CN114016010A - Acidic pore-finishing agent and surface metallization treatment process method of inorganic non-metallic base material - Google Patents
Acidic pore-finishing agent and surface metallization treatment process method of inorganic non-metallic base material Download PDFInfo
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- CN114016010A CN114016010A CN202111308483.8A CN202111308483A CN114016010A CN 114016010 A CN114016010 A CN 114016010A CN 202111308483 A CN202111308483 A CN 202111308483A CN 114016010 A CN114016010 A CN 114016010A
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- acid
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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
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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
Abstract
The invention discloses an acidic pore-forming agent and a surface metallization processing method of an inorganic non-metallic substrate, the adsorption of the introduced ionic liquid on the PCB surface follows a Langmuir adsorption model, the adsorption of the ionic liquid on the PCB is mainly physical adsorption, and the ionic liquid is a cathode corrosion inhibitor and a surfactant, can be used as a PCB active agent, is especially applied to chemical copper plating in a horizontal continuous transmission operation mode, improves the hole metallization quality of a high-performance circuit board, and has excellent corrosion inhibition effect, and the invention adopts graphene oxide as a repairing agent, effectively reduces the average roughness of the PCB surface by utilizing the ultrahigh specific surface area and the nanometer property thereof, enables the hole surface of the PCB layer to be flat, simultaneously uses an organic acid which is easier to clean, is difficult to cause residue compared with an alkaline substance, and has better cleaning effect on the copper surface oxide of the circuit board by the organic acid, the binding force between the plating layer and the copper surface can be improved.
Description
Technical Field
The invention relates to the technical field of preparation of inorganic non-metallic substrates, in particular to an acidic pore-forming agent and a surface metallization treatment process method of an inorganic non-metallic substrate.
Background
The inorganic non-metal substrate, namely the printed circuit board, is called as the printed board for short, the insulating board is a basic material for manufacturing the PCB, the printed board is cut into a certain size, a plurality of patterns which can conduct electricity are arranged on the board, and a plurality of holes are distributed on the board and are used for replacing a chassis for installing electronic components or integrated circuits, so that the mutual connection of the electronic components is realized.
The hole metallization process is used as a core process for manufacturing the printed circuit board, and a conductive layer is plated on the hole wall of an insulated PCB by mainly using methods of chemical copper plating and electrolytic copper plating so that the interlayer leads are mutually communicated. The pore-modifying agent commonly used in the prior art is an alkaline pore-modifying agent, which generally comprises inorganic base or organic amine base substances and cationic high-molecular surfactants (such as quaternized imidazole cations or gemini cationic surfactants) as described in patent documents CN201510024735, CN201710208305, CN201810499344 and CN201310566173, and has the function of adjusting the surface charge of the non-conductive substrate in the PCB hole by utilizing the strong cationic property of the cationic surfactants under alkaline conditions.
Patent document CN109679775A discloses an acidic pore-forming agent for circuit board hole metallization process and a method for preparing a circuit board, the pore-forming agent comprises acid, hyperbranched polymer using polyamine as an initiator, wetting agent and deionized water, compared with the basic pore-forming agent used in the prior art, the acidic pore-forming agent adopts organic carboxylic acid which is easy to clean as a cleaning aid, and hyperbranched polymer having strong cationic property under acidic condition as a surface charge modifier of a dielectric material, and is easy to clean, so that the problems of difficult cleaning of the basic pore-forming agent, abnormal quality of circuit board empty metallization caused by excessive adsorption of a palladium activator due to easy residual of excessive surface charge modifier and the like can be improved. However, acid in the acidic pore-forming agent can damage the surface of the circuit board to a certain extent, and meanwhile, the hyperbranched polymer can also generate aggregative aggregation at different parts and influence the pore structure to a certain extent, which is not beneficial to the uniformity of copper plating on the surface layer of the circuit board.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide an acidic pore-forming agent and a surface metallization treatment process method of an inorganic non-metallic substrate, which solve the problem of uneven copper plating of a surface coating.
In order to achieve the purpose, the invention adopts the following technical scheme:
an acidic pore-modifying agent comprising an ionic liquid, an organic acid, a repairing agent and deionized water, wherein the ionic liquid is one or more of trioctyl dodecyl ammonium bis (trifluoromethanesulfonyl) imide, trioctyl tetradecyl ammonium bis (trifluoromethanesulfonyl) imide and trioctyl benzyl ammonium bis (trifluoromethanesulfonyl) imide.
Preferably, the concentration of the ionic liquid is 200-400g/L, the concentration of the organic acid is 30-50g/L, and the concentration of the repairing agent is 1-5 g/L.
Preferably, the preparation method of the metal complex is as follows:
(1) adding zinc nitrate hexahydrate into deionized water to obtain a solution A;
(2) adding phytic acid into an equal volume of methanol solution in a separate container to obtain solution B;
(3) and uniformly mixing the solution A and the solution B, adding NaOH and 4, 4-bipyridine, carrying out ultrasonic oscillation for 3min, uniformly dispersing into a suspension, carrying out hydrothermal reaction, keeping the mixture in an oven at 120 ℃ for 1 day, naturally cooling and centrifuging, and washing the product for three times by using a mixture of methanol and water in a volume ratio of 1:1 to remove residual impurities to obtain the metal complex.
Preferably, the mass ratio of the zinc nitrate hexahydrate to the deionized water is 280-320: 10-20.
Preferably, the amount of phytic acid added is 300-400 g.
Preferably, the mass ratio of NaOH to 4, 4-bipyridine is 50-150: 300-400.
Preferably, the organic acid is selected from at least one of formic acid, acetic acid, glycolic acid, citric acid, methanesulfonic acid, benzenesulfonic acid, p-toluenesulfonic acid, hydroxyethylidene diphosphonic acid or aminotrimethylene phosphonic acid.
Preferably, the repair agent is graphene oxide.
The invention also provides a surface metallization processing method of the inorganic non-metal substrate, which comprises the step of soaking the circuit board in the acidic pore-forming agent for processing and then carrying out a pore metallization process.
Preferably, the soaking temperature is 20-50 deg.C, and the soaking time is 1-5 min.
Compared with the prior art, the invention has the following beneficial effects:
(1) the invention provides an acidic pore-forming agent and a surface metallization treatment process method of an inorganic non-metallic substrate, wherein heteroatoms such as O, P, N in a metal complex are easily filled in unoccupied 3d orbitals outside the metal atoms due to the existence of lone-pair electrons, the heteroatoms and the PCB surface form coordination bonds, the adsorption of the metal complex on the PCB surface follows a Langmuir adsorption model, the adsorption of the metal complex on the PCB is mainly physical adsorption, and the metal complex can be used as a PCB active agent, is especially applied to chemical copper plating in a horizontal continuous transmission operation mode, improves the hole metallization quality of a high-performance circuit board, and has an excellent corrosion inhibition effect.
(2) The invention provides an acidic pore-forming agent and a surface metallization treatment process method of an inorganic non-metallic substrate.
(3) The invention provides an acidic pore-forming agent and a surface metallization treatment process method of an inorganic non-metallic substrate.
(4) The invention provides an acidic pore-forming agent and a surface metallization treatment process method of an inorganic non-metallic substrate.
Detailed Description
The present invention will be described in more detail with reference to specific preferred embodiments, but the present invention is not limited to the following embodiments.
It should be noted that, unless otherwise specified, the chemical reagents involved in the present invention are commercially available.
The specific implementation mode is as follows:
(1) preparing an acidic pore-adjusting agent: adding ionic liquid, organic acid and a repairing agent into deionized water, and stirring and mixing uniformly to obtain the acidic pore-forming agent, wherein the preparation method of the ionic liquid comprises the following steps:
adding trioctylamine and dodecyl bromine into a DMF solvent, carrying out reflux reaction under the protection of nitrogen, after the reaction is finished, cooling a reaction product to room temperature, standing, carrying out solid-liquid separation, recrystallizing ethyl acetate to obtain a white solid, then adding the white solid and lithium bistrifluoromethanesulfonylimide into a methanol solvent, stirring for reaction, then cooling to room temperature, drying an organic phase, concentrating the solvent, adding dichloromethane, washing with deionized water, concentrating the solvent to obtain a colorless viscous liquid, and then carrying out vacuum drying on the colorless viscous liquid to obtain an ionic liquid;
(2) preparation of the metal complex:
adding 302mg of zinc nitrate hexahydrate into 15mg of deionized water to obtain a solution A, adding 355.5mg of phytic acid into an equal volume of methanol solution in a separate container to obtain a solution B, uniformly mixing the solution A and the solution B, adding 100mg of NaOH and 390.5mg of 4, 4-bipyridine, carrying out ultrasonic oscillation for 3min, uniformly dispersing into a suspension, carrying out hydrothermal reaction, keeping the mixture in an oven at 120 ℃ for 1 day, naturally cooling and centrifuging, washing the product for three times by using a mixture of methanol and water with a volume ratio of 1:1 to remove residual impurities to obtain a metal complex;
(3) the chemical copper plating process comprises the following steps: the sample is a copper-clad plate with holes, the thickness of which is 2mm, the aperture of which is 0.2mm and the thickness of which is 10:1, and the substrate material is provided by Jing Pont electronics Limited in Shenzhen City.
The existing circuit board hole metallization process mainly comprises the following processing flows:
swelling → water washing → degumming → water washing → neutralization → water washing → whole hole → water washing → micro-etching → water washing → presoaking → activation → water washing → acceleration → water washing → chemical copper → water washing → drying.
In this embodiment, except for the pore-forming process, the products of the corresponding process are treated by the pore-metallization process, the pore-forming agent is treated by the above-mentioned examples and comparative examples, and the test results are analyzed after the samples are sequentially treated by the above-mentioned processes.
The operation conditions of the specific main process of the hole metallization process flow are as follows:
a. expansion: swelling the mixture at 70 ℃ for 3 minutes by using a swelling solution;
b. removing glue: oxidizing and removing the resin swelled in the hole by using potassium permanganate at 75 ℃ under an alkaline condition to increase the roughness of the hole wall, and treating for 8 minutes;
c. neutralizing, namely neutralizing and reducing residual permanganate and manganese oxide by using 5% of ethanol, 3% of hydrogen peroxide and 92% of water at room temperature, cleaning the hole wall, and treating for 1 minute;
d. hole trimming: the specific examples and comparative examples of the acidic pore-conditioning agent described herein were pore wall conditioned at 50 ℃ and degreased on the board surface for 2 minutes;
e. micro-etching: at room temperature, a mixed solution of 10% of sulfuric acid, 12% of sodium persulfate and 78% of water is used for treatment for 1 minute;
f. pre-dipping: soaking 20% of sodium chloride, 5% of hydrochloric acid and 75% of water at room temperature for 30 seconds;
g. and (3) activation: treating by using 23% of palladium chloride, 5% of hydrochloric acid and 72% of water, wherein the preferable operation temperature is 30-60 ℃, the treatment time is generally 1-6 minutes, and the cost is generally not more than 2 minutes;
h. accelerating: treating with 10% hydrochloric acid at 45 deg.C for 40 s;
i. chemical copper plating: processing for 4 minutes in chemical copper plating solution at 38 ℃, washing and drying to finish the whole processing flow.
The specific operation example according to the above flow is as follows:
example 1
Adding 200g of ionic liquid bis (trifluoromethane sulfonyl) imide trioctyl dodecylammonium, 10g of acetic acid, 10g of glycolic acid, 10g of hydroxyethylidene diphosphonic acid and 1g of graphene oxide into 1L of deionized water, and uniformly stirring and mixing to obtain an acidic pore-adjusting agent;
and (3) heating the prepared hole-finishing agent to 50 ℃ for later use, treating the through hole copper-clad plate with the thickness of 2.0mm to be tested according to the hole metallization process of the steps a-i, and drying the sample for test evaluation after copper plating is completed.
Example 2
Adding 300g of ionic liquid bis (trifluoromethane sulfonyl) imide trioctyl tetradecyl ammonium, 20g of methanesulfonic acid, 10g of citric acid, 10g of hydroxyethylidene diphosphonic acid and 2g of graphene oxide into 1L of deionized water, and uniformly stirring and mixing to obtain an acidic pore-adjusting agent;
and (3) heating the prepared hole-finishing agent to 50 ℃ for later use, treating the through hole copper-clad plate with the thickness of 2.0mm to be tested according to the hole metallization process of the steps a-i, and drying the sample for test evaluation after copper plating is completed.
Example 3
Adding 400g of ionic liquid bis (trifluoromethane sulfonyl) imide trioctyl dodecylammonium, 10g of formic acid, 10g of methanesulfonic acid, 30g of aminotrimethylene phosphonic acid and 3g of graphene oxide into 1L of deionized water, and uniformly stirring and mixing to obtain an acidic pore-adjusting agent;
and (3) heating the prepared hole-finishing agent to 50 ℃ for later use, treating the through hole copper-clad plate with the thickness of 2.0mm to be tested according to the hole metallization process of the steps a-i, and drying the sample for test evaluation after copper plating is completed.
Example 4
Adding 200g of ionic liquid bis (trifluoromethane sulfonyl) imide trioctyl dodecylammonium, 10g of acetic acid, 10g of benzenesulfonic acid, 10g of p-toluenesulfonic acid and 4g of graphene oxide into 1L of deionized water, and uniformly stirring and mixing to obtain an acidic pore-adjusting agent;
and (3) heating the prepared hole-finishing agent to 50 ℃ for later use, treating the through hole copper-clad plate with the thickness of 2.0mm to be tested according to the hole metallization process of the steps a-i, and drying the sample for test evaluation after copper plating is completed.
Example 5
Adding 300g of ionic liquid bis (trifluoromethane sulfonyl) imide trioctyl tetradecyl ammonium, 10g of citric acid, 10g of formic acid, 10g of glycolic acid and 5g of graphene oxide into 1L of deionized water, and stirring and mixing uniformly to obtain an acidic pore-adjusting agent;
and (3) heating the prepared hole-finishing agent to 50 ℃ for later use, treating the through hole copper-clad plate with the thickness of 2.0mm to be tested according to the hole metallization process of the steps a-i, and drying the sample for test evaluation after copper plating is completed.
Example 6
Adding 400g of ionic liquid bis (trifluoromethane sulfonyl) imide trioctylbenzyl ammonium, 10g of citric acid, 10g of methanesulfonic acid, 10g of hydroxyethylidene diphosphonic acid and 3g of graphene oxide into 1L of deionized water, and uniformly stirring and mixing to obtain an acidic pore-adjusting agent;
and (3) heating the prepared hole-finishing agent to 50 ℃ for later use, treating the through hole copper-clad plate with the thickness of 2.0mm to be tested according to the hole metallization process of the steps a-i, and drying the sample for test evaluation after copper plating is completed.
Comparative example 1
Taking 10% of alkaline pore-forming agent of the Shenzhen Tianxi technology sold in the market, and preparing the alkaline pore-forming agent into the pore-forming agent by using deionized water according to the operation guidance configuration;
heating the prepared pore-adjusting agent to 50 ℃ for standby. And c, treating the copper-clad plate with the thickness of 2.0mm to be tested according to the hole metallization process of the steps a-i, and drying the sample for test evaluation after copper plating is completed.
Comparative example 2
An acidic pore-adjusting agent is prepared according to the scheme disclosed in patent document CN201510024735, and the prepared pore-adjusting agent is heated to 50 ℃ for standby. And c, treating the copper-clad plate with the thickness of 2.0mm to be tested according to the hole metallization process of the steps a-i, and drying the sample for test evaluation after copper plating is completed.
The through hole plating backlight effect evaluation is carried out on the samples prepared in the examples 1-6 and the comparative examples 1-2, whether the surface of the base material of the whole through hole can be uniformly covered is evaluated according to the backlight grade of the plated sample through hole, so that the treatment effect of the pore-finishing agent and the regeneration effect of the pore-finishing agent are reflected, and the backlight grade standard is classified into 0-5 grade according to the expression method of the American military standard MIL-P4.8.7.2 on backlight grading; taking down a through hole area of each example sample, observing a cross section of the through hole at a multiplying power of 100 under a transmission mode of a metallographic microscope, comparing the number and the form of light transmission points of the cross section with a backlight grade graph to obtain a grade judgment result, and if no light is observed, completely displaying black on the cross section, wherein the backlight grade is 5 grades; if the light is completely transmitted without any dark area, no copper metal is deposited on the surface of the substrate, and the backlight level is 0; if a dark area and an area with light transmission exist at the same time, grading judgment is carried out from 0.5-4.75 grade according to comparison with a standard graphic, and the activation effect and performance of the pore-forming agent can be judged according to the judgment of the backlight grade, wherein the higher the backlight grade is, the more complete the coverage of the catalytic particles in the pore-forming agent is, the better the activation effect is; the lower the backlight grade is, the light leakage is caused, which indicates that the catalytic effect of the pore-adjusting agent is poor or the catalytic performance is reduced, thereby indicating the performance and stability of the pore-adjusting agent and the regenerated pore-adjusting agent, generally speaking, the backlight grade needs to reach more than 4.0 grade to meet the requirement of circuit board pore metallization.
The samples prepared in this example and comparative example were observed for delamination after plating using a 50-fold mirror, and the results are shown in the following table:
as can be seen from the table, in the present embodiment, after the acidic pore-forming agent and the electroless copper plating are used, the backlight level of the copper-plated covering substrate in the through hole can reach more than 4.5 levels, which indicates that the pore-forming agent has good covering and adjusting functions, and after the acidic pore-forming agent is used, the hole is easy to clean, the probability of excessive adsorption of the palladium activator is low, the palladium adsorption amount is appropriate, the hole is smooth, the binding force is better, the comparative example 1 uses the alkaline pore-forming agent, and the backlight level can meet the backlight level requirement under normal conditions; comparative example 2 using the alkaline pore-adjusting agent disclosed in the prior art, the backlight effect could not meet the quality requirement.
Finally, it is to be noted that: the above examples do not limit the invention in any way. It will be apparent to those skilled in the art that various modifications and improvements can be made to the present invention. Accordingly, any modification or improvement made without departing from the spirit of the present invention is within the scope of the claimed invention.
Claims (10)
1. An acidic pore-modifying agent, which is characterized by comprising a metal complex, an organic acid, a repairing agent and deionized water, wherein the metal complex is synthesized by reacting zinc nitrate hexahydrate and phytic acid through a solvothermal method in the presence of 4, 4-bipyridine.
2. The acidic pore-regulating agent as claimed in claim 1, wherein the concentration of the metal complex is 200-400g/L, the concentration of the organic acid is 30-50g/L, and the concentration of the repairing agent is 1-5 g/L.
3. The acidic pore-modifying agent according to claim 1, wherein the metal complex is prepared by the following method:
(1) adding zinc nitrate hexahydrate into deionized water to obtain a solution A;
(2) adding phytic acid into an equal volume of methanol solution in a separate container to obtain solution B;
(3) and uniformly mixing the solution A and the solution B, adding NaOH and 4, 4-bipyridine, carrying out ultrasonic oscillation for 3min, uniformly dispersing into a suspension, carrying out hydrothermal reaction, keeping the mixture in an oven at 120 ℃ for 1 day, naturally cooling and centrifuging, and washing the product for three times by using a mixture of methanol and water in a volume ratio of 1:1 to remove residual impurities to obtain the metal complex.
4. The acidic pore-forming agent as claimed in claim 3, wherein the mass ratio of zinc nitrate hexahydrate to deionized water is 280-320: 10-20.
5. The acidic pore-regulating agent according to claim 3, wherein the amount of phytic acid added is 300-400 g.
6. The acidic pore-modifying agent according to claim 3, wherein the mass ratio of NaOH to 4, 4-bipyridine is 50-150: 300-400.
7. The acidic pore-modifying agent of claim 1, wherein said organic acid is selected from at least one of formic acid, acetic acid, glycolic acid, citric acid, methanesulfonic acid, benzenesulfonic acid, p-toluenesulfonic acid, hydroxyethylenediphosphonic acid, and aminotrimethylenephosphonic acid.
8. The acidic pore-modifying agent according to claim 1, wherein said repair agent is graphene oxide.
9. A process for metallizing the surface of an inorganic non-metallic substrate, which comprises the step of treating the substrate by immersing the substrate in the acidic pore-forming agent according to any one of claims 1 to 8, and then subjecting the substrate to a pore-metallization process.
10. The process of claim 9, wherein the soaking temperature is 20-50 ℃ and the soaking time is 1-5 min.
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| US5503877A (en) * | 1989-11-17 | 1996-04-02 | Atotech Deutschalnd Gmbh | Complex oligomeric or polymeric compounds for the generation of metal seeds on a substrate |
| JP2003181476A (en) * | 2001-12-18 | 2003-07-02 | Azusaa:Kk | Method for decomposing chelating agent |
| WO2005090539A1 (en) * | 2004-03-18 | 2005-09-29 | Henkel Kommanditgesellschaft Auf Aktien | Composition for producing ph jump |
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