CN117385345A - Preparation method and application of electroless nickel gold activator - Google Patents
Preparation method and application of electroless nickel gold activator Download PDFInfo
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- CN117385345A CN117385345A CN202311339442.4A CN202311339442A CN117385345A CN 117385345 A CN117385345 A CN 117385345A CN 202311339442 A CN202311339442 A CN 202311339442A CN 117385345 A CN117385345 A CN 117385345A
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- parts
- circuit board
- printed circuit
- activator
- solution
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- 239000012190 activator Substances 0.000 title claims abstract description 58
- MSNOMDLPLDYDME-UHFFFAOYSA-N gold nickel Chemical compound [Ni].[Au] MSNOMDLPLDYDME-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 42
- 238000007747 plating Methods 0.000 claims abstract description 29
- 239000000126 substance Substances 0.000 claims abstract description 25
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 21
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 60
- TXUICONDJPYNPY-UHFFFAOYSA-N (1,10,13-trimethyl-3-oxo-4,5,6,7,8,9,11,12,14,15,16,17-dodecahydrocyclopenta[a]phenanthren-17-yl) heptanoate Chemical compound C1CC2CC(=O)C=C(C)C2(C)C2C1C1CCC(OC(=O)CCCCCC)C1(C)CC2 TXUICONDJPYNPY-UHFFFAOYSA-N 0.000 claims description 57
- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims description 57
- 239000001119 stannous chloride Substances 0.000 claims description 57
- 235000011150 stannous chloride Nutrition 0.000 claims description 57
- 238000002156 mixing Methods 0.000 claims description 50
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 42
- 238000003756 stirring Methods 0.000 claims description 40
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 37
- 239000000758 substrate Substances 0.000 claims description 35
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 33
- 238000004140 cleaning Methods 0.000 claims description 26
- 238000001035 drying Methods 0.000 claims description 26
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 claims description 24
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 23
- KMUONIBRACKNSN-UHFFFAOYSA-N potassium dichromate Chemical compound [K+].[K+].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O KMUONIBRACKNSN-UHFFFAOYSA-N 0.000 claims description 22
- 239000012153 distilled water Substances 0.000 claims description 21
- 239000011780 sodium chloride Substances 0.000 claims description 21
- 239000011889 copper foil Substances 0.000 claims description 20
- 239000000919 ceramic Substances 0.000 claims description 19
- 238000009713 electroplating Methods 0.000 claims description 18
- 238000003825 pressing Methods 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 15
- TVQLLNFANZSCGY-UHFFFAOYSA-N disodium;dioxido(oxo)tin Chemical compound [Na+].[Na+].[O-][Sn]([O-])=O TVQLLNFANZSCGY-UHFFFAOYSA-N 0.000 claims description 13
- 238000002791 soaking Methods 0.000 claims description 13
- CYEJMVLDXAUOPN-UHFFFAOYSA-N 2-dodecylphenol Chemical compound CCCCCCCCCCCCC1=CC=CC=C1O CYEJMVLDXAUOPN-UHFFFAOYSA-N 0.000 claims description 12
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 12
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 12
- 229940079864 sodium stannate Drugs 0.000 claims description 12
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 11
- 229910000365 copper sulfate Inorganic materials 0.000 claims description 11
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 11
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 11
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 11
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 9
- 239000012298 atmosphere Substances 0.000 claims description 9
- 238000000151 deposition Methods 0.000 claims description 9
- 238000007731 hot pressing Methods 0.000 claims description 9
- 229910052708 sodium Inorganic materials 0.000 claims description 9
- 239000011734 sodium Substances 0.000 claims description 9
- 239000011248 coating agent Substances 0.000 claims description 8
- 238000000576 coating method Methods 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- NRTDAKURTMLAFN-UHFFFAOYSA-N potassium;gold(3+);tetracyanide Chemical compound [K+].[Au+3].N#[C-].N#[C-].N#[C-].N#[C-] NRTDAKURTMLAFN-UHFFFAOYSA-N 0.000 claims description 8
- 238000004321 preservation Methods 0.000 claims description 8
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 claims description 4
- 229910000397 disodium phosphate Inorganic materials 0.000 claims description 3
- 235000019800 disodium phosphate Nutrition 0.000 claims description 3
- XTFKWYDMKGAZKK-UHFFFAOYSA-N potassium;gold(1+);dicyanide Chemical compound [K+].[Au+].N#[C-].N#[C-] XTFKWYDMKGAZKK-UHFFFAOYSA-N 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 2
- 238000013329 compounding Methods 0.000 claims 1
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 abstract description 37
- 239000003795 chemical substances by application Substances 0.000 abstract description 34
- 230000003213 activating effect Effects 0.000 abstract description 32
- 229910052763 palladium Inorganic materials 0.000 abstract description 18
- 230000004913 activation Effects 0.000 abstract description 12
- 230000000694 effects Effects 0.000 abstract description 5
- 229910052751 metal Inorganic materials 0.000 abstract description 4
- 239000002184 metal Substances 0.000 abstract description 4
- 150000002739 metals Chemical class 0.000 abstract description 2
- 238000009792 diffusion process Methods 0.000 abstract 1
- 238000001994 activation Methods 0.000 description 13
- 230000000052 comparative effect Effects 0.000 description 8
- 230000008021 deposition Effects 0.000 description 7
- 150000003839 salts Chemical class 0.000 description 6
- 239000002253 acid Substances 0.000 description 5
- 229910052802 copper Inorganic materials 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 238000007772 electroless plating Methods 0.000 description 3
- 238000001465 metallisation Methods 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000007639 printing Methods 0.000 description 2
- 239000004593 Epoxy Substances 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 125000003636 chemical group Chemical group 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- SFXJSNATBHJIDS-UHFFFAOYSA-N disodium;dioxido(oxo)tin;trihydrate Chemical compound O.O.O.[Na+].[Na+].[O-][Sn]([O-])=O SFXJSNATBHJIDS-UHFFFAOYSA-N 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 150000002500 ions Chemical group 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
Classifications
-
- 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
- C23C18/1803—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces
- C23C18/1824—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces by chemical pretreatment
- C23C18/1837—Multistep pretreatment
- C23C18/1844—Multistep pretreatment with use of organic or inorganic compounds other than metals, first
-
- 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
- C23C18/1646—Characteristics of the product obtained
- C23C18/165—Multilayered product
- C23C18/1653—Two or more layers with at least one layer obtained by electroless plating and one layer obtained by electroplating
-
- 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
- C23C18/34—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents
- C23C18/36—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents using hypophosphites
-
- 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
- C23C28/021—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 including at least one metal alloy layer
-
- 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
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F1/00—Etching metallic material by chemical means
- C23F1/10—Etching compositions
- C23F1/14—Aqueous compositions
- C23F1/16—Acidic compositions
- C23F1/18—Acidic compositions for etching copper or alloys thereof
-
- 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
- C25D3/56—Electroplating: Baths therefor from solutions of alloys
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K3/00—Apparatus or processes for manufacturing printed circuits
- H05K3/10—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern
- H05K3/18—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern using precipitation techniques to apply the conductive material
- H05K3/188—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern using precipitation techniques to apply the conductive material by direct electroplating
Abstract
The invention relates to the field of preparation of printed circuit boards, and discloses a preparation method and application of a electroless nickel gold activator. The printed circuit board is an important part in electronic components, and has the main functions of achieving the effect of connecting the electronic components by electrically connecting the printed circuit board, replacing a chassis of the electronic components by arranging a metalized hole on the printed circuit board, and the activation step has important significance; according to the invention, a metal plating distribution mode is adopted for the printed circuit board, so that the occurrence of a diffusion phenomenon between metals is prevented, a chemical nickel Jin Huohua agent containing metal palladium is firstly used as a main activating component of the activating agent on the selection of the activating agent, the activating performance of the plating activating agent is enhanced, the uneven and black layer phenomena are avoided, the activating performance of the activating agent is improved, and the comprehensive performance of the circuit board is enhanced.
Description
Technical Field
The invention relates to the technical field of printed circuit boards, and discloses a preparation method and application of a electroless nickel gold activator.
Background
Because of the rapid development of high-tech industries such as computers and communications, higher requirements are placed on printed circuit boards in which important electronic components are located, the important process in the printed circuit board is hole metallization, and the activation process is an important step of hole metallization, which provides good catalysis for subsequent electroless plating, and the more the number of apertures of the circuit board, the smaller the aperture, and the better the electrical performance and reliability of the circuit board.
The electroless nickel gold is a common circuit board printing process, and aims to ensure that metals cannot diffuse mutually and improve the performance of a printing plate, a layer of metal ions with activation performance is deposited on the surface of a printed circuit board material, and the activation liquid mainly used for a common printed circuit board is an ion and colloid palladium solution, but the problems that palladium metal ions are unevenly distributed on the surface of the circuit board and the prior art is difficult to realize good activation effect on micro holes exist, and the performance and the subsequent processing process of the circuit board are seriously affected.
Disclosure of Invention
The invention aims to provide a preparation method and application of a electroless nickel gold activator, which are used for solving the problems in the background technology.
In order to solve the technical problems, the invention provides the following technical scheme:
a preparation method of a electroless nickel gold activator is characterized in that: the method comprises the following steps:
s1: adding stannous chloride solution into hydrochloric acid solution, stirring until the stannous chloride solution is completely dissolved, continuously adding sodium stannate, uniformly mixing to obtain solution 1, dissolving palladium chloride into another hydrochloric acid solution, continuously stirring until the stannous chloride is completely dissolved, adding the stannous chloride at a constant temperature, stirring until the stannous chloride is completely dissolved, slowly adding the solution 1, keeping the temperature at 30-40 ℃ and the water bath at 60-70 ℃ for 4-6 hours, and obtaining an activator A;
s2: mixing concentrated hydrochloric acid solution with distilled water, adding palladium chloride and stannous chloride, stirring uniformly, adding sodium chloride solution, stirring continuously, and maintaining the temperature in a constant-temperature water bath to obtain an activator B;
s3: taking a ceramic plate and a copper foil, coating the copper foil on the upper and lower surfaces of the ceramic plate, performing double-sided hot pressing, heating to 200-350 ℃ under the protection of vacuum atmosphere, pressurizing to 20-35 MPa, and pressing for 20-25 h to obtain a printed circuit board substrate;
s4: placing the printed circuit board substrate obtained by pressing into microetching solution obtained by mixing potassium dichromate, concentrated sulfuric acid and distilled water, and taking out after 3-4 min;
s5: mixing an activating agent A with an activating agent B to obtain a chemical nickel Jin Huohua agent, taking the prepared printed circuit board substrate, soaking the printed circuit board substrate in the chemical nickel gold activating agent, taking out the printed circuit board substrate, and cleaning and drying the printed circuit board substrate to obtain an activated printed circuit board;
s6: mixing sulfuric acid solution, sodium chloride, dodecylphenol polyoxyethylene ether, sodium hydrogen phosphate and nickel sulfate, placing the mixture into a printed circuit board, carrying out chemical nickel plating under the conditions that the temperature is 80-90 ℃ and the pH is 8.5-9.5, depositing for 5-25 min, taking out, cleaning and drying;
s7: mixing gold potassium cyanide solution, sodium dodecyl sulfate and copper sulfate, electroplating the printed circuit board soaked in S4 at 50-60 deg.c, pH 5.0 and current density of 2A/dm 2 And (3) electroplating for 15-20 min, taking out, cleaning and drying to obtain the nickel-gold activated printed circuit board.
More preferably, in S1, the components are: according to the weight portions, 10 to 20 portions of stannous chloride solution, 50 to 100 portions of 300mL/L hydrochloric acid solution, 1 to 2 portions of sodium stannate, 0.1 to 1 portion of palladium chloride and 10 to 20 portions of stannous chloride.
More optimally, in S2, the concentration of the concentrated hydrochloric acid solution is 37 percent, the constant temperature is 40-60 ℃, and the heat preservation time is 4-5 hours.
More preferably, in S2, the components are: according to the weight portions, 5 to 20 portions of concentrated hydrochloric acid solution, 5 to 20 portions of distilled water, 0.1 to 1 portion of palladium chloride, 2 to 20 portions of stannous chloride and 150 to 200 portions of sodium chloride.
More preferably, the weight ratio of palladium chloride to stannous chloride is 1:20.
More preferably, in S4, the microetching solution comprises the following components: 10-15 parts of potassium dichromate, 9-18 parts of concentrated sulfuric acid and 85-120 parts of distilled water.
More preferably, in S5, the components are: according to parts by weight, 20-35 parts of activator A and 30-50 parts of activator B, and the soaking time is 20-35 minutes.
More preferably, in S6, the components are: 60-80 parts of sulfuric acid solution, 0.5-1 part of sodium chloride solution, 0.5-1 part of dodecylphenol polyoxyethylene ether, 5-10 parts of sodium hydrophosphate and 1-5 parts of nickel sulfate solution.
More preferably, in S7, the components are: according to the weight portions, 2 to 7 portions of potassium gold cyanide solution, 10 to 15 portions of sodium dodecyl sulfate and 10 to 15 portions of copper sulfate.
Compared with the prior art, the invention has the following beneficial effects:
(1) The most important step of electroless copper plating is activation, the performances of the electroless copper plating layer, such as binding force, uniformity and the like, depend on the activation process, but the acid-based colloidal palladium and the salt-based colloidal palladium have better stability and catalytic activity, palladium metal particles are adsorbed on the surface of the hole wall of the printed circuit board after the printed circuit board is immersed in a colloidal palladium solution to form a catalytic activation layer, so that the activation performance and adhesive force of the electroless plating layer on the surface of a substrate are improved, and the effect of hole metallization is improved;
(2) The prepared acid-based colloidal palladium and salt-based colloidal palladium have good activity and stability, and can obviously improve the quality of the electroless copper plating layer; the salt-based colloidal palladium has better epoxy friendliness, and the mixed system has good activity and stability, and also has better activation performance and environmental friendliness by mixing the acid-based colloidal palladium with the salt-based colloidal palladium in a certain proportion;
(3) The activating agent containing palladium element is used as an important step in each step of electroless nickel gold plating process, nickel in the electroless plating solution is reduced to elemental nickel under the catalysis of palladium to be plated on the printed circuit board, then gold is deposited through displacement reaction, the existence of palladium ensures the surface uniformity in the subsequent steps, and the phenomenon of black disks on the surface of the printed circuit board is prevented.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The preparation method of the electroless nickel gold activator and the preparation process of the electroless nickel gold activator application comprise the following chemicals:
the following components in parts by mass:
sodium stannate: CAS:12058-66-1, shanghai Ala Biochemical technology Co., ltd., palladium chloride: CAS:7647-10-1, model: FLQ-Pd106, shanghai Fuli Hydrogen New energy science and technology Co., ltd., stannous chloride: CAS:7772-99-8, merck life sciences, sodium stannate: CAS:12209-98-2, merck life sciences, ceramic plate: model: HS-48, 95 porcelain, thickness: 3mm, yixing city Heisen ceramic technology Co., ltd., copper foil: thickness: 0.1mm, shenzhen Jin Xin Chengjingjingjingjingsha, dodecylphenol polyoxyethylene ether: CAS:9002-93-1, sodium hydrogen phosphate, a company of the chemical group of Morse (Shandong): CAS:7558-79-4, baizhu (Shanghai) biotechnology Co., ltd., potassium gold cyanide: CAS:13967-50-5.
Example 1:
s1: adding 15 parts of stannous chloride solution into 75 parts of 300mL/L hydrochloric acid solution, stirring until the stannous chloride solution is completely dissolved, continuously adding 1.5 parts of sodium stannate, uniformly mixing to obtain solution 1, dissolving 0.5 part of palladium chloride into the other hydrochloric acid solution, continuously stirring until the stannous chloride is completely dissolved, adding 15 parts of stannous chloride at a constant temperature, stirring until the stannous chloride is completely dissolved, slowly adding the solution 1, keeping the temperature at 40 ℃ and keeping the water bath at 70 ℃ for 6 hours to obtain an activator A;
s2: mixing 10 parts of concentrated hydrochloric acid solution with 10 parts of distilled water, adding 0.5 part of palladium chloride and 10 parts of stannous chloride, uniformly stirring, adding 150 parts of sodium chloride solution, continuously stirring, and carrying out water bath heat preservation at the constant temperature of 40 ℃ for 5 hours to obtain an activator B;
s3: copper foil is coated on the upper surface and the lower surface of the ceramic plate to carry out double-sided hot pressing, the copper foil is heated to 200 ℃ under the protection of vacuum atmosphere, the copper foil is pressurized to 25MPa, and the printed circuit board base material is obtained after 25 hours of pressing;
s4: placing the printed circuit board substrate obtained by pressing into microetching solution obtained by mixing 10 parts of potassium dichromate, 10 parts of concentrated sulfuric acid and 100 parts of distilled water, and taking out after 3 min;
s5: taking 20 parts of an activating agent A and 48 parts of an activating agent B, uniformly mixing to obtain a chemical nickel Jin Huohua agent, taking the prepared printed circuit board substrate, soaking the printed circuit board substrate in the chemical nickel gold activating agent for 25min, taking out, cleaning and drying to obtain an activated printed circuit board;
s6: mixing 75 parts of sulfuric acid solution, 0.8 part of sodium chloride, 0.8 part of dodecylphenol polyoxyethylene ether, 9 parts of sodium hydrophosphate and 3 parts of nickel sulfate, carrying out chemical nickel plating at the temperature of 85 ℃ and the pH value of 9, taking out after 15min of deposition, cleaning and drying;
s7: mixing 5 parts of gold potassium cyanide solution, 12 parts of sodium dodecyl sulfate and 13 parts of copper sulfate uniformly, and then placing the printed circuit board soaked in the S4 into a reactor for electroplating at the temperature of 60 ℃, the pH value of 5.0 and the current density of 2A/dm 2 And (3) electroplating for 20min, taking out, cleaning and drying to obtain the nickel-gold activated printed circuit board.
Example 2:
s1: preparation of activator A: adding 15 parts of stannous chloride solution into 75 parts of 300mL/L hydrochloric acid solution, stirring until the stannous chloride solution is completely dissolved, continuously adding 1.5 parts of sodium stannate, uniformly mixing to obtain solution 1, dissolving 0.5 part of palladium chloride into the other hydrochloric acid solution, continuously stirring until the stannous chloride is completely dissolved, adding 15 parts of stannous chloride at a constant temperature, stirring until the stannous chloride is completely dissolved, slowly adding the solution 1, keeping the temperature at 40 ℃ and keeping the water bath at 70 ℃ for 6 hours to obtain an activator A;
s2: mixing 10 parts of concentrated hydrochloric acid solution with 10 parts of distilled water, adding 0.5 part of palladium chloride and 10 parts of stannous chloride, uniformly stirring, adding 150 parts of sodium chloride solution, continuously stirring, and carrying out water bath heat preservation at the constant temperature of 40 ℃ for 5 hours to obtain an activator B;
s3: taking a ceramic plate and copper foil, coating the copper foil on the upper and lower surfaces of the ceramic plate, performing double-sided hot pressing, heating to 200 ℃ under the protection of vacuum atmosphere, pressurizing to 25MPa, and pressing for 25 hours to obtain a printed circuit board substrate;
s4: placing the printed circuit board substrate obtained by pressing into microetching solution obtained by mixing 10 parts of potassium dichromate, 10 parts of concentrated sulfuric acid and 100 parts of distilled water, and taking out after 3 min;
s5: taking 20 parts of an activating agent A and 48 parts of an activating agent B, uniformly mixing to obtain a chemical nickel Jin Huohua agent, taking the prepared printed circuit board substrate, soaking the printed circuit board substrate in the chemical nickel gold activating agent for 10min, taking out, cleaning and drying to obtain an activated printed circuit board;
s6: mixing 75 parts of sulfuric acid solution, 0.8 part of sodium chloride, 0.8 part of dodecylphenol polyoxyethylene ether, 9 parts of sodium hydrophosphate and 3 parts of nickel sulfate, carrying out chemical nickel plating at the temperature of 85 ℃ and the pH value of 9, taking out after 15min of deposition, cleaning and drying;
s7: mixing 5 parts of gold potassium cyanide solution, 12 parts of sodium dodecyl sulfate and 13 parts of copper sulfate uniformly, and then placing the printed circuit board soaked in the S4 into a reactor for electroplating at the temperature of 60 ℃, the pH value of 5.0 and the current density of 2A/dm 2 And (3) electroplating for 20min, taking out, cleaning and drying to obtain the nickel-gold activated printed circuit board.
Example 3:
s1: preparation of activator A: adding 15 parts of stannous chloride solution into 75 parts of 300mL/L hydrochloric acid solution, stirring until the stannous chloride solution is completely dissolved, continuously adding 1.5 parts of sodium stannate, uniformly mixing to obtain solution 1, dissolving 0.5 part of palladium chloride into the other hydrochloric acid solution, continuously stirring until the stannous chloride is completely dissolved, adding 15 parts of stannous chloride at a constant temperature, stirring until the stannous chloride is completely dissolved, slowly adding the solution 1, keeping the temperature at 40 ℃ and keeping the water bath at 70 ℃ for 6 hours to obtain an activator A;
s2: mixing 10 parts of concentrated hydrochloric acid solution with 10 parts of distilled water, adding 0.5 part of palladium chloride and 10 parts of stannous chloride, uniformly stirring, adding 150 parts of sodium chloride solution, continuously stirring, and carrying out water bath heat preservation at the constant temperature of 40 ℃ for 5 hours to obtain an activator B;
s3: taking a ceramic plate and copper foil, coating the copper foil on the upper and lower surfaces of the ceramic plate, performing double-sided hot pressing, heating to 200 ℃ under the protection of vacuum atmosphere, pressurizing to 25MPa, and pressing for 25 hours to obtain a printed circuit board substrate;
s4: placing the printed circuit board substrate obtained by pressing into microetching solution obtained by mixing 10 parts of potassium dichromate, 10 parts of concentrated sulfuric acid and 100 parts of distilled water, and taking out after 3 min;
s5: taking 20 parts of an activating agent A and 48 parts of an activating agent B, uniformly mixing to obtain a chemical nickel Jin Huohua agent, taking the prepared printed circuit board substrate, soaking the printed circuit board substrate in the chemical nickel gold activating agent for 35min, taking out, cleaning and drying to obtain an activated printed circuit board;
s6: mixing 75 parts of sulfuric acid solution, 0.8 part of sodium chloride, 0.8 part of dodecylphenol polyoxyethylene ether, 9 parts of sodium hydrophosphate and 3 parts of nickel sulfate, carrying out chemical nickel plating at the temperature of 85 ℃ and the pH value of 9, taking out after 15min of deposition, cleaning and drying;
s7: mixing 5 parts of gold potassium cyanide solution, 12 parts of sodium dodecyl sulfate and 13 parts of copper sulfate uniformly, and then placing the printed circuit board soaked in the S4 into a reactor for electroplating at the temperature of 60 ℃, the pH value of 5.0 and the current density of 2A/dm 2 And (3) electroplating for 20min, taking out, cleaning and drying to obtain the nickel-gold activated printed circuit board.
Comparative example 1: the number of parts of activator A in S5 is increased on the basis of example 1:
s1: preparation of activator A: adding 15 parts of stannous chloride solution into 75 parts of 300mL/L hydrochloric acid solution, stirring until the stannous chloride solution is completely dissolved, continuously adding 1.5 parts of sodium stannate, uniformly mixing to obtain solution 1, dissolving 0.5 part of palladium chloride into the other hydrochloric acid solution, continuously stirring until the stannous chloride is completely dissolved, adding 15 parts of stannous chloride at a constant temperature, stirring until the stannous chloride is completely dissolved, slowly adding the solution 1, keeping the temperature at 40 ℃ and keeping the water bath at 70 ℃ for 6 hours to obtain an activator A;
s2: mixing 10 parts of concentrated hydrochloric acid solution with 10 parts of distilled water, adding 0.5 part of palladium chloride and 10 parts of stannous chloride, uniformly stirring, adding 150 parts of sodium chloride solution, continuously stirring, and carrying out water bath heat preservation at the constant temperature of 40 ℃ for 5 hours to obtain an activator B;
s3: taking a ceramic plate and copper foil, coating the copper foil on the upper and lower surfaces of the ceramic plate, performing double-sided hot pressing, heating to 200 ℃ under the protection of vacuum atmosphere, pressurizing to 25MPa, and pressing for 25 hours to obtain a printed circuit board substrate;
s4: placing the printed circuit board substrate obtained by pressing into microetching solution obtained by mixing 10 parts of potassium dichromate, 10 parts of concentrated sulfuric acid and 100 parts of distilled water, and taking out after 3 min;
s5: taking 30 parts of an activating agent A and 48 parts of an activating agent B, uniformly mixing to obtain a chemical nickel Jin Huohua agent, taking the prepared printed circuit board substrate, soaking the printed circuit board substrate in the chemical nickel gold activating agent for 25min, taking out, cleaning and drying to obtain an activated printed circuit board;
s6: mixing 75 parts of sulfuric acid solution, 0.8 part of sodium chloride, 0.8 part of dodecylphenol polyoxyethylene ether, 9 parts of sodium hydrophosphate and 3 parts of nickel sulfate, carrying out chemical nickel plating at the temperature of 85 ℃ and the pH value of 9, taking out after 15min of deposition, cleaning and drying;
s7: mixing 5 parts of gold potassium cyanide solution, 12 parts of sodium dodecyl sulfate and 13 parts of copper sulfate uniformly, and then placing the printed circuit board soaked in the S4 into a reactor for electroplating at the temperature of 60 ℃, the pH value of 5.0 and the current density of 2A/dm 2 And (3) electroplating for 20min, taking out, cleaning and drying to obtain the nickel-gold activated printed circuit board.
Comparative example 2: increasing the fraction of activator B in S5 on the basis of example 2:
s1: preparation of activator A: adding 15 parts of stannous chloride solution into 75 parts of 300mL/L hydrochloric acid solution, stirring until the stannous chloride solution is completely dissolved, continuously adding 1.5 parts of sodium stannate, uniformly mixing to obtain solution 1, dissolving 0.5 part of palladium chloride into the other hydrochloric acid solution, continuously stirring until the stannous chloride is completely dissolved, adding 15 parts of stannous chloride at a constant temperature, stirring until the stannous chloride is completely dissolved, slowly adding the solution 1, keeping the temperature at 40 ℃ and keeping the water bath at 70 ℃ for 6 hours to obtain an activator A;
s2: mixing 10 parts of concentrated hydrochloric acid solution with 10 parts of distilled water, adding 0.5 part of palladium chloride and 10 parts of stannous chloride, uniformly stirring, adding 150 parts of sodium chloride solution, continuously stirring, and carrying out water bath heat preservation at the constant temperature of 40 ℃ for 5 hours to obtain an activator B;
s3: taking a ceramic plate and copper foil, coating the copper foil on the upper and lower surfaces of the ceramic plate, performing double-sided hot pressing, heating to 200 ℃ under the protection of vacuum atmosphere, pressurizing to 25MPa, and pressing for 25 hours to obtain a printed circuit board substrate;
s4: placing the printed circuit board substrate obtained by pressing into microetching solution obtained by mixing 10 parts of potassium dichromate, 10 parts of concentrated sulfuric acid and 100 parts of distilled water, and taking out after 3 min;
s5: taking 20 parts of an activating agent A and 60 parts of an activating agent B, uniformly mixing to obtain a chemical nickel Jin Huohua agent, taking the prepared printed circuit board substrate, soaking the printed circuit board substrate in the chemical nickel gold activating agent for 25min, taking out, cleaning and drying to obtain an activated printed circuit board;
s6: mixing 75 parts of sulfuric acid solution, 0.8 part of sodium chloride, 0.8 part of dodecylphenol polyoxyethylene ether, 9 parts of sodium hydrophosphate and 3 parts of nickel sulfate, carrying out chemical nickel plating at the temperature of 85 ℃ and the pH value of 9, taking out after 15min of deposition, cleaning and drying;
s7: mixing 5 parts of gold potassium cyanide solution, 12 parts of sodium dodecyl sulfate and 13 parts of copper sulfate uniformly, and then placing the printed circuit board soaked in the S4 into a reactor for electroplating at the temperature of 60 ℃, the pH value of 5.0 and the current density of 2A/dm 2 And (3) electroplating for 20min, taking out, cleaning and drying to obtain the nickel-gold activated printed circuit board.
Comparative example 3: the parts of activator A, B in S5 are simultaneously increased on the basis of example 1:
s1: preparation of activator A: adding 15 parts of stannous chloride solution into 75 parts of 300mL/L hydrochloric acid solution, stirring until the stannous chloride solution is completely dissolved, continuously adding 1.5 parts of sodium stannate, uniformly mixing to obtain solution 1, dissolving 0.5 part of palladium chloride into the other hydrochloric acid solution, continuously stirring until the stannous chloride is completely dissolved, adding 15 parts of stannous chloride at a constant temperature, stirring until the stannous chloride is completely dissolved, slowly adding the solution 1, keeping the temperature at 40 ℃ and keeping the water bath at 70 ℃ for 6 hours to obtain an activator A;
s2: mixing 10 parts of concentrated hydrochloric acid solution with 10 parts of distilled water, adding 0.5 part of palladium chloride and 10 parts of stannous chloride, uniformly stirring, adding 150 parts of sodium chloride solution, continuously stirring, and carrying out water bath heat preservation at the constant temperature of 40 ℃ for 5 hours to obtain an activator B;
s3: taking a ceramic plate and copper foil, coating the copper foil on the upper and lower surfaces of the ceramic plate, performing double-sided hot pressing, heating to 200 ℃ under the protection of vacuum atmosphere, pressurizing to 25MPa, and pressing for 25 hours to obtain a printed circuit board substrate;
s4: placing the printed circuit board substrate obtained by pressing into microetching solution obtained by mixing 10 parts of potassium dichromate, 10 parts of concentrated sulfuric acid and 100 parts of distilled water, and taking out after 3 min;
s5: taking 25 parts of an activating agent A and 60 parts of an activating agent B, uniformly mixing to obtain a chemical nickel Jin Huohua agent, taking the prepared printed circuit board substrate, soaking the printed circuit board substrate in the chemical nickel gold activating agent for 25min, taking out, cleaning and drying to obtain an activated printed circuit board;
s6: mixing 75 parts of sulfuric acid solution, 0.8 part of sodium chloride, 0.8 part of dodecylphenol polyoxyethylene ether, 9 parts of sodium hydrophosphate and 3 parts of nickel sulfate, carrying out chemical nickel plating at the temperature of 85 ℃ and the pH value of 9, taking out after 15min of deposition, cleaning and drying;
s7: mixing 5 parts of gold potassium cyanide solution, 12 parts of sodium dodecyl sulfate and 13 parts of copper sulfate uniformly, and then placing the printed circuit board soaked in the S4 into a reactor for electroplating at the temperature of 60 ℃, the pH value of 5.0 and the current density of 2A/dm 2 And (3) electroplating for 20min, taking out, cleaning and drying to obtain the nickel-gold activated printed circuit board.
Comparative example 4: activator A, B was not prepared on the basis of example 1:
s1: taking a ceramic plate and copper foil, coating the copper foil on the upper and lower surfaces of the ceramic plate, performing double-sided hot pressing, heating to 200 ℃ under the protection of vacuum atmosphere, pressurizing to 25MPa, and pressing for 25 hours to obtain a printed circuit board substrate;
s2: placing the printed circuit board substrate obtained by pressing into microetching solution obtained by mixing 10 parts of potassium dichromate, 10 parts of concentrated sulfuric acid and 100 parts of distilled water, and taking out after 3 min;
s3: mixing 75 parts of sulfuric acid solution, 0.8 part of sodium chloride, 0.8 part of dodecylphenol polyoxyethylene ether, 9 parts of sodium hydrophosphate and 3 parts of nickel sulfate, carrying out chemical nickel plating at the temperature of 85 ℃ and the pH value of 9, taking out after 15min of deposition, cleaning and drying;
s4: take 5 parts of cyanidation Jin JiarongMixing the solution, 12 parts of sodium dodecyl sulfate and 13 parts of copper sulfate uniformly, and then placing the printed circuit board soaked in the S4 into a reactor for electroplating at a temperature of 60 ℃, a pH value of 5.0 and a current density of 2A/dm 2 And (3) electroplating for 20min, taking out, cleaning and drying to obtain the nickel-gold activated printed circuit board.
Experiment: (1) Taking an activated printed circuit board with the size of 19mm multiplied by 627mm multiplied by 3mm as a basis of the embodiment 1, carrying out electroless nickel plating, and recording the time for starting generating bubbles;
(2) Based on example 1, the activated printed circuit board with the size of 19mm multiplied by 627mm multiplied by 3mm is taken and put into plating solution for electroless nickel plating, and after 50s, the printed circuit board is taken out and dried, and the area of plating leakage is observed and recorded. Wherein, the area of the missed plating is smaller than 2% of the area of the circuit board, namely the missed plating does not occur, and the missed plating area exceeds 2% to occur; the data obtained are shown in the following table:
table 1 performance test data
| Bubble generation time/s | Surface condition | |
| Example 1 | 7.5 | No plating leakage occurs |
| Example 2 | 7.9 | No plating leakage occurs |
| Example 3 | 8.1 | No plating leakage occurs |
| Comparative example 1 | 9.9 | No plating leakage occurs |
| Comparative example 2 | 10.6 | No plating leakage occurs |
| Comparative example 3 | 10.2 | No plating leakage occurs |
| Comparative example 4 | 12.3 | No plating leakage occurs |
Conclusion: as can be seen from comparison of the data in Table 1, the soaking time of the printed circuit board in the prepared activator is an important condition affecting the activating performance of the activator, and too long time can lead to excessive activating steps, too short time can lead to incomplete activation, which indicates that the soaking time can lead to the degradation of the activating performance, and the soaking time is the optimal time.
As can be seen from the comparison example, the presence of the acid-based colloidal palladium and the salt-based colloidal palladium can improve the activation performance of the activator, and meanwhile, the addition ratio and the part of the acid-based colloidal palladium and the salt-based colloidal palladium can greatly influence the activation performance of the activator, thereby influencing the comprehensive performance of the printed circuit board.
In conclusion, the data show that the preparation method and the application of the electroless nickel gold activator provided by the invention can prepare the activator with better performance and the printed circuit board with better activation performance.
Finally, it should be noted that: the foregoing description is only a preferred embodiment of the present invention, and the present invention is not limited thereto, but it is to be understood that modifications and equivalents of some of the technical features described in the foregoing embodiments may be made by those skilled in the art, although the present invention has been described in detail with reference to the foregoing embodiments. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A preparation method of a electroless nickel gold activator is characterized in that: the method comprises the following steps:
step 1: adding stannous chloride solution into hydrochloric acid solution, stirring until the stannous chloride solution is completely dissolved, continuously adding sodium stannate, uniformly mixing to obtain solution 1, dissolving palladium chloride into another hydrochloric acid solution, continuously stirring until the stannous chloride is completely dissolved, adding the stannous chloride at a constant temperature, stirring until the stannous chloride is completely dissolved, slowly adding the solution 1, keeping the temperature at 30-40 ℃ and the water bath at 60-70 ℃ for 4-6 hours, and obtaining an activator A;
step 2: mixing concentrated hydrochloric acid solution with distilled water, adding palladium chloride and stannous chloride, stirring uniformly, adding sodium chloride solution, stirring continuously, and maintaining the temperature in a constant-temperature water bath to obtain an activator B;
step 3: compounding the activator A and the activator B to obtain the electroless nickel gold activator.
2. The method for preparing the electroless nickel gold activator according to claim 1, wherein the method comprises the following steps: in the step 1, the components are as follows: according to the weight portions, 10 to 20 portions of stannous chloride solution, 50 to 100 portions of 300mL/L hydrochloric acid solution, 1 to 2 portions of sodium stannate, 0.1 to 1 portion of palladium chloride and 10 to 20 portions of stannous chloride.
3. The method for preparing the electroless nickel gold activator according to claim 1, wherein the method comprises the following steps: in the step 2, the concentration of the concentrated hydrochloric acid solution is 37%, the constant temperature is 40-60 ℃, and the heat preservation time is 4-5 h.
4. A method for preparing a electroless nickel gold activator according to claim 3, wherein: in the step 2, the components are as follows: according to the weight portions, 5 to 20 portions of concentrated hydrochloric acid solution, 5 to 20 portions of distilled water, 0.1 to 1 portion of palladium chloride, 2 to 20 portions of stannous chloride and 150 to 200 portions of sodium chloride.
5. The method for preparing the electroless nickel gold activator according to claim 4, wherein the method comprises the following steps: the weight ratio of palladium chloride to stannous chloride is 1:20.
6. The use of the electroless nickel gold activator prepared by the method according to any one of claims 1 to 5, characterized in that: the method comprises the following steps:
s1: taking a ceramic plate and a copper foil, coating the copper foil on the upper and lower surfaces of the ceramic plate, performing double-sided hot pressing, heating to 200-350 ℃ under the protection of vacuum atmosphere, pressurizing to 20-35 MPa, and pressing for 20-25 h to obtain a printed circuit board substrate;
s2: placing the printed circuit board substrate obtained by pressing into microetching solution obtained by mixing potassium dichromate, concentrated sulfuric acid and distilled water, and taking out after 3-4 min;
s3: soaking the prepared printed circuit board substrate in a electroless nickel gold activator, taking out, cleaning and drying to obtain an activated printed circuit board;
s4: mixing sulfuric acid solution, sodium chloride, dodecylphenol polyoxyethylene ether, sodium hydrogen phosphate and nickel sulfate, placing the mixture into a printed circuit board, carrying out chemical nickel plating under the conditions that the temperature is 80-90 ℃ and the pH is 8.5-9.5, depositing for 5-25 min, taking out, cleaning and drying;
s5: mixing gold potassium cyanide solution, sodium dodecyl sulfate and copper sulfate, electroplating the printed circuit board soaked in S4 at 50-60 deg.c, pH 5.0 and current density of 2A/dm 2 And (3) electroplating for 15-20 min, taking out, cleaning and drying to obtain the nickel-gold activated printed circuit board.
7. The use of an electroless nickel gold activator according to claim 6, wherein: in S2, the microetching solution comprises the following components: 10-15 parts of potassium dichromate, 9-18 parts of concentrated sulfuric acid and 85-120 parts of distilled water.
8. The use of an electroless nickel gold activator according to claim 6, wherein: in the S3, the electroless nickel gold activator comprises 20-35 parts of activator A and 30-50 parts of activator B in parts by weight, and the soaking time is 20-35 min.
9. The use of an electroless nickel gold activator according to claim 6, wherein: s4, the components are as follows: 60-80 parts of sulfuric acid solution, 0.5-1 part of sodium chloride solution, 0.5-1 part of dodecylphenol polyoxyethylene ether, 5-10 parts of sodium hydrophosphate and 1-5 parts of nickel sulfate solution.
10. The use of an electroless nickel gold activator according to claim 6, wherein: s5, the components are as follows: according to the weight portions, 2 to 7 portions of potassium gold cyanide solution, 10 to 15 portions of sodium dodecyl sulfate and 10 to 15 portions of copper sulfate.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104152874A (en) * | 2014-07-20 | 2014-11-19 | 烟台恒迪克能源科技有限公司 | Printed circuit board chemical copper plating activation solution |
| CN104630857A (en) * | 2014-12-13 | 2015-05-20 | 重庆浩立塑胶有限公司 | Palladium chloride activator for plastic electroplating process |
| CN106591809A (en) * | 2016-12-26 | 2017-04-26 | 长沙理工大学 | Low-concentration colloid palladium activation solution for printed circuit board electroless copper |
| CN107245707A (en) * | 2017-06-23 | 2017-10-13 | 湖北共铭电路有限公司 | A kind of pcb board chemical nickel and gold technique |
| CN108330474A (en) * | 2018-02-08 | 2018-07-27 | 中山市鑫鸿顺新材料有限公司 | A kind of activator and preparation method thereof for chemical nickel gold |
-
2023
- 2023-10-17 CN CN202311339442.4A patent/CN117385345A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104152874A (en) * | 2014-07-20 | 2014-11-19 | 烟台恒迪克能源科技有限公司 | Printed circuit board chemical copper plating activation solution |
| CN104630857A (en) * | 2014-12-13 | 2015-05-20 | 重庆浩立塑胶有限公司 | Palladium chloride activator for plastic electroplating process |
| CN106591809A (en) * | 2016-12-26 | 2017-04-26 | 长沙理工大学 | Low-concentration colloid palladium activation solution for printed circuit board electroless copper |
| CN107245707A (en) * | 2017-06-23 | 2017-10-13 | 湖北共铭电路有限公司 | A kind of pcb board chemical nickel and gold technique |
| CN108330474A (en) * | 2018-02-08 | 2018-07-27 | 中山市鑫鸿顺新材料有限公司 | A kind of activator and preparation method thereof for chemical nickel gold |
Non-Patent Citations (5)
| Title |
|---|
| 丁雨: "印刷线路板化学镀铜活化剂-胶体钯的研究", 《中国优秀硕士学位论文全文数据库 工程科技I辑》, no. 9, 15 September 2012 (2012-09-15), pages 9 - 10 * |
| 何为: "《印刷电路基础：原理、工艺技术及应用》", 31 January 2022, 北京：机械工业出版社, pages: 189 - 190 * |
| 何家禧: "《职业危害风险评估与防控》", 30 April 2016, 北京：中国环境出版社, pages: 326 - 327 * |
| 姜培安等: "《印制电路设计标准手册》", 31 March 1993, 宇航出版社出版, pages: 139 - 140 * |
| 强颖怀: "《材料表面工程技术》", 31 May 2016, 徐州：中国矿业大学出版社, pages: 50 - 51 * |
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