinghuana is 3g/L～4g/L in the described sodium borohydride solution, and concentration sodium hydroxide is 8g/L～12g/L.Other are identical with embodiment one or two.
Embodiment four: this embodiment with one of embodiment one to three difference is: the chemical nickel-plating plating solution described in the step 4 is mixed by single nickel salt, sodium-acetate, ammonium chloride, inferior sodium phosphate, lactic acid, thiocarbamide, ammoniacal liquor and deionized water; And the concentration of single nickel salt is 25g/L～35g/L in the described chemical nickel-plating plating solution; The concentration of sodium-acetate is 15g/L～25g/L; The concentration of ammonium chloride is 20g/L～30g/L; The concentration of inferior sodium phosphate is 25g/L～35g/L, and concentration of lactic acid is 15g/L～20g/L, and the concentration of thiocarbamide is 1.5 * 10
-3G/L～2.5 * 10
-3G/L, the concentration of ammoniacal liquor is 45g/L～55g/L, and the pH of described chemical nickel-plating plating solution is 8.0～9.0.Other are identical with embodiment one to three.
Adopt following verification experimental verification effect of the present invention:
Test one: a kind of method of carbon fiber surface chemical nickel plating, specifically accomplish according to the following steps:
One, surface treatment: 1. remove glue: with acetone is solvent, and adopting soxhlet extraction is condensing reflux 30h under 75 ℃ of water bath condition with thomel in temperature, obtains except that the thomel behind the glue; 2. oil removing: will place concentration except that the thomel behind the glue is the sodium hydroxide solution of 1mol/L; Low whipping speed is to boil 150min under the 80 commentaries on classics/min then; It is in the 1mol/L hydrochloric acid soln that taking-up is placed on concentration; Low whipping speed is to boil 15min under the 80 commentaries on classics/min then, obtains the thomel behind the surface degreasing after the taking-up; Two, roughening treatment: thomel behind the surface degreasing is immersed in the concentrated nitric acid, and sealing, under 90 ℃ of water bath condition, flood 30min then; Obtain thomel after the alligatoring after the taking-up; Be the ultrasonic down auxiliary of 40kHz in frequency then, thomel after the acidifying of employing distilled water wash, the liquid to washing is till the neutrality; Be to be dried to constant weight under 80 ℃ in temperature again, promptly obtain thomel after the clean alligatoring; Three, activation treatment: immerse thomel after the alligatoring in the activation solution approximately; Infiltrating time is 9min; Taking-up drains the back and adopts zero(ppm) water I washing 3s, immerses and carries out reduction reaction in the sodium borohydride solution, and the recovery time is 10min; Adopt zero(ppm) water II washing 3s after taking-up drains once more, promptly obtain thomel after the activation; Four, nickel plating: thomel after the activation is immersed in the chemical nickel-plating plating solution; And be that chemical nickel plating is 25min under 70 ℃ of water bath condition in temperature; Take out the back and adopt distilled water wash; Till the liquid clarification, be to be dried to constant weight under 60 ℃ in temperature again after washing to the washing that obtains, promptly accomplish the carbon fiber surface chemical nickel plating.
The fine quality of carbon is 1g: 350mL with the ratio of activation solution volume after the alligatoring described in this embodiment step 3; The volume ratio of activation solution described in this embodiment step 3 and zero(ppm) water I is 10: 10; The fine quality of carbon is 1g: 75mL with the ratio of sodium borohydride solution volume after the alligatoring described in this embodiment step 3; The volume ratio of sodium borohydride solution described in this embodiment step 3 and zero(ppm) water II is 25: 10.
The thomel quality is 1g: 1500mL with the ratio of chemical nickel-plating plating solution volume after the activation described in this embodiment step 4.
Activation solution described in this testing sequence three is mixed by single nickel salt, sodium-acetate, ammonium chloride, inferior sodium phosphate, lactic acid, thiocarbamide, ammoniacal liquor and deionized water; And the concentration of single nickel salt is 30g/L in the described activation solution, and the concentration of sodium-acetate is 20g/L, and the concentration of ammonium chloride is 25g/L, and the concentration of inferior sodium phosphate is 305g/L, and concentration of lactic acid is 17.5g/L, and the concentration of thiocarbamide is 2.0 * 10
-3G/L, the concentration of ammoniacal liquor is 50g/L; And the pH of described activation solution is 8.5.
Sodium borohydride solution described in this testing sequence three is mixed by Peng Qinghuana, sodium hydroxide and deionized water; And the concentration of Peng Qinghuana is 3.5g/L in the described sodium borohydride solution, and concentration sodium hydroxide is 10g/L.
Chemical nickel-plating plating solution described in this testing sequence four is mixed by single nickel salt, sodium-acetate, ammonium chloride, inferior sodium phosphate, lactic acid, thiocarbamide, ammoniacal liquor and deionized water; And the concentration of single nickel salt is 30g/L in the described activation solution; The concentration of sodium-acetate is 20g/L, and the concentration of ammonium chloride is 25g/L, and the concentration of inferior sodium phosphate is 305g/L; Concentration of lactic acid is 17.5g/L, and the concentration of thiocarbamide is 2.0 * 10
-3G/L, the concentration of ammoniacal liquor is 50g/L; And the pH of described activation solution is 8.5.
Adopt this testing sequence of sem observation one to obtain thomel and this testing sequence three behind the surface degreasing and obtain thomel after the activation; As shown in Figures 2 and 3; Fig. 2 is the 10000 times of apparent patterns of thomel amplification after this testing sequence one obtains surface degreasing; Fig. 3 is that this testing sequence three obtains that thomel amplifies 5000 times of apparent patterns after the activation, can knowledge through Fig. 2 and Fig. 3, thomel through roughening treatment, activation solution adsorb and sodium borohydride reduction after the surface separate out a large amount of metallic nickel autocatalysis site; As the attachment point of Wasserstoffatoms that inferior sodium phosphate discharges in the nickel process, reached the purpose of thomel electroless plating front activating.
Adopt this test of sem observation to obtain accomplishing the thomel of carbon fiber surface chemical nickel plating; Like Fig. 4 and shown in Figure 5; Fig. 4 is 5000 times of apparent patterns of thomel amplification that this test obtains accomplishing the carbon fiber surface chemical nickel plating; Fig. 5 is 1000 times of apparent patterns of thomel amplification that this test obtains accomplishing the carbon fiber surface chemical nickel plating; Can knowledge through Fig. 4 and Fig. 5, thomel reacts in chemical nickel-plating plating solution and obtains comparatively ideal light close coating after the activation, and gained carbon fiber surface nickel coatings thickness reaches micron order behind the chemical nickel plating.
Adopt X-ray diffractometer to detect this testing sequence one and obtain the thomel that thomel and this test behind the surface degreasing obtains accomplishing the carbon fiber surface chemical nickel plating, detected result is as shown in Figure 6, and a among Fig. 6 representes that this testing sequence one obtains the XRD figure of the thomel behind the surface degreasing; A among Fig. 6 representes that this test obtains accomplishing the XRD figure of the thomel of carbon fiber surface chemical nickel plating; Can be known that by Fig. 6 the thomel characteristic diffraction peak is located about 2 θ=26.8 °, the shared ratio of thomel peak area that this test obtains accomplishing the carbon fiber surface chemical nickel plating is significantly less than the thomel proportion after this testing sequence one obtains surface degreasing; This explanation carbon fiber surface is evenly coated by nickel dam; The diffraction peak of nickel 51.8 °, is located for 76.3 ° 44.5 ° of 2 θ ≈ in the chemical plating; They are respectively Ni (111); The diffraction angle of Ni (200) and Ni (220), nickel peak area proportion is bigger, and this explanation carbon fiber surface coating has certain thickness.
Claims (4)
1. the method for a carbon fiber surface chemical nickel plating is characterized in that the method for carbon fiber surface chemical nickel plating is accomplished according to the following steps:
One, surface treatment: 1. remove glue: with acetone is solvent, and adopting soxhlet extraction is condensing reflux 12h～48h under 70 ℃～80 ℃ water bath condition with thomel in temperature, obtains except that the thomel behind the glue; 2. oil removing: will place concentration except that the thomel behind the glue is the sodium hydroxide solution of 0.8mol/L～1.2mol/L; Low whipping speed is to boil 10min～20min under 40 commentaries on classics/min～130 commentaries on classics/min then; It is in 0.8mol/L～1.2mol/L hydrochloric acid soln that taking-up is placed on concentration; Low whipping speed is to boil 10min～20min under 40 commentaries on classics/min～130 commentaries on classics/min then, obtains the thomel behind the surface degreasing after the taking-up; Two, roughening treatment: thomel behind the surface degreasing is immersed in the concentrated nitric acid, and sealing, under 80 ℃～100 ℃ water bath condition, flood 20min～40min then; Obtain thomel after the alligatoring after the taking-up; Be the ultrasonic down auxiliary of 30kHz～50kHz in frequency then, thomel after the acidifying of employing distilled water wash, the liquid to washing is till the neutrality; Be to be dried to constant weight under 70 ℃～90 ℃ in temperature again, promptly obtain thomel after the clean alligatoring; Three, activation treatment: thomel after the alligatoring is immersed in the activation solution; Infiltrating time is 4min～14min; Taking-up drains the back and adopts zero(ppm) water I washing 1s～5s, immerses and carries out reduction reaction in the sodium borohydride solution, and the recovery time is 8min～12min; Adopt zero(ppm) water II washing 1s～5s after taking-up drains once more, promptly obtain thomel after the activation; Four, nickel plating: thomel after the activation is immersed in the chemical nickel-plating plating solution; And be that chemical nickel plating is 20min～30min under 65 ℃～75 ℃ water bath condition in temperature; Take out the back and adopt distilled water wash; Till the liquid clarification, be to be dried to constant weight under 50 ℃～70 ℃ in temperature again after washing to the washing that obtains, promptly accomplish the carbon fiber surface chemical nickel plating; The fine quality of carbon is 1g with the ratio of activation solution volume after the alligatoring described in the step 3: (200mL～500mL); The volume ratio of activation solution described in the step 3 and zero(ppm) water I is (4～16): 10; The fine quality of carbon is 1g with the ratio of sodium borohydride solution volume after the alligatoring described in the step 3: (50mL～100mL); The volume ratio of sodium borohydride solution described in the step 3 and zero(ppm) water II is (20～30): 10; The thomel quality is 1g with the ratio of chemical nickel-plating plating solution volume after the activation described in the step 4: (1000mL～2000mL).
2. the method for a kind of carbon fiber surface chemical nickel plating according to claim 1 is characterized in that the activation solution described in the step 3 is mixed by single nickel salt, sodium-acetate, ammonium chloride, inferior sodium phosphate, lactic acid, thiocarbamide, ammoniacal liquor and deionized water; And the concentration of single nickel salt is 25g/L～35g/L in the described activation solution; The concentration of sodium-acetate is 15g/L～25g/L, and the concentration of ammonium chloride is 20g/L～30g/L, and the concentration of inferior sodium phosphate is 25g/L～35g/L; Concentration of lactic acid is 15g/L～20g/L, and the concentration of thiocarbamide is 1.5 * 10
-3G/L～2.5 * 10
-3G/L, the concentration of ammoniacal liquor is 45g/L～55g/L; And the pH of described activation solution is 8.0～9.0.
3. the method for a kind of carbon fiber surface chemical nickel plating according to claim 2 is characterized in that the sodium borohydride solution described in the step 3 is mixed by Peng Qinghuana, sodium hydroxide and deionized water; And the concentration of Peng Qinghuana is 3g/L～4g/L in the described sodium borohydride solution, and concentration sodium hydroxide is 8g/L～12g/L.
4. according to the method for claim 1,2 or 3 described a kind of carbon fiber surface chemical nickel platings; It is characterized in that the chemical nickel-plating plating solution described in the step 4 is mixed by single nickel salt, sodium-acetate, ammonium chloride, inferior sodium phosphate, lactic acid, thiocarbamide, ammoniacal liquor and deionized water; And the concentration of single nickel salt is 25g/L～35g/L in the described chemical nickel-plating plating solution; The concentration of sodium-acetate is 15g/L～25g/L, and the concentration of ammonium chloride is 20g/L～30g/L, and the concentration of inferior sodium phosphate is 25g/L～35g/L; Concentration of lactic acid is 15g/L～20g/L, and the concentration of thiocarbamide is 1.5 * 10
-3G/L～2.5 * 10
-3G/L, the concentration of ammoniacal liquor is 45g/L～55g/L, and the pH of described chemical nickel-plating plating solution is 8.0～9.0.
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| CN103160826A (en) * | 2013-03-22 | 2013-06-19 | 西北工业大学 | Preparation method of continuous carbon fiber surface pyrolytic carbon/nickel composite coating |
| CN103484842A (en) * | 2013-09-11 | 2014-01-01 | 昆山市万丰制衣有限责任公司 | Copper plating process for surface of carbon fiber |
| CN103643503A (en) * | 2013-11-25 | 2014-03-19 | 中国科学院山西煤炭化学研究所 | Processing method for silane coupling agent modified carbon fiber surface |
| CN103981513A (en) * | 2014-05-30 | 2014-08-13 | 北京理工大学 | Chemical nickel plating method on carbon fiber surface |
| CN104088138A (en) * | 2014-07-08 | 2014-10-08 | 山东建筑大学 | Preparation method of copper-zinc-iron ternary alloy chemical plating layer on surface of aramid fiber |
| CN104313516A (en) * | 2014-10-24 | 2015-01-28 | 苏州吴创材料科技发展有限公司 | Rare earth added carbon fiber aluminum matrix composite material for car doors and preparation method thereof |
| CN104448840A (en) * | 2015-01-19 | 2015-03-25 | 中国科学院长春应用化学研究所 | Preparation method of filing type electromagnetic shielding silicon rubber |
| CN105107509A (en) * | 2015-09-08 | 2015-12-02 | 徐金富 | Flexible loading type carbon fiber loaded CoB catalyst and preparation method thereof |
| CN105200761A (en) * | 2015-10-13 | 2015-12-30 | 四川大学 | Palladium-free activation chemical nickel-plating method for electromagnetic shielding polyphenylene sulfide fiber |
| CN105803433A (en) * | 2016-04-20 | 2016-07-27 | 青岛科技大学 | Aluminum oxide ceramic surface palladium-free activating and chemical nickel-plating technology |
| CN106436287A (en) * | 2016-09-28 | 2017-02-22 | 天津工业大学 | Method for depositing metal on carbon fiber surfaces |
| CN106801335A (en) * | 2016-12-12 | 2017-06-06 | 东莞市佳乾新材料科技有限公司 | A kind of preparation method of high performance surface nickel-coated carbon fibers |
| CN106835684A (en) * | 2017-03-02 | 2017-06-13 | 昆明理工大学 | A kind of carbon fiber surface coats processing method |
| CN106906646A (en) * | 2017-03-02 | 2017-06-30 | 昆明理工大学 | A kind of carbon fiber surface metallization treating method |
| CN107058986A (en) * | 2017-04-10 | 2017-08-18 | 河南科技大学 | A kind of method of Electroless Nickel Plating on Carbon Fiber |
| CN107868947A (en) * | 2017-11-23 | 2018-04-03 | 广东工业大学 | A kind of activating solution and preparation method thereof and no-palladium activating chemical nickel plating method |
| CN108797097A (en) * | 2018-05-08 | 2018-11-13 | 哈尔滨理工大学 | A kind of preparation of graphene/carbon nano-fiber composite material |
| CN108978178A (en) * | 2018-08-06 | 2018-12-11 | 合肥岑遥新材料科技有限公司 | A kind of activating process of carbon fiber |
| CN109136889A (en) * | 2017-06-27 | 2019-01-04 | 罗奕兵 | A kind of cobalt-nickel-phosphor catalytic reactor and production method |
| CN109666261A (en) * | 2018-12-21 | 2019-04-23 | 河南扬博防雷科技有限公司 | A kind of carbon fiber lift lightning arrester, preparation method and application |
| CN109943870A (en) * | 2017-12-21 | 2019-06-28 | 宜兴市宜泰碳纤维织造有限公司 | A kind of carbon fiber surface copper plating process |
| CN112331378A (en) * | 2020-11-19 | 2021-02-05 | 中国工程物理研究院应用电子学研究所 | Flexible wearable conductive material with Joule heating performance and preparation method thereof |
| CN112482024A (en) * | 2020-11-26 | 2021-03-12 | 南京信息工程大学 | Preparation method of copper-plated carbon fabric electromagnetic shielding material |
| CN112962088A (en) * | 2021-02-03 | 2021-06-15 | 合肥华清方兴表面技术有限公司 | Carbon fiber metallization surface treatment method for invisible airplane |
| CN112992558A (en) * | 2021-02-07 | 2021-06-18 | 东华大学 | Preparation method of metal-based carbon fiber composite electrode, product and application thereof |
| CN113059155A (en) * | 2021-03-22 | 2021-07-02 | 东北大学 | Preparation method of nickel-coated graphite composite powder material for conductive silica gel |
| CN113604192A (en) * | 2021-08-31 | 2021-11-05 | 广州市白云化工实业有限公司 | High-temperature addition type organic silicon electromagnetic shielding adhesive and preparation method thereof |
| CN113717470A (en) * | 2021-11-01 | 2021-11-30 | 苏州度辰新材料有限公司 | Permanent antistatic master batch for polypropylene film, preparation method thereof and film |
| CN114974918A (en) * | 2022-02-16 | 2022-08-30 | 上海应用技术大学 | Composite material of carbon fiber surface loaded with reduced titanium dioxide and preparation and application thereof |
| CN115537117A (en) * | 2022-10-05 | 2022-12-30 | 复旦大学义乌研究院 | Silicone rubber light ablation-resistant electromagnetic shielding coating material and application thereof |
| CN116496073A (en) * | 2023-05-16 | 2023-07-28 | 醴陵千汇实业有限公司 | Blank pug for extrusion molding of cup lugs |
| CN114974918B (en) * | 2022-02-16 | 2024-04-26 | 上海应用技术大学 | Composite material of carbon fiber surface loaded with reduced titanium dioxide and preparation and application thereof |
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| CN103160826A (en) * | 2013-03-22 | 2013-06-19 | 西北工业大学 | Preparation method of continuous carbon fiber surface pyrolytic carbon/nickel composite coating |
| CN103160826B (en) * | 2013-03-22 | 2015-06-17 | 西北工业大学 | Preparation method of continuous carbon fiber surface pyrolytic carbon/nickel composite coating |
| CN103484842A (en) * | 2013-09-11 | 2014-01-01 | 昆山市万丰制衣有限责任公司 | Copper plating process for surface of carbon fiber |
| CN103643503A (en) * | 2013-11-25 | 2014-03-19 | 中国科学院山西煤炭化学研究所 | Processing method for silane coupling agent modified carbon fiber surface |
| CN103981513A (en) * | 2014-05-30 | 2014-08-13 | 北京理工大学 | Chemical nickel plating method on carbon fiber surface |
| CN104088138A (en) * | 2014-07-08 | 2014-10-08 | 山东建筑大学 | Preparation method of copper-zinc-iron ternary alloy chemical plating layer on surface of aramid fiber |
| CN104313516B (en) * | 2014-10-24 | 2016-05-25 | 苏州吴创材料科技发展有限公司 | Arrangements for automotive doors adds carbon fiber aluminum-based compound material and preparation method thereof with rare earth |
| CN104313516A (en) * | 2014-10-24 | 2015-01-28 | 苏州吴创材料科技发展有限公司 | Rare earth added carbon fiber aluminum matrix composite material for car doors and preparation method thereof |
| CN104448840B (en) * | 2015-01-19 | 2017-01-18 | 中国科学院长春应用化学研究所 | Preparation method of filing type electromagnetic shielding silicon rubber |
| CN104448840A (en) * | 2015-01-19 | 2015-03-25 | 中国科学院长春应用化学研究所 | Preparation method of filing type electromagnetic shielding silicon rubber |
| CN105107509A (en) * | 2015-09-08 | 2015-12-02 | 徐金富 | Flexible loading type carbon fiber loaded CoB catalyst and preparation method thereof |
| CN105200761A (en) * | 2015-10-13 | 2015-12-30 | 四川大学 | Palladium-free activation chemical nickel-plating method for electromagnetic shielding polyphenylene sulfide fiber |
| CN105803433A (en) * | 2016-04-20 | 2016-07-27 | 青岛科技大学 | Aluminum oxide ceramic surface palladium-free activating and chemical nickel-plating technology |
| CN106436287A (en) * | 2016-09-28 | 2017-02-22 | 天津工业大学 | Method for depositing metal on carbon fiber surfaces |
| CN106801335A (en) * | 2016-12-12 | 2017-06-06 | 东莞市佳乾新材料科技有限公司 | A kind of preparation method of high performance surface nickel-coated carbon fibers |
| CN106835684A (en) * | 2017-03-02 | 2017-06-13 | 昆明理工大学 | A kind of carbon fiber surface coats processing method |
| CN106906646A (en) * | 2017-03-02 | 2017-06-30 | 昆明理工大学 | A kind of carbon fiber surface metallization treating method |
| CN107058986B (en) * | 2017-04-10 | 2019-08-06 | 河南科技大学 | A kind of method of Electroless Nickel Plating on Carbon Fiber |
| CN107058986A (en) * | 2017-04-10 | 2017-08-18 | 河南科技大学 | A kind of method of Electroless Nickel Plating on Carbon Fiber |
| CN109136889A (en) * | 2017-06-27 | 2019-01-04 | 罗奕兵 | A kind of cobalt-nickel-phosphor catalytic reactor and production method |
| CN107868947A (en) * | 2017-11-23 | 2018-04-03 | 广东工业大学 | A kind of activating solution and preparation method thereof and no-palladium activating chemical nickel plating method |
| CN107868947B (en) * | 2017-11-23 | 2023-09-19 | 广东工业大学 | Activating solution, preparation method thereof and palladium-free activated chemical nickel plating method |
| CN109943870A (en) * | 2017-12-21 | 2019-06-28 | 宜兴市宜泰碳纤维织造有限公司 | A kind of carbon fiber surface copper plating process |
| CN108797097A (en) * | 2018-05-08 | 2018-11-13 | 哈尔滨理工大学 | A kind of preparation of graphene/carbon nano-fiber composite material |
| CN108978178A (en) * | 2018-08-06 | 2018-12-11 | 合肥岑遥新材料科技有限公司 | A kind of activating process of carbon fiber |
| CN109666261A (en) * | 2018-12-21 | 2019-04-23 | 河南扬博防雷科技有限公司 | A kind of carbon fiber lift lightning arrester, preparation method and application |
| CN112331378B (en) * | 2020-11-19 | 2022-03-01 | 中国工程物理研究院应用电子学研究所 | Flexible wearable conductive material with Joule heating performance and preparation method thereof |
| CN112331378A (en) * | 2020-11-19 | 2021-02-05 | 中国工程物理研究院应用电子学研究所 | Flexible wearable conductive material with Joule heating performance and preparation method thereof |
| CN112482024A (en) * | 2020-11-26 | 2021-03-12 | 南京信息工程大学 | Preparation method of copper-plated carbon fabric electromagnetic shielding material |
| CN112962088A (en) * | 2021-02-03 | 2021-06-15 | 合肥华清方兴表面技术有限公司 | Carbon fiber metallization surface treatment method for invisible airplane |
| CN112992558A (en) * | 2021-02-07 | 2021-06-18 | 东华大学 | Preparation method of metal-based carbon fiber composite electrode, product and application thereof |
| CN112992558B (en) * | 2021-02-07 | 2022-04-05 | 东华大学 | Preparation method of metal-based carbon fiber composite electrode, product and application thereof |
| CN113059155A (en) * | 2021-03-22 | 2021-07-02 | 东北大学 | Preparation method of nickel-coated graphite composite powder material for conductive silica gel |
| CN113604192A (en) * | 2021-08-31 | 2021-11-05 | 广州市白云化工实业有限公司 | High-temperature addition type organic silicon electromagnetic shielding adhesive and preparation method thereof |
| CN113717470B (en) * | 2021-11-01 | 2022-02-08 | 苏州度辰新材料有限公司 | Permanent antistatic master batch for polypropylene film, preparation method thereof and film |
| CN113717470A (en) * | 2021-11-01 | 2021-11-30 | 苏州度辰新材料有限公司 | Permanent antistatic master batch for polypropylene film, preparation method thereof and film |
| CN114974918A (en) * | 2022-02-16 | 2022-08-30 | 上海应用技术大学 | Composite material of carbon fiber surface loaded with reduced titanium dioxide and preparation and application thereof |
| CN114974918B (en) * | 2022-02-16 | 2024-04-26 | 上海应用技术大学 | Composite material of carbon fiber surface loaded with reduced titanium dioxide and preparation and application thereof |
| CN115537117A (en) * | 2022-10-05 | 2022-12-30 | 复旦大学义乌研究院 | Silicone rubber light ablation-resistant electromagnetic shielding coating material and application thereof |
| CN116496073A (en) * | 2023-05-16 | 2023-07-28 | 醴陵千汇实业有限公司 | Blank pug for extrusion molding of cup lugs |
| CN116496073B (en) * | 2023-05-16 | 2024-04-02 | 醴陵千汇实业有限公司 | Blank pug for extrusion molding of cup lugs |
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