CN112064026A - Novel copper surface roughness corrosion stabilizer and preparation method thereof - Google Patents
Novel copper surface roughness corrosion stabilizer and preparation method thereof Download PDFInfo
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- CN112064026A CN112064026A CN202010765969.3A CN202010765969A CN112064026A CN 112064026 A CN112064026 A CN 112064026A CN 202010765969 A CN202010765969 A CN 202010765969A CN 112064026 A CN112064026 A CN 112064026A
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- Prior art keywords
- stabilizer
- copper surface
- hydrogen peroxide
- surface roughness
- bite
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- Pending
Links
- 239000003381 stabilizer Substances 0.000 title claims abstract description 51
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 41
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 40
- 239000010949 copper Substances 0.000 title claims abstract description 40
- 238000005260 corrosion Methods 0.000 title claims abstract description 25
- 230000007797 corrosion Effects 0.000 title claims abstract description 21
- 230000003746 surface roughness Effects 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title abstract description 10
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 56
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000008367 deionised water Substances 0.000 claims abstract description 15
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000003112 inhibitor Substances 0.000 claims abstract description 11
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims description 21
- 238000003756 stirring Methods 0.000 claims description 18
- GTKOKCQMHAGFSM-UHFFFAOYSA-N 1-methyltetrazol-5-amine Chemical compound CN1N=NN=C1N GTKOKCQMHAGFSM-UHFFFAOYSA-N 0.000 claims description 12
- LXBGSDVWAMZHDD-UHFFFAOYSA-N 2-methyl-1h-imidazole Chemical compound CC1=NC=CN1 LXBGSDVWAMZHDD-UHFFFAOYSA-N 0.000 claims description 12
- ULRPISSMEBPJLN-UHFFFAOYSA-N 2h-tetrazol-5-amine Chemical compound NC1=NN=NN1 ULRPISSMEBPJLN-UHFFFAOYSA-N 0.000 claims description 12
- PAFZNILMFXTMIY-UHFFFAOYSA-N cyclohexylamine Chemical compound NC1CCCCC1 PAFZNILMFXTMIY-UHFFFAOYSA-N 0.000 claims description 12
- RWNUSVWFHDHRCJ-UHFFFAOYSA-N 1-butoxypropan-2-ol Chemical compound CCCCOCC(C)O RWNUSVWFHDHRCJ-UHFFFAOYSA-N 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 6
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 claims description 5
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 4
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims description 3
- 150000001875 compounds Chemical class 0.000 claims description 2
- 238000005530 etching Methods 0.000 abstract description 5
- 150000002391 heterocyclic compounds Chemical class 0.000 abstract description 3
- 238000000354 decomposition reaction Methods 0.000 abstract description 2
- 229910021645 metal ion Inorganic materials 0.000 abstract description 2
- 230000003628 erosive effect Effects 0.000 abstract 4
- 238000005457 optimization Methods 0.000 description 7
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000011889 copper foil Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 150000003071 polychlorinated biphenyls Chemical class 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F1/00—Etching metallic material by chemical means
- C23F1/10—Etching compositions
- C23F1/14—Aqueous compositions
- C23F1/16—Acidic compositions
- C23F1/18—Acidic compositions for etching copper or alloys thereof
-
- 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
- H05K3/02—Apparatus or processes for manufacturing printed circuits in which the conductive material is applied to the surface of the insulating support and is thereafter removed from such areas of the surface which are not intended for current conducting or shielding
- H05K3/06—Apparatus or processes for manufacturing printed circuits in which the conductive material is applied to the surface of the insulating support and is thereafter removed from such areas of the surface which are not intended for current conducting or shielding the conductive material being removed chemically or electrolytically, e.g. by photo-etch process
- H05K3/067—Etchants
Abstract
The invention discloses a novel copper surface roughness biting and eroding stabilizer and a preparation method thereof, wherein the biting and eroding stabilizer comprises 3-10% of sulfuric acid, 3-8% of hydrogen peroxide, 0.5-1% of hydrogen peroxide stabilizer, 1-3% of corrosion inhibitor, 3-5% of microetching stabilizer and 75-90% of deionized water, the stabilizer can be added to obviously inhibit the self-decomposition of hydrogen peroxide in the biting and eroding stabilizer, the use stability and the quality guarantee period of the biting and eroding stabilizer are improved, and the N-containing heterocyclic compound is added to effectively adsorb at a place with high current density during etching, so that metal ions can be deposited at a place with low current density, and the concave part of a plate surface can be leveled.
Description
Technical Field
The invention relates to the technical field of copper surface corrosion inhibitors, in particular to a novel copper surface roughness corrosion inhibitor and a preparation method thereof.
Background
Printed circuit boards are providers of electrical connection of electronic components, and as electronic products are developed in a direction of being lighter, smaller and thinner, PCBs are also required to be developed in a direction of being higher in density and finer, whereas printed circuit boards with high density and finer require PCB circuits to be finer, the finer circuits are closely related to surface copper thickness, and the thicker the copper thickness is, the more difficult it is to manufacture the finer circuits.
The existing PCB copper surface processing is mainly formic acid and stabilizer two-dosage type copper surface etching agent, and the roughness of the copper surface is not high. After the copper surface corrosion stabilizer is subjected to corrosion treatment, when the micro-corrosion amount is 20UM, the roughness of the copper surface can only reach RA: 0.1-0.15, RZ: 1.0-1.3, the oxidation resistance of the copper surface is poor, and the copper surface of the carrier is oxidized and blackened immediately when the copper surface corrosion stabilizer is output from the coarse liquid medicine cylinder; the roughness uniformity of the copper surface corrosion stabilizer is poor, and the roughness of 12 points of the existing copper surface corrosion stabilizer tested on the copper surface only reaches 70 percent of uniformity.
In conclusion, the chemical copper surface treatment of the PCB process has insufficient roughness, poor oxidation resistance and low roughness uniformity.
Disclosure of Invention
The invention aims to provide a novel copper surface roughness undercut stabilizer and a preparation method thereof, so as to solve the problems in the background technology.
In order to achieve the purpose, the invention adopts the technical scheme that: a novel copper surface roughness corrosion stabilizer comprises, by mass, 3-10% of sulfuric acid, 3-8% of hydrogen peroxide, 0.5-1% of a hydrogen peroxide stabilizer, 1-3% of a corrosion inhibitor, 3-5% of a microetching stabilizer and 75-90% of deionized water.
As further optimization, the novel copper surface roughness bite stabilizer comprises, by mass, 8% of sulfuric acid, 6% of hydrogen peroxide, 1% of a hydrogen peroxide stabilizer, 2% of a corrosion inhibitor, 5% of a microetching stabilizer and 78% of deionized water.
As a further optimization, the volume fraction of the sulfuric acid is 98%; the volume fraction of the hydrogen peroxide is 30%.
As further optimization, the hydrogen peroxide stabilizer is one of ethylene glycol methyl ether, diethylene glycol and propylene glycol butyl ether.
As a further optimization, the corrosion inhibitor is one of cyclohexylamine, diethanolamine and triethanolamine.
As a further optimization, the microetching stabilizer is a compound of 2-methylimidazole, 5-aminotetrazole and 5-amino-1-methyltetrazole.
As further optimization, the mass ratio of the 2-methylimidazole, the 5-aminotetrazole and the 5-amino-1-methyltetrazole is 1 (1-2) to (1-2).
The invention also provides a preparation method of the novel copper surface roughness bite-corrosion stabilizer, which comprises the following steps,
s1) weighing the components according to the mass fraction;
s2) sequentially adding deionized water, a corrosion inhibitor and a microetching stabilizer, then slowly adding sulfuric acid, uniformly stirring, adding a hydrogen peroxide stabilizer and hydrogen peroxide, and uniformly stirring to obtain a finished product.
As a further optimization, the method of the invention S2 adopts room temperature feeding, and the stirring speed is 50-60 times/min.
Compared with the prior art, the invention has the beneficial effects that:
1. the stabilizer is at least one selected from ethylene glycol methyl ether, diethylene glycol and propylene glycol butyl ether, can obviously inhibit the self-decomposition of hydrogen peroxide in the bite stabilizer, improves the use stability of the bite stabilizer and prolongs the shelf life;
2. by adding the N-containing heterocyclic compound, the N-containing heterocyclic compound can be effectively adsorbed at a place with high current density during etching, and metal ions are favorably deposited at a place with low current density, so that the concave part of the plate surface is leveled, and the uniformity of roughness is improved.
Drawings
FIG. 1 is an electron microscope scanning image of a copper surface with a microetching rate of 20 μ "according to the present invention.
FIG. 2 is an electron microscope scanning of a copper surface with a microetching rate of 30 μ "according to the present invention.
FIG. 3 is an electron microscope scan of a copper surface with a microetching rate of 40 μ "according to the present invention.
Detailed Description
The following are specific embodiments of the present invention, and the technical solutions of the present invention will be further described with reference to the drawings, but the present invention is not limited to these embodiments.
Example 1
A novel copper surface roughness bite-etching stabilizer comprises, by mass, 8% of sulfuric acid, 6% of hydrogen peroxide, 1% of diethylene glycol, 2% of cyclohexylamine, 1% of 2-methylimidazole, 2% of 5-aminotetrazole, 2% of 5-amino-1-methyltetrazole and 78% of deionized water.
The preparation method comprises the following steps: s1) weighing the components according to the mass fraction; s2) sequentially adding deionized water, cyclohexylamine, 2-methylimidazole, 5-aminotetrazole and 5-amino-1-methyltetrazole at room temperature, slowly adding sulfuric acid, stirring uniformly, adding diethylene glycol and hydrogen peroxide, and stirring uniformly to obtain a finished product; the stirring speed is 50-60 times/min.
Example 2
A novel copper surface roughness bite-etching stabilizer comprises, by mass, 5% of sulfuric acid, 5% of hydrogen peroxide, 0.5% of propylene glycol butyl ether, 2.5% of cyclohexylamine, 1% of 2-methylimidazole, 1% of 5-aminotetrazole, 1% of 5-amino-1-methyltetrazole and 84% of deionized water.
The preparation method comprises the following steps: s1) weighing the components according to the mass fraction; s2) sequentially adding deionized water, cyclohexylamine, 2-methylimidazole, 5-aminotetrazole and 5-amino-1-methyltetrazole at room temperature, slowly adding sulfuric acid, stirring uniformly, adding propylene glycol butyl ether and hydrogen peroxide, and stirring uniformly to obtain a finished product; the stirring speed is 50-60 times/min.
Example 3
A novel copper surface roughness corrosion stabilizer comprises, by mass, 7% of sulfuric acid, 2% of hydrogen peroxide, 1% of diethylene glycol, 3% of diethanolamine, 1% of 2-methylimidazole, 1% of 5-aminotetrazole, 1% of 5-amino-1-methyltetrazole and 84% of deionized water.
The preparation method comprises the following steps: s1) weighing the components according to the mass fraction; s2) sequentially adding deionized water, propylene glycol butyl ether, 2-methylimidazole, 5-aminotetrazole and 5-amino-1-methyltetrazole at room temperature, slowly adding sulfuric acid, stirring uniformly, adding diethylene glycol and hydrogen peroxide, and stirring uniformly to obtain a finished product; the stirring speed is 50-60 times/min.
Example 4
A novel copper surface roughness corrosion stabilizer comprises, by mass, 8% of sulfuric acid, 7% of hydrogen peroxide, 1% of ethylene glycol monomethyl ether, 1% of triethanolamine, 1% of 2-methylimidazole, 2% of 5-aminotetrazole, 1% of 5-amino-1-methyltetrazole and 79% of deionized water.
The preparation method comprises the following steps: s1) weighing the components according to the mass fraction; s2) sequentially adding deionized water, triethanolamine, 2-methylimidazole, 5-aminotetrazole and 5-amino-1-methyltetrazole at room temperature, slowly adding sulfuric acid, stirring uniformly, adding ethylene glycol monomethyl ether and hydrogen peroxide, and stirring uniformly to obtain a finished product; the stirring speed is 50-60 times/min.
Application examples
A bite stabilizer was prepared according to the formulation of example 1, and 1/3oz of 4cm X5 cm double-sided electrolytic copper foil was immersed at 25 ℃ for 1min, taken out and dried with hot air, and SEM photograph was taken using Nitachi S-3000N.
As shown in fig. 1 to 3, the microetching rates were 20 μ ", 30 μ", and 40 μ ", respectively, and it can be seen from the drawings that the undercut copper face can be formed into a honeycomb-like uniform rough surface.
The specific embodiments described herein are merely illustrative of the spirit of the invention. Various modifications or additions may be made to the described embodiments or alternatives may be employed by those skilled in the art without departing from the spirit or ambit of the invention as defined in the appended claims.
Claims (9)
1. The novel copper surface roughness bite-corrosion stabilizer is characterized by comprising, by mass, 3-10% of sulfuric acid, 3-8% of hydrogen peroxide, 0.5-1% of hydrogen peroxide stabilizer, 1-3% of corrosion inhibitor, 3-5% of microetching stabilizer and 75-90% of deionized water.
2. The novel copper surface roughness bite stabilizer according to claim 1, characterized by comprising, by mass, 8% of sulfuric acid, 6% of hydrogen peroxide, 1% of a hydrogen peroxide stabilizer, 2% of a corrosion inhibitor, 5% of a microetching stabilizer, and 78% of deionized water.
3. The novel copper surface roughness bite stabilizer according to claim 1, characterized in that the volume fraction of sulfuric acid is 98%; the volume fraction of the hydrogen peroxide is 30%.
4. The novel copper surface roughness bite stabilizer according to claim 1, wherein the hydrogen peroxide stabilizer is one of ethylene glycol methyl ether, diethylene glycol and propylene glycol butyl ether.
5. The novel copper surface roughness bite stabilizer according to claim 1, wherein the corrosion inhibitor is one of cyclohexylamine, diethanolamine and triethanolamine.
6. The novel copper surface roughness bite stabilizer according to claim 1, wherein the microetching stabilizer is a compound of 2-methylimidazole, 5-aminotetrazole and 5-amino-1-methyltetrazole.
7. The novel copper surface roughness bite-corrosion stabilizer as claimed in claim 6, wherein the mass ratio of the 2-methylimidazole, the 5-aminotetrazole and the 5-amino-1-methyltetrazole is 1 (1-2) to (1-2).
8. A method for preparing the novel copper surface roughness bite stabilizer according to any one of claims 1 to 7, characterized by comprising the steps of,
s1) weighing the components according to the mass fraction;
s2) sequentially adding deionized water, a corrosion inhibitor and a microetching stabilizer, then slowly adding sulfuric acid, uniformly stirring, adding a hydrogen peroxide stabilizer and hydrogen peroxide, and uniformly stirring to obtain a finished product.
9. The method for preparing the novel copper surface roughness bite stabilizer according to claim 8, characterized in that the addition is carried out at room temperature, and the stirring speed is 50-60 times/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010765969.3A CN112064026A (en) | 2020-08-03 | 2020-08-03 | Novel copper surface roughness corrosion stabilizer and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010765969.3A CN112064026A (en) | 2020-08-03 | 2020-08-03 | Novel copper surface roughness corrosion stabilizer and preparation method thereof |
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| Publication Number | Publication Date |
|---|---|
| CN112064026A true CN112064026A (en) | 2020-12-11 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN202010765969.3A Pending CN112064026A (en) | 2020-08-03 | 2020-08-03 | Novel copper surface roughness corrosion stabilizer and preparation method thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113445052A (en) * | 2021-07-28 | 2021-09-28 | 南通群安电子材料有限公司 | Differential etching solution suitable for MSAP (multiple-site-sensitive protection) process |
| CN114016031A (en) * | 2021-10-22 | 2022-02-08 | 深圳市松柏实业发展有限公司 | Fast etching liquid and preparation method thereof |
| CN114574863A (en) * | 2022-03-10 | 2022-06-03 | 上海富柏化工有限公司 | Low-loss black hole micro-etching solution and preparation method and application thereof |
| CN114686885A (en) * | 2022-06-02 | 2022-07-01 | 深圳市板明科技股份有限公司 | Copper surface super-roughening solution for circuit board, preparation method and application thereof |
| CN114807942A (en) * | 2022-03-07 | 2022-07-29 | 上海富柏化工有限公司 | Sodium persulfate microetching additive and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4917758A (en) * | 1988-05-20 | 1990-04-17 | Mitsubishi Gas Chemical Company, Inc. | Method for preparing thin copper foil-clad substrate for circuit boards |
| US5800859A (en) * | 1994-12-12 | 1998-09-01 | Price; Andrew David | Copper coating of printed circuit boards |
| US20020084441A1 (en) * | 2000-01-07 | 2002-07-04 | Roger Bernards | Method for roughening copper surfaces for bonding to substrates |
| CN109097776A (en) * | 2018-07-17 | 2018-12-28 | 东莞市广华化工有限公司 | A kind of microetch subtracts copper annex solution and technique |
| CN110079804A (en) * | 2019-06-17 | 2019-08-02 | 广州三孚新材料科技股份有限公司 | Copper surface micro-etching agent and preparation method thereof |
| CN110913596A (en) * | 2019-12-10 | 2020-03-24 | 深圳市板明科技有限公司 | Copper-reducing microetching agent and preparation method thereof |
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2020
- 2020-08-03 CN CN202010765969.3A patent/CN112064026A/en active Pending
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| US4917758A (en) * | 1988-05-20 | 1990-04-17 | Mitsubishi Gas Chemical Company, Inc. | Method for preparing thin copper foil-clad substrate for circuit boards |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113445052A (en) * | 2021-07-28 | 2021-09-28 | 南通群安电子材料有限公司 | Differential etching solution suitable for MSAP (multiple-site-sensitive protection) process |
| CN114016031A (en) * | 2021-10-22 | 2022-02-08 | 深圳市松柏实业发展有限公司 | Fast etching liquid and preparation method thereof |
| CN114807942A (en) * | 2022-03-07 | 2022-07-29 | 上海富柏化工有限公司 | Sodium persulfate microetching additive and application thereof |
| CN114807942B (en) * | 2022-03-07 | 2024-02-13 | 上海富柏化工有限公司 | Sodium persulfate microetching additive and application thereof |
| CN114574863A (en) * | 2022-03-10 | 2022-06-03 | 上海富柏化工有限公司 | Low-loss black hole micro-etching solution and preparation method and application thereof |
| CN114574863B (en) * | 2022-03-10 | 2023-12-01 | 上海富柏化工有限公司 | Low-loss black hole microetching solution and preparation method and application thereof |
| CN114686885A (en) * | 2022-06-02 | 2022-07-01 | 深圳市板明科技股份有限公司 | Copper surface super-roughening solution for circuit board, preparation method and application thereof |
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Application publication date: 20201211 |