CN113005437B - Chemical gold-precipitating liquid for printed circuit board - Google Patents
Chemical gold-precipitating liquid for printed circuit board Download PDFInfo
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- CN113005437B CN113005437B CN202110209518.6A CN202110209518A CN113005437B CN 113005437 B CN113005437 B CN 113005437B CN 202110209518 A CN202110209518 A CN 202110209518A CN 113005437 B CN113005437 B CN 113005437B
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- gold
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- circuit board
- palladium
- printed circuit
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Classifications
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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
- 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
- C23C18/42—Coating with noble metals
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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
- 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
- C23F11/00—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent
- C23F11/08—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent in other liquids
- C23F11/10—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent in other liquids using organic inhibitors
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- 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
- H05K3/40—Forming printed elements for providing electric connections to or between printed circuits
- H05K3/42—Plated through-holes or plated via connections
- H05K3/422—Plated through-holes or plated via connections characterised by electroless plating method; pretreatment therefor
-
- 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
- H05K2203/00—Indexing scheme relating to apparatus or processes for manufacturing printed circuits covered by H05K3/00
- H05K2203/07—Treatments involving liquids, e.g. plating, rinsing
- H05K2203/0703—Plating
- H05K2203/072—Electroless plating, e.g. finish plating or initial plating
Abstract
The invention relates to the technical field of circuit board production, in particular to a chemical gold-depositing solution for a printed circuit board, which comprises 1-10g/L of water-soluble gold salt, 1-10g/L of complexing agent, 1-10g/L of complexing stabilizer, 1-100ppm of grain refiner, 1-10g/L of PH buffer, 1-10g/L of conductive salt and 1-10g/L of corrosion inhibitor, wherein the complexing agent is selected from one or a combination of more of cyanide ions, sulfite ions, thiosulfate ions, ammonia, ethylenediamine, citrate, tartrate, phosphate, borate, ethylenediamine tetraacetic acid, thiosulfate, organic phosphonic acid, 2-amino n-butanol and isobutanolamine, the chemical gold-depositing solution mainly solves the problem of palladium corrosion of conventional chemical palladium-plating gold, and avoids poor weldability of the chemical palladium-plating gold caused by palladium corrosion, the weather resistance condition is poor, the quality and the reliability of the product can not meet the requirement of high weldability, the corrosion resistance of the chemical palladium-plated gold can be greatly improved, and the gold surface can keep excellent weldability for a long time.
Description
Technical Field
The invention relates to the technical field of circuit board production, in particular to a chemical gold-precipitating solution for a printed circuit board.
Background
Printed Circuit Boards (PCBs) are components that are commonly required for various electronic devices in the information society. Through holes and blind holes are generally arranged on the PCB for circuit connection. In the PCB manufacturing process, the blind holes are processed by operations of electroless copper plating, nickel-gold (chemical gold) deposition and the like.
However, the applicant has found that the reason for the difficult gold plating is that, in the case of the electroless nickel gold plating of the blind hole, the gold plating is difficult: when the gold is dissolved, bubbles are hidden in the blind holes, so that the liquid medicine exchange is blocked, and the situation of liquid medicine exchange blocking also exists in the subsequent gold leaching process.
Electroless nickel-gold is prepared by replacing palladium on the surface of copper by chemical reaction, then plating a nickel-phosphorus alloy layer on the basis of palladium core, and then plating a gold layer on the surface of nickel by replacement reaction. At present, the gold deposition of the nickel-gold is carried out by two processes of substitution and half-reduction mixed bath construction.
Electroless nickel gold is mainly used for surface treatment of circuit boards, for preventing copper on the surface of circuit boards from being oxidized or corroded, and for soldering and application to contacts (e.g., keys, gold fingers on memory chips, etc.).
The chemical immersion of Ni and Au is also called electroless Ni immersion Au or chemical Ni immersion Au. The method is a surface coating process which deposits a layer of nickel on the surface of bare copper under the acidic condition through the catalytic action of palladium and then deposits a layer of thin gold through a displacement reaction, wherein the gold layer provides a good electrical connectivity layer as a barrier layer to prevent the diffusion of copper, thereby avoiding the pollution of solder to the copper layer in the welding and rework operation processes.
Disclosure of Invention
The invention aims to provide the chemical gold-precipitating solution for the printed circuit board, which effectively relieves corrosion and has better use feeling.
In order to solve the technical problems, the invention adopts the technical scheme that: a chemical gold deposition solution for a printed circuit board comprises the following components in parts by weight:
1-10g/L of water-soluble gold salt, 1-10g/L of complexing agent, 1-10g/L of complexing stabilizer, 1-100ppm of grain refiner, 1-10g/L of pH buffer, 1-10g/L of conductive salt and 1-10g/L of corrosion inhibitor.
Further, the corrosion inhibitor comprises the following components in percentage by weight: 3-5% of polyepoxysuccinate, 2-5% of gluconate and 88-95% of fatty alcohol polyoxyethylene phosphate.
Furthermore, the corrosion inhibitor also comprises 1-2% by mass of triethanolamine.
Further, the complexing agent is selected from one or more of cyanide ions, sulfite ions, thiosulfate ions, ammonia, ethylenediamine, citrate, tartrate, phosphate, borate, ethylenediamine tetraacetic acid, thiosulfate, organic phosphonic acid, 2-amino-n-butanol and isobutanolamine.
Further, the complexing stabilizer comprises methacrylic acid, crotonic acid and polyethyleneimine.
Further, the grain refiner is selected from one of sodium thiosulfate, potassium thiosulfate, sodium dithionate and potassium dithionate.
Further, the conductive salt is selected from one of potassium citrate, sodium citrate, ammonium chloride and ammonium sulfate.
Further, the pH value buffering agent is selected from one or more of sodium succinate, borax, sodium acetate, sodium propionate and sodium malonate.
Further, the water-soluble gold salt is one of gold potassium cyanide, gold sodium sulfite, gold potassium thiosulfate, gold chloride salt and gold thiomalate salt.
Compared with the prior art, the invention has the advantages and positive effects that:
the invention provides a chemical gold deposition solution for printed circuit boards, which mainly solves the problem of palladium corrosion of conventional chemical palladium-gold plating, avoids poor weldability and poor weather resistance of the chemical palladium-gold plating caused by the palladium corrosion, can greatly improve the corrosion resistance of the chemical palladium-gold plating, enables a gold surface to keep excellent welding performance for a long time, enables gold to be stably replaced on a palladium layer of a substrate through a complexing agent and a complexing stabilizer, can form a corrosion inhibition film on the gold surface through a corrosion inhibitor, can reduce the gold corrosion, enables the corrosion inhibitor to be soaked in holes of a metal layer in the gold deposition process, has long-time corrosion inhibition effect, eliminates the defects of insufficient soldering, missing soldering, poor welding reliability and the like, improves the product quality and the product reliability, and has no pollution in the production process, is suitable for industrial production.
Detailed Description
For a better understanding of the present invention, the present invention is further described below in conjunction with specific embodiments.
The method comprises the following steps: cleaning a chemical palladium plating tank of a chemical palladium-gold plating production line, continuously circularly cleaning with deionized water, and draining the cleaning water;
step two: adding a chemical palladium plating solution into a chemical palladium plating tank, wherein the chemical palladium plating solution comprises a palladium compound, a hypophosphorous acid compound, a boron hydride compound, a composite complexing agent and a complexing stabilizer, the pH value of the chemical palladium plating solution is adjusted by a sodium hydroxide solution to be 10, the specific gravity of the chemical palladium plating solution is 1.16g/cm3, the composite complexing agent comprises ethylenediamine, 2-amino n-butyl alcohol and isobutanolamine, and the composite stabilizer comprises methacrylic acid, crotonic acid and polyethyleneimine;
step three: adjusting the temperature to 65 ℃, starting a circulating filter pump, and simultaneously opening a gas stirring valve to stir air;
step four: washing the printed circuit board with water for 30 minutes by using deionized water, removing surface floating soil, carrying out acid washing, removing surface oxides, washing with water again to remove acid, placing the washed printed circuit board into a chemical palladium plating tank, and carrying out chemical palladium plating for 10 minutes;
step five: taking out the printed circuit board subjected to chemical palladium plating, washing for 2min, placing the printed circuit board into a chemical gold plating tank at room temperature for chemical gold plating by using the chemical gold deposition solution provided by the invention, taking out the printed circuit board subjected to chemical gold plating, washing with water, drying by using hot air at 78 ℃ for 2min at 60 ℃ and 85 ℃ for 4 min, and transferring to a shape processing procedure, wherein the thickness of a palladium plating layer is 1 micron.
Example 1:
10g/L of water-soluble gold salt, 1g/L of complexing agent, 1g/L of complexing stabilizer, 1ppm of grain refiner, 1g/L of PH buffer, 1g/L of conductive salt and 1g/L of corrosion inhibitor.
The complexing agent is selected from the group consisting of cyanide ions, sulfite ions, and thiosulfate ions.
The complexing stabilizer comprises methacrylic acid, crotonic acid and polyethyleneimine.
The grain refiner is sodium thiosulfate; the conductive salt is selected from potassium citrate.
The pH buffer is selected from sodium succinate, borax, and sodium acetate.
The corrosion inhibitor comprises 5% of polyepoxysuccinate, 5% of gluconate, 88% of fatty alcohol polyoxyethylene phosphate and 2% of triethanolamine.
The water-soluble gold salt was gold potassium cyanide, as experimental group a.
Example 2:
5g/L of water-soluble gold salt, 2g/L of complexing agent, 3g/L of complexing stabilizer, 50ppm of grain refiner, 4g/L of PH buffer, 6g/L of conductive salt and 7g/L of corrosion inhibitor.
The complexing agent is a combination of ammonia, ethylenediamine, citrate, tartrate and phosphate.
The complexing stabilizer comprises methacrylic acid, crotonic acid and polyethyleneimine.
The grain refiner is potassium thiosulfate and the conductive salt is sodium citrate.
The pH buffer is a combination of sodium propionate and sodium malonate.
The corrosion inhibitor comprises 4% of polyepoxysuccinate, 3% of gluconate, 92% of fatty alcohol polyoxyethylene phosphate and 1% of triethanolamine.
The water-soluble gold salt was gold sodium sulfite as experimental group B.
Example 3:
1g/L of water-soluble gold salt, 10g/L of complexing agent, 10g/L of complexing stabilizer, 100ppm of grain refiner, 10g/L of PH buffer, 10g/L of conductive salt and 10g/L of corrosion inhibitor.
The complexing agent is the combination of organic phosphonic acid, 2-amino n-butyl alcohol and isobutanolamine.
The complexing stabilizer comprises methacrylic acid, crotonic acid and polyethyleneimine.
The grain refiner is sodium dithionate and the conductive salt is ammonium chloride.
The pH buffer is a combination of borax, sodium acetate and sodium propionate.
The corrosion inhibitor comprises 3.5 percent of polyepoxysuccinate, 4 percent of gluconate, 91 percent of fatty alcohol polyoxyethylene phosphate and 1.5 percent of triethanolamine.
The water-soluble gold salt was thiomalic acid gold salt, as experimental group C.
Example 4:
7g/L of water-soluble gold salt, 5g/L of complexing agent, 4g/L of complexing stabilizer, 100ppm of grain refiner, 6g/L of PH buffer, 5g/L of conductive salt and 5g/L of corrosion inhibitor.
The complexing agent is a combination of phosphate, borate, ethylene diamine tetraacetic acid and thiosulfate.
The complexing stabilizer comprises methacrylic acid, crotonic acid and polyethyleneimine.
The grain refiner is potassium dithionate, and the conductive salt is ammonium sulfate.
The pH buffer is a combination of sodium acetate, sodium propionate, and sodium malonate.
The corrosion inhibitor comprises 3% of polyepoxysuccinate, 2% of gluconate and 95% of fatty alcohol polyoxyethylene phosphate.
The water-soluble gold salt was a gold chloride salt as experimental group D.
Example 5:
the effect of experimental groups a-D was tested.
Carrying out chemical deposition on the experimental groups A-D, and counting the thickness of the gold layer after 5 minutes of depositing the gold layer to obtain the gold plating rate of the chemical gold plating solution;
respectively putting the experimental groups A-D into a salt spray resistant test box, and measuring the time of corrosion on the surface of the experimental groups A-D;
the welding performance is judged, the welding regularity is measured, the shaking condition of the welding point in a period of time after welding is judged by shaking the welding point, and the result is shown in table 1.
Table 1: results of the experiment
The table 1 shows that the electroless gold plating solution for the printed circuit board provided by the invention mainly solves the problem of palladium corrosion of the conventional electroless palladium-gold plating, avoids poor weldability and poor weather resistance of the electroless palladium-gold plating caused by palladium corrosion, ensures that the quality and reliability of the product cannot meet the requirements of high weldability, can greatly improve the corrosion resistance of the electroless palladium-gold plating, enables the gold surface to keep excellent welding performance for a long time, and eliminates the defects of insufficient welding, missing welding, poor welding reliability and the like, thereby improving the quality and reliability of the product, ensuring that the production process is pollution-free, and being suitable for industrial production.
The embodiments of the present invention have been described in detail, but the description is only for the preferred embodiments of the present invention and should not be construed as limiting the scope of the present invention. All equivalent changes and modifications made within the scope of the present invention are also within the scope of the present invention.
Claims (5)
1. A chemical gold-precipitating liquid for printed circuit boards is characterized in that: the composition comprises the following components in percentage by concentration:
1-10g/L of water-soluble gold salt, 1-10g/L of complexing agent, 1-10g/L of complexing stabilizer, 1-100ppm of grain refiner, 1-10g/L of pH buffering agent, 1-10g/L of conductive salt and 1-10g/L of corrosion inhibitor; the complexing stabilizer comprises methacrylic acid, crotonic acid and polyethyleneimine; the grain refiner is selected from one of sodium thiosulfate, potassium thiosulfate, sodium dithionate and potassium dithionate;
the corrosion inhibitor comprises the following components in percentage by weight: 3-5% of polyepoxysuccinate, 2-5% of gluconate and 88-95% of fatty alcohol polyoxyethylene phosphate; the corrosion inhibitor also comprises 1-2% of triethanolamine by mass percent;
the chemical gold immersion process of the printed circuit board comprises the following steps:
the method comprises the following steps: cleaning a chemical palladium plating tank of a chemical palladium-gold plating production line, continuously circularly cleaning with deionized water, and draining the cleaning water;
step two: adding chemical palladium plating solution into the chemical palladium plating tank, wherein the chemical palladium plating solution comprises a palladium compound, a hypophosphorous acid compound, a boron hydride compound, a composite complexing agent and a complexing stabilizer, and adjusting the pH value of the chemical palladium plating solution by using sodium hydroxide solution to ensure that the pH value of the chemical palladium plating solution is 10 and the specific gravity is 1.16g/cm3The composite complexing agent comprises ethylenediamine, 2-amino n-butyl alcohol and isobutanolamine, and the composite stabilizer comprises methacrylic acid, crotonic acid and polyethyleneimine;
step three: adjusting the temperature to 65 ℃, starting a circulating filter pump, and simultaneously opening a gas stirring valve to stir air;
step four: washing the printed circuit board with water for 30 minutes by using deionized water, removing surface floating soil, carrying out acid washing, removing surface oxides, washing with water again to remove acid, placing the washed printed circuit board into a chemical palladium plating tank, and carrying out chemical palladium plating for 10 minutes;
step five: and taking out the printed circuit board subjected to chemical palladium plating, washing with water for 2min, placing the printed circuit board into a chemical gold plating tank at room temperature, performing chemical gold plating by using the chemical gold immersion liquid, taking out the printed circuit board subjected to chemical gold plating, washing with water, drying with hot air at 78 ℃ for 2min at 60 ℃ and 85 ℃ for 4 min, and transferring to a shape processing procedure, wherein the thickness of a palladium plating layer is 1 micron.
2. The electroless gold plating solution for printed wiring boards according to claim 1, wherein:
the complexing agent is selected from one or more of cyanide ions, sulfite ions, thiosulfate ions, ammonia, ethylenediamine, citrate, tartrate, phosphate, borate, ethylenediamine tetraacetic acid, thiosulfate, organic phosphonic acid, 2-amino n-butanol and isobutanolamine.
3. The electroless gold plating solution for printed wiring boards according to claim 1, wherein: the conductive salt is selected from one of potassium citrate, sodium citrate, ammonium chloride and ammonium sulfate.
4. The electroless gold plating solution for printed wiring boards according to claim 1, wherein:
the pH buffering agent is selected from one or more of sodium succinate, borax, sodium acetate, sodium propionate and sodium malonate.
5. The electroless gold plating solution for printed wiring boards according to claim 1, wherein: the water-soluble gold salt is one of gold potassium cyanide, gold sodium sulfite, gold potassium thiosulfate, gold chloride salt and gold thiomalate salt.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202110209518.6A CN113005437B (en) | 2021-02-24 | 2021-02-24 | Chemical gold-precipitating liquid for printed circuit board |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202110209518.6A CN113005437B (en) | 2021-02-24 | 2021-02-24 | Chemical gold-precipitating liquid for printed circuit board |
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| CN113005437B true CN113005437B (en) | 2021-12-24 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115198257B (en) * | 2022-07-12 | 2024-02-02 | 深圳创智芯联科技股份有限公司 | Environment-friendly cyanide-free gold-depositing solution for wafer packaging and electroless plating method |
| CN117580267B (en) * | 2024-01-16 | 2024-03-26 | 珠海斯美特电子材料有限公司 | Gold plating process of printed circuit board |
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| CN108822991B (en) * | 2018-07-23 | 2020-06-26 | 维达纸业(浙江)有限公司 | Felt cleaning agent and application thereof |
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| CN1407132A (en) * | 2001-07-02 | 2003-04-02 | 希普雷公司 | Nonelectrolytic gold plating liquid and method thereof |
| JP2004149824A (en) * | 2002-10-29 | 2004-05-27 | Murata Mfg Co Ltd | Gold plating liquid, plating method using the gold plating liquid, method of producing electronic component, and electronic component |
| CN101634021A (en) * | 2008-07-24 | 2010-01-27 | 罗门哈斯电子材料有限公司 | Electroless gold plating solution |
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