CN105386048A - Gold plating method for nanosilicon dioxide-epoxy resin composite material - Google Patents

Gold plating method for nanosilicon dioxide-epoxy resin composite material Download PDF

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CN105386048A
CN105386048A CN201510844454.1A CN201510844454A CN105386048A CN 105386048 A CN105386048 A CN 105386048A CN 201510844454 A CN201510844454 A CN 201510844454A CN 105386048 A CN105386048 A CN 105386048A
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solution
epoxy resin
composite material
test piece
resin composite
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CN105386048B (en
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帅和平
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SHENZHEN RUN SUN CHEMICAL TECHNOLOGY Co Ltd
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SHENZHEN RUN SUN CHEMICAL TECHNOLOGY Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/02—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings only including layers of metallic material
    • C23C28/023—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings only including layers of metallic material only coatings of metal elements only
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
    • C23C18/1601—Process or apparatus
    • C23C18/1633—Process of electroless plating
    • C23C18/1635—Composition of the substrate
    • C23C18/1639—Substrates other than metallic, e.g. inorganic or organic or non-conductive
    • C23C18/1641—Organic substrates, e.g. resin, plastic
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
    • C23C18/18—Pretreatment of the material to be coated
    • C23C18/20—Pretreatment of the material to be coated of organic surfaces, e.g. resins
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
    • C23C18/18—Pretreatment of the material to be coated
    • C23C18/20—Pretreatment of the material to be coated of organic surfaces, e.g. resins
    • C23C18/2006—Pretreatment of the material to be coated of organic surfaces, e.g. resins by other methods than those of C23C18/22 - C23C18/30
    • C23C18/2046—Pretreatment of the material to be coated of organic surfaces, e.g. resins by other methods than those of C23C18/22 - C23C18/30 by chemical pretreatment
    • C23C18/2073—Multistep pretreatment
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
    • C23C18/18—Pretreatment of the material to be coated
    • C23C18/20—Pretreatment of the material to be coated of organic surfaces, e.g. resins
    • C23C18/22—Roughening, e.g. by etching
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
    • C23C18/31—Coating with metals
    • C23C18/32—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00—Electroplating: Baths therefor
    • C25D3/02—Electroplating: Baths therefor from solutions
    • C25D3/12—Electroplating: Baths therefor from solutions of nickel or cobalt
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00—Electroplating: Baths therefor
    • C25D3/02—Electroplating: Baths therefor from solutions
    • C25D3/48—Electroplating: Baths therefor from solutions of gold
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/10—Electroplating with more than one layer of the same or of different metals
    • C25D5/12—Electroplating with more than one layer of the same or of different metals at least one layer being of nickel or chromium

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  • Engineering & Computer Science (AREA)
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  • General Chemical & Material Sciences (AREA)
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  • Inorganic Chemistry (AREA)
  • Electroplating Methods And Accessories (AREA)
  • Chemically Coating (AREA)

Abstract

The invention provides a gold plating method for a nanosilicon dioxide-epoxy resin composite material. The gold plating method includes the following step: (1) a swelling agent is added into an alkaline oil removing solution to obtain an oil removing swelling solution, a test piece of the nanosilicon dioxide-epoxy resin composite material is placed into the oil removing swelling solution, oil removing is carried at the temperature ranging from 70 DEG C to 80 DEG C for 10 min to 30 min, and then the test piece is taken out and washed to be clean; (2) the test piece obtained after oil removing swelling processing is placed into an alkaline coarsening solution, coarsening processing is carried out at the temperature ranging from 55 DEG C to 75 DEG C for 5 min to 15 min, and then the test piece is taken out and washed to be clean, wherein the alkaline coarsening solution is prepared from 5-15 g/L of potassium permanganate, 2-5 g/L of sodium hydroxide and deionized water; (3) neutralization is carried out; (4) acid pickling is carried out; (5) activating is carried out; (6) chemical nickel-plating is carried out; (7) electro nickelling is carried out; and (8) electrogilding is carried out. The plating layer stability of the nanosilicon dioxide-epoxy resin composite material obtained with the method is good.

Description

The gold plating method of nano silicon-epoxy resin composite material
Technical field
Composite material surface processing technology field of the present invention, is specifically related to a kind of gold plating method of nano silicon-epoxy resin composite material.
Background technology
Nano silicon is unformed white powder, there is the hydroxyl of a large amount of undersaturated residual bond and different bond styles in its molecular structure, and molecular structure is three-dimensional chain-like structure.Can there is bonding action in some group of this structure and resin, thus greatly improve hardness and the intensity of material.Meanwhile, Nano-meter SiO_2 2particle is little due to size, will be distributed in the space of polymer key, making the intensity of polymkeric substance, toughness, ductility all significantly improve thus when adopting suitable mode and resin compounded.
Epoxy resin has excellent cementability, chemical stability, mechanical property and lower shrinkage, the easily advantage such as processing and low cost, is used widely in fields such as tackiness agent, building, space flight and aviation, coating, electric and advanced composite materials.But, because pure epoxy resin has higher crosslinking structure, there is the shortcomings such as matter is crisp, resistance to fatigue, toughness difference, be difficult to the service requirements meeting engineering, make it apply and be subject to certain restrictions.Therefore, modification is carried out to epoxy resin, to improve one of its performance focus becoming research.
Nano silicon-epoxy resin composite material needs to carry out surface modification usually.In technique, because nano silicon-epoxy resin composite material obtains high quality, the overlay coating difficulty of high reliability is comparatively large, and surfacing process is unreasonable, and coating coating adhesion is not high.Existing nano silicon-epoxy resin composite material is with sulfuric acid/chromic acid alligatoring in roughening process, and the composite material surface after process is combination gold-plated with follow-up nickel plating not easily, and big for environment pollution.
Summary of the invention
For solving the problems such as existing nano silicon-epoxy resin composite material surface modification difficulty is large, binding force of cladding material is poor, the present invention proposes a kind of gold plating method of nano silicon-epoxy resin composite material, its coating good stability of gold-plated nano silicon-epoxy resin composite material that the method obtains.
Technical scheme of the present invention is achieved in that
A gold plating method for nano silicon-epoxy resin composite material, comprises the following steps:
1) alkaline degreasing activates with expansion
Swelling agent is added in alkaline degreasing solution and obtains oil removing expansion solutions, oil removing expansion solutions is put in the test piece of nano silicon-epoxy resin composite material, be 70-80 DEG C in temperature and carry out oil removing 10-30min, then take out washing totally;
2) alkaline alligatoring
Alkaline roughening solution is put in test piece through oil removing expansion process, and at temperature 55-75 DEG C of roughening treatment 5-15min, then take out washing totally, wherein alkaline roughening solution is by 5-15g/L potassium permanganate, 2-5g/L sodium hydroxide and deionized water preparation composition;
3) neutralize
Room temperature, with neutralizer in the test piece of roughening treatment and 1-3min;
4) pickling
Room temperature, carries out washing by soaking 1-3min with acid to the test piece after neutralization;
5) activate
Activated solution is put in test piece after pickling and activates 3-8min, then washing is clean;
6) chemical nickel plating
Test piece after activation is put into the chemical nickel-plating solution plating 20-40min of temperature 75-85 DEG C, then wash with water clean;
7) electronickelling
Test piece after chemical nickel plating being put into nickel plating solution in temperature is 30-60 DEG C of plating 20-40min, current density 10-30A/dm 2, then washing is clean;
8) electrogilding
Test piece through electronickelling being put into gold-plating solution in temperature is 50-55 DEG C of plating 20-40min, current density 0.3-0.5A/dm 2, then washing is clean, dry.
Further, described alkaline degreasing solution is by 5-10g/L sodium hydroxide, and 20-30g/L sodium carbonate, 20-30g/L sodium phosphate, 1-3g/L tensio-active agent and deionized water preparation composition, described alkaline degreasing solution and described swelling agent mass ratio are 1:1.5-3.
Further, described tensio-active agent is sodium laurylsulfonate or sodium stearate, and described swelling agent is anti-plain boiled water.
Further, described neutralizer is organic bases.
Further, the hydrofluoric acid of described acid to be mass concentration be 1-3%.
Further, described activated solution is by 0.15-0.35g/LPdCl 2, 5-15ml/LHCl and deionized water are prepared and are formed.
Further, described chemical nickel-plating solution is by 20-40g/LNiSO 46H 2o, 5-15g/LCH 3cOONa, 5-15g/LNaH 2pO 2form with deionized water.
Further, described nickel plating solution by 5-30g/L nickelous chloride, 50-150g/L nickel sulfamic acid, 20-100g/L boric acid, 0.5-3g/L phenyl aldehyde, 0.5-10g/L polyethoxye amine concentration is, 0.5-10g/L naphthols and deionized water form, and the pH value of described nickel plating solution is 3-6.
Further, described gold-plating solution by 8-12g/L without cyanogen gold salt, 30-50g/LNa 2sO 3, 12-18g/L quadrol, 25-35g/LNa 2sO 4, 25-35ppm aluminium Ti, B grain graining agent, 35-45ppm Tert. Butyl Hydroquinone, 40-60ppm butylated hydroxytoluene, 0.3-0.8g/L benzotriazole, 1.2-1.8g/L trolamine, 10-20g/L SODIUM PHOSPHATE, MONOBASIC and deionized water form, the pH value of described gold-plating solution is 7.8-8.2.
Beneficial effect of the present invention:
1, swelling agent is added in alkaline degreasing solution and obtains oil removing expansion solutions by the present invention, and swelling agent can allow epoxy resin is fluffy is conducive to the gold-plated process of follow-up nickel plating.
2, the present invention's alkalescence roughening solution is by 5-15g/L potassium permanganate, and 2-5g/L sodium hydroxide and deionized water preparation composition, instead of traditional sulfuric acid/chromic acid, not only environmental protection, and be conducive to the follow-up modifying surface to matrix material.
Embodiment
Embodiment 1
A gold plating method for nano silicon-epoxy resin composite material, comprises the following steps:
1) alkaline degreasing activates with expansion
Anti-plain boiled water is added in alkaline degreasing solution and obtains oil removing expansion solutions, oil removing expansion solutions is put in the test piece of nano silicon-epoxy resin composite material, be 80 DEG C in temperature and carry out oil removing 30min, then take out washing totally; Wherein, described alkaline degreasing solution by 10g/L sodium hydroxide, 30g/L sodium carbonate, 20g/L sodium phosphate, 3g/L sodium laurylsulfonate and deionized water preparation composition, alkaline degreasing solution and anti-plain boiled water mass ratio are 1:2;
2) alkaline alligatoring
Alkaline roughening solution is put in test piece through oil removing expansion process, at temperature 65 DEG C of roughening treatment 10min, then take out washing totally, washing time is 5min, wherein alkaline roughening solution is by 10g/L potassium permanganate, 3g/L sodium hydroxide and deionized water preparation composition;
3) neutralize
Room temperature, with organic bases in the test piece of roughening treatment and 3min;
4) pickling
Room temperature, carries out washing by soaking 3min with mass concentration 1% hydrofluoric acid to the test piece after neutralization;
5) activate
Activated solution is put in test piece after pickling and activates 8min, then washing is clean, and washing time is 5min; Wherein activated solution is by 0.35g/LPdCl 2, 15ml/LHCl and deionized water are prepared and are formed;
6) chemical nickel plating
Test piece after activation is put into the chemical nickel-plating solution plating 40min of temperature 85 DEG C, then wash with water clean, washing time is 15min; Wherein chemical nickel-plating solution is by 40g/LNiSO 46H 2o, 5g/LCH 3cOONa, 15g/LNaH 2pO 2form with deionized water;
7) electronickelling
Test piece after chemical nickel plating being put into nickel plating solution in temperature is 45 DEG C of plating 20-40min, current density 15A/dm 2, then washing is clean, and washing time is 5min; Wherein nickel plating solution is by 30g/L nickelous chloride, 90g/L nickel sulfamic acid, 60g/L boric acid, 2.5g/L phenyl aldehyde, and 6.5g/L polyethoxye amine concentration is that 5.5g/L naphthols and deionized water form, and the pH value of described nickel plating solution is 4.5;
8) electrogilding
Test piece through electronickelling being put into gold-plating solution in temperature is 52 DEG C of plating 20-40min, current density 0.3A/dm 2, then washing is clean, dry.Wherein gold-plating solution by 8g/L without cyanogen gold salt, 30g/LNa 2sO 3, 12g/L quadrol, 35g/LNa 2sO 4, 35ppm aluminium Ti, B grain graining agent, 45ppm Tert. Butyl Hydroquinone, 60ppm butylated hydroxytoluene, 0.5g/L benzotriazole, 1.5g/L trolamine, 15g/L SODIUM PHOSPHATE, MONOBASIC and deionized water form, the pH value of described gold-plating solution is 7.8.
Embodiment 2
A gold plating method for nano silicon-epoxy resin composite material, comprises the following steps:
1) alkaline degreasing activates with expansion
Anti-plain boiled water is added in alkaline degreasing solution and obtains oil removing expansion solutions, oil removing expansion solutions is put in the test piece of nano silicon-epoxy resin composite material, be 80 DEG C in temperature and carry out oil removing 30min, then take out washing totally; Wherein, described alkaline degreasing solution by 10g/L sodium hydroxide, 20g/L sodium carbonate, 30g/L sodium phosphate, 3g/L sodium laurylsulfonate and deionized water preparation composition, alkaline degreasing solution and anti-plain boiled water mass ratio are 1:3;
2) alkaline alligatoring
Alkaline roughening solution is put in test piece through oil removing expansion process, at temperature 75 DEG C of roughening treatment 15min, then take out washing totally, washing time is 15min, wherein alkaline roughening solution is by 15g/L potassium permanganate, 5g/L sodium hydroxide and deionized water preparation composition;
3) neutralize
Room temperature, with organic bases in the test piece of roughening treatment and 3min;
4) pickling
Room temperature, carries out washing by soaking 2min with mass concentration 2% hydrofluoric acid to the test piece after neutralization;
5) activate
Activated solution is put in test piece after pickling and activates 6min, then washing is clean, and washing time is 15min; Wherein activated solution is by 0.25g/LPdCl 2, 10ml/LHCl and deionized water are prepared and are formed;
6) chemical nickel plating
Test piece after activation is put into the chemical nickel-plating solution plating 40min of temperature 85 DEG C, then wash with water clean, washing time is 15min; Wherein chemical nickel-plating solution is by 40g/LNiSO 46H 2o, 15g/LCH 3cOONa, 10g/LNaH 2pO 2form with deionized water;
7) electronickelling
Test piece after chemical nickel plating being put into nickel plating solution in temperature is 50 DEG C of plating 20-40min, current density 15A/dm 2, then washing is clean, and washing time is 5min; Wherein nickel plating solution is by 20g/L nickelous chloride, 80g/L nickel sulfamic acid, 60g/L boric acid, 1.5g/L phenyl aldehyde, and 6.0g/L polyethoxye amine concentration is that 4.5g/L naphthols and deionized water form, and the pH value of described nickel plating solution is 5.5;
8) electrogilding
Test piece through electronickelling being put into gold-plating solution in temperature is 55 DEG C of plating 20-40min, current density 0.3A/dm 2, then washing is clean, dry.Wherein gold-plating solution by 12g/L without cyanogen gold salt, 50g/LNa 2sO 3, 18g/L quadrol, 25g/LNa 2sO 4, 35ppm aluminium Ti, B grain graining agent, 45ppm Tert. Butyl Hydroquinone, 60ppm butylated hydroxytoluene, 0.5g/L benzotriazole, 1.5g/L trolamine, 20g/L SODIUM PHOSPHATE, MONOBASIC and deionized water form, the pH value of described gold-plating solution is 8.0.
Embodiment 3
A gold plating method for nano silicon-epoxy resin composite material, comprises the following steps:
1) alkaline degreasing activates with expansion
Anti-plain boiled water is added in alkaline degreasing solution and obtains oil removing expansion solutions, oil removing expansion solutions is put in the test piece of nano silicon-epoxy resin composite material, be 70 DEG C in temperature and carry out oil removing 10min, then take out washing totally; Wherein, described alkaline degreasing solution is by 5g/L sodium hydroxide, and 30g/L sodium carbonate, 30g/L sodium phosphate, 1g/L sodium laurylsulfonate and deionized water preparation composition, alkaline degreasing solution and anti-plain boiled water mass ratio are 1:1.5.
2) alkaline alligatoring
Alkaline roughening solution is put in test piece through oil removing expansion process, at temperature 55 DEG C of roughening treatment 10min, then take out washing totally, washing time is 15min, wherein alkaline roughening solution is by 10g/L potassium permanganate, 3g/L sodium hydroxide and deionized water preparation composition;
3) neutralize
Room temperature, with organic bases in the test piece of roughening treatment and 2min;
4) pickling
Room temperature, carries out washing by soaking 2min with mass concentration 3% hydrofluoric acid to the test piece after neutralization;
5) activate
Activated solution is put in test piece after pickling and activates 5min, then washing is clean, and washing time is 15min; Wherein activated solution is by 0.15g/LPdCl 2, 10ml/LHCl and deionized water are prepared and are formed;
6) chemical nickel plating
Test piece after activation is put into the chemical nickel-plating solution plating 40min of temperature 80 DEG C, then wash with water clean, washing time is 15min; Wherein chemical nickel-plating solution is by 35g/LNiSO 46H 2o, 10g/LCH 3cOONa, 5g/LNaH 2pO 2form with deionized water;
7) electronickelling
Test piece after chemical nickel plating being put into nickel plating solution in temperature is 50 DEG C of plating 20-40min, current density 15A/dm 2, then washing is clean, and washing time is 5min; Wherein nickel plating solution is by 25g/L nickelous chloride, 100g/L nickel sulfamic acid, 80g/L boric acid, 2.5g/L phenyl aldehyde, and 3.5g/L polyethoxye amine concentration is that 5g/L naphthols and deionized water form, and the pH value of described nickel plating solution is 4;
8) electrogilding
Test piece through electronickelling being put into gold-plating solution in temperature is 55 DEG C of plating 20-40min, current density 0.3A/dm 2, then washing is clean, dry.Wherein gold-plating solution by 10g/L without cyanogen gold salt, 40g/LNa 2sO 3, 15g/L quadrol, 30g/LNa 2sO 4, 30ppm aluminium Ti, B grain graining agent, 40ppm Tert. Butyl Hydroquinone, 50ppm butylated hydroxytoluene, 0.5g/L benzotriazole, 1.5g/L trolamine, 15g/L SODIUM PHOSPHATE, MONOBASIC and deionized water form, the pH value of described gold-plating solution is 8.2.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.

Claims (9)

1. a gold plating method for nano silicon-epoxy resin composite material, is characterized in that, comprises the following steps:
1) alkaline degreasing activates with expansion
Swelling agent is added in alkaline degreasing solution and obtains oil removing expansion solutions, oil removing expansion solutions is put in the test piece of nano silicon-epoxy resin composite material, be 70-80 DEG C in temperature and carry out oil removing 10-30min, then take out washing totally;
2) alkaline alligatoring
Alkaline roughening solution is put in test piece through oil removing expansion process, and at temperature 55-75 DEG C of roughening treatment 5-15min, then take out washing totally, wherein alkaline roughening solution is by 5-15g/L potassium permanganate, 2-5g/L sodium hydroxide and deionized water preparation composition;
3) neutralize
Room temperature, with neutralizer in the test piece of roughening treatment and 1-3min;
4) pickling
Room temperature, carries out washing by soaking 1-3min with acid to the test piece after neutralization;
5) activate
Activated solution is put in test piece after pickling and activates 3-8min, then washing is clean;
6) chemical nickel plating
Test piece after activation is put into the chemical nickel-plating solution plating 20-40min of temperature 75-85 DEG C, then wash with water clean;
7) electronickelling
Test piece after chemical nickel plating being put into nickel plating solution in temperature is 30-60 DEG C of plating 20-40min, current density 10-30A/dm 2, then washing is clean;
8) electrogilding
Test piece through electronickelling being put into gold-plating solution in temperature is 50-55 DEG C of plating 20-40min, current density 0.3-0.5A/dm 2, then washing is clean, dry.
2. the gold plating method of nano silicon-epoxy resin composite material according to claim 1, it is characterized in that, described alkaline degreasing solution is by 5-10g/L sodium hydroxide, 20-30g/L sodium carbonate, 20-30g/L sodium phosphate, 1-3g/L tensio-active agent and deionized water preparation composition, described alkaline degreasing solution and described swelling agent mass ratio are 1:1.5-3.
3. the gold plating method of nano silicon-epoxy resin composite material according to claim 2, is characterized in that, described tensio-active agent is sodium laurylsulfonate or sodium stearate, and described swelling agent is anti-plain boiled water.
4. the gold plating method of nano silicon-epoxy resin composite material according to claim 1 and 2, is characterized in that, described neutralizer is organic bases.
5. the gold plating method of nano silicon-epoxy resin composite material according to claim 1 and 2, is characterized in that, the hydrofluoric acid of described acid to be mass concentration be 1-3%.
6. the gold plating method of nano silicon-epoxy resin composite material according to claim 1 and 2, is characterized in that, described activated solution is by 0.15-0.35g/LPdCl 2, 5-15ml/LHCl and deionized water are prepared and are formed.
7. the gold plating method of nano silicon-epoxy resin composite material according to claim 1 and 2, is characterized in that, described chemical nickel-plating solution is by 20-40g/LNiSO 46H 2o, 5-15g/LCH 3cOONa, 5-15g/LNaH 2pO 2form with deionized water.
8. the gold plating method of nano silicon-epoxy resin composite material according to claim 1 and 2, it is characterized in that, described nickel plating solution is by 5-30g/L nickelous chloride, 50-150g/L nickel sulfamic acid, 20-100g/L boric acid, 0.5-3g/L phenyl aldehyde, 0.5-10g/L polyethoxye amine concentration is, 0.5-10g/L naphthols and deionized water form, and the pH value of described nickel plating solution is 3-6.
9. the gold plating method of nano silicon-epoxy resin composite material according to claim 1 and 2, is characterized in that, described gold-plating solution by 8-12g/L without cyanogen gold salt, 30-50g/LNa 2sO 3, 12-18g/L quadrol, 25-35g/LNa 2sO 4, 25-35ppm aluminium Ti, B grain graining agent, 35-45ppm Tert. Butyl Hydroquinone, 40-60ppm butylated hydroxytoluene, 0.3-0.8g/L benzotriazole, 1.2-1.8g/L trolamine, 10-20g/L SODIUM PHOSPHATE, MONOBASIC and deionized water form, the pH value of described gold-plating solution is 7.8-8.2.
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CN102936726A (en) * 2012-11-20 2013-02-20 合肥工业大学 Multiple-layer metallization processing method for epoxy resin package electronic component surface
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CN105714345A (en) * 2016-04-14 2016-06-29 中山品高电子材料有限公司 Method of silver electroplating on nickel of LED bracket
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