CN102086517A - Chemical nickel-plating method for carbon fiber - Google Patents
Chemical nickel-plating method for carbon fiber Download PDFInfo
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- CN102086517A CN102086517A CN2009102206120A CN200910220612A CN102086517A CN 102086517 A CN102086517 A CN 102086517A CN 2009102206120 A CN2009102206120 A CN 2009102206120A CN 200910220612 A CN200910220612 A CN 200910220612A CN 102086517 A CN102086517 A CN 102086517A
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Abstract
The invention discloses a chemical nickel-plating method for carbon fiber, which is designed for overcoming the disadvantages of high cost, a large number of process steps and poor operability existing in the prior art. In the method, a chemical plating process is adopted; and a pre-treatment is performed on a raw material and chemical plating solution is prepared before the chemical plating. The pre-treatment process comprises the steps of: calcining by using a muffle furnace to remove glue; soaking in solution of absolute ethanol to remove oil; performing surface roughening and activating treatment by using solution of sodium hydroxide and solution of silver ammonia; sensitizing by using a sensitizer, namely stannous chloride; and performing surface reduction by using solution of sodium hypophosphite. The chemical plating solution consists of nickel sulfate hexahydrate, sodium hypophosphite, sodium pyrophosphate and sodium citrate. The chemical nickel-plating on the carbon fiber is finished by placing a pre-treatment product of the chemical plating into the chemical plating solution, and reacting, standing, filtering and drying under a chemical plating condition. The method has the characteristics that: the product has a uniform surface, a compact plating layer and uniform particles.
Description
Technical field
The invention belongs to field of compound material, relate to a kind of chemical nickel plating method of carbon fiber
Background technology
Metal-based carbon fiber composite material has premium propertiess such as high specific strength, high ratio modulus and good toughness, has broad application prospects in aerospace, biomaterial and civilian industry field.Carbon fiber with surface metalation is made filler, and prepared shielding material has good shield effectiveness, can be used as the absorbing material of aircraft; The metallizing carbon fiber is woven into fabric by certain way, can make the three-dimensional bait body of emulation, and the counterradar reconnaissance and the counter that are used for high-tech war are led.But, volatile in Ni-Speed in the existing chemical nickel plating method owing to the noxious solvent that adopts the hydrofluoric acid acid etching, and adopt the Palladous chloride activation treatment, existing for this reason method cost is higher, and processing step is many, poor operability.
Summary of the invention
The present invention seeks in order to solve in the existing chemical plating method, owing to adopt the noxious solvent of hydrofluoric acid acid etching, volatile in Ni-Speed, and employing Palladous chloride activation treatment, cost is higher, and processing step is many, deficiencies such as poor operability, a kind of chemical nickel plating method of carbon fiber is provided, and its preparation process is as follows:
The first step: to the pre-treatment of matrix
(1) technology of removing photoresist is earlier removed photoresist carbon fiber with the retort furnace high temperature sintering; Remove photoresist condition: temperature 200-500 ℃, time 5-30min;
(2) oil removing process adds the carbon fiber that obtains in the step (1) in the oil removal treatment liquid dehydrated alcohol; The oil removing condition: room temperature, under the condition of power 500W, magnetic agitation disperses to make first reaction solution behind the reaction 30-60min; First reaction solution is washed acquisition first product, and the washing condition is diluted first reaction solution at ambient temperature with deionized water, adds the 800-1000ml deionized water and dilute in every 100ml first reaction solution; Behind the sedimentation 60-90min supernatant liquid is removed, repeated 2-3 back and obtain first product;
(3) preparation roughening treatment liquid roughening treatment liquid is made up of sodium hydroxide (NaOH) and deionized water; Add 2-3g sodium hydroxide (NaOH) in the deionized water of consumption: 100ml;
(4) roughening process adds first product in the roughening treatment liquid; The alligatoring condition is under the condition of room temperature, power 500W, and magnetic agitation disperses to make second reaction solution behind the reaction 20-60min; Second reaction solution is carried out suction filtration obtain second product, the suction filtration condition is at ambient temperature, and the vacuum tightness of regulating suction filtration vacuum instrument be-0.1MPa acquisition second product behind the suction filtration time 5-10min;
(5) preparation sensitization treatment solution sensitization treatment solution is by tin protochloride (SnCl
22H
2O) and deionized water form; Add 2-3g tin protochloride (SnCl in the deionized water of consumption: 100ml
22H
2O);
(6) sensitization technology adds second product in the sensitization treatment solution, and the sensitization condition is under the condition of room temperature, power 500W, and magnetic agitation disperses to make the 3rd reaction solution behind the reaction 20-60min; The 3rd reaction solution is carried out suction filtration obtain third product, the suction filtration condition is at ambient temperature, and the vacuum tightness of adjusting suction filtration vacuum instrument is-0.1MPa to obtain third product behind the suction filtration time 5-10min;
(7) preparation activation treatment liquid activation treatment liquid is by Silver Nitrate (AgNO
3), sodium hydroxide (NaOH), ammoniacal liquor (NH
4OH) and deionized water form; Add 1-5g Silver Nitrate (AgNO in the deionized water of consumption: 100ml
3) and 1.5-3.5g sodium hydroxide (NaOH), ammoniacal liquor (NH
4OH) an amount of;
(8) activating process adds third product in the activation treatment liquid, and activation condition is under the condition of room temperature, power 500W, and magnetic agitation disperses to make the 4th reaction solution behind the reaction 30-180min;
The 4th reaction solution is carried out suction filtration obtain the 4th product, the suction filtration condition is at ambient temperature, and the vacuum tightness of regulating suction filtration vacuum instrument be-0.1MPa acquisition the 4th product behind the suction filtration time 5-10min;
(9) preparation reduction treatment solution reduction treatment solution is made up of sodium hypophosphite and deionized water; Add the 1-5g sodium hypophosphite in the deionized water of consumption: 100ml; Reductive condition: under the condition of room temperature, power 500W, magnetic agitation disperses to make the 5th reaction solution behind the reaction 4-6min; The 5th reaction solution is carried out suction filtration obtain the 5th product, the suction filtration condition is at ambient temperature, and the vacuum tightness of regulating suction filtration vacuum instrument be-0.1MPa acquisition the 5th product behind the suction filtration time 5-10min; The 5th product is put into loft drier, behind dry 5h under 90 ℃ the condition, make the 6th product;
Second step: electroless plating is handled
(1) preparation chemical plating fluid chemical plating fluid is made up of nickel sulfate hexahydrate, inferior sodium phosphate, trisodium phosphate, Trisodium Citrate and deionized water; Consumption: 2-4g nickel sulfate hexahydrate, 2-4g inferior sodium phosphate, 2-4g trisodium phosphate, 1-3g Trisodium Citrate join respectively in the deionized water of 100ml; In chemical plating fluid, add the pH=9.5-10.5 that ammoniacal liquor is regulated described chemical plating fluid, obtain chemical plating fluid;
(2) chemical plating technology is put into chemical plating fluid with the 6th product, and the electroless plating condition is under the condition of 70 ℃-90 ℃ of temperature, power 500W, and magnetic agitation leaves standstill 3-5min and makes the 6th reaction solution after disperseing reaction 60-120min; The 6th reaction solution is carried out suction filtration obtain the 7th product, the suction filtration condition: at ambient temperature, the vacuum tightness of regulating suction filtration vacuum instrument is-0.1MPa to obtain the 7th product behind the suction filtration time 5-10min; The 7th product is put into loft drier, behind dry 4-5h under 90-110 ℃ the condition, make the 8th product, promptly coat layer of metal nickel, finish chemical nickel plating carbon fiber at carbon fiber surface.
Characteristics of the present invention and beneficial effect: cost is low, and is simple to operate, effectively the use range of enhanced carbon fiber.Mainly be that this method does not have volatile noxious solvent, the useless hydrofluoric acid acid etching of present method step; And while low price avoids using the Palladous chloride activation treatment, and replace with Silver Nitrate; Technology is simple, and is workable.
Description of drawings:
Fig. 1 carbon fiber chemical nickel plating sem photograph
Fig. 2 carbon fiber chemical nickel plating energy spectrum analysis figure
Embodiment:
A kind of chemical nickel plating method of carbon fiber, its preparation process is as follows:
The first step: to the pre-treatment of matrix
(1) technology of removing photoresist is earlier removed photoresist carbon fiber with the retort furnace high temperature sintering; Remove photoresist condition: temperature 200-500 ℃, time 5-30min;
(2) oil removing process adds the carbon fiber that obtains in the step (1) in the oil removal treatment liquid dehydrated alcohol; The oil removing condition: room temperature, under the condition of power 500W, magnetic agitation disperses to make first reaction solution behind the reaction 30-60min; First reaction solution is washed acquisition first product, and the washing condition is diluted first reaction solution at ambient temperature with deionized water, adds the 800-1000ml deionized water and dilute in every 100ml first reaction solution; Behind the sedimentation 60-90min supernatant liquid is removed, repeated 2-3 back and obtain first product;
(3) preparation roughening treatment liquid roughening treatment liquid is made up of sodium hydroxide (NaOH) and deionized water; Add 2-3g sodium hydroxide (NaOH) in the deionized water of consumption: 100ml;
(4) roughening process adds first product in the roughening treatment liquid; The alligatoring condition is under the condition of room temperature, power 500W, and magnetic agitation disperses to make second reaction solution behind the reaction 20-60min; Second reaction solution is carried out suction filtration obtain second product, the suction filtration condition is at ambient temperature, and the vacuum tightness of regulating suction filtration vacuum instrument be-0.1MPa acquisition second product behind the suction filtration time 5-10min;
(5) preparation sensitization treatment solution sensitization treatment solution is by tin protochloride (SnCl
22H
2O) and deionized water form; Add 2-3g tin protochloride (SnCl in the deionized water of consumption: 100ml
22H
2O);
(6) sensitization technology adds second product in the sensitization treatment solution, and the sensitization condition is under the condition of room temperature, power 500W, and magnetic agitation disperses to make the 3rd reaction solution behind the reaction 20-60min; The 3rd reaction solution is carried out suction filtration obtain third product, the suction filtration condition is at ambient temperature, and the vacuum tightness of adjusting suction filtration vacuum instrument is-0.1MPa to obtain third product behind the suction filtration time 5-10min;
(7) preparation activation treatment liquid activation treatment liquid is by Silver Nitrate (AgNO
3), sodium hydroxide (NaOH), ammoniacal liquor (NH
4OH) and deionized water form; Add 1-5g Silver Nitrate (AgNO in the deionized water of consumption: 100ml
3) and 1.5-3.5g sodium hydroxide (NaOH), ammoniacal liquor (NH
4OH) an amount of;
(8) activating process adds third product in the activation treatment liquid, and activation condition is under the condition of room temperature, power 500W, and magnetic agitation disperses to make the 4th reaction solution behind the reaction 30-180min; The 4th reaction solution is carried out suction filtration obtain the 4th product, the suction filtration condition is at ambient temperature, and the vacuum tightness of regulating suction filtration vacuum instrument be-0.1MPa acquisition the 4th product behind the suction filtration time 5-10min;
(9) preparation reduction treatment solution reduction treatment solution is made up of sodium hypophosphite and deionized water; Add the 1-5g sodium hypophosphite in the deionized water of consumption: 100ml; Reductive condition: under the condition of room temperature, power 500W, magnetic agitation disperses to make the 5th reaction solution behind the reaction 4-6min; The 5th reaction solution is carried out suction filtration obtain the 5th product, the suction filtration condition is at ambient temperature, and the vacuum tightness of regulating suction filtration vacuum instrument be-0.1MPa acquisition the 5th product behind the suction filtration time 5-10min; The 5th product is put into loft drier, behind dry 5h under 90 ℃ the condition, make the 6th product;
Second step: electroless plating is handled
(1) preparation chemical plating fluid chemical plating fluid is made up of nickel sulfate hexahydrate, inferior sodium phosphate, trisodium phosphate, Trisodium Citrate and deionized water; Consumption: 2-4g nickel sulfate hexahydrate, 2-4g inferior sodium phosphate, 2-4g trisodium phosphate, 1-3g Trisodium Citrate join respectively in the deionized water of 100ml; In chemical plating fluid, add ammoniacal liquor and regulate described chemical plating fluid pH=9.5-10.5, obtain chemical plating fluid;
(2) chemical plating technology is put into chemical plating fluid with the 6th product, and the electroless plating condition is under the condition of 70 ℃-90 ℃ of temperature, power 500W, and magnetic agitation leaves standstill 3-5min and makes the 6th reaction solution after disperseing reaction 60-120min; The 6th reaction solution is carried out suction filtration obtain the 7th product, the suction filtration condition: at ambient temperature, the vacuum tightness of regulating suction filtration vacuum instrument is-0.1MPa to obtain the 7th product behind the suction filtration time 5-10min; The 7th product is put into loft drier, behind dry 4-5h under 90-110 ℃ the condition, make the 8th product, promptly coat layer of metal nickel, finish chemical nickel plating carbon fiber at carbon fiber surface.
Embodiment 1
A kind of chemical nickel plating method of carbon fiber:
The first step: to the pre-treatment of matrix
Carbon fiber is placed in the retort furnace, 400 ℃ of temperature, after high temperature sintering removes photoresist under the time 30min condition, 25 ℃ of room temperatures, under the condition of power 500W, places dehydrated alcohol to soak, magnetic agitation is disperseed reaction 30min, obtains first reaction solution; Adding the 900ml deionized water in every 100ml first reaction solution dilutes; Behind the sedimentation 80min supernatant liquid is removed, repeated 2-3 back and obtain first product; Roughening treatment, magnetic agitation is disperseed reaction 30min after-filtration in 30g/L sodium hydroxide (NaOH) solution, and regulating the vacuum tightness of filtering the vacuum instrument is-0.1MPa to obtain second product behind the suction filtration time 8min; Sensitization is handled, at 30g/L tin protochloride (SnCl
22H
2O) flood in the sensitizing solution, magnetic agitation disperses to filter behind the reaction 30min, and the vacuum tightness of regulating suction filtration vacuum instrument is-0.1MPa to obtain third product behind the suction filtration time 8min; Activation treatment is at 40g/L Silver Nitrate (AgNO
3) and 25g/L sodium hydroxide (NaOH), ammoniacal liquor (NH
4OH) activation treatment in an amount of silver ammino solution, magnetic agitation disperse to filter behind the reaction 150min, and the vacuum tightness of regulating suction filtration vacuum instrument be-0.1MPa acquisition the 4th product behind the suction filtration time 8min; Reduction is handled, and reduces in 20 gram/L sodium hypophosphite solution, and magnetic agitation disperses to filter behind the reaction 5min, and the vacuum tightness of regulating suction filtration vacuum instrument is-0.1MPa to obtain the 5th product behind the suction filtration time 8min; The 5th product is put into loft drier, behind dry 5h under 90 ℃ the condition, make the 6th product.
Second step: electroless plating is handled
Chemical plating fluid is by 28g/L nickel sulfate hexahydrate (NiSO
46H
2O), 26g/L inferior sodium phosphate (NaH
2PO
2), 26g/L trisodium phosphate (NaAC), 15g/L Trisodium Citrate and deionized water form; In chemical plating fluid, add the pH=9.5-10.5 that ammoniacal liquor is regulated chemical plating fluid, the 6th product is put into chemical plating fluid, under the condition of 80 ℃ of temperature, power 500W, after magnetic agitation is disperseed reaction 120min, leaving standstill 5min filters again, the vacuum tightness of regulating suction filtration vacuum instrument is-0.1MPa to obtain the 7th product behind the suction filtration time 8min; The 7th product is put into loft drier, behind dry 4h under 90 ℃ the condition, coat layer of metal nickel, finish chemical nickel plating carbon fiber at carbon fiber surface.
Embodiment 2
A kind of chemical nickel plating method of carbon fiber, its preparation process is as follows:
The first step: to the pre-treatment of matrix
Carbon fiber is calcined 5min under 300 ℃ in stove; Soaked in absolute ethyl alcohol 60min; Under the room temperature, in the NaOH of 30g/L solution, stir the 30min after-filtration; Under the room temperature, at the SnCL of 30g/L
2Flood 30min in the sensitizing solution, filter; The configuration silver ammino solution stirs 2h under the room temperature, filters; NaH at 20g/L
2PO
2Reduce 5min in the solution, filter;
Second step: electroless plating is handled
Configuration plating bath (28g/L NiSO
46H
2O, 26g/L NaH
2PO
2, 26g/L NaAC, 15g/L Trisodium Citrate), carbon fiber is poured in the plating bath, be heated to 80 ℃ of whiles with stirring, reaction 2h.Other are with embodiment 1.
Embodiment 3
A kind of chemical nickel plating method of carbon fiber, its preparation process is as follows:
The first step: to the pre-treatment of matrix
Carbon fiber is calcined 5min under 400 ℃ in stove; Soaked in absolute ethyl alcohol 60min; Under the room temperature, in the NaOH of 20g/L solution, stir the 30min after-filtration; Under the room temperature, at the SnCL of 20g/L
2Flood 30min in the sensitizing solution, filter; The configuration silver ammino solution stirs 1h under the room temperature, filters; NaH at 10g/L
2PO
2Reduce 3min in the solution, filter.
Second step: electroless plating is handled
Configuration plating bath (40g/L NiSO
46H
2O, 40g/L NaH
2PO
2, 40g/L NaAC, 30g/L Trisodium Citrate), carbon fiber is poured in the plating bath, be heated to 90 ℃ of whiles with stirring, reaction 1h.Other are with embodiment 1.
Embodiment 4
A kind of chemical nickel plating method of carbon fiber, its preparation process is as follows:
The first step: to the pre-treatment of matrix
Carbon fiber is calcined 20min under 500 ℃ in stove; Soaked in absolute ethyl alcohol 30min; Under the room temperature, in the NaOH of 20g/L solution, stir the 20min after-filtration; Under the room temperature, at the SnCL of 20g/L
2Flood 20min in the sensitizing solution, filter; The configuration silver ammino solution stirs 2h under the room temperature, filters; NaH at 20g/L
2PO
2Reduce 4min in the solution, filter.
Second step: electroless plating is handled
Configuration plating bath (20g/L NiSO
46H
2O, 20g/L NaH
2PO
2, 20g/L NaAC, 10g/L Trisodium Citrate), carbon fiber is poured in the plating bath, be heated to 70 ℃ of whiles with stirring, reaction 2h.Other are with embodiment 1.
Claims (1)
1. the chemical nickel plating method of a carbon fiber, its preparation process is as follows:
The first step: to the pre-treatment of matrix
(1) technology of removing photoresist is earlier removed photoresist carbon fiber with the retort furnace high temperature sintering; Remove photoresist condition: temperature 200-500 ℃, time 5-30min;
(2) oil removing process adds the carbon fiber that obtains in the step (1) in the oil removal treatment liquid dehydrated alcohol; The oil removing condition: room temperature, under the condition of power 500W, magnetic agitation disperses to make first reaction solution behind the reaction 30-60min; First reaction solution is washed acquisition first product, and the washing condition is diluted first reaction solution at ambient temperature with deionized water, adds the 800-1000ml deionized water and dilute in every 100ml first reaction solution; Behind the sedimentation 60-90min supernatant liquid is removed, repeated 2-3 back and obtain first product;
(3) preparation roughening treatment liquid roughening treatment liquid is made up of sodium hydroxide (NaOH) and deionized water; Add 2-3g sodium hydroxide (NaOH) in the deionized water of consumption: 100ml;
(4) roughening process adds first product in the roughening treatment liquid; The alligatoring condition is under the condition of room temperature, power 500W, and magnetic agitation disperses to make second reaction solution behind the reaction 20-60min; Second reaction solution is carried out suction filtration obtain second product, the suction filtration condition is at ambient temperature, and the vacuum tightness of regulating suction filtration vacuum instrument be-0.1MPa acquisition second product behind the suction filtration time 5-10min;
(5) preparation sensitization treatment solution sensitization treatment solution is by tin protochloride (SnCl
22H
2O) and deionized water form; Add 2-3g tin protochloride (SnCl in the deionized water of consumption: 100ml
22H
2O);
(6) sensitization technology adds second product in the sensitization treatment solution, and the sensitization condition is under the condition of room temperature, power 500W, and magnetic agitation disperses to make the 3rd reaction solution behind the reaction 20-60min; The 3rd reaction solution is carried out suction filtration obtain third product, the suction filtration condition is at ambient temperature, and the vacuum tightness of adjusting suction filtration vacuum instrument is-0.1MPa to obtain third product behind the suction filtration time 5-10min;
(7) preparation activation treatment liquid activation treatment liquid is by Silver Nitrate (AgNO
3), sodium hydroxide (NaOH), ammoniacal liquor (NH
4OH) and deionized water form; Add 1-5g Silver Nitrate (AgNO in the deionized water of consumption: 100ml
3) and 1.5-3.5g sodium hydroxide (NaOH), ammoniacal liquor (NH
4OH) an amount of;
(8) activating process adds third product in the activation treatment liquid, and activation condition is under the condition of room temperature, power 500W, and magnetic agitation disperses to make the 4th reaction solution behind the reaction 30-180min; The 4th reaction solution is carried out suction filtration obtain the 4th product, the suction filtration condition is at ambient temperature, and the vacuum tightness of regulating suction filtration vacuum instrument be-0.1MPa acquisition the 4th product behind the suction filtration time 5-10min;
(9) preparation reduction treatment solution reduction treatment solution is made up of sodium hypophosphite and deionized water; Add the 1-5g sodium hypophosphite in the deionized water of consumption: 100ml; Reductive condition: under the condition of room temperature, power 500W, magnetic agitation disperses to make the 5th reaction solution behind the reaction 4-6min; The 5th reaction solution is carried out suction filtration obtain the 5th product, the suction filtration condition is at ambient temperature, and the vacuum tightness of regulating suction filtration vacuum instrument be-0.1MPa acquisition the 5th product behind the suction filtration time 5-10min; The 5th product is put into loft drier, behind dry 5h under 90 ℃ the condition, make the 6th product;
Second step: electroless plating is handled
(1) preparation chemical plating fluid chemical plating fluid is made up of nickel sulfate hexahydrate, inferior sodium phosphate, trisodium phosphate, Trisodium Citrate and deionized water; Consumption: add the 2-4g nickel sulfate hexahydrate in the 100ml deionized water; Add the 2-4g inferior sodium phosphate in the 100ml deionized water; Add the 2-4g trisodium phosphate in the 100ml deionized water; 1-3g Trisodium Citrate in the 100ml deionized water; In chemical plating fluid, add ammoniacal liquor and regulate described chemical plating fluid pH=9.5-10.5, obtain chemical plating fluid;
(2) chemical plating technology is put into chemical plating fluid with the 6th product, and the electroless plating condition is under the condition of 70 ℃-90 ℃ of temperature, power 500W, and magnetic agitation leaves standstill 3-5min and makes the 6th reaction solution after disperseing reaction 60-120min; The 6th reaction solution is carried out suction filtration obtain the 7th product, the suction filtration condition: at ambient temperature, the vacuum tightness of regulating suction filtration vacuum instrument is-0.1MPa to obtain the 7th product behind the suction filtration time 5-10min; The 7th product is put into loft drier, behind dry 4-5h under 90-110 ℃ the condition, make the 8th product, promptly coat layer of metal nickel, finish chemical nickel plating carbon fiber at carbon fiber surface.
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|---|---|---|---|
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- 2009-12-08 CN CN200910220612A patent/CN102086517B/en not_active Expired - Fee Related
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