CN109797384A - A kind of printed wiring board copper antioxidation agent and preparation method thereof - Google Patents
A kind of printed wiring board copper antioxidation agent and preparation method thereof Download PDFInfo
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- CN109797384A CN109797384A CN201910146009.6A CN201910146009A CN109797384A CN 109797384 A CN109797384 A CN 109797384A CN 201910146009 A CN201910146009 A CN 201910146009A CN 109797384 A CN109797384 A CN 109797384A
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- sodium
- printed wiring
- wiring board
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Abstract
The present invention relates to the technical fields of printed wiring board production, more particularly to a kind of printed wiring board copper antioxidation agent and preparation method thereof, it can be under the premise of same operation processing, can reducing treated, there is oxidative phenomena in copper face, and the duration for preventing color changeable effect can be extended, it is easy to operate；Raw material including following ratio: organic acid 2-3%；Ethyl alcohol 1.2-1.3%；Hydrogen peroxidase 10 .4-0.7%；Benzimidizole derivatives 0.1-0.3%；Benzotriazole Derivative salt 0.1-0.3%；Sodium sulphate 0.2-0.4%；Sodium molybdate 0.1-0.3%；Potassium chloride 0.2-0.4%；Sodium hypophosphite 0.05-0.10%；Sodium potassium tartrate tetrahydrate 0.05-0.10%；Cobalt chloride 0.05-0.10%；Deionized water surplus；Preparation method are as follows: hydrogen peroxide, benzimidizole derivatives, Benzotriazole Derivative salt, sodium sulphate, sodium molybdate, potassium chloride, sodium hypophosphite, sodium potassium tartrate tetrahydrate and cobalt chloride are added in portions of de-ionized water, mixing 10-20min is stirred at 50-60 DEG C；Organic acid and ethyl alcohol is added, and is cooled to progress mixed processing 60-80min at 45 DEG C ± 3 DEG C；Deionized water is supplied, and is cooled down.
Description
Technical field
The present invention relates to the technical fields of printed wiring board production, more particularly to a kind of printed wiring board copper face oxygen
Agent and preparation method thereof.
Background technique
Printed wiring board, i.e. PCB circuit board, also known as printed circuit board are the suppliers of electronic component electrical connection,
In manufacture and assembling process, to improve the planarization of welding surface, reducing cost and meeting the requirement of environmental protection, therefore in its production
It needs to carry out anti-oxidation processing to copper sheet used in it in the process, is not in oxidation to guarantee it in subsequent use process
Phenomena such as with discoloration, in existing antioxidant use process, by copper face using washing after antioxidant processing using 70-80
DEG C hot blast drying, copper sheet overlaps when there is moisture at the copper sheet edge after hot blast drying, after lower plate place 20min after
Will appear oxidative phenomena, and it prevents the color changeable effect duration shorter, be easy to its it is subsequent processing and using etc. cause
It influences.
Summary of the invention
In order to solve the above technical problems, the present invention provide one kind can same operation processing under the premise of, it is possible to reduce place
There is oxidative phenomena in copper face after reason, and can extend the duration for preventing color changeable effect, printed wiring easy to operate
Plate copper antioxidation agent and preparation method thereof.
A kind of printed wiring board copper antioxidation agent of the invention, the raw material including following ratio:
Organic acid 2-3%；
Ethyl alcohol 1.2-1.3%；
Hydrogen peroxidase 10 .4-0.7%；
Benzimidizole derivatives 0.1-0.3%；
Benzotriazole Derivative salt 0.1-0.3%；
Sodium sulphate 0.2-0.4%；
Sodium molybdate 0.1-0.3%；
Potassium chloride 0.2-0.4%；
Sodium hypophosphite 0.05-0.10%；
Sodium potassium tartrate tetrahydrate 0.05-0.10%；
Cobalt chloride 0.05-0.10%；
Deionized water surplus.
A kind of printed wiring board copper antioxidation agent of the invention, it is preferred that the raw material including following ratio:
Organic acid 2.45-2.6%；
Ethyl alcohol 1.24-1.26%；
Hydrogen peroxidase 10 .5-0.6%；
Benzimidizole derivatives 0.18-0.21%；
Benzotriazole Derivative salt 0.18-0.21%；
Sodium sulphate 0.29-0.32%；
Sodium molybdate 0.18-0.24%；
Potassium chloride 0.27-0.31%；
Sodium hypophosphite 0.07-0.08%；
Sodium potassium tartrate tetrahydrate 0.07-0.08%；
Cobalt chloride 0.07-0.08%；
Deionized water surplus.
A kind of printed wiring board copper antioxidation agent of the invention, the organic acid are formic acid, acetic acid, hydroxy ethylidene two
The mixture of any one or more in phosphonic acids and propionic acid.
A kind of printed wiring board copper antioxidation agent of the invention, the benzimidizole derivatives be band alkyl, phenyl,
The mixture of one of alkylene, halogen, sulfonic monosubstituted polysubstituted or compound substituted benzimidazole or multiple groups.
A kind of printed wiring board copper antioxidation agent of the invention, the Benzotriazole Derivative salt are benzothiazole
Sodium.
A kind of preparation method of printed wiring board copper antioxidation agent of the invention, comprising the following steps:
(1) weigh respectively hydrogen peroxide, benzimidizole derivatives, Benzotriazole Derivative salt, sodium sulphate, sodium molybdate,
Potassium chloride, sodium hypophosphite, sodium potassium tartrate tetrahydrate and cobalt chloride, and be added into portions of de-ionized water, it is stirred at 50-60 DEG C
Mixing 10-20min is mixed, until being uniformly mixed；
(2) organic acid and ethyl alcohol are added into mixed liquor obtained in step (1), and is cooled at 45 DEG C ± 3 DEG C and carries out
Mixed processing 60-80min；
(3) deionized water is supplied, and the mixed solution after the completion of mixing is cooled to room temperature, obtains antioxidant.
Compared with prior art the invention has the benefit that in the present invention addition band alkyl, phenyl, alkylene, halogen,
One of sulfonic monosubstituted polysubstituted or compound substituted benzimidazole or the mixture of multiple groups are as benzimidazole
Derivative can react with copper face, generate fine and close organic-metallic complex compound, and copper sheet surface is made to form one layer of oxygen
The protective film of change, so as under the premise of same operation is handled, before the margin residual moisture by high temperature drying back plate
It puts, it is possible to reduce oxidative phenomena occurs in lamination part after copper face lower plate that treated, reduces the sulfide in air to copper face
Autoxidation phenomenon, and the duration for preventing color changeable effect can be extended, and since it can be used at normal temperature,
Therefore its is easy to operate.
Specific embodiment
With reference to embodiment, the embodiment of the present invention is furthur described in detail.Following embodiment is used for
Illustrate the present invention, but is not intended to limit the scope of the invention.
Embodiment 1
The mixture of any one or more in formic acid, acetic acid, 1-hydroxy ethylidene-1,1-diphosphonic acid and propionic acid is as organic
Acid starting material, and select with alkyl, phenyl, alkylene, halogen, sulfonic monosubstituted polysubstituted or compound substituted benzo miaow
One of azoles or the mixture of multiple groups are as benzimidizole derivatives raw material.
A kind of preparation method of printed wiring board copper antioxidation agent, comprising the following steps:
(1) weigh respectively 0.4% hydrogen peroxide, 0.1% benzimidizole derivatives, 0.1% benzothiazole sodium,
0.2% sodium sulphate, 0.1% sodium molybdate, 0.2% potassium chloride, 0.05% sodium hypophosphite, 0.05% sodium potassium tartrate tetrahydrate
Cobalt chloride with 0.05%, and is added into portions of de-ionized water, mixing 10-20min is stirred at 50-60 DEG C, directly
Extremely it is uniformly mixed；
(2) 2% organic acid and 1.2% ethyl alcohol are added into mixed liquor obtained in step (1), and is cooled to 45 DEG C
Mixed processing 60-80min is carried out at ± 3 DEG C；
(3) deionized water is supplied, and the mixed solution after the completion of mixing is cooled to room temperature, obtains antioxidant.
Embodiment 2
The mixture of any one or more in formic acid, acetic acid, 1-hydroxy ethylidene-1,1-diphosphonic acid and propionic acid is as organic
Acid starting material, and select with alkyl, phenyl, alkylene, halogen, sulfonic monosubstituted polysubstituted or compound substituted benzo miaow
One of azoles or the mixture of multiple groups are as benzimidizole derivatives raw material.
A kind of preparation method of printed wiring board copper antioxidation agent, comprising the following steps:
(1) weigh respectively 0.45% hydrogen peroxide, 0.14% benzimidizole derivatives, 0.14% benzothiazole
Sodium, 0.25% sodium sulphate, 0.14% sodium molybdate, 0.23% potassium chloride, 0.06% sodium hypophosphite, 0.06% winestone
Sour potassium sodium and 0.06% cobalt chloride, and be added into portions of de-ionized water, mixing 10- be stirred at 50-60 DEG C
20min, until being uniformly mixed；
(2) 2.23% organic acid and 1.12% ethyl alcohol are added into mixed liquor obtained in step (1), and is cooled to
Mixed processing 60-80min is carried out at 45 DEG C ± 3 DEG C；
(3) deionized water is supplied, and the mixed solution after the completion of mixing is cooled to room temperature, obtains antioxidant.
Embodiment 3
The mixture of any one or more in formic acid, acetic acid, 1-hydroxy ethylidene-1,1-diphosphonic acid and propionic acid is as organic
Acid starting material, and select with alkyl, phenyl, alkylene, halogen, sulfonic monosubstituted polysubstituted or compound substituted benzo miaow
One of azoles or the mixture of multiple groups are as benzimidizole derivatives raw material.
A kind of preparation method of printed wiring board copper antioxidation agent, comprising the following steps:
(1) weigh respectively 0.5% hydrogen peroxide, 0.18% benzimidizole derivatives, 0.18% benzothiazole sodium,
0.29% sodium sulphate, 0.18% sodium molybdate, 0.27% potassium chloride, 0.07% sodium hypophosphite, 0.07% tartaric acid
Potassium sodium and 0.07% cobalt chloride, and be added into portions of de-ionized water, mixing 10- be stirred at 50-60 DEG C
20min, until being uniformly mixed；
(2) 2.45% organic acid and 1.24% ethyl alcohol are added into mixed liquor obtained in step (1), and is cooled to
Mixed processing 60-80min is carried out at 45 DEG C ± 3 DEG C；
(3) deionized water is supplied, and the mixed solution after the completion of mixing is cooled to room temperature, obtains antioxidant.
Embodiment 4
The mixture of any one or more in formic acid, acetic acid, 1-hydroxy ethylidene-1,1-diphosphonic acid and propionic acid is as organic
Acid starting material, and select with alkyl, phenyl, alkylene, halogen, sulfonic monosubstituted polysubstituted or compound substituted benzo miaow
One of azoles or the mixture of multiple groups are as benzimidizole derivatives raw material.
A kind of preparation method of printed wiring board copper antioxidation agent, comprising the following steps:
(1) weigh respectively 0.55% hydrogen peroxide, 0.19% benzimidizole derivatives, 0.19% benzothiazole
Sodium, 0.31% sodium sulphate, 0.21% sodium molybdate, 0.29% potassium chloride, 0.075% sodium hypophosphite, 0.075% wine
Stone acid potassium sodium and 0.075% cobalt chloride, and be added into portions of de-ionized water, mixing 10- be stirred at 50-60 DEG C
20min, until being uniformly mixed；
(2) 2.53% organic acid and 1.25% ethyl alcohol are added into mixed liquor obtained in step (1), and is cooled to
Mixed processing 60-80min is carried out at 45 DEG C ± 3 DEG C；
(3) deionized water is supplied, and the mixed solution after the completion of mixing is cooled to room temperature, obtains antioxidant.
Embodiment 5
The mixture of any one or more in formic acid, acetic acid, 1-hydroxy ethylidene-1,1-diphosphonic acid and propionic acid is as organic
Acid starting material, and select with alkyl, phenyl, alkylene, halogen, sulfonic monosubstituted polysubstituted or compound substituted benzo miaow
One of azoles or the mixture of multiple groups are as benzimidizole derivatives raw material.
A kind of preparation method of printed wiring board copper antioxidation agent, comprising the following steps:
(1) weigh respectively 0.6% hydrogen peroxide, 0.21% benzimidizole derivatives, 0.21% benzothiazole sodium,
0.32% sodium sulphate, 0.24% sodium molybdate, 0.31% potassium chloride, 0.08% sodium hypophosphite, 0.08% tartaric acid
Potassium sodium and 0.08% cobalt chloride, and be added into portions of de-ionized water, mixing 10- be stirred at 50-60 DEG C
20min, until being uniformly mixed；
(2) 2.6% organic acid and 1.26% ethyl alcohol are added into mixed liquor obtained in step (1), and is cooled to
Mixed processing 60-80min is carried out at 45 DEG C ± 3 DEG C；
(3) deionized water is supplied, and the mixed solution after the completion of mixing is cooled to room temperature, obtains antioxidant.
Embodiment 6
The mixture of any one or more in formic acid, acetic acid, 1-hydroxy ethylidene-1,1-diphosphonic acid and propionic acid is as organic
Acid starting material, and select with alkyl, phenyl, alkylene, halogen, sulfonic monosubstituted polysubstituted or compound substituted benzo miaow
One of azoles or the mixture of multiple groups are as benzimidizole derivatives raw material.
A kind of preparation method of printed wiring board copper antioxidation agent, comprising the following steps:
(1) weigh respectively 0.65% hydrogen peroxide, 0.25% benzimidizole derivatives, 0.25% benzothiazole
Sodium, 0.36% sodium sulphate, 0.27% sodium molybdate, 0.36% potassium chloride, 0.08% sodium hypophosphite, 0.08% winestone
Sour potassium sodium and 0.08% cobalt chloride, and be added into portions of de-ionized water, mixing 10- be stirred at 50-60 DEG C
20min, until being uniformly mixed；
(2) 2.8% organic acid and 1.28% ethyl alcohol are added into mixed liquor obtained in step (1), and is cooled to
Mixed processing 60-80min is carried out at 45 DEG C ± 3 DEG C；
(3) deionized water is supplied, and the mixed solution after the completion of mixing is cooled to room temperature, obtains antioxidant.
Embodiment 7
The mixture of any one or more in formic acid, acetic acid, 1-hydroxy ethylidene-1,1-diphosphonic acid and propionic acid is as organic
Acid starting material, and select with alkyl, phenyl, alkylene, halogen, sulfonic monosubstituted polysubstituted or compound substituted benzo miaow
One of azoles or the mixture of multiple groups are as benzimidizole derivatives raw material.
A kind of preparation method of printed wiring board copper antioxidation agent, comprising the following steps:
(1) weigh respectively 0.7% hydrogen peroxide, 0.3% benzimidizole derivatives, 0.3% benzothiazole sodium,
0.4% sodium sulphate, 0.3% sodium molybdate, 0.4% potassium chloride, 0.1% sodium hypophosphite, 0.1% sodium potassium tartrate tetrahydrate and
0.1% cobalt chloride, and be added into portions of de-ionized water, mixing 10-20min is stirred at 50-60 DEG C, until mixed
It closes uniform；
(2) 3% organic acid and 1.13% ethyl alcohol are added into mixed liquor obtained in step (1), and is cooled to 45
Mixed processing 60-80min is carried out at DEG C ± 3 DEG C；
(3) deionized water is supplied, and the mixed solution after the completion of mixing is cooled to room temperature, obtains antioxidant.
Comparative example 1
A kind of preparation method of printed wiring board copper antioxidation agent, comprising the following steps:
(1) 0.55% hydrogen peroxide, 0.19% benzothiazole sodium, 0.31% sodium sulphate, 0.21% are weighed respectively
Sodium molybdate, 0.29% potassium chloride, 0.075% sodium hypophosphite, 0.075% sodium potassium tartrate tetrahydrate and 0.075% chlorination
Cobalt, and be added into portions of de-ionized water, mixing 10-20min is stirred at 50-60 DEG C, until being uniformly mixed；
(2) 2.53% organic acid and 1.25% ethyl alcohol are added into mixed liquor obtained in step (1), and is cooled to
Mixed processing 60-80min is carried out at 45 DEG C ± 3 DEG C；
(3) deionized water is supplied, and the mixed solution after the completion of mixing is cooled to room temperature, obtains antioxidant.
Comparative example 2
A kind of preparation method of printed wiring board copper antioxidation agent, comprising the following steps:
(1) weigh respectively 0.55% hydrogen peroxide, 0.19% benzimidizole derivatives, 0.31% sodium sulphate,
0.21% sodium molybdate, 0.29% potassium chloride, 0.075% sodium hypophosphite, 0.075% sodium potassium tartrate tetrahydrate and 0.075%
Cobalt chloride, and be added into portions of de-ionized water, mixing 10-20min be stirred at 50-60 DEG C, until mixing is equal
It is even；
(2) 2.53% organic acid and 1.25% ethyl alcohol are added into mixed liquor obtained in step (1), and is cooled to
Mixed processing 60-80min is carried out at 45 DEG C ± 3 DEG C；
(3) deionized water is supplied, and the mixed solution after the completion of mixing is cooled to room temperature, obtains antioxidant.
Comparative example 3
A kind of preparation method of printed wiring board copper antioxidation agent, comprising the following steps:
(1) 0.55% hydrogen peroxide, 0.31% sodium sulphate, 0.21% sodium molybdate, 0.29% chlorine are weighed respectively
Change potassium, 0.075% sodium hypophosphite, 0.075% sodium potassium tartrate tetrahydrate and 0.075% cobalt chloride, and be added into part go
In ionized water, mixing 10-20min is stirred at 50-60 DEG C, until being uniformly mixed；
(2) 2.53% organic acid and 1.25% ethyl alcohol are added into mixed liquor obtained in step (1), and is cooled to
Mixed processing 60-80min is carried out at 45 DEG C ± 3 DEG C；
(3) deionized water is supplied, and the mixed solution after the completion of mixing is cooled to room temperature, obtains antioxidant.
The copper sheet surface that the copper antioxidation agent that above embodiments and comparative example are prepared is used in printed wiring board is resisted
Oxidation processes carry out the processing of 1-5min to copper sheet at normal temperature, and to treated, copper sheet is tested, and obtains following knot
Fruit:
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, without departing from the technical principles of the invention, several improvements and modifications, these improvements and modifications can also be made
Also it should be regarded as protection scope of the present invention.
Claims (6)
1. a kind of printed wiring board copper antioxidation agent, which is characterized in that the raw material including following ratio:
Organic acid 2-3%；
Ethyl alcohol 1.2-1.3%；
Hydrogen peroxidase 10 .4-0.7%；
Benzimidizole derivatives 0.1-0.3%；
Benzotriazole Derivative salt 0.1-0.3%；
Sodium sulphate 0.2-0.4%；
Sodium molybdate 0.1-0.3%；
Potassium chloride 0.2-0.4%；
Sodium hypophosphite 0.05-0.10%；
Sodium potassium tartrate tetrahydrate 0.05-0.10%；
Cobalt chloride 0.05-0.10%；
Deionized water surplus.
2. a kind of printed wiring board copper antioxidation agent as described in claim 1, which is characterized in that it is preferred, including with
The raw material of lower ratio:
Organic acid 2.45-2.6%；
Ethyl alcohol 1.24-1.26%；
Hydrogen peroxidase 10 .5-0.6%；
Benzimidizole derivatives 0.18-0.21%；
Benzotriazole Derivative salt 0.18-0.21%；
Sodium sulphate 0.29-0.32%；
Sodium molybdate 0.18-0.24%；
Potassium chloride 0.27-0.31%；
Sodium hypophosphite 0.07-0.08%；
Sodium potassium tartrate tetrahydrate 0.07-0.08%；
Cobalt chloride 0.07-0.08%；
Deionized water surplus.
3. a kind of printed wiring board copper antioxidation agent as described in any one of claim 1 and 2, which is characterized in that institute
Stating organic acid is the mixture of any one or more in formic acid, acetic acid, 1-hydroxy ethylidene-1,1-diphosphonic acid and propionic acid.
4. a kind of printed wiring board copper antioxidation agent as described in any one of claim 1 and 2, which is characterized in that institute
Stating benzimidizole derivatives is with alkyl, phenyl, alkylene, halogen, sulfonic monosubstituted polysubstituted or compound substituted
The mixture of one of benzimidazole or multiple groups.
5. a kind of printed wiring board copper antioxidation agent as described in any one of claim 1 and 2, which is characterized in that institute
Stating Benzotriazole Derivative salt is benzothiazole sodium.
6. a kind of preparation method of printed wiring board copper antioxidation agent, which comprises the following steps:
(1) hydrogen peroxide, benzimidizole derivatives, Benzotriazole Derivative salt, sodium sulphate, sodium molybdate, chlorination are weighed respectively
Potassium, sodium hypophosphite, sodium potassium tartrate tetrahydrate and cobalt chloride, and be added into portions of de-ionized water, it is stirred at 50-60 DEG C mixed
10-20min is closed, until being uniformly mixed；
(2) organic acid and ethyl alcohol are added into mixed liquor obtained in step (1), and is cooled at 45 DEG C ± 3 DEG C and is mixed
Handle 60-80min；
(3) deionized water is supplied, and the mixed solution after the completion of mixing is cooled to room temperature, obtains antioxidant.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910146009.6A CN109797384A (en) | 2019-02-27 | 2019-02-27 | A kind of printed wiring board copper antioxidation agent and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910146009.6A CN109797384A (en) | 2019-02-27 | 2019-02-27 | A kind of printed wiring board copper antioxidation agent and preparation method thereof |
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| Publication Number | Publication Date |
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| CN109797384A true CN109797384A (en) | 2019-05-24 |
Family
ID=66561387
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
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| CN201910146009.6A Pending CN109797384A (en) | 2019-02-27 | 2019-02-27 | A kind of printed wiring board copper antioxidation agent and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113737167A (en) * | 2021-09-22 | 2021-12-03 | 东莞市四辉表面处理科技有限公司 | Copper material antioxidant and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS57170592A (en) * | 1981-04-15 | 1982-10-20 | Nippon Denkai Kk | Copper foil for printed circuit |
| CN1955341A (en) * | 2005-10-25 | 2007-05-02 | 李碧洁 | Copper antioxidation agent suitable for multiple high temp leadless welding |
| CN101962766A (en) * | 2009-07-22 | 2011-02-02 | 深圳市正天伟科技有限公司 | Copper plated organic coating preparation for preventing copper surface from oxidation |
| CN104046996A (en) * | 2014-06-23 | 2014-09-17 | 梧州恒声电子科技有限公司 | Copper antioxidant and preparation method thereof |
| CN105671538A (en) * | 2016-01-08 | 2016-06-15 | 滁州嘉泰科技有限公司 | Compound organic solderability preservatives (OSP) treating agent for lead-free printed circuit board (PCB) |
-
2019
- 2019-02-27 CN CN201910146009.6A patent/CN109797384A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS57170592A (en) * | 1981-04-15 | 1982-10-20 | Nippon Denkai Kk | Copper foil for printed circuit |
| CN1955341A (en) * | 2005-10-25 | 2007-05-02 | 李碧洁 | Copper antioxidation agent suitable for multiple high temp leadless welding |
| CN101962766A (en) * | 2009-07-22 | 2011-02-02 | 深圳市正天伟科技有限公司 | Copper plated organic coating preparation for preventing copper surface from oxidation |
| CN104046996A (en) * | 2014-06-23 | 2014-09-17 | 梧州恒声电子科技有限公司 | Copper antioxidant and preparation method thereof |
| CN105671538A (en) * | 2016-01-08 | 2016-06-15 | 滁州嘉泰科技有限公司 | Compound organic solderability preservatives (OSP) treating agent for lead-free printed circuit board (PCB) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113737167A (en) * | 2021-09-22 | 2021-12-03 | 东莞市四辉表面处理科技有限公司 | Copper material antioxidant and preparation method thereof |
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