CN108034973B - Direct electroplating hole metallization solution for printed circuit board and preparation method - Google Patents
Direct electroplating hole metallization solution for printed circuit board and preparation method Download PDFInfo
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- CN108034973B CN108034973B CN201711277707.7A CN201711277707A CN108034973B CN 108034973 B CN108034973 B CN 108034973B CN 201711277707 A CN201711277707 A CN 201711277707A CN 108034973 B CN108034973 B CN 108034973B
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- additive
- printed circuit
- hole metallization
- circuit board
- metallization solution
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- 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
- C25D5/54—Electroplating of non-metallic surfaces
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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
- C23C18/38—Coating with copper
Abstract
The embodiment of the invention provides a direct electroplating hole metallization solution of a printed circuit board and a preparation method, and relates to the technical field of printed circuit boards. The composition comprises the following components in percentage by mass: 1-5% of carbon black, 0.1-1.5% of a first additive, 0.2-0.8% of a second additive, 0.1-0.3% of a third additive, 0.5-3.5% of an alkaline buffer salt, 0.01-0.5% of an antibacterial agent and 90-99% of water, wherein the first additive has a structural formula of R (OR ') nX, wherein R is alkyl OR aryl, R' is alkyl, n is 5-80, X is sulfate radical OR phosphate radical, and the second additive has a structural formula of R (OR ') n, wherein R is aryl, and R' is alkyl; n is 30-80, and the third additive is at least one of polypropylene glycol, glycerol and polyethylene glycol. The hole metallization solution of the printed circuit board can improve the performance of the hole metallization solution of the printed circuit board and prolong the service life of the printed circuit board.
Description
Technical Field
The invention belongs to the technical field of printed circuit boards, and particularly relates to a direct electroplating hole metallization solution of a printed circuit board and a preparation method thereof.
Background
Prior to electroplating of the printed circuit board, a dedicated circuit board printing hole metallization solution is typically used. The traditional hole metallization chemical copper plating is a chemical reaction process, and formaldehyde contained in the solution is harmful to the environment and has carcinogenic risk. The complexing agent is not easy to carry out biodegradation, and the wastewater treatment is difficult. Meanwhile, the chemical copper plating solution has poor stability, easy decomposition, various process flows and difficult operation and maintenance. The direct electroplating hole metallization solution for circuit board printing is in physical form in the adsorption process, and does not generate chemical reaction, and the phenomenon that other components are consumed due to the chemical reaction does not exist. The solution is simple and reliable to use and maintain.
The existing direct plating hole metallization solution for printed circuit boards generally comprises high-purity and high-carbon powder, a surfactant and a water-soluble high molecular compound. However, the carbon black of the prior hole metallization solution of the printed circuit board is difficult to disperse and easy to agglomerate, and can lose efficacy after being placed for a period of time.
Disclosure of Invention
The invention provides a hole metallization solution of a printed circuit board and a preparation method thereof, aiming at solving the problem that the hole metallization solution of the printed circuit board is easy to lose efficacy due to the fact that carbon black in the hole metallization solution of the existing printed circuit board is difficult to disperse and easy to agglomerate.
The invention provides a hole metallization solution of a printed circuit board, which comprises the following components in percentage by mass:
1-5% of carbon black, 0.1-1.5% of first additive, 0.2-0.8% of second additive, 0.1-0.3% of third additive, 0.5-3.5% of alkaline buffer salt, 0.01-0.5% of antibacterial agent and 90-99% of water;
wherein the first additive has a structural formula of R (OR') nX, wherein R is alkyl OR aryl; r' is alkyl, n is 5-80, X is sulfate or phosphate radical;
the second additive is represented by the structural formula R (OR ') n, wherein R is aryl, and R' is alkyl; n is 30 to 80;
the third additive is at least one of polypropylene glycol, glycerol and polyethylene glycol. A second aspect of the invention provides a method of preparing a hole metallization solution for a printed circuit board, the method comprising:
respectively weighing the following components in percentage by mass: 1-5% of carbon black, 0.1-1.5% of first additive, 0.2-0.8% of second additive, 0.1-0.3% of third additive, 0.5-3.5% of alkaline buffer salt, 0.01-0.5% of antibacterial agent and 90-99% of water;
adding carbon black and a second additive into water to prepare a suspension;
adding a first additive and alkaline buffer salt into the suspension, grinding for 0.5-4 hours, and adding a third additive in a grinding process for multiple times to form a dispersion liquid, wherein the addition amount of the alkaline buffer salt is 50-70% of the mass of the first additive;
adding alkaline buffer salt and an antibacterial agent into the dispersion liquid to obtain a hole metallization solution of the printed circuit board;
wherein the mass fraction of the carbon black is 1-5%, the mass fraction of the first additive is 0.1-1.5%, the mass fraction of the second additive is 0.2-0.8%, the mass fraction of the third additive is 0.1-0.3%, the mass fraction of the alkaline buffer salt is 0.5-3.5%, the mass fraction of the antibacterial agent is 0.01-0.5%, and the mass fraction of the water is 90-99%;
the first additive is of a structural formula R (OR') nX, wherein R is alkyl OR aryl; r' is alkyl, n is 5-80, X is sulfate or phosphate radical;
the second additive is represented by the structural formula R (OR ') n, wherein R is aryl, and R' is alkyl; n is 30 to 80;
the third additive is at least one of polypropylene glycol, glycerol and polyethylene glycol.
According to the hole metallization solution of the printed circuit board and the preparation method, the first additive adopted in the hole metallization solution of the printed circuit board is an anionic surfactant, belongs to polyether salt, is ionized in water to form anions, can be well dissolved in water, adsorbs functional groups in carbon black and large pi bonds on the inner plane of the carbon black, and enables carbon black powder to be dispersed in the water. In addition, the first additive belongs to long-chain high molecular polymer, and can enhance the steric hindrance of carbon black particles and protect the carbon black particles from flocculation. The second additive is that polyphenyl polyether and carbon black both contain polyaromatic rings, and the second additive is mutually attracted by forming relatively stronger large pi bonds, is cooperated with the first additive to stably disperse the carbon black, and then can enhance the acting force among the first additive, the second additive and the solvent through the hydrogen bond action and dipole-dipole action among the third additive, so that the additives are better dissolved into the solvent water to form a highly stable dispersion system. The system is uniform, the suspension performance is improved, no precipitation is caused, and the physicochemical properties of the whole system are the same. Thus, the life of the hole metallization solution of the printed circuit board can be greatly increased.Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention.
Fig. 1 is a scanning electron microscope image of a printed circuit board after drying a hole metallization solution according to embodiment 3 of the present invention.
Fig. 2 is a graph showing the particle size of the hole metallization solution of the printed circuit board prepared in example 3 of the present invention.
Detailed Description
In order to make the objects, features and advantages of the present invention more obvious and understandable, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention, and it is apparent that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a hole metallization solution of a printed circuit board, which comprises the following components in percentage by mass:
1-5% of carbon black, 0.1-1.5% of first additive, 0.2-0.8% of second additive, 0.1-0.3% of third additive, 0.5-3.5% of alkaline buffer salt, 0.01-0.5% of antibacterial agent and 90-99% of water;
wherein, the first additive has a structural formula of R (OR') nX, wherein R is alkyl OR aryl; r' is alkyl; n is 5 to 80; x is sulfate or phosphate;
the second additive is of the structural formula R (OR') n, wherein R is aryl; r' is alkyl; n is 30-80.
The third additive is at least one of polypropylene glycol, glycerol and polyethylene glycol.
The hole metallization solution of the printed circuit board is in the hole metallization solution of the printed circuit board;
specifically, the first additive is polyether salt which is an anionic surfactant and can be at least one of dodecyl polyoxyethylene ether sulfate, octadecyl polyoxypropylene ether phosphate and octyl polyoxyethylene ether phosphate. For example, sodium laureth sulfate, potassium laureth sulfate, sodium octadecylpolyoxypropylene ether phosphate, potassium octylpolyoxyethylene ether phosphate. The first additive is an anionic surfactant, which is ionized in water to form anions, and the anions are well dissolved in water to adsorb functional groups in the carbon black and large pi bonds on the internal plane of the carbon black, so that carbon black powder is dispersed in the water; on the other hand, the polyether salt belongs to a long-chain high molecular polymer, and enhances the steric hindrance of carbon black particles, thereby protecting the carbon black particles from flocculation.
Preferably, the first addition is potassium octyl polyoxyethylene ether phosphate.
Specifically, the second additive belongs to the polyphenyl polyether which is a nonionic surfactant and can be at least one of phenylbutyl polyoxyethylene ether, naphthyl ethyl polyoxypropylene ether and phenethyl polyoxypropylene ether. The second additive polyphenyl polyether and carbon black both contain aromatic rings, and are mutually attracted by forming relatively stronger large pi bonds to cooperate with the first additive to stably disperse the carbon black.
Preferably, the second additive is phenylbutylpolyoxyethylene ether.
In practical application, the third additive can enhance the acting force between the first additive and the second additive and the solvent through the hydrogen bond action and dipole-dipole action among the cosolvents, so that the additives are better dissolved into the solvent water to form a highly stable dispersion system. The system is uniform, the suspension performance is improved, no precipitation is caused, and the physicochemical properties of the whole system are the same. Thus, the life of the hole metallization solution of the printed circuit board can be greatly increased.
Specifically, the alkaline buffer salt is one of potassium carbonate, sodium carbonate, potassium carbonate-potassium bicarbonate, dipotassium hydrogen phosphate-potassium dihydrogen phosphate, borax-calcium chloride, borax-sodium carbonate, and ammonia water-ammonium chloride. Preferably, the alkaline buffer salt is potassium carbonate-potassium bicarbonate, and after the alkaline buffer salt is added, the pH value of the solution can be adjusted to 9.5-12.5, preferably 11, so that the surface of the carbon black particles is negative in charge, and the carbon black particles are adsorbed on the pore walls.
Specifically, the antibacterial agent is at least one of imidazole, isothiazolone and dodecyl dimethyl benzyl ammonium bromide. The antibacterial agent can prevent the growth and reproduction of microorganisms in water and reduce the pollution of the microorganisms to the solution.
The invention also provides a method for preparing the hole metallization solution of the printed circuit board,
respectively weighing the following components in percentage by mass: 1-5% of carbon black, 0.1-1.5% of first additive, 0.2-0.8% of second additive, 0.1-0.3% of third additive, 0.5-3.5% of alkaline buffer salt, 0.01-0.5% of antibacterial agent and 90-99% of water;
adding carbon black and a second additive into water to prepare a suspension;
adding a first additive and an alkaline buffer solution salt into the suspension for grinding for 0.5-4 hours, and adding a third additive for multiple times in the grinding process to form a dispersion liquid;
the adding amount of the alkaline buffer salt is 50-70% of the mass of the first additive. Preferably, the alkaline buffer salt is potassium carbonate or sodium carbonate, and the addition amount is 60% of the mass of the first additive.
Adding the rest alkaline buffer salt and the antibacterial agent into the dispersion liquid to obtain a hole metallization solution of the printed circuit board;
wherein the first additive has a structural formula of R (OR') nX, wherein R is alkyl OR aryl; r' is alkyl, n is 5-80, X is sulfate or phosphate radical;
the second additive is represented by the structural formula R (OR ') n, wherein R is aryl, and R' is alkyl; n is 30 to 80;
the third additive is at least one of polypropylene glycol, glycerol and polyethylene glycol. The water used in the method meets the three-level water standard of China laboratory water country, and mainly aims to prevent excessive Ca ions and Mg ions in the water from forming scale, accelerate the agglomeration of carbon black and further influence the stability of the hole metallization solution of the printed circuit board.
Preferably, the grinding time in the step one is 1-3 hours, and the number of times of adding the cosolvent is 2-5 times.
Comparative example 1
Adding 20g of carbon black and 20g of second additive phenylbutylethylene ether into 938g of water to prepare suspension; adding 10g of potassium carbonate powder into the suspension, grinding for 3 hours, and adding 1.5g of polypropylene glycol every 1 hour to form a uniform dispersion liquid;
6g of potassium carbonate-potassium bicarbonate (which can be prepared into a solution) and 3g of imidazole are added into the dispersion liquid, and the mixture is uniformly stirred to form the hole metallization solution of the printed circuit board.
Comparative example 2
Adding 20g of carbon black and 20g of naphthyl ethyl polyoxypropylene ether into 938g of water to prepare a suspension; adding 10g of sodium bicarbonate powder into the suspension, grinding for 3 hours, and adding 1.5g of polypropylene glycol every 1 hour to form a uniform dispersion liquid;
6g of potassium carbonate-potassium bicarbonate (which can be prepared into a solution) and 3g of imidazole are added into the dispersion liquid, and the mixture is uniformly stirred to form the hole metallization solution of the printed circuit board.
Example 1
Adding 20g of carbon black and 10g of phenethyl polyoxypropylene ether into 938g of water to prepare a suspension; adding 10g of sodium octyl polyoxyethylene ether phosphate and 6g of potassium hydroxide powder into the suspension, grinding for 3 hours, and adding 1.5g of polypropylene glycol every 1 hour to form uniform dispersion liquid;
6g of dipotassium hydrogen phosphate-potassium dihydrogen phosphate (which can be prepared into a solution) and 3g of imidazole are added into the dispersion liquid, and the mixture is stirred uniformly to form a hole metallization solution of the printed circuit board.
Example 2
Adding 20g of carbon black and 20g of naphthyl ethyl polyoxypropylene ether into 938g of water to prepare a suspension; adding 10g of potassium octadecyl polyoxypropylene ether phosphate and 2g of sodium hydroxide powder into the suspension, grinding for 3 hours, and adding 1.5g of polypropylene glycol every 1 hour to form a uniform dispersion liquid;
6g of potassium carbonate-potassium bicarbonate (which can be prepared into a solution) and 3g of imidazole are added into the dispersion liquid, and the mixture is uniformly stirred to form the hole metallization solution of the printed circuit board.
Example 3
Adding 20g of carbon black and 18g of phenylbutyl polyoxyethylene ether into 1000g of water to prepare suspension; adding 10g of potassium dodecyl polyoxyethylene sulfate and 5g of sodium carbonate powder into the suspension, grinding for 3 hours, and adding 1.5g of polypropylene glycol every 1 hour to form uniform dispersion liquid;
6g of sodium carbonate (which can be prepared into a solution) and 3g of imidazole are added into the dispersion liquid, and the mixture is uniformly stirred to form the hole metallization solution of the printed circuit board. The hole metallization solution of the printed circuit boards prepared in comparative examples 1-2 and examples 1-3 is placed for 300 days, no agglomeration phenomenon occurs, and the performance is stable. After the printed circuit board is placed for 600 days, precipitates appear at the bottoms of the comparative examples 1 and 2, and the agglomeration phenomenon does not appear in the examples 1 to 3, which shows that the effect of the hole metallization solution of the printed circuit board prepared by simultaneously adding the first additive and the second additive is better than that of the printed circuit board prepared by independently adding one additive. In addition, a particle size test and a drying test are performed on the hole metallization solution of the printed circuit board prepared in example 3, and then a scanning electron microscope test is performed, as shown in the figure, fig. 1 is an electron microscope image of the hole metallization solution test of the printed circuit board prepared in example 3 of the present invention, and fig. 2 is a particle size test chart of the hole metallization solution of the printed circuit board prepared in example 3 of the present invention. It can be seen from the figure that the material dispersion in the hole metallization solution of the printed circuit board is relatively uniform. Furthermore, the average particle size of the carbon black is less than 100nm, which is far below the commercial maturity product. The method can not only improve the dispersibility of the hole metallization solution of the printed circuit board, but also reduce the particle size of the carbon black, thereby having better stability.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (6)
1. A hole metallization solution for a printed circuit board, characterized in that the hole metallization solution comprises the following components in mass fraction:
1-5% of carbon black, 0.1-1.5% of a first additive, 0.2-0.8% of a second additive, 0.1-0.3% of a third additive, 0.5-3.5% of an alkaline buffer salt, 0.01-0.5% of an antibacterial agent and 90-99% of water, wherein the sum of the mass fractions of the components in the pore metallization solution is 100%;
wherein, the first additive has a structural formula of R (OR') nX, wherein R is alkyl OR aryl; r' is alkyl, n is 5-80, X is sulfate or phosphate radical; the first additive is at least one of octadecyl polyoxypropylene phosphate and octyl polyoxyethylene ether phosphate;
the second additive has a structural formula of R (OR ') n, wherein R is aryl and R' is alkyl; n is 30 to 80; the second additive is at least one of phenylbutyl polyoxyethylene ether, naphthyl ethyl polyoxypropylene ether and phenethyl polyoxypropylene ether;
the third additive is at least one of polypropylene glycol and glycerol.
2. The hole metallization solution of claim 1 wherein the basic buffer salt is at least one of potassium carbonate, sodium carbonate, potassium carbonate-bicarbonate, dipotassium hydrogen phosphate-monopotassium phosphate, borax-calcium chloride, borax-sodium carbonate, and ammonia-ammonium chloride.
3. The hole metallization solution of claim 1 wherein the antimicrobial agent is at least one of an imidazole, an isothiazolone, and a dodecyl dimethyl benzyl ammonium bromide antimicrobial agent.
4. A method of preparing a hole metallization solution for a printed circuit board, the method comprising:
respectively weighing the following components in percentage by mass: 1-5% of carbon black, 0.1-1.5% of first additive, 0.2-0.8% of second additive, 0.1-0.3% of third additive, 0.5-3.5% of alkaline buffer salt, 0.01-0.5% of antibacterial agent and 90-99% of water, wherein the sum of the mass fractions of the weighed components is 100%;
adding carbon black and a second additive into water to prepare a suspension;
adding a first additive and alkaline buffer salt into the suspension, grinding for 0.5-4 hours, and adding a third additive in a grinding process for multiple times to form a dispersion liquid, wherein the addition amount of the alkaline buffer salt is 50-70% of the mass of the first additive;
adding the rest alkaline buffer salt and the antibacterial agent into the dispersion liquid to obtain a hole metallization solution of the printed circuit board;
wherein, the first additive has a structural formula of R (OR ') nX, wherein R is alkyl OR aryl, R' is alkyl, n is 5-80, and X is sulfate OR phosphate; the first additive is at least one of octadecyl polyoxypropylene phosphate and octyl polyoxyethylene ether phosphate;
the second additive is represented by the structural formula R (OR ') n, wherein R is aryl, and R' is alkyl; n is 30 to 80; the second additive is at least one of phenylbutyl polyoxyethylene ether, naphthyl ethyl polyoxypropylene ether and phenethyl polyoxypropylene ether;
the third additive is at least one of polypropylene glycol, glycerol and polyethylene glycol.
5. The method of preparing a hole metallization solution of claim 4, wherein the alkaline buffer salt is at least one of potassium carbonate-bicarbonate, dipotassium hydrogen phosphate-dihydrogen phosphate, borax-calcium chloride, borax-sodium carbonate, and ammonia-ammonium chloride.
6. The method of preparing a hole metallization solution of claim 4, wherein the antimicrobial agent is at least one of an imidazole, an isothiazolone, and a dodecyl dimethyl benzyl ammonium bromide antimicrobial agent.
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| CN112867285B (en) * | 2020-12-29 | 2022-10-04 | 深圳市贝加电子材料有限公司 | Conductive graphite hole metallization solution and preparation method and application thereof |
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| US4724005A (en) * | 1985-11-29 | 1988-02-09 | Olin Hunt Specialty Products Inc. | Liquid carbon black dispersion |
| CN101165820B (en) * | 2006-10-18 | 2011-08-24 | 比亚迪股份有限公司 | Carbon black conductive fluid |
| CN104818506A (en) * | 2015-05-28 | 2015-08-05 | 哈尔滨工业大学 | Solution for metalizing printed circuit board hole |
| CN106535505B (en) * | 2016-11-23 | 2019-04-02 | 昆山尚宇电子科技有限公司 | Blank hole liquid for printed board manufacture |
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Denomination of invention: Direct plating hole metallization solution and preparation method for printed circuit board Effective date of registration: 20210622 Granted publication date: 20200428 Pledgee: Shenzhen hi tech investment small loan Co.,Ltd. Pledgor: SHENZHEN BAIKAL ELECTRONICS Co.,Ltd. Registration number: Y2021980005086 |