CN103668199B - The method of carbon fiber/cyanate ester resin composite material nickel plating - Google Patents
The method of carbon fiber/cyanate ester resin composite material nickel plating Download PDFInfo
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Abstract
The invention discloses the method for carbon fiber/cyanate ester resin composite material nickel plating, first use the method for electroless plating at material surface nickel preplating the carbon fiber/cyanate ester resin composite material through pre-treatment, then adopt electric plating method to continue nickel plating.Electroless plating combines with plating by the present invention, first use the method nickel preplating of electroless plating, material surface is made to have the uniform conductive layer of one deck, then electric plating method is adopted to thicken nickel dam, both ensure that the even of nickel layer, in turn ensure that coating has enough thickness, solve prior art and occur to during carbon fiber/cyanate ester resin composite material plating nickel on surface the problem that plating leakage and coating are too thin, obtain evenly and enough thick coating, coating is even, complete, without plating leakage phenomenon, good with base material bonding force, seamless existence, meet the working conditions of aerospace light microscopic, and plating and electroless plating production cost low, can be mass.
Description
Technical field
The invention belongs to non-metal material surface processing technology field, be specifically related to the method for a kind of carbon fiber/cyanate ester resin composite material nickel plating.
Background technology
Remote sensing realizes the Main Means to military target investigation, and the level of remote sensing camera determines the modernization level of a national national defence.Since the eighties in last century, remote sensing camera competitively develops between countries in the world, most is representative is the SPOT5(2001 of the U.S., 2.5 meters of resolving power), IKNOS(1999,1 meter of resolving power), KH-12(2007,0.1 meter of resolving power) etc. camera, pedestrian's quantity and the vehicle fleet size of ground and sensitizing range can be investigated, substantially increase the level of detail of military intelligence, thus heavy caliber high-definition remote sensing camera is the demand of future military struggle.But the raising of resolving power means the increase of camera weight, bring a series of technical barrier to load, satellite platform development, carrying capacity, thus the lightweight of heavy caliber high resolution camera is the inevitable requirement of camera development.
The lightweight of principal reflection mirror is the light-weighted key of camera, and lightweight mode is generally divided into two kinds, and the first adopts traditional specular material to carry out structure lightened design, its two be adopt more excellent performance, the material that density is less realizes light-weight design.Structure lightened ratio is limited to scantlings of the structure, and loss of weight is than limited, and comparatively speaking excellent novel material can increase substantially lightweight ratio.Carbon-fibre composite has excellent specific rigidity, there is light weight, high strength, high rigidity, particularly there are a series of excellent properties such as low-down thermal expansivity, be specially adapted to space structure, also be applicable to the exigent Space Optical System of precision and stability, become the designing material of following heavy caliber ultra lightweighting camera speculum.
Carbon-fibre composite before use often must through corresponding surface treatment to meet it to the adaptability of environment and security.Carbon fiber surface method for metallising is a lot, have physical vapor deposition (PVD), chemical vapour deposition (CVD), ion implantation, ion extractuin, laser surface modification etc., but use these methods have cost high, the shortcoming such as cannot to produce in enormous quantities.Compared with aforesaid method, electroless plating, plating make the most economical a kind of simple method again of carbon-fibre composite surface metalation, it has unique advantage, and its is suitable for, and matrix is wide, convenient for production, all platings and covering power is good, change Coating composition and massfraction can realize several functions.Adopt the method for electroless plating at carbon-fibre composite plating nickel on surface, coating and carbon-fibre composite surface bonding good, both can ensure that carbon-fibre composite had original machinery, physicals, can change again the wettability of carbon-fibre composite and metal, but the thickness of chemical Ni-plating layer there is certain restriction; Electrochemical plating have that equipment is simple, cost is low, can quantity-produced feature, be a kind of method had a extensive future, but carbon-fibre composite surface conductivity is bad, directly adopts plating to be difficult to avoid plating leakage.
Summary of the invention
The object of this invention is to provide the method for a kind of carbon fiber/cyanate ester resin composite material nickel plating, solve prior art and occur to during carbon fiber/cyanate ester resin composite material plating nickel on surface the problem that plating leakage and coating are too thin.
The technical solution adopted in the present invention is: the method for carbon fiber/cyanate ester resin composite material nickel plating, first use the method for electroless plating at material surface nickel preplating the carbon fiber/cyanate ester resin composite material through pre-treatment, then adopt electric plating method to continue nickel plating.
Feature of the present invention is also,
Pre-treatment specifically comprises the following steps:
A, oil removing: carbon fiber/cyanate ester resin composite material is soaked in acetone, the washing of taking-up distilled water, drying after ultrasonic 10 ~ 20min;
B, alligatoring: the material obtained by step a is immersed in the nitric acid of 35%, heating in water bath to 40 DEG C, with distilled water washing, drying after insulation 15 ~ 20min;
C, sensitization: be dissolved in by tin protochloride in concentrated hydrochloric acid, add tin grain, obtains sensitizing solution with distilled water diluting to volume required, and the material obtained by step b soaks taking-up distilled water hydrostatic rinsing after 10 ~ 25min, drying in sensitizing solution;
D, activation: be dissolved in by Palladous chloride in concentrated hydrochloric acid, obtain activation solution with distilled water diluting to volume required, and the material obtained by step c soaks taking-up distilled water washing after 15 ~ 25min, drying in activation solution;
E, reduction: be soak 1 ~ 2min in the ortho phosphorous acid sodium water solution of 1% in concentration under the material room temperature that steps d is obtained.
In step c, the concentration of tin protochloride is 15g/L, and the concentration of concentrated hydrochloric acid is 40mL/L, and tin grain concentration is 15 ~ 20g/L, and soaking temperature is 28 ~ 32 DEG C.
In steps d, the concentration of Palladous chloride is 0.3g/L, and the concentration of concentrated hydrochloric acid is 10mL/L, and soaking temperature is 28 ~ 32 DEG C.
The concrete operations of electroless plating are: the chemical plating fluid carbon fiber/cyanate ester resin composite material through pre-treatment being put into 85 ~ 90 DEG C, take out after soaking 85 ~ 95min, dry after cleaning with distilled water.
Chemical plating fluid consists of: sulfur acid nickel 23 ~ 27g, sodium hypophosphite 23 ~ 27g, lactic acid 22 ~ 26mL, propanedioic acid 4 ~ 6g, sodium-acetate 12 ~ 18g in 1L chemical plating fluid, surplus is distilled water, and use ammoniacal liquor to regulate chemical plating fluid to make its pH value be 6.0, the loading capacity of chemical plating fluid is 0.5 ~ 1.43dm
2/ L.
The concrete operations of plating are: nickel metal is connected on anode, and the carbon fiber/cyanate ester resin composite material through electroless plating is connected on negative electrode, passes to 1.5A/dm
2electric current, then negative electrode, anode are put into respectively the electroplate liquid of 60 DEG C, interpole gap 30 ~ 50mm, and ensure the two poles of the earth parallel, take out after 11 ~ 13h.
Electroplate liquid consists of: sulfur acid nickel 260 ~ 300g, nickelous chloride 35 ~ 45g, boric acid 35 ~ 45g, asccharin 1.0 ~ 1.5g, 1 in 1L electroplate liquid, 4-butynediol 0.1 ~ 0.3g, tonka bean camphor 0.1 ~ 0.3g, sodium lauryl sulphate 0.1 ~ 0.3g, surplus is distilled water, and the loading capacity of electroplate liquid is 0.5 ~ 1.43dm
2/ L.
The invention has the beneficial effects as follows: the method for carbon fiber of the present invention/cyanate ester resin composite material nickel plating, electroless plating is combined with plating, first use the method nickel preplating of electroless plating, material surface is made to have the uniform conductive layer of one deck, then electric plating method is adopted to thicken nickel dam, both ensure that the even of nickel layer, in turn ensure that coating has enough thickness, solve prior art and occur to during carbon fiber/cyanate ester resin composite material plating nickel on surface the problem that plating leakage and coating are too thin, obtain evenly and enough thick coating, coating is even, complete, without plating leakage phenomenon, good with base material bonding force, seamless existence, and plating and electroless plating production cost low, can be mass.
Accompanying drawing explanation
Fig. 1 is the SEM figure after the embodiment of the present invention 1 carbon fiber/cyanate ester resin composite material electroless plating;
Fig. 2 is the sectional drawing after the embodiment of the present invention 1 carbon fiber/cyanate ester resin composite material electroless plating;
Fig. 3 is the sectional drawing after the first electroless plating re-plating of the embodiment of the present invention 1 carbon fiber/cyanate ester resin composite material.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in detail.
The method of carbon fiber of the present invention/cyanate ester resin composite material nickel plating, first uses the method for electroless plating at material surface nickel preplating the carbon fiber/cyanate ester resin composite material through pre-treatment, then adopts electric plating method to continue nickel plating.
Concrete operation step is as follows:
Step 1, pre-treatment,
A, oil removing: carbon fiber/cyanate ester resin composite material is soaked in acetone, the washing of taking-up distilled water, drying after ultrasonic 10 ~ 20min;
B, alligatoring: the material obtained by step a is immersed in the nitric acid of 35%, heating in water bath to 40 DEG C, with distilled water washing, drying after insulation 15 ~ 20min;
C, sensitization: tin protochloride is dissolved in concentrated hydrochloric acid, add tin grain, sensitizing solution is obtained to volume required with distilled water diluting, the concentration of tin protochloride is 15g/L, the concentration of concentrated hydrochloric acid is 40mL/L, the concentration of tin grain is 15 ~ 20g/L, and control temperature is 28 ~ 32 DEG C, and the material obtained by step b soaks taking-up distilled water hydrostatic rinsing after 10 ~ 25min, drying in sensitizing solution;
D, activation: Palladous chloride is dissolved in concentrated hydrochloric acid, activation solution is obtained to volume required with distilled water diluting, the concentration of Palladous chloride is 0.3g/L, the concentration of concentrated hydrochloric acid is 10mL/L, control temperature is 28 ~ 32 DEG C, and the material obtained by step c soaks taking-up distilled water washing after 15 ~ 25min, dry in activation solution;
E, reduction: be soak 1 ~ 2min in the ortho phosphorous acid sodium water solution of 1% in concentration under the material room temperature that steps d is obtained;
Step 2, electroless plating,
A, chemical plating fluid consist of: sulfur acid nickel 23 ~ 27g, sodium hypophosphite 23 ~ 27g, lactic acid 22 ~ 26mL, propanedioic acid 4 ~ 6g, sodium-acetate 12 ~ 18g in 1L chemical plating fluid, surplus is distilled water, and use ammoniacal liquor to regulate chemical plating fluid to make its pH value be 6.0, the loading capacity of chemical plating fluid is 0.5 ~ 1.43dm
2/ L;
B, according to above-mentioned composition configuration chemical plating fluid: the volume first calculating required plating solution according to plating solution loading capacity, takes single nickel salt, sodium hypophosphite, lactic acid, propanedioic acid, sodium-acetate, dissolves respectively with a small amount of distilled water; Respectively the propanedioic acid of dissolving and lactic acid are added in the sodium-acetate of dissolving; By consoluet single nickel salt, join in solution obtained in the previous step lentamente; By consoluet sodium hypophosphite, under stirring tempestuously, join in solution obtained in the previous step lentamente; Use distilled water by solution dilution obtained in the previous step to volume required; Ammoniacal liquor is used to regulate solution obtained in the previous step to pH value to be 6.0;
C, nickel plating: the chemical plating fluid carbon fiber/cyanate ester resin composite material through pre-treatment being put into 85 ~ 90 DEG C, take out after soaking 85 ~ 95min, dry after cleaning with distilled water;
Step 3, plating,
A, electroplate liquid consist of: sulfur acid nickel 260 ~ 300g, nickelous chloride 35 ~ 45g, boric acid 35 ~ 45g, asccharin 1.0 ~ 1.5g, 1 in 1L electroplate liquid, 4-butynediol 0.1 ~ 0.3g, tonka bean camphor 0.1 ~ 0.3g, sodium lauryl sulphate 0.1 ~ 0.3g, surplus is distilled water, and the loading capacity of electroplate liquid is 0.5 ~ 1.43dm
2/ L;
B, according to above-mentioned composition configuration electroplate liquid: the volume first calculating required plating solution according to plating solution loading capacity, takes single nickel salt and nickelous chloride, and the distilled water adding 1/3rd dissolves; Take the boric acid of aequum, add 1/3rd boiling water and stir until it dissolves; The boric acid solution of dissolving is slowly added in the nickel salt solution of dissolving; Take sodium lauryl sulphate, add minor amount of water and make it in the pasty state, then add proper amount of boiling water or solution is boiled again and make it dissolve completely, sodium dodecyl sulfate solution is added in solution obtained in the previous step; Take required asccharin, Isosorbide-5-Nitrae-butynediol, tonka bean camphor, pour in solution obtained in the previous step again after dissolving with distilled water respectively, last adding distil water is to volume required;
C, nickel plating: nickel metal is connected on anode, the carbon fiber/cyanate ester resin composite material through electroless plating is connected on negative electrode, passes to 1.5A/dm
2electric current, then negative electrode, anode are put into respectively the electroplate liquid of 60 DEG C, interpole gap 30 ~ 50mm, and ensure the two poles of the earth parallel, take out after 11 ~ 13h.
Embodiment 1
Adopt the carbon fiber/cyanate ester resin composite sheet of 25mm × 25mm × 5mm; Plating area is 0.175dm
2, plating solution loading capacity refers to the ratio of workpiece plating area and plating solution volume, is 0.5dm according to plating solution loading capacity
2/ L calculates required chemical plating fluid and electroplate liquid volume is 350mL.
Step 1, pre-treatment,
A, oil removing: carbon fiber/cyanate ester resin composite material is immersed in 350mL acetone, the washing of taking-up distilled water, drying after ultrasonic 20min;
B, alligatoring: the material obtained by step a is immersed in the nitric acid of 350mL35%, heating in water bath to 40 DEG C, with distilled water washing, drying after insulation 20min;
C, sensitization: 5.25g tin protochloride is dissolved in 14mL concentrated hydrochloric acid, add 7g tin grain, obtain sensitizing solution with distilled water diluting to 350mL, control temperature is 30 DEG C, and the material obtained by step b soaks taking-up distilled water hydrostatic rinsing after 15min, drying in sensitizing solution;
D, activation: 0.105g Palladous chloride is dissolved in 3.5mL concentrated hydrochloric acid, obtains activation solution with distilled water diluting to 350mL, control temperature is 30 DEG C, and the material obtained by step c soaks taking-up distilled water washing after 15min, dry in activation solution;
E, reduction: 3.5g inferior sodium phosphate is added distillation dissolved dilution to 350mL, under material room temperature steps d obtained, in ortho phosphorous acid sodium solution, soak 1min;
Step 2, electroless plating,
A, configuration 350mL chemical plating fluid: get 8.75g single nickel salt, 8.75g sodium hypophosphite, 8.75mL lactic acid, 2.1g propanedioic acid, 5.25g sodium-acetate, dissolve with a small amount of distilled water respectively; Respectively the propanedioic acid of dissolving and lactic acid are added in the sodium-acetate of dissolving; By consoluet single nickel salt, join in solution obtained in the previous step lentamente; By consoluet sodium hypophosphite, under stirring tempestuously, join in solution obtained in the previous step lentamente; Use distilled water by solution dilution obtained in the previous step to 350mL; Ammoniacal liquor is used to regulate solution obtained in the previous step to pH value to be 6.0;
B, nickel plating: the chemical plating fluid carbon fiber/cyanate ester resin composite material through pre-treatment being put into 90 DEG C, take out after soaking 90min, dry after cleaning with distilled water;
Step 3, plating,
A, configuration 350mL electroplate liquid: take 98g single nickel salt and 14g nickelous chloride, the distilled water adding 116mL dissolves; Take 14g boric acid, add 116mL boiling water and stir until it dissolves; The boric acid solution of dissolving is slowly added in the single nickel salt of dissolving and the mixing solutions of nickelous chloride; Take 0.07g sodium lauryl sulphate, add minor amount of water and make it in the pasty state, then add 3mL boiling water or solution is boiled again and make it dissolve completely, sodium dodecyl sulfate solution is added in solution obtained in the previous step; Take 0.42g asccharin, 0.07g1,4-butynediol, 0.07g tonka bean camphor, pour in solution obtained in the previous step again after dissolving with distilled water respectively, last adding distil water is to 350mL;
B, nickel plating: nickel metal is connected on anode, the carbon fiber/cyanate ester resin composite material through electroless plating is connected on negative electrode, passes to 1.5A/dm
2electric current, then negative electrode, anode are put into respectively the electroplate liquid of 60 DEG C, interpole gap 40mm, and ensure that the two poles of the earth are parallel, take out the thickness of coating that can obtain light after 12h and be about the nickel layer of 411 μm.
As seen from Figure 1, even, complete at the coating of material surface deposition after the embodiment of the present invention 1 carbon fiber/cyanate ester resin composite material electroless plating, without plating leakage phenomenon, and coating is made up of cellular structure; As seen from Figure 2,33 μm are about in the thickness of coating of material surface deposition after the embodiment of the present invention 1 carbon fiber/cyanate ester resin composite material electroless plating, and be combined well with matrix surface, seamless existence, through the phase composite of energy spectrum analysis coating surface thing, know that coating is Ni-P alloy, and be complete non-crystalline state; As seen from Figure 3, technology that the embodiment of the present invention 1 adopts electroless plating to add plating is Ni layer at carbon fiber/cyanate ester resin composite material surface deposition, coating is even, complete, without plating leakage phenomenon, and thickness of coating is about 411 μm, being combined well with matrix surface, seamless existence, is pure Ni through energy spectrum analysis electrolytic coating.
Embodiment 2
Adopt the carbon fiber/cyanate ester resin composite sheet of diameter d=130mm, thickness t=5mm; Plating area is 2.86dm
2, plating solution loading capacity refers to the ratio of workpiece plating area and plating solution volume, is 1.43dm according to plating solution loading capacity
2/ L calculates required chemical plating fluid and electroplate liquid volume is 2L.
Step 1, pre-treatment,
A, oil removing: carbon fiber/cyanate ester resin composite material is immersed in 2L acetone, the washing of taking-up distilled water, drying after ultrasonic 15min;
B, alligatoring: the material obtained by step a is immersed in the nitric acid of 2L35%, heating in water bath to 40 DEG C, with distilled water washing, drying after insulation 15min;
C, sensitization: 30g tin protochloride is dissolved in 80mL concentrated hydrochloric acid, add 30g tin grain, obtain sensitizing solution with distilled water diluting to 2L, control temperature is 28 DEG C, and the material obtained by step b soaks taking-up distilled water hydrostatic rinsing after 25min, drying in sensitizing solution;
D, activation: 0.6g Palladous chloride is dissolved in 20mL concentrated hydrochloric acid, obtains activation solution with distilled water diluting to 2L, control temperature is 28 DEG C, and the material obtained by step c soaks taking-up distilled water washing after 25min, dry in activation solution;
E, reduction: 20g inferior sodium phosphate is added distillation dissolved dilution to 2L, under material room temperature steps d obtained, in ortho phosphorous acid sodium solution, soak 2min;
Step 2, electroless plating,
A, configuration 2L chemical plating fluid: get 46g single nickel salt, 46g sodium hypophosphite, 52mL lactic acid, 10g propanedioic acid, 36g sodium-acetate, dissolve with a small amount of distilled water respectively; Respectively the propanedioic acid of dissolving and lactic acid are added in the sodium-acetate of dissolving; By consoluet single nickel salt, join in solution obtained in the previous step lentamente; By consoluet sodium hypophosphite, under stirring tempestuously, join in solution obtained in the previous step lentamente; Use distilled water by solution dilution obtained in the previous step to 2L; Ammoniacal liquor is used to regulate solution obtained in the previous step to pH value to be 6.0;
B, nickel plating: the chemical plating fluid carbon fiber/cyanate ester resin composite material through pre-treatment being put into 85 DEG C, take out after soaking 85min, dry after cleaning with distilled water;
Step 3, plating,
A, configuration 2L electroplate liquid: take 600g single nickel salt and 90g nickelous chloride, the distilled water adding 666mL dissolves; Take 90g boric acid, add 666mL boiling water and stir until it dissolves; The boric acid solution of dissolving is slowly added in the single nickel salt of dissolving and the mixing solutions of nickelous chloride; Take 0.6g sodium lauryl sulphate, add minor amount of water and make it in the pasty state, then add 10mL boiling water or solution is boiled again and make it dissolve completely, sodium dodecyl sulfate solution is added in solution obtained in the previous step; Take 2.0g asccharin, 0.6g1,4-butynediol, 0.6g tonka bean camphor, pour in solution obtained in the previous step again after dissolving with distilled water respectively, last adding distil water is to 2L;
B, nickel plating: nickel metal is connected on anode, the carbon fiber/cyanate ester resin composite material through electroless plating is connected on negative electrode, passes to 1.5A/dm
2electric current, then negative electrode, anode are put into respectively the electroplate liquid of 60 DEG C, interpole gap 50mm, and ensure the two poles of the earth parallel, take out after 11h.
Embodiment 3
Adopt the carbon fiber/cyanate ester resin composite sheet of 20mm × 20mm × 5mm; Plating area is 0.12dm
2, plating solution loading capacity refers to the ratio of workpiece plating area and plating solution volume, is 1.2dm according to plating solution loading capacity
2/ L calculates required chemical plating fluid and electroplate liquid volume is 100mL.
Step 1, pre-treatment,
A, oil removing: carbon fiber/cyanate ester resin composite material is immersed in 100mL acetone, the washing of taking-up distilled water, drying after ultrasonic 10min;
B, alligatoring: the material obtained by step a is immersed in the nitric acid of 100mL35%, heating in water bath to 40 DEG C, with distilled water washing, drying after insulation 18min;
C, sensitization: 1.5g tin protochloride is dissolved in 4mL concentrated hydrochloric acid, add 1.8g tin grain, obtain sensitizing solution with distilled water diluting to 100mL, control temperature is 32 DEG C, and the material obtained by step b soaks taking-up distilled water hydrostatic rinsing after 10min, drying in sensitizing solution;
D, activation: 0.03g Palladous chloride is dissolved in 1mL concentrated hydrochloric acid, obtains activation solution with distilled water diluting to 100mL, control temperature is 32 DEG C, and the material obtained by step c soaks taking-up distilled water washing after 20min, dry in activation solution;
E, reduction: 1g inferior sodium phosphate is added distillation dissolved dilution to 100mL, under material room temperature steps d obtained, in ortho phosphorous acid sodium solution, soak 1.5min;
Step 2, electroless plating,
A, configuration 100mL chemical plating fluid: get 2.7g single nickel salt, 2.7g sodium hypophosphite, 2.2mL lactic acid, 0.4g propanedioic acid, 1.2g sodium-acetate, dissolve with a small amount of distilled water respectively; Respectively the propanedioic acid of dissolving and lactic acid are added in the sodium-acetate of dissolving; By consoluet single nickel salt, join in solution obtained in the previous step lentamente; By consoluet sodium hypophosphite, under stirring tempestuously, join in solution obtained in the previous step lentamente; Use distilled water by solution dilution obtained in the previous step to 100mL; Ammoniacal liquor is used to regulate solution obtained in the previous step to pH value to be 6.0;
B, nickel plating: the chemical plating fluid carbon fiber/cyanate ester resin composite material through pre-treatment being put into 88 DEG C, take out after soaking 95min, dry after cleaning with distilled water;
Step 3, plating,
A, configuration 100mL electroplate liquid: take 26g single nickel salt and 3.5g nickelous chloride, the distilled water adding 33mL dissolves; Take 3.5g boric acid, add 33mL boiling water and stir until it dissolves; The boric acid solution of dissolving is slowly added in the single nickel salt of dissolving and the mixing solutions of nickelous chloride; Take 0.01g sodium lauryl sulphate, add minor amount of water and make it in the pasty state, then add 1mL boiling water or solution is boiled again and make it dissolve completely, sodium dodecyl sulfate solution is added in solution obtained in the previous step; Take 0.15g asccharin, 0.01g1,4-butynediol, 0.01g tonka bean camphor, pour in solution obtained in the previous step again after dissolving with distilled water respectively, last adding distil water is to 100mL volume;
B, nickel plating: nickel metal is connected on anode, the carbon fiber/cyanate ester resin composite material through electroless plating is connected on negative electrode, passes to 1.5A/dm
2electric current, then negative electrode, anode are put into respectively the electroplate liquid of 60 DEG C, interpole gap 30mm, and ensure the two poles of the earth parallel, take out after 13h.
Embodiment 4
Adopt the carbon fiber/cyanate ester resin composite sheet of diameter d=80mm, thickness t=5mm, plating area is 1.13dm
2, plating solution loading capacity refers to the ratio of workpiece plating area and plating solution volume, is 1.13dm according to plating solution loading capacity
2/ L calculates required chemical plating fluid and electroplate liquid volume is 1L.
Step 1, pre-treatment,
A, oil removing: carbon fiber/cyanate ester resin composite material is immersed in 1L acetone, the washing of taking-up distilled water, drying after ultrasonic 17min;
B, alligatoring: the material obtained by step a is immersed in the nitric acid of 1L35%, heating in water bath to 40 DEG C, with distilled water washing, drying after insulation 16min;
C, sensitization: 15g tin protochloride is dissolved in 40mL concentrated hydrochloric acid, add 16g tin grain, obtain sensitizing solution with distilled water diluting to 1L, control temperature is 30 DEG C, and the material obtained by step b soaks taking-up distilled water hydrostatic rinsing after 20min, drying in sensitizing solution;
D, activation: 0.3g Palladous chloride is dissolved in 10mL concentrated hydrochloric acid, obtains activation solution with distilled water diluting to 1L, control temperature is 28 DEG C, and the material obtained by step c soaks taking-up distilled water washing after 22min, dry in activation solution;
E, reduction: 10g inferior sodium phosphate is added distillation dissolved dilution to 1L, under material room temperature steps d obtained, in ortho phosphorous acid sodium solution, soak 1min;
Step 2, electroless plating,
A, configuration 1L chemical plating fluid: get 24g single nickel salt, 24g sodium hypophosphite, 23mL lactic acid, 6g propanedioic acid, 17g sodium-acetate, dissolve with a small amount of distilled water respectively; Respectively the propanedioic acid of dissolving and lactic acid are added in the sodium-acetate of dissolving; By consoluet single nickel salt, join in solution obtained in the previous step lentamente; By consoluet sodium hypophosphite, under stirring tempestuously, join in solution obtained in the previous step lentamente; Use distilled water by solution dilution obtained in the previous step to 1L; Ammoniacal liquor is used to regulate solution obtained in the previous step to pH value to be 6.0;
B, nickel plating: the chemical plating fluid carbon fiber/cyanate ester resin composite material through pre-treatment being put into 87 DEG C, take out after soaking 90min, dry after cleaning with distilled water;
Step 3, plating,
A, configuration 1L electroplate liquid: take 280g single nickel salt and 42g nickelous chloride, the distilled water adding 333mL dissolves; Take 42g boric acid, add 333mL boiling water and stir until it dissolves; The boric acid solution of dissolving is slowly added in the single nickel salt of dissolving and the mixing solutions of nickelous chloride; Take 0.2g sodium lauryl sulphate, add minor amount of water and make it in the pasty state, then add 5mL boiling water or solution is boiled again and make it dissolve completely, sodium dodecyl sulfate solution is added in solution obtained in the previous step; Take 1.4g asccharin, 0.2g1,4-butynediol, 0.2g tonka bean camphor, pour in solution obtained in the previous step again after dissolving with distilled water respectively, last adding distil water is to 1L;
B, nickel plating: nickel metal is connected on anode, the carbon fiber/cyanate ester resin composite material through electroless plating is connected on negative electrode, passes to 1.5A/dm
2electric current, then negative electrode, anode are put into respectively the electroplate liquid of 60 DEG C, interpole gap 45mm, and ensure the two poles of the earth parallel, take out after 12h.
The method of carbon fiber of the present invention/cyanate ester resin composite material nickel plating, electroless plating is combined with plating, first use the method nickel preplating of electroless plating, material surface is made to have the uniform conductive layer of one deck, then electric plating method is adopted to thicken nickel dam, both ensure that the even of nickel layer, in turn ensure that coating has enough thickness, existing data shows that coating is generally tens microns to tens microns, the method that the present invention is combined with plating by electroless plating, coating is made to reach about 400 μm, chemical plating is Ni-P alloy, electrolytic coating is pure Ni, good with base material bonding force, seamless existence, and coating surface is bright, no significant defect, meet aerospace light microscopic working conditions, coating is even, complete, without plating leakage phenomenon, and plating and electroless plating production cost low, can be mass.
Claims (7)
1. the method for carbon fiber/cyanate ester resin composite material nickel plating, is characterized in that, first uses the method for electroless plating at material surface nickel preplating the carbon fiber/cyanate ester resin composite material through pre-treatment, then adopts electric plating method to continue nickel plating;
Described pre-treatment specifically comprises the following steps:
A, oil removing: carbon fiber/cyanate ester resin composite material is soaked in acetone, the washing of taking-up distilled water, drying after ultrasonic 10 ~ 20min;
B, alligatoring: be immersed in the nitric acid of 35% by the material that described step a obtains, heating in water bath to 40 DEG C, with distilled water washing, drying after insulation 15 ~ 20min;
C, sensitization: be dissolved in by tin protochloride in concentrated hydrochloric acid, add tin grain, obtains sensitizing solution with distilled water diluting to volume required, and the material obtained by described step b soaks taking-up distilled water hydrostatic rinsing after 10 ~ 25min, drying in sensitizing solution;
D, activation: be dissolved in by Palladous chloride in concentrated hydrochloric acid, obtain activation solution with distilled water diluting to volume required, and the material obtained by described step c soaks taking-up distilled water washing after 15 ~ 25min, drying in activation solution;
E, reduction: be soak 1 ~ 2min in the ortho phosphorous acid sodium water solution of 1% in concentration under the material room temperature that described steps d is obtained.
2. the method for carbon fiber/cyanate ester resin composite material nickel plating as claimed in claim 1, it is characterized in that, in described step c, the concentration of tin protochloride is 15g/L, and the concentration of described concentrated hydrochloric acid is 40mL/L, described tin grain concentration is 15 ~ 20g/L, and described soaking temperature is 28 ~ 32 DEG C.
3. the method for carbon fiber/cyanate ester resin composite material nickel plating as claimed in claim 1, it is characterized in that, in described steps d, the concentration of Palladous chloride is 0.3g/L, and the concentration of described concentrated hydrochloric acid is 10mL/L, and described soaking temperature is 28 ~ 32 DEG C.
4. the method for carbon fiber/cyanate ester resin composite material nickel plating as claimed in claim 1, it is characterized in that, the concrete operations of described electroless plating are: the chemical plating fluid carbon fiber/cyanate ester resin composite material through pre-treatment being put into 85 ~ 90 DEG C, take out after soaking 85 ~ 95min, dry after cleaning with distilled water.
5. the method for carbon fiber/cyanate ester resin composite material nickel plating as claimed in claim 4, it is characterized in that, described chemical plating fluid consists of: sulfur acid nickel 23 ~ 27g, sodium hypophosphite 23 ~ 27g, lactic acid 22 ~ 26mL, propanedioic acid 4 ~ 6g, sodium-acetate 12 ~ 18g in 1L chemical plating fluid, surplus is distilled water, and use ammoniacal liquor to regulate described chemical plating fluid to make its pH value be 6.0, the loading capacity of described chemical plating fluid is 0.5 ~ 1.43dm
2/ L.
6. the method for carbon fiber/cyanate ester resin composite material nickel plating as claimed in claim 1, it is characterized in that, the concrete operations of described plating are: nickel metal is connected on anode, and the carbon fiber/cyanate ester resin composite material through electroless plating is connected on negative electrode, passes to 1.5A/dm
2electric current, then negative electrode, anode are put into respectively the electroplate liquid of 60 DEG C, interpole gap 30 ~ 50mm, and ensure the two poles of the earth parallel, take out after 11 ~ 13h.
7. the method for carbon fiber/cyanate ester resin composite material nickel plating as claimed in claim 6, it is characterized in that, described electroplate liquid consists of: sulfur acid nickel 260 ~ 300g, nickelous chloride 35 ~ 45g, boric acid 35 ~ 45g, asccharin 1.0 ~ 1.5g, 1 in 1L electroplate liquid, 4-butynediol 0.1 ~ 0.3g, tonka bean camphor 0.1 ~ 0.3g, sodium lauryl sulphate 0.1 ~ 0.3g, surplus is distilled water, and the loading capacity of described electroplate liquid is 0.5 ~ 1.43dm
2/ L.
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| CN104131271A (en) * | 2014-07-21 | 2014-11-05 | 西安理工大学 | Method for low-temperature alkaline nickel plating of carbon fiber/cyanate resin composite material |
| CN106148919B (en) * | 2015-03-25 | 2018-10-16 | 中国科学院深圳先进技术研究院 | Porous nickel paper and preparation method thereof, electrode slice and preparation method thereof |
| CN105734535B (en) * | 2016-03-18 | 2019-03-05 | 大连理工大学 | A method of improving composite material nickel coating bond strength |
| CN108400339B (en) * | 2018-02-28 | 2020-05-05 | 湖北大学 | Preparation method and application of nickel cloth current collector |
| CN113668020B (en) * | 2021-08-03 | 2022-10-11 | 安徽三宝棉纺针织投资有限公司 | Preparation method of carbon fiber fabric electroplating solution |
| CN113668026B (en) * | 2021-08-03 | 2022-10-11 | 安徽三宝棉纺针织投资有限公司 | Preparation method of multifunctional carbon fiber fabric |
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| CN102086517A (en) * | 2009-12-08 | 2011-06-08 | 沈阳临德陶瓷研发有限公司 | Chemical nickel-plating method for carbon fiber |
| CN103305820A (en) * | 2013-06-09 | 2013-09-18 | 西北工业大学 | Plating solution for chemically plated bottom nickel and electroplated nickel of carbon fiber cyanate ester-based composite material, and plating method thereof |
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| CN103305820A (en) * | 2013-06-09 | 2013-09-18 | 西北工业大学 | Plating solution for chemically plated bottom nickel and electroplated nickel of carbon fiber cyanate ester-based composite material, and plating method thereof |
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