CN109252165A - A kind of preparation method for subtracting copper liquid subtracting copper composition and include the composition - Google Patents
A kind of preparation method for subtracting copper liquid subtracting copper composition and include the composition Download PDFInfo
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- CN109252165A CN109252165A CN201810901746.8A CN201810901746A CN109252165A CN 109252165 A CN109252165 A CN 109252165A CN 201810901746 A CN201810901746 A CN 201810901746A CN 109252165 A CN109252165 A CN 109252165A
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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
- 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
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- Organic Chemistry (AREA)
- Preventing Corrosion Or Incrustation Of Metals (AREA)
Abstract
The invention discloses a kind of preparation methods for subtracting copper liquid for subtracting copper composition and include the composition, of the invention subtracts copper composition by weight, by following material composition: 0-10 parts of cyclohexylamine, 0-6 parts of isopropylamine, 20-50 parts of glyoxaline compound, 30-70 parts of deionized water.The weight ratio for subtracting each substance in copper liquid of the invention is sulfuric acid: subtracting copper composition: hydrogen peroxide 10-30:10-30:50-150.Subtract copper liquid according to prepared by the present invention, and carry out subtracting Copper treatment according to the copper liquid that subtracts that the preparation method for subtracting copper liquid in invention obtains, subtract that copper is high-efficient, and by learning that each dot thickness of the wiring board after subtracting Copper treatment is uniform to 9 mensurations of wiring board.
Description
Technical field
The present invention relates to circuit board etching field, subtracts copper composition more particularly to a kind of and include subtracting for the composition
The preparation method of copper liquid.
Background technique
With advances in technology and requirement of the people to electronic product is higher and higher, thus it is higher to need wiring board to have
Integrated level.It quickly prints in order to ensure the accurate of wiring board, has been unable to satisfy by traditional wiring board printing technology
The requirement of the High precision and integrated level of circuit board.Wiring board printing process more common at present uses laser imaging, and right
The very high wiring board of accuracy is prepared after wiring board exposure, development and etching.Usually before being exposed to wiring board, need pair
Wiring board carries out pad pasting processing, and antiultraviolet film is sticked to complete subsequent exposure development operation in assist side surface.Thus, pad pasting
Technique influences wiring board processing quality very big.Since the difference in thickness of the original material surface each point of wiring board is larger, such as
Fruit, which is not pocessed, will will affect pad pasting effect.Thus, it carries out subtracting Copper treatment it is generally necessary to treat pad pasting wiring board in practice.
Copper liquid must be subtracted and completed using special by subtracting Copper treatment, preferably subtract copper liquid need targetedly by copper in wiring board from
Son is dissolved out, and is not simple corrosive liquid, and in ideal conditions, the PCB surface after subtracting Copper treatment should have
Certain roughness, this can guarantee the stability of subsequent pad pasting.However, improper if subtracting Copper treatment, it will cause route
Plate became uneven influences subsequent film coating process in turn, makes a big impact to wiring board quality.
Summary of the invention
There is provided one kind the present invention solves the technical problem of the present invention may be implemented uniformly to subtract copper effect and will not make
At PCB surface thickness have big difference subtract copper composition and include the composition the preparation method for subtracting copper liquid.
In order to solve the above technical problems, one technical scheme adopted by the invention is that: the present invention provides one kind to subtract copper group
Object is closed, by weight, by following material composition: 0-10 parts of cyclohexylamine, 0-6 parts of isopropylamine, glyoxaline compound 20-50
Part, 30-70 parts of deionized water.
Preferably, the glyoxaline compound includes I-hydroxybenzotriazole monohydrate, and 2,4- methylimidazoles, 5,6-
Dimethyl -1,2,3- benzotriazole hydrate, ethyl imidazol(e), ethylmethylimidazolium, hydroxyl benzimidazole and 1, in 2,4- triazoles
It is at least one.
Preferably, further including sulfuric acid.
Preferably, described subtracts copper composition, and by weight, by following material composition: 6-10 parts of cyclohexylamine, isopropyl
2-5 parts of amine, 2-5 parts of I-hydroxybenzotriazole monohydrate, 2,4- 3-7 parts of methylimidazoles, 5,6- dimethyl -1,2,3- benzo
2-5 parts of triazole hydrate, 2-4 parts of ethyl imidazol(e), 1-5 parts of ethylmethylimidazolium, 3-15 parts of hydroxyl benzimidazole, 1,2,4- triazole 7-
25 parts, 3-9 parts of sulfuric acid, 30-70 parts of deionized water.
Preferably, including the preparation method for subtracting copper liquid for subtracting copper composition, include the following steps:
(1) preparation subtracts copper liquid: each raw material for subtracting copper liquid in claim 1-4 is sequentially added in reaction kettle, is stirred evenly, it is standby
With；
(2) appropriate amount of deionized water is added into reaction kettle；
(3) 60% sulfuric acid V1 parts by volume is added into reaction kettle；
(4) step (1) is added into reaction kettle subtracts copper liquid V2 parts by volume, stirs evenly；
(5) 35% hydrogen peroxide V3 parts by volume is added into reaction kettle；
(6) CuSO is added into reaction kettle4·5H2O, and add pure water to 1000 parts by volume, CuSO in final system4·5H2O
Concentration is M g/L, is stirred evenly.
Preferably, the V1 is 10-30 parts by volume, the V2 is 10-30 parts by volume, and the V3 is 50-150 parts by volume,
The M is 10-50.
The beneficial effects of the present invention are: the copper liquid that subtracts for wiring board processing of the invention utilizes cyclohexylamine and isopropylamine
Its rate of etch to copper ion in wiring board is increased, in addition, of the invention subtracting in copper liquid formula is added to glyoxaline compound,
So that assist side surface forms one layer of cross-linked layer to ensure that PCB surface has centainly coarse when carrying out subtracting Copper treatment
Degree.According to the present invention to subtract the route plate thickness that copper liquid subtract after Copper treatment uniform, subtracts copper and works well.
Detailed description of the invention
To describe the technical solutions in the embodiments of the present invention more clearly, make required in being described below to embodiment
Attached drawing is briefly described, it should be apparent that, drawings in the following description are only some embodiments of the invention, for
For those of ordinary skill in the art, without creative efforts, it can also be obtained according to these attached drawings other
Attached drawing, in which:
Fig. 1 is subtracting the compound proportion for subtracting copper composition and sulfuric acid and hydrogen peroxide in copper liquid and subtracting copper effect for 1-6 of the embodiment of the present invention
Fruit assessment figure.
Specific embodiment
The technical scheme in the embodiments of the invention will be clearly and completely described below, it is clear that described implementation
Example is only a part of the embodiments of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is common
Technical staff's all other embodiment obtained without making creative work belongs to the model that the present invention protects
It encloses.
Of the invention subtracts copper composition for wiring board processing, and cyclohexylamine and isopropylamine is selected to increase it to copper
Etching efficiency subtracts in copper composite formula and selects glyoxaline compound that assist side surface is made to form copper crosslinking net layer, really
Protecting PCB surface has certain roughness.
The copper composition that subtracts of the invention is used in compounding when carrying out subtracting Copper treatment with sulfuric acid and hydrogen peroxide, sulfuric acid and double
Oxygen water and the compound proportion for subtracting copper liquid have larger impact to copper effect is subtracted.Meanwhile in order to reach subtract copper effect and subtract copper cost it
Between balance, it is determined that the preferable compound proportion for subtracting copper liquid Yu sulfuric acid and hydrogen peroxide of the invention.
The effect for subtracting copper liquid is determined to use following analysis method in the present invention:
Subtract the measurement test of copper rate: wiring board in homogeneous thickness being cleaned up, weight M is measured after drying1(kg), wiring board is measured
Length L(m), the width W(m of wiring board), under 30 degrees Celsius, after PCB surface in homogeneous thickness is sprayed above-mentioned compounding
Subtract Copper treatment liquid, after processing 1 minute, measure weight M with after drying after clear water irrigation lines plate surface2(kg), according to following
Formula calculating subtracts copper rate:
Subtract copper rate (micron)=(M1- M2)×10000/(L×W×8.92×2)。
Subtract copper effect test: subtracting the test of Copper treatment rear board the thickness uniformity: the wiring board by subtracting Copper treatment is adopted
The thickness of 9 side amount wiring boards is uniformly chosen in the circuit board using CMI measuring instrument with 9 mensurations.It is being tested
When, it is averaged after selecting 10 wiring boards to be handled.
For the content that the present invention will be described in detail, it is as follows now to enumerate embodiment:
Embodiment 1
Each substance in copper composite formula that subtracts of the present embodiment by weight, is prepared according to the following formulation: 6 parts of isopropylamine,
2 parts of I-hydroxybenzotriazole monohydrate, 2,4- 3 parts of methylimidazoles, 5,6- dimethyl -1,2,3- benzotriazole hydrate 2
Part, 2 parts of ethyl imidazol(e), 1 part of ethylmethylimidazolium, 3 parts of hydroxyl benzimidazole, 1,2,4- 7 parts of triazole, 3 parts of sulfuric acid, deionized water
30 parts.
The preparation method for subtracting copper liquid of the present embodiment carries out as follows:
(1) preparation subtracts copper composition: each raw material for subtracting copper composition is sequentially added in A reaction kettle, is stirred evenly, it is spare；
(2) appropriate amount of deionized water is added into B reaction kettle；
(3) 60% sulfuric acid, 10 parts by volume is added into B reaction kettle；
(4) step (1) is added into B reaction kettle subtracts 10 parts by volume of copper liquid, stirs evenly；
(5) 35% 50 parts by volume of hydrogen peroxide is added into B reaction kettle；
(6) CuSO is added into B reaction kettle4·5H2O, and add pure water to 1000 parts by volume, CuSO in final system4·5H2O
Addition concentration is 10 g/L, is stirred evenly.
Embodiment 2
Each substance in copper composite formula that subtracts of the present embodiment by weight, is prepared according to the following formulation: 3 parts of cyclohexylamine,
5 parts of isopropylamine, 3 parts of I-hydroxybenzotriazole monohydrate, 2,4- 4 parts of methylimidazoles, 5,6- dimethyl -1,2,3- benzo
3 parts of triazole hydrate, 3 parts of ethyl imidazol(e), 3 parts of ethylmethylimidazolium, 5 parts of hydroxyl benzimidazole, 1,2,4- 25 parts of triazole, sulfuric acid
5 parts, 45 parts of deionized water.
The preparation method for subtracting copper liquid of the present embodiment carries out as follows:
(1) preparation subtracts copper composition: each raw material for subtracting copper liquid is sequentially added in A reaction kettle, is stirred evenly, it is spare；
(2) appropriate amount of deionized water is added into B reaction kettle；
(3) 60% sulfuric acid, 15 parts by volume is added into B reaction kettle；
(4) step (1) is added into B reaction kettle subtracts 16 parts by volume of copper liquid, stirs evenly；
(5) 35% 70 parts by volume of hydrogen peroxide is added into B reaction kettle；
(6) CuSO is added into B reaction kettle4·5H2O, and add pure water to 100 parts by volume, CuSO in final system4·5H2O
Addition concentration is 20 g/L, is stirred evenly.
Embodiment 3
Each substance in copper composite formula that subtracts of the present embodiment by weight, is prepared according to the following formulation: 5 parts of cyclohexylamine,
4 parts of isopropylamine, 5 parts of I-hydroxybenzotriazole monohydrate, 2,4- 6 parts of methylimidazoles, 5,6- dimethyl -1,2,3- benzo
4 parts of triazole hydrate, 4 parts of ethyl imidazol(e), 4 parts of ethylmethylimidazolium, 7 parts of hydroxyl benzimidazole, 1,2,4- 15 parts of triazole, sulfuric acid
6 parts, 60 parts of deionized water.
The preparation method for subtracting copper liquid of the present embodiment carries out as follows:
(1) preparation subtracts copper composition: each raw material for subtracting copper liquid is sequentially added in A reaction kettle, is stirred evenly, it is spare；
(2) appropriate amount of deionized water is added into B reaction kettle；
(3) 60% sulfuric acid, 20 parts by volume is added into B reaction kettle；
(4) step (1) is added into B reaction kettle subtracts 22 parts by volume of copper liquid, stirs evenly；
(5) 35% 90 parts by volume of hydrogen peroxide is added into B reaction kettle；
(6) CuSO is added into B reaction kettle4·5H2O, and add pure water to 1000 parts by volume, CuSO in final system4·5H2O
Addition concentration is 30 g/L, is stirred evenly.
Embodiment 4
Each substance in copper composite formula that subtracts of the present embodiment by weight, is prepared according to the following formulation: 6 parts of cyclohexylamine,
3 parts of isopropylamine, 2 parts of I-hydroxybenzotriazole monohydrate, 2,4- 7 parts of methylimidazoles, 5,6- dimethyl -1,2,3- benzo
5 parts of triazole hydrate, 3 parts of ethyl imidazol(e), 5 parts of ethylmethylimidazolium, 10 parts of hydroxyl benzimidazole, 1,2,4- 18 parts of triazole, sulfuric acid
7 parts, 70 parts of deionized water.
The preparation method for subtracting copper liquid of the present embodiment carries out as follows:
(1) preparation subtracts copper composition: each raw material for subtracting copper liquid is sequentially added in A reaction kettle, is stirred evenly, it is spare；
(2) appropriate amount of deionized water is added into B reaction kettle；
(3) 60% sulfuric acid, 28 parts by volume is added into B reaction kettle；
(4) step (1) is added into B reaction kettle subtracts 22 parts by volume of copper liquid, stirs evenly；
(5) 35% 110 parts by volume of hydrogen peroxide is added into B reaction kettle；
(6) CuSO is added into B reaction kettle4·5H2O, and add pure water to 1000 parts by volume, CuSO in final system4·5H2O
Addition concentration is 40 g/L, is stirred evenly.
Embodiment 5
Each substance in copper composite formula that subtracts of the present embodiment by weight, is prepared according to the following formulation: 8 parts of cyclohexylamine,
2 parts of isopropylamine, 3 parts of I-hydroxybenzotriazole monohydrate, 2,4- 5 parts of methylimidazoles, 5,6- dimethyl -1,2,3- benzo
5 parts of triazole hydrate, 2 parts of ethyl imidazol(e), 3 parts of ethylmethylimidazolium, 11 parts of hydroxyl benzimidazole, 1,2,4- 21 parts of triazole, sulfuric acid
8 parts, 70 parts of deionized water.
The preparation method for subtracting copper liquid of the present embodiment carries out as follows:
(1) preparation subtracts copper composition: each raw material for subtracting copper liquid is sequentially added in A reaction kettle, is stirred evenly, it is spare；
(2) appropriate amount of deionized water is added into B reaction kettle；
(3) 60% sulfuric acid, 30 parts by volume is added into B reaction kettle；
(4) step (1) is added into B reaction kettle subtracts 30 parts by volume of copper liquid, stirs evenly；
(5) 35% 130 parts by volume of hydrogen peroxide is added into B reaction kettle；
(6) CuSO is added into B reaction kettle4·5H2O, and add pure water to 1000 parts by volume, CuSO in final system4·5H2O
Addition concentration is 50 g/L, is stirred evenly.
Embodiment 6
Each substance in copper composite formula that subtracts of the present embodiment by weight, is prepared according to the following formulation: 10 parts of cyclohexylamine,
1 part of isopropylamine, 4 parts of I-hydroxybenzotriazole monohydrate, 2,4- 6 parts of methylimidazoles, 5,6- dimethyl -1,2,3- benzo
3 parts of triazole hydrate, 4 parts of ethyl imidazol(e), 2 parts of ethylmethylimidazolium, 15 parts of hydroxyl benzimidazole, 1,2,4- 12 parts of triazole, sulfuric acid
9 parts, 55 parts of deionized water.
The preparation method for subtracting copper liquid of the present embodiment carries out as follows:
(1) preparation subtracts copper composition: each raw material for subtracting copper liquid is sequentially added in A reaction kettle, is stirred evenly, it is spare；
(2) appropriate amount of deionized water is added into B reaction kettle；
(3) 60% sulfuric acid, 23 parts by volume is added into B reaction kettle；
(4) step (1) is added into B reaction kettle subtracts 25 parts by volume of copper liquid, stirs evenly；
(5) 35% 150 parts by volume of hydrogen peroxide is added into B reaction kettle；
(6) CuSO is added into B reaction kettle4·5H2O, and add pure water to 1000 parts by volume, CuSO in final system4·5H2O
Addition concentration is 35 g/L, is stirred evenly.
The formula composition for subtracting copper composition in embodiment 1-6 is as shown in table 1, and subtracting for embodiment 1-6 subtracts copper combination in copper liquid
The compound proportion of object and sulfuric acid and hydrogen peroxide and to subtract copper recruitment evaluation as shown in Table 2 and Fig. 1.
1 embodiment 1-6's of table subtracts copper composite formula composition table
Subtract the compound proportion of copper composition and sulfuric acid and hydrogen peroxide in 2 various embodiments of the present invention of table and subtracts copper recruitment evaluation
The copper that subtracts for subtracting copper liquid in various embodiments of the present invention works well, and 1 minutes only need to be acted on copper sheet can make to subtract
Copper rate reaches 12 microns or more, and by learning to 9 mensurations of wiring board, each dot thickness phase of the wiring board after subtracting Copper treatment
It is poor little.
The above description is only an embodiment of the present invention, is not intended to limit the scope of the invention, all to utilize this hair
Equivalent structure or equivalent flow shift made by bright description is applied directly or indirectly in other relevant technology necks
Domain is included within the scope of the present invention.
Claims (6)
1. one kind subtracts copper composition, by weight, by following material composition: 0-10 parts of cyclohexylamine, 0-6 parts of isopropylamine, imidazoles
20-50 parts of class compound, 30-70 parts of deionized water.
2. according to claim 1 subtract copper composition, which is characterized in that the glyoxaline compound includes 1- hydroxy benzo
Triazole monohydrate, 2,4- methylimidazoles, 5,6- dimethyl -1,2,3- benzotriazole hydrate, ethyl imidazol(e), ethyl-methyl
Imidazoles, hydroxyl benzimidazole and 1, at least one of 2,4- triazoles.
3. according to claim 2 subtract copper composition, which is characterized in that further include sulfuric acid.
4. according to claim 3 subtract copper composition, by weight, by following material composition: 6-10 parts of cyclohexylamine,
2-5 parts of isopropylamine, 2-5 parts of I-hydroxybenzotriazole monohydrate, 2,4- 3-7 parts of methylimidazoles, 5,6- dimethyl -1,2,3-
2-5 parts of benzotriazole hydrate, 2-4 parts of ethyl imidazol(e), 1-5 parts of ethylmethylimidazolium, 3-15 parts of hydroxyl benzimidazole, 1,2,4- tri-
7-25 parts of azoles, 3-9 parts of sulfuric acid, 30-70 parts of deionized water.
5. comprising just like the preparation side for subtracting copper liquid for subtracting copper composition described in any one of claim 1-4 claim
Method, which comprises the steps of:
(1) preparation subtracts copper liquid: each raw material for subtracting copper liquid in claim 1-4 is sequentially added in reaction kettle, is stirred evenly, it is standby
With；
(2) appropriate amount of deionized water is added into reaction kettle；
(3) 60% sulfuric acid V1 parts by volume is added into reaction kettle；
(4) step (1) is added into reaction kettle subtracts copper liquid V2 parts by volume, stirs evenly；
(5) 35% hydrogen peroxide V3 parts by volume is added into reaction kettle；
(6) CuSO is added into reaction kettle4·5H2O, and add pure water to 1000 parts by volume, CuSO in final system4·5H2O is dense
Degree is M g/L, is stirred evenly.
6. the preparation method according to claim 5 for subtracting copper liquid, which is characterized in that the V1 is 10-30 parts by volume, described
V2 is 10-30 parts by volume, and the V3 is 50-150 parts by volume, and the M is 10-50.
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| CN201810901746.8A CN109252165A (en) | 2018-08-09 | 2018-08-09 | A kind of preparation method for subtracting copper liquid subtracting copper composition and include the composition |
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| CN201810901746.8A CN109252165A (en) | 2018-08-09 | 2018-08-09 | A kind of preparation method for subtracting copper liquid subtracting copper composition and include the composition |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111148378A (en) * | 2020-01-09 | 2020-05-12 | 深圳市景旺电子股份有限公司 | Manufacturing method of local thick copper plate |
| 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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| CN1324959A (en) * | 1999-10-29 | 2001-12-05 | 希普雷公司 | Supplement method for bath |
| CN107151795A (en) * | 2017-06-02 | 2017-09-12 | 苏州晶瑞化学股份有限公司 | A kind of copper-molybdenum alloy film etching solution |
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2018
- 2018-08-09 CN CN201810901746.8A patent/CN109252165A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1324959A (en) * | 1999-10-29 | 2001-12-05 | 希普雷公司 | Supplement method for bath |
| CN107151795A (en) * | 2017-06-02 | 2017-09-12 | 苏州晶瑞化学股份有限公司 | A kind of copper-molybdenum alloy film etching solution |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111148378A (en) * | 2020-01-09 | 2020-05-12 | 深圳市景旺电子股份有限公司 | Manufacturing method of local thick copper plate |
| CN111148378B (en) * | 2020-01-09 | 2021-04-06 | 深圳市景旺电子股份有限公司 | Manufacturing method of local thick copper plate |
| 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 |
| CN114686885B (en) * | 2022-06-02 | 2022-08-19 | 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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