CN110049637B - Brown oxidation treatment process of PCB substrate - Google Patents
Brown oxidation treatment process of PCB substrate Download PDFInfo
- Publication number
- CN110049637B CN110049637B CN201910426583.7A CN201910426583A CN110049637B CN 110049637 B CN110049637 B CN 110049637B CN 201910426583 A CN201910426583 A CN 201910426583A CN 110049637 B CN110049637 B CN 110049637B
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- pcb substrate
- browning
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Classifications
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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
- H05K3/38—Improvement of the adhesion between the insulating substrate and the metal
- H05K3/381—Improvement of the adhesion between the insulating substrate and the metal by special treatment of the substrate
-
- 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
- H05K2203/0779—Treatments involving liquids, e.g. plating, rinsing characterised by the specific liquids involved
- H05K2203/0786—Using an aqueous solution, e.g. for cleaning or during drilling of holes
- H05K2203/0789—Aqueous acid solution, e.g. for cleaning or etching
-
- 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
- H05K2203/0779—Treatments involving liquids, e.g. plating, rinsing characterised by the specific liquids involved
- H05K2203/0786—Using an aqueous solution, e.g. for cleaning or during drilling of holes
- H05K2203/0793—Aqueous alkaline solution, e.g. for cleaning or etching
-
- 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
- H05K2203/0779—Treatments involving liquids, e.g. plating, rinsing characterised by the specific liquids involved
- H05K2203/0786—Using an aqueous solution, e.g. for cleaning or during drilling of holes
- H05K2203/0796—Oxidant in aqueous solution, e.g. permanganate
Abstract
The invention discloses a browning treatment process of a PCB substrate, which comprises the following steps of 1) washing with acid liquor; 2) overflow water washing; 3) washing with alkali liquor; 4) pre-soaking with pure water; 5) browning with a browning agent; 6) drying and 7) cooling; wherein the acid solution is sulfuric acid containing an acidification additive; the alkali liquor comprises the following materials in parts by weight: 5-8 parts of phosphate, 5-8 parts of isomeric alcohol polyoxyethylene ether sodium sulfate, 3-4 parts of dodecyl benzene sulfonate, and 90-100 parts of hydrofluoric acid and water; the browning agent comprises the following raw materials (by mass concentration): 30-50mg/L of nitric acid, 5-8mg/L of potassium permanganate, 10-30mg/L of polyethylene glycol monomethyl ether, 10-30mg/L of halogen ions and 10-20mg/L of azoles, and adding water to 1L. Through the mode, the invention improves the browning uniformity of the PCB substrate by improving the formula of the acid solution, the alkali solution and the browning agent, further provides the binding force between the PCB substrate and PP, and is beneficial to enterprises to manufacture multilayer circuit boards.
Description
Technical Field
The invention belongs to the technical field of PCB (printed circuit board) pretreatment, and particularly relates to a browning treatment process of a PCB substrate.
Background
The PCB substrate needs to be subjected to browning pretreatment before being pressed with PP, browning is to remove foreign matters such as oxides, grease, residual dry films and fingerprint marks on the surface of the PCB substrate through acid-base washing, and the roughness of the copper surface is increased through chemical reaction of liquid medicine and the copper surface of the PCB substrate, so that the effects of activating the copper surface and roughening the surface of the copper surface are achieved, the binding force between the PP and the PCB substrate is increased, and the PCB substrate is suitable for manufacturing multilayer circuit boards.
Chinese patent CN 1564650A discloses a browning treatment fluid for improving the binding force between the copper surface of the inner layer of the circuit board and a polymeric material, which comprises sulfuric acid, hydrogen peroxide, sodium chloride, water-soluble methoxylated polyethylene glycol, corrosion inhibitors indole, triazolylmethane, 4-substituted benzotriazoles or 5-methyl-1-substituted benzotriazoles + 1-substituted benzotriazoles or a combination of the corrosion inhibitor compounds, and is used for improving the binding force between the copper surface of the inner layer of the circuit board and the polymeric material.
Therefore, the quality of browning directly affects the bonding degree between PP and the substrate during pressing, and therefore, the quality of browning (factors such as selection of alkali solution, selection of acid solution, and temperature) is a primary task of browning.
Disclosure of Invention
The invention mainly solves the technical problem of providing a browning treatment process for a PCB substrate, which improves the browning treatment uniformity of the PCB substrate by improving the formula of acid liquid, alkali liquid and a browning agent, further provides the binding force between the PCB substrate and PP, and is beneficial to enterprises to manufacture multilayer circuit boards.
In order to solve the technical problems, the invention adopts a technical scheme that: the brown oxidation treatment process of the PCB substrate comprises the following steps:
1) acid liquor washing: soaking the PCB substrate in acid liquor at 20-30 deg.C for 1-2 min;
2) and (3) overflow water washing: washing the PCB substrate washed by the acid liquor with deionized water at normal temperature;
3) washing with alkali liquor: soaking the washed PCB substrate in alkali liquor for 2-3min, wherein the temperature of the alkali liquor is 40-50 ℃;
4) pre-soaking with pure water: soaking the PCB substrate washed by the alkali liquor in deionized water at normal temperature for 1-2 min;
5) browning with a browning agent: soaking the PCB substrate subjected to secondary water washing in a browning agent for 1-2min, wherein the temperature of the browning agent is 25-35 ℃;
6) drying: drying the browned PCB substrate;
7) and (3) cooling: cooling the dried PCB substrate;
wherein the content of the first and second substances,
the acid liquor is sulfuric acid containing an acidification additive, the concentration of the sulfuric acid is 3-5%, and the mass concentration of the acid liquor is 3-7%;
the alkali liquor comprises the following materials in parts by weight: 5-8 parts of phosphate, 5-8 parts of isomeric alcohol polyoxyethylene ether sodium sulfate, 3-4 parts of dodecyl benzene sulfonate, and 90-100 parts of hydrofluoric acid and water, wherein the concentration of the hydrofluoric acid is 40%, and the mass concentration of the alkali liquor is 3-7%;
the browning agent comprises the following raw materials (by mass concentration): 30-50mg/L of nitric acid, 5-8mg/L of potassium permanganate, 10-30mg/L of polyethylene glycol monomethyl ether, 10-30mg/L of halogen ions and 10-20mg/L of azoles, and adding water to 1L, wherein the mass concentration of the browning agent is 15-20%.
The invention adopts a further technical scheme for solving the technical problem that:
further, the preparation method of the alkali liquor comprises the following steps:
(1) adding water into a water bath, and heating to 40-50 deg.C;
(2) under the conditions, adding the isomeric alcohol polyoxyethylene ether sodium sulfate (added according to the weight portion) into a water bath gradually for dissolving;
(3) adding the solution obtained in the step (2) into a stirrer, continuously adding phosphate and dodecyl benzene sulfonate in parts by weight according to a certain proportion, uniformly stirring at the stirring speed of 1000-1100rpm for 40-50 min;
(4) and (4) slowly dropwise adding hydrofluoric acid into the mixed solution obtained in the step (3), and measuring the pH value to be 8-9.
Further, the preparation method of the browning agent comprises the following steps: adding nitric acid, potassium permanganate, polyethylene glycol monomethyl ether, halogen ions, azole and water into a reaction kettle, stirring at a constant speed, simultaneously blowing nitrogen to remove oxygen for 10-15min, and finally sealing the reaction kettle for 20-30 min.
Further, the drying specifically comprises the following steps: firstly, drying with cold air for 30-50min by using an air cooler, and then drying with hot air for 1-2 h.
Further, the cooling is performed by a natural cooling method.
Further, the cooling is to cool the PCB substrate by using an inert gas cooling method.
Further, the inert gas is carbon dioxide or nitrogen.
Further, the azole is at least one of methylimidazole, benzotriazole, 5-methylbenzotriazole and thiazole.
Further, the temperature for drying by hot air is 70-80 degrees.
Further, the acidifying additive comprises higher fatty alcohol-polyvinyl ether and dimethyl dicarbonate.
The invention has the beneficial effects that: the invention improves the components of acid liquor, alkali liquor and browning agent, and improves the oil stain removal rate of the surface of the PCB substrate, the cleaning degree of a surface oxidation layer and the browning uniformity of a copper surface; and when drying, firstly drying by cold air and then drying by hot air can avoid the board explosion of the product; the cooling is natural cooling or inert gas cooling to protect the protective film formed on the surface of the copper surface.
Detailed Description
The following detailed description of the preferred embodiments of the present invention is provided to enable those skilled in the art to more readily understand the advantages and features of the present invention, and to clearly and unequivocally define the scope of the present invention.
Example (b): the invention discloses a browning treatment process of a PCB (printed circuit board) substrate, which comprises the following steps of:
1) acid liquor washing: soaking the PCB substrate in acid liquor at 20-30 deg.C for 1-2 min;
2) and (3) overflow water washing: washing the PCB substrate washed by the acid liquor with deionized water at normal temperature;
3) washing with alkali liquor: soaking the washed PCB substrate in alkali liquor for 2-3min, wherein the temperature of the alkali liquor is 40-50 ℃;
4) pre-soaking with pure water: soaking the PCB substrate washed by the alkali liquor in deionized water at normal temperature for 1-2 min;
5) browning with a browning agent: soaking the PCB substrate subjected to secondary water washing in a browning agent for 1-2min, wherein the temperature of the browning agent is 25-35 ℃;
6) drying: drying the browned PCB substrate;
7) and (3) cooling: cooling the dried PCB substrate;
wherein the content of the first and second substances,
the acid liquor is sulfuric acid containing an acidification additive, the concentration of the sulfuric acid is 3-5%, and the mass concentration of the acid liquor is 3-7%;
the alkali liquor comprises the following materials in parts by weight: 5-8 parts of phosphate, 5-8 parts of isomeric alcohol polyoxyethylene ether sodium sulfate, 3-4 parts of dodecyl benzene sulfonate, and 90-100 parts of hydrofluoric acid and water, wherein the concentration of the hydrofluoric acid is 40%, and the mass concentration of the alkali liquor is 3-7%;
the browning agent comprises the following raw materials (by mass concentration): 30-50mg/L of nitric acid, 5-8mg/L of potassium permanganate, 10-30mg/L of polyethylene glycol monomethyl ether, 10-30mg/L of halogen ions and 10-20mg/L of azoles, and adding water to 1L, wherein the mass concentration of the browning agent is 15-20%.
The preparation method of the alkali liquor comprises the following steps:
(1) adding water into a water bath, and heating to 40-50 deg.C;
(2) under the conditions, adding the isomeric alcohol polyoxyethylene ether sodium sulfate (added according to the weight portion) into a water bath gradually for dissolving;
(3) adding the solution obtained in the step (2) into a stirrer, continuously adding phosphate and dodecyl benzene sulfonate in parts by weight according to a certain proportion, uniformly stirring at the stirring speed of 1000-1100rpm for 40-50 min;
(4) and (4) slowly dropwise adding hydrofluoric acid into the mixed solution obtained in the step (3), and measuring the pH value to be 8-9.
The preparation method of the browning agent comprises the following steps: adding nitric acid, potassium permanganate, polyethylene glycol monomethyl ether, halogen ions, azole and water into a reaction kettle, stirring at a constant speed, simultaneously blowing nitrogen to remove oxygen for 10-15min, and finally sealing the reaction kettle for 20-30 min.
The drying comprises the following specific steps: firstly, drying with cold air for 30-50min by using an air cooler, and then drying with hot air for 1-2 h.
The cooling is performed by a natural cooling method.
And the cooling is to cool the PCB substrate by adopting an inert gas cooling method.
The inert gas is carbon dioxide or nitrogen.
The azole is at least one of methylimidazole, benzotriazole, 5-methylbenzotriazole and thiazole.
The temperature for drying the hot air is 70-80 degrees.
The acidification additive comprises high-carbon fatty alcohol-polyvinyl ether and dimethyl dicarbonate.
The working principle of the invention is as follows:
the invention improves the components of acid liquor, alkali liquor and browning agent, and improves the oil stain removal rate of the surface of the PCB substrate, the cleaning degree of a surface oxidation layer and the browning uniformity of a copper surface; and when drying, firstly drying by cold air and then drying by hot air can avoid the board explosion of the product; the cooling is natural cooling or inert gas cooling to protect the protective film formed on the surface of the copper surface.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications made by the present invention in the equivalent structure or directly or indirectly applied to other related technical fields are included in the scope of the present invention.
Claims (5)
1. A browning treatment process of a PCB substrate is characterized by comprising the following steps: the method comprises the following steps:
1) acid liquor washing: soaking the PCB substrate in acid liquor at 20-30 deg.C for 1-2 min;
2) and (3) overflow water washing: washing the PCB substrate washed by the acid liquor with deionized water at normal temperature;
3) washing with alkali liquor: soaking the washed PCB substrate in alkali liquor for 2-3min, wherein the temperature of the alkali liquor is 40-50 ℃;
4) pre-soaking with pure water: soaking the PCB substrate washed by the alkali liquor in deionized water at normal temperature for 1-2 min;
5) browning with a browning agent: soaking the PCB substrate subjected to secondary water washing in a browning agent for 1-2min, wherein the temperature of the browning agent is 25-35 ℃;
6) drying: drying the browned PCB substrate;
7) and (3) cooling: cooling the dried PCB substrate;
wherein the content of the first and second substances,
the acid liquor is sulfuric acid containing an acidification additive, the concentration of the sulfuric acid is 3-5%, and the mass concentration of the acid liquor is 3-7%;
the alkali liquor comprises the following materials in parts by weight: 5-8 parts of phosphate, 5-8 parts of isomeric alcohol polyoxyethylene ether sodium sulfate, 3-4 parts of dodecyl benzene sulfonate, and 90-100 parts of hydrofluoric acid and water, wherein the concentration of the hydrofluoric acid is 40%, and the mass concentration of the alkali liquor is 3-7%;
the browning agent comprises the following raw materials in percentage by mass: 30-50mg/L of nitric acid, 5-8mg/L of potassium permanganate, 10-30mg/L of polyethylene glycol monomethyl ether, 10-30mg/L of halogen ions and 10-20mg/L of azoles, and adding water to 1L, wherein the mass concentration of the browning agent is 15-20%;
the preparation method of the alkali liquor comprises the following steps:
(1) adding water into a water bath, and heating to 40-50 deg.C;
(2) under the conditions, adding the isomeric alcohol polyoxyethylene ether sodium sulfate which is added according to the weight portion ratio into a water bath gradually for dissolving;
(3) adding the solution obtained in the step (2) into a stirrer, continuously adding phosphate and dodecyl benzene sulfonate in parts by weight according to a certain proportion, uniformly stirring at the stirring speed of 1000-1100rpm for 40-50 min;
(4) slowly dropwise adding hydrofluoric acid into the mixed solution obtained in the step (3), and measuring the pH value to be 8-9;
the preparation method of the browning agent comprises the following steps: adding nitric acid, potassium permanganate, polyethylene glycol monomethyl ether, halogen ions, azole and water into a reaction kettle, stirring at a constant speed, simultaneously blowing nitrogen to remove oxygen for 10-15min, and finally sealing the reaction kettle for 20-30 min;
the acidification additive comprises high-carbon fatty alcohol-polyvinyl ether and dimethyl dicarbonate;
the cooling is to cool the PCB substrate by adopting an inert gas cooling method;
the inert gas is carbon dioxide or nitrogen.
2. The browning processing technology of a PCB substrate according to claim 1, wherein: the drying comprises the following specific steps: firstly, drying with cold air for 30-50min by using an air cooler, and then drying with hot air for 1-2 h.
3. The browning processing technology of a PCB substrate according to claim 1, wherein: the cooling is performed by a natural cooling method.
4. The browning processing technology of a PCB substrate according to claim 1, wherein: the azole is at least one of methylimidazole, benzotriazole, 5-methylbenzotriazole and thiazole.
5. The browning processing technology of claim 2, wherein: the temperature for drying the hot air is 70-80 degrees.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910426583.7A CN110049637B (en) | 2019-05-22 | 2019-05-22 | Brown oxidation treatment process of PCB substrate |
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| CN201910426583.7A CN110049637B (en) | 2019-05-22 | 2019-05-22 | Brown oxidation treatment process of PCB substrate |
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| CN110049637A CN110049637A (en) | 2019-07-23 |
| CN110049637B true CN110049637B (en) | 2020-11-06 |
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| CN111867275B (en) * | 2020-07-31 | 2021-08-24 | 国网河南省电力公司西峡县供电公司 | Browning method for improving interlayer binding force of printed circuit board |
| CN113056115A (en) * | 2021-03-18 | 2021-06-29 | 广德扬升电子科技有限公司 | Browning treatment process for 5G high-frequency multilayer printed circuit board |
| CN114501831B (en) * | 2022-01-28 | 2023-09-15 | 南京欣达飞科技股份有限公司 | Automatic brown chemical processing system of PCB base plate |
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| CN1079112C (en) * | 1999-09-22 | 2002-02-13 | 赵中夏 | Descaling agent for cleaning |
| TW200417628A (en) * | 2002-09-09 | 2004-09-16 | Shipley Co Llc | Improved cleaning composition |
| KR100838066B1 (en) * | 2006-07-14 | 2008-06-16 | 삼성에스디아이 주식회사 | Organic light emitting device |
| CN100491595C (en) * | 2007-04-16 | 2009-05-27 | 重庆大学 | Acid pickling inhibitor and preparation method thereof |
| TWI456093B (en) * | 2012-06-26 | 2014-10-11 | Dexnano Chemicals Co Ltd | Method for black chromium oxide and black chromium oxide electroplating layer thereof |
| JP6163803B2 (en) * | 2013-03-14 | 2017-07-19 | 味の素株式会社 | Resin composition |
| CN203814061U (en) * | 2014-04-10 | 2014-09-03 | 深圳市迅捷兴电路技术有限公司 | Brown oxidation copper ion concentration control device |
| CN105714280A (en) * | 2016-04-06 | 2016-06-29 | 武汉创新特科技有限公司 | Browning treatment liquid for printed circuit board |
| CN107190254B (en) * | 2017-05-22 | 2019-04-23 | 博敏电子股份有限公司 | A kind of novel brownification treatment fluid of printed circuit board |
| CN108179426A (en) * | 2018-03-05 | 2018-06-19 | 苏州科技大学 | A kind of copper and its alloy pickling corrosion inhibiter and preparation method thereof |
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