CN107400893B - Fine circuit film removing liquid and film removing process - Google Patents
Fine circuit film removing liquid and film removing process Download PDFInfo
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- CN107400893B CN107400893B CN201710622922.XA CN201710622922A CN107400893B CN 107400893 B CN107400893 B CN 107400893B CN 201710622922 A CN201710622922 A CN 201710622922A CN 107400893 B CN107400893 B CN 107400893B
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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
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
- C23G1/14—Cleaning or pickling metallic material with solutions or molten salts with alkaline solutions
- C23G1/20—Other heavy metals
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Abstract
The invention provides a fine circuit film stripping liquid and a film stripping process. The fine circuit stripping solution comprises, by weight, 10-50% of organic base, 1-5% of ammonia water, 1-5% of tetramethylammonium hydroxide, 20-30% of DMSO (dimethyl sulfoxide), and 1-3% of NMP. The fine circuit stripping liquid disclosed by the invention is thorough in stripping and high in stripping efficiency, and can completely strip a copper surface and a wrapped dry film within 15-90 s at the temperature of 40-65 ℃; the cost is low, and 1-3 wt% of NMP solvent is used as an auxiliary agent in the mixed solution for secondary film stripping, so that the dosage of a main solvent DMSO can be greatly reduced, and the cost of the film stripping solution is greatly reduced.
Description
Technical Field
The invention belongs to the technical field of circuit board treatment agents, and relates to a fine circuit film stripping liquid and a film stripping process.
Background
Pcb (printed Circuit board), which is called printed Circuit board in chinese, is an important electronic component, is a support for electronic components, and is a carrier for electrical connection of electronic components. It is called a "printed" circuit board because it is made using electronic printing.
In the PCB manufacturing process, a fine circuit dry film process which is a key for pattern transfer cannot completely avoid the condition that an electroplated layer forms a so-called mushroom on a dry film due to the difference of electroplating distribution in the subsequent electroplating process, and the wrapped dry film is difficult to be cleanly removed in the film removing process to cause short circuit of a circuit or the defect of dog teeth.
The film removing method is characterized in that an alkaline film removing liquid is utilized to neutralize resin containing acid groups, so that the resin is dissolved out, a dry film is separated from a copper surface, and the film removing liquid is often used in the manufacturing and production of electronic product circuits. At present, sodium hydroxide is generally adopted, when the membrane is removed, the membrane is too thick (80 microns), the capability of the liquid medicine for attacking and eroding the dry membrane is weak, the dry membrane can be removed in more than 20 minutes, and the production efficiency is reduced. In addition, in the film stripping process, as the wafers are soaked in the sodium hydroxide solution for a long time, the copper surface is easy to generate an oxidant, and the film stripping is difficult, so that the incomplete etching is caused.
CN104195558A discloses a film removing liquid, which is composed of the following raw materials in parts by weight: 80 to 85 percent of potassium hydroxide; 8.5 to 15 percent of triethanolamine; emulsifier OP21 is 1% -2%; ethylene glycol monobutyl ether is 0.3 to 0.5 percent; 2 to 3 percent of methanol; the acetone is 0.5-1%, the film removing liquid can remove the dry film on the copper surface within 5min, and the removing efficiency of the wrapped dry film needs to be improved.
Disclosure of Invention
Aiming at the defects of the prior art, one of the purposes of the invention is to provide a fine circuit film stripping liquid which is thorough in film stripping and high in film stripping efficiency, can completely strip a copper surface and a wrapped dry film within 15-90 s at 40-65 ℃, and is low in cost.
In order to achieve the purpose, the invention adopts the following technical scheme:
the fine circuit film removing liquid comprises the following components in percentage by weight:
the balance being deionized water.
In the invention, the film removing liquid comprises the following components in percentage by weight:
10-50% of organic base, for example, 10%, 15%, 20%, 25%, 30%, 35%, 40%, 45%, 50%, preferably 20-40% by weight of organic base;
1-5% of ammonia water, for example, 1%, 1.5%, 2%, 2.5%, 3%, 3.5%, 4%, 4.5%, 5%, preferably 2-3% of ammonia water;
1-5% of tetramethylammonium hydroxide, for example, 1%, 1.5%, 2%, 2.5%, 3%, 3.5%, 4%, 4.5%, 5%, preferably 2-4% by weight of tetramethylammonium hydroxide;
DMSO 20-30%, for example, DMSO accounts for 20%, 21%, 22%, 23%, 24%, 25%, 26%, 27%, 28%, 29%, 30%;
NMP 1-3%, for example NMP weight percentage is 1%, 1.2%, 1.5%, 1.6%, 1.8%, 2%, 2.2%, 2.3%, 2.5%, 2.6%, 2.8%, 2.9%, 3%.
According to the invention, the film removing liquid comprises the following substances in percentage by weight:
the balance being deionized water.
According to the invention, the organic base comprises, by weight, 5-30% of monoethanolamine, 2-10% of choline and 1-5% of tetramethylammonium hydroxide; for example, the weight percentage of monoethanolamine is 5%, 10%, 15%, 20%, 25%, 30%; the weight percentage of the choline is 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9% and 10%; the weight percentage of the tetramethyl ammonium hydroxide is 1%, 2%, 3%, 4% and 5%.
According to the invention, the organic base comprises, by weight, 10-20% of monoethanolamine, 3-6% of choline and 2-4% of tetramethylammonium hydroxide.
In the invention, the organic alkali consists of the following substances in percentage by weight: 5-30% of monoethanolamine, 2-10% of choline, 1-5% of tetramethylammonium hydroxide and the balance of deionized water.
The invention also aims to provide a film stripping process adopting the film stripping liquid for the fine circuit, which comprises the following steps:
1) according to the weight percentage, 10-50% of organic base is added into 1-5% of ammonia water to prepare a mixed solution for stripping a dry film on the copper surface of the PCB fine circuit substrate;
2) according to the weight percentage, 1-5% of tetramethyl ammonium hydroxide is used as a base solution, 20-30% of dimethyl sulfoxide (DMSO for short) is used as a main solvent, 1-3% of N-methyl pyrrolidone (NMP for short) is used as an auxiliary agent, and a mixed solution is prepared to carry out secondary film removal on the copper surface subjected to film removal in the step 1).
In step 1) of the invention, the organic alkali is used for breaking and dropping the dry film; the addition of the ammonia greatly accelerates the removal speed of most dry films.
Through the secondary film removing process in the step 2), a small amount of residual dry films on the side of the circuit surrounded by the electroplated layer are completely dissolved and then removed. Therefore, the dry film is completely removed by the two-step film removing process. The fine circuit can be a high-end PCB fine circuit and an IC carrier plate.
The film removing temperature in the steps 1) and 2) is 40-65 ℃, for example, the film removing temperature is 40 ℃, 45 ℃, 50 ℃, 55 ℃, 60 ℃ and 65 ℃.
In step 1), the thickness of the dry film is 15 to 100 μm, for example, the thickness of the dry film is 15 μm, 20 μm, 25 μm, 30 μm, 35 μm, 40 μm, 45 μm, 50 μm, 55 μm, 60 μm, 65 μm, 70 μm, 75 μm, 80 μm, 85 μm, 90 μm, 95 μm, 100 μm.
The mixed solution in the step 1) comprises 20-40% of organic base, 1-5% of ammonia water and the balance of deionized water in parts by weight.
The mixed solution in the step 2) is prepared by taking 1-5% of tetramethyl ammonium hydroxide as a base solution, 20-30% of DMSO as a main solvent, 1-3% of NMP as an auxiliary agent and the balance of deionized water in parts by weight.
Dimethyl sulfoxide (DMSO for short) and N-methylpyrrolidone (NMP for short) are used as solvents of the membrane stripping liquid in the step 2) of the invention, and a small amount of NMP solvent is used as an auxiliary agent to greatly reduce the concentration of a main solvent DMSO, so that the dosage of DMSO can be greatly reduced to 20-30% by adding 1-3% of NMP, and if the NMP auxiliary agent is lacked, the dosage of DMSO is usually required to be more than 95% to be effective, so that the cost of the membrane stripping liquid can be greatly reduced.
Compared with the prior art, the invention has the beneficial effects that:
(1) the fine circuit stripping liquid disclosed by the invention is thorough in stripping and high in stripping efficiency, and can completely strip the copper surface and the wrapped dry film within 15-90 s at the temperature of 40-65 ℃.
(2) The fine line stripping liquid disclosed by the invention is low in cost, and in a mixed solution of secondary stripping, 1-3% of NMP solvent in percentage by weight is used as an auxiliary agent, so that the consumption of a main solvent DMSO can be greatly reduced, and the cost of the stripping liquid is greatly reduced.
Detailed Description
The technical solution of the present invention is further explained by the following embodiments.
Example 1
The film-fading liquid of the embodiment comprises the following components in percentage by weight: 30% of organic base, 2% of ammonia water, 3% of tetramethylammonium hydroxide, 25% of DMSO, 3% of NMP and the balance of deionized water.
The film stripping process of the embodiment comprises the following steps:
1) according to the weight percentage, adding 30% of organic base into 2% of ammonia water, and the balance being deionized water to prepare a mixed solution for stripping a dry film on the copper surface of the PCB fine circuit substrate;
2) according to the weight percentage, 3% of tetramethyl ammonium hydroxide is used as a base solution, 25% of DMSO is used as a main solvent, 3% of NMP is used as an auxiliary agent, and the balance is deionized water, so that a mixed solution is prepared, and secondary film stripping is carried out on the copper surface subjected to film stripping in the step 1).
The thickness of the dry film is 50 mu m, the film stripping temperature is 50 ℃, and the time used by the whole film stripping process is 23 s; after complete film stripping, the surface of the copper surface is bright and has no residual dry film.
Example 2
The film-fading liquid of the embodiment comprises the following components in percentage by weight: 40% of organic base, 1% of ammonia water, 5% of tetramethylammonium hydroxide, 30% of DMSO, 1% of NMP and the balance of deionized water.
The film stripping process of the embodiment comprises the following steps:
1) according to the weight percentage, 40% of organic base is added into 1% of ammonia water, and the balance is deionized water to prepare mixed liquid for stripping a dry film on the copper surface of the PCB fine circuit substrate;
2) according to the weight percentage, 5% of tetramethyl ammonium hydroxide is used as a base solution, 30% of DMSO is used as a main solvent, 1% of NMP is used as an auxiliary agent, and the balance is deionized water, so that a mixed solution is prepared, and secondary film stripping is carried out on the copper surface subjected to film stripping in the step 1).
The thickness of the dry film is 80 mu m, the film stripping temperature is 30 ℃, and the time used by the whole film stripping process is 55 s; after complete film stripping, the surface of the copper surface is bright and has no residual dry film.
Example 3
The film-fading liquid of the embodiment comprises the following components in percentage by weight: 20% of organic base, 3% of ammonia water, 2% of tetramethylammonium hydroxide, 22% of DMSO, 2% of NMP and the balance of deionized water.
The film stripping process of the embodiment comprises the following steps:
1) according to the weight percentage, 20% of organic base is added into 3% of ammonia water, and the balance is deionized water to prepare mixed liquid for stripping a dry film on the copper surface of the PCB fine circuit substrate;
2) according to the weight percentage, 2% of tetramethyl ammonium hydroxide is used as a base solution, 22% of DMSO is used as a main solvent, 2% of NMP is used as an auxiliary agent, and the balance is deionized water, so that a mixed solution is prepared, and secondary film stripping is carried out on the copper surface subjected to film stripping in the step 1).
The thickness of the dry film is 100 mu m, the film stripping temperature is 50 ℃, and the time used by the whole film stripping process is 86 s; after complete film stripping, the surface of the copper surface is bright and has no residual dry film.
Example 4
The film-fading liquid of the embodiment comprises the following components in percentage by weight: 10% of organic base, 4% of ammonia water, 4% of tetramethylammonium hydroxide, 30% of DMSO, 1% of NMP and the balance of deionized water.
The film stripping process of the embodiment comprises the following steps:
1) according to the weight percentage, 10% of organic base is added into 4% of ammonia water, and the balance is deionized water to prepare mixed liquid for stripping a dry film on the copper surface of the PCB fine circuit substrate;
2) according to the weight percentage, 4% of tetramethyl ammonium hydroxide is used as a base solution, 30% of DMSO is used as a main solvent, 1% of NMP is used as an auxiliary agent, and the balance is deionized water, so that a mixed solution is prepared, and secondary film stripping is carried out on the copper surface subjected to film stripping in the step 1).
The thickness of the dry film is 15 mu m, the film stripping temperature is 40 ℃, and the time used by the whole film stripping process is 15 s; after complete film stripping, the surface of the copper surface is bright and has no residual dry film.
Example 5
The film-fading liquid of the embodiment comprises the following components in percentage by weight: 45% of organic base, 2% of ammonia water, 3% of tetramethylammonium hydroxide, 25% of DMSO, 3% of NMP and the balance of deionized water.
The film stripping process of the embodiment comprises the following steps:
1) adding 45% of organic base into 2% of ammonia water and the balance of deionized water according to the weight percentage to prepare mixed liquid for stripping a dry film on the copper surface of the PCB fine circuit substrate;
2) according to the weight percentage, 3% of tetramethyl ammonium hydroxide is used as a base solution, 25% of DMSO is used as a main solvent, 3% of NMP is used as an auxiliary agent, and the balance is deionized water, so that a mixed solution is prepared, and secondary film stripping is carried out on the copper surface subjected to film stripping in the step 1).
The thickness of the dry film is 50 mu m, the film stripping temperature is 50 ℃, and the time used by the whole film stripping process is 30 s; after complete film stripping, the surface of the copper surface is bright and has no residual dry film.
Example 6
The film-fading liquid of the embodiment comprises the following components in percentage by weight: 25% of organic base, 2% of ammonia water, 3% of tetramethylammonium hydroxide, 25% of DMSO, 3% of NMP and the balance of deionized water.
The film stripping process of the embodiment comprises the following steps:
1) according to the weight percentage, 2% ammonia water and the balance of deionized water are added into 25% of organic base to prepare mixed liquid for stripping a dry film on the copper surface of the PCB fine circuit substrate;
2) according to the weight percentage, 3% of tetramethyl ammonium hydroxide is used as a base solution, 25% of DMSO is used as a main solvent, 3% of NMP is used as an auxiliary agent, and the balance is deionized water, so that a mixed solution is prepared, and secondary film stripping is carried out on the copper surface subjected to film stripping in the step 1).
The thickness of the dry film is 75 mu m, the film stripping temperature is 60 ℃, and the time used by the whole film stripping process is 33 s; after complete film stripping, the surface of the copper surface is bright and has no residual dry film.
Comparative example 1
The film-fading liquid of the embodiment comprises the following components in percentage by weight: 30% of organic base, 3% of tetramethylammonium hydroxide, 25% of DMSO, 3% of NMP and the balance of deionized water.
The film stripping process of the embodiment comprises the following steps:
1) adding 30% of organic base into the balance of deionized water according to the weight percentage to prepare mixed liquid for stripping a dry film on the copper surface of the PCB fine circuit substrate;
2) according to the weight percentage, 3% of tetramethyl ammonium hydroxide is used as a base solution, 25% of DMSO is used as a main solvent, 3% of NMP is used as an auxiliary agent, and the balance is deionized water, so that a mixed solution is prepared, and secondary film stripping is carried out on the copper surface subjected to film stripping in the step 1).
The thickness of the dry film is 80 mu m, the film stripping temperature is 50 ℃, and the time used by the whole film stripping process is 110 s; after complete film stripping, the surface of the copper surface is blackened and no residual dry film exists.
Comparative example 2
The film-fading liquid of the embodiment comprises the following components in percentage by weight: 15% of organic base, 2% of tetramethylammonium hydroxide, 80% of DMSO and the balance of deionized water.
The film stripping process of the embodiment comprises the following steps:
1) adding 15% of organic base into the balance of deionized water according to the weight percentage to prepare mixed liquid for stripping a dry film on the copper surface of the PCB fine circuit substrate;
2) according to the weight percentage, 2% of tetramethyl ammonium hydroxide is used as a base solution, 80% of DMSO is used as a main solvent, and the balance is deionized water, so that a mixed solution is prepared, and secondary film stripping is carried out on the copper surface subjected to film stripping in the step 1).
The thickness of the dry film is 100 mu m, the film stripping temperature is 55 ℃, and the time used by the whole film stripping process is 120 s; after complete stripping, the surface of the copper surface is blackened, and a small amount of dry film sandwiched by the copper surface is not stripped.
Comparative example 3
The film-fading liquid of the embodiment comprises the following components in percentage by weight: 18% of organic base, 5% of ammonia water, 5% of tetramethylammonium hydroxide, 70% of DMSO and the balance of deionized water.
The film stripping process of the embodiment comprises the following steps:
1) according to the weight percentage, 18% of organic base is added into 5% of ammonia water, and the balance is deionized water to prepare mixed liquid for stripping a dry film on the copper surface of the PCB fine circuit substrate;
2) according to the weight percentage, 5% of tetramethyl ammonium hydroxide is used as a base solution, 70% of DMSO is used as a main solvent, and the balance is deionized water, so that a mixed solution is prepared, and secondary film stripping is carried out on the copper surface subjected to film stripping in the step 1).
The thickness of the dry film is 50 mu m, the film stripping temperature is 60 ℃, and the time used by the whole film stripping process is 100 s; after complete stripping, the surface of the copper surface is bright, and a small amount of dry film clamped by the copper surface is not stripped.
The applicant states that the present invention is illustrated by the above examples to show the detailed process equipment and process flow of the present invention, but the present invention is not limited to the above detailed process equipment and process flow, i.e. it does not mean that the present invention must rely on the above detailed process equipment and process flow to be implemented. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
Claims (7)
1. The film stripping process of the fine line film stripping liquid is characterized by comprising the following steps:
1) according to the weight percentage, 10-50% of organic base is added into 1-5% of ammonia water to prepare a mixed solution for stripping a dry film on the copper surface of the PCB fine circuit substrate;
2) according to the weight percentage, 1-5% of tetramethyl ammonium hydroxide is used as a base solution, 20-30% of DMSO is used as a main solvent, 1-3% of NMP is used as an auxiliary agent, and a mixed solution is prepared to carry out secondary film stripping on the copper surface subjected to film stripping in the step 1);
the organic base comprises, by weight, 5-30% of monoethanolamine, 2-10% of choline and 1-5% of tetramethylammonium hydroxide.
2. The film stripping process according to claim 1, wherein the organic base comprises, by weight, 10-20% of monoethanolamine, 3-6% of choline, and 2-4% of tetramethylammonium hydroxide.
3. The process for stripping film according to claim 1, wherein the organic base comprises the following substances in percentage by weight: 5-30% of monoethanolamine, 2-10% of choline, 1-5% of tetramethylammonium hydroxide and the balance of deionized water.
4. The de-filming process according to claim 1, wherein the de-filming temperature in step 1) and step 2) is 40-65 ℃.
5. The film stripping process according to claim 1, wherein in step 1), the thickness of the dry film is 15-100 μm.
6. The film fading process according to claim 1, wherein the mixed solution in the step 1) comprises 20-40% of organic base, 1-5% of ammonia water and the balance of deionized water in parts by weight.
7. The film fading process according to claim 1, wherein the mixed solution in the step 2) comprises, by weight, 1-5% of tetramethylammonium hydroxide as a base solution, 20-30% of DMSO as a main solvent, 1-3% of NMP as an auxiliary agent, and the balance of deionized water.
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| CN201710622922.XA CN107400893B (en) | 2017-07-27 | 2017-07-27 | Fine circuit film removing liquid and film removing process |
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| CN109371406B (en) * | 2018-11-23 | 2020-09-11 | 东南大学 | Stripping method for sulfide soft coating cutter |
| CN110597026B (en) * | 2019-09-26 | 2022-11-29 | 上海富柏化工有限公司 | Dry film removing process for flexible circuit board |
| CN111031694A (en) * | 2019-12-31 | 2020-04-17 | 江门市华锐铝基板股份公司 | Film stripping liquid and film stripping method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2017126652A1 (en) * | 2016-01-20 | 2017-07-27 | 日揮プラントイノベーション株式会社 | Liquid detergent composition for removing sludge and hard films formed in system containing heavy hydrocarbon or element imparting polarity to molecule, and cleaning method using same |
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| CN101578341A (en) * | 2008-01-07 | 2009-11-11 | 巴斯夫欧洲公司 | Composition and method for stripping organic coatings |
| CN102634809B (en) * | 2012-04-27 | 2013-11-13 | 东莞市广华化工有限公司 | Secondary dry film removing liquid |
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| WO2017126652A1 (en) * | 2016-01-20 | 2017-07-27 | 日揮プラントイノベーション株式会社 | Liquid detergent composition for removing sludge and hard films formed in system containing heavy hydrocarbon or element imparting polarity to molecule, and cleaning method using same |
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Effective date of registration: 20220729 Address after: 201599 block s, room 359, unit 5, building 1, 688 Qiushi Road, Jinshanwei Town, Jinshan District, Shanghai Patentee after: Shanghai Tiancheng Chemical Co.,Ltd. Address before: Building 4, No. 1088, Yinzhong South Road, Hedong Industrial Park, Wuzhong Economic Development Zone, Suzhou City, Jiangsu Province Patentee before: SUZHOU SKYCHEM LTD. |