CN110093637A - For flexibility coat copper plate, the electrolytic copper foil of flexible printed-circuit board and preparation method - Google Patents
For flexibility coat copper plate, the electrolytic copper foil of flexible printed-circuit board and preparation method Download PDFInfo
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- CN110093637A CN110093637A CN201910500393.5A CN201910500393A CN110093637A CN 110093637 A CN110093637 A CN 110093637A CN 201910500393 A CN201910500393 A CN 201910500393A CN 110093637 A CN110093637 A CN 110093637A
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- copper foil
- electrolytic copper
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- circuit board
- flexible printed
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D1/00—Electroforming
- C25D1/04—Wires; Strips; Foils
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
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- Organic Chemistry (AREA)
- Electroplating And Plating Baths Therefor (AREA)
- Electroplating Methods And Accessories (AREA)
Abstract
The present invention relates to a kind of electrolytic copper foils and preparation method thereof, for flexibility coat copper plate, flexible printed-circuit board, electrolytic copper foil room temperature tensile strength is 350MPa or more, room temperature elongation percentage >=6%, tensile strength is greater than elongation percentage >=10% after 300MPa, heating after electrolytic copper foil heating, electrolytic copper foil hair side roughness Rz≤2.0 μm, electrolytic copper foil glossiness are 100-500.Electrolytic copper foil produced by the invention has lower profile, and surface microstructure is smooth, and tensile strength and elongation percentage can reach the processing request as flexible print wiring board basis material.
Description
Technical field
The present invention relates to flexible electrolytic copper foil manufacturing technology fields, it particularly relates to a kind of electrolytic copper foil and its preparation
Method.
Background technique
In recent years, since the fast development of electronic technology, electronics and electrical instrument are gradually sent out to light, thin, short, smallization direction
Exhibition.Therefore, printed wiring board is put forward new requirements, flexible print wiring board is with soft, light, thin and flexibility is special
Point is widely used at present in the electronic products such as aerospace, mobile phone laptop, LCD TV.As flexible printing
The conductor material of circuit board and flexibility coat copper plate, also there is specific requirement to electrolytic copper foil.In general, flexible print wiring board electricity consumption
Solution copper foil should have compared with low profile, and higher ductility, low roughness and higher tensile strength only meet these characteristics
It is corresponding with miniaturization and high performance to be just able to satisfy formation in limited mounting space on a printed-wiring board for electrolytic copper foil
Circuit.
To obtain compared with high-tensile and compared with the electrolytic copper foil of low profile and surface roughness, need by specific addition
Agent, different additives play different effects during electro-deposition.It is to promote the copper foil crystal grain center of area raw such as leveling agent
Long a kind of additive；Brightener is that copper foil hair side (face M) is promoted to play bright a kind of additive rapidly；Inhibitor is also called off
Position agent, is to aid in other functional additives and is attached to a kind of auxiliary additive of cathode roller surface everywhere.Different additives are pressed
It combines, plays the role of to the intensity of copper foil, hardness and smooth sense vital according to different ratios.
Existing electrolytic copper foil can't meet well compared with low profile, higher ductility, low roughness and compared with highly resistance
The characteristic of tensile strength.
For the problems in the relevant technologies, currently no effective solution has been proposed.
Summary of the invention
For above-mentioned technical problem in the related technology, the present invention proposes a kind of electrolytic copper foil and preparation method thereof, can
Overcome the above-mentioned deficiency of the prior art.
To realize the above-mentioned technical purpose, the technical scheme of the present invention is realized as follows:
It is a kind of for flexibility coat copper plate, the electrolytic copper foil of flexible printed-circuit board, for flexibility coat copper plate, flexible printing electricity
Road plate, the electrolytic copper foil room temperature tensile strength is 350MPa or more, room temperature elongation percentage >=6%, after the electrolytic copper foil heating
Tensile strength is greater than elongation percentage >=10% after 300MPa, heating, electrolytic copper foil hair side roughness Rz≤2.0 μm, the electricity
Solution copper foil glossiness is 100-500.
Preferably, the condition of the heating is 150 DEG C, 30 minutes.
A kind of preparation side for flexibility coat copper plate, the electrolytic copper foil of flexible printed-circuit board as described in claim 1
Method, comprising the following steps:
S1, the pot for smelted copper containing sulfuric acid is added in copper, prepares main electrolyte；
S2, main electrolyte are mixed to get electrolyte after multistage filtering with additive, and the additive includes A agent, B agent, C
Agent, chloride ion, the A agent be nitrogen-containing heterocycle compound containing sulfydryl, the B agent be organic divalent sulfur compound, the C agent be containing
Nitrogenous natural or synthetic high-molecular compound, copper ion in the electrolyte, sulfuric acid, chloride ion, A agent, B agent, C agent concentration point
It Wei not 50-100g/L, 80-140g/L, 20-100mg/L, 1-50mg/L, 3-70mg/L, 5-70mg/L；
S3, electrolyte is squeezed into electrolytic cell after heat exchanger exchanges heat to certain temperature；
S4, temperature be 30-70 DEG C, current density 30-85A/dm2In the environment of carry out electrolytic preparation original foil；
S5, post-processing is carried out to former foil, obtains finished product.
Preferably, this method is suitable for the production of 9-20 μm of electrolytic copper foil.
Preferably, in S3 step, electrolysis cathode is seamless roller formula titanium roller, and anode electrolytic cell is dimensionally stable anode.
Preferably, the A agent be 2- mercaptobenzoxazole, 2-mercaptobenzimidazole, 2- sulfydryl -5- benzimidazole sulfonic acid or
One or more mixtures of person its salt, 2-mercaptobenzothiazole.
Preferably, the B agent is 3-sulfydryl-1-propane sulfonic acid sodium, sodium polydithio-dipropyl sulfonate, mercapto propane sulfonic acid
The mixture of one or more of sodium.
Preferably, the C agent is one or more mixtures of collagen, polyethyleneimine, polyethers ammonia.
Preferably, the content of A agent is 1-15mg/L in the electrolyte.
Preferably, the S5 step specifically: after the former foil surface treated of preparation, using copper foil as cathode, through one
Serial plating bath plates various metals film cuts into the finished product of different wide cuts using drying after winding.
Beneficial effects of the present invention: the organic additive of certain content is added in foil process, controls initial nucleus number
Amount and grain growth direction, effectively improve flexibility, ductility, reduce roughness.It is surface-treated by high-chemical-resistance
Technology, by the way that minor metallic element is electroplated, improves high temperature chemical-resistance, makes copper foil no matter normal in surface treatment procedure
Peel strength all with higher under temperature or high temperature, meets the processing request of flexible print wiring board.
The electrolytic copper foil of additive compound technology and production technology through the invention, production has lower profile, table
Face crystal grain is smooth, and tensile strength and elongation percentage can reach the processing request as flexible print wiring board basis material.
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 embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is common
Technical staff's every other embodiment obtained, shall fall within the protection scope of the present invention.
A kind of electrolytic copper foil according to embodiments of the present invention, room temperature tensile strength are that can reach 350MPa or more, are added
Hot (150 DEG C, 30 minutes) tensile strength is greater than 300MPa (the 85% of room temperature tensile strength value) afterwards；Room temperature elongation percentage >=6%, adds
(150 DEG C, 30 minutes) elongation percentage >=10% after heat；Hair side roughness Rz≤2.5 μm, glossiness 100-500.The following are the electrolysis
The embodiment of the specific preparation method of copper foil.
Embodiment 1
Metal copper simple substance is added in the pot for smelted copper containing sulfuric acid, high temperature air is blasted with screw rod blower, by copper dissolution system
The standby main electrolyte of acid copper sulfate, main electrolyte are mixed to get electrolyte, gained electrolysis after multistage filtering with additive solution
In liquid, the composition of copper ion concentration 85g/L, acid content 100g/L, other additives are:
2-mercaptobenzimidazole: 2mg/L；
3-sulfydryl-1-propane sulfonic acid sodium: 30mg/L；
Collagen (number-average molecular weight 3000-5000): 20mg/L；
Polyethyleneimine (category molecular weight 3000): 10mg/L；
Chloride ion: 25mg/L；
Above-mentioned electrolyte exchanges heat through heat exchanger to 50 DEG C, squeezes into electrolytic cell.Electric tank cathode is seamless roller formula titanium roller, sun
Extremely size limits anode.In 55A/dm2Current density under, in 50 DEG C of progress electrolytic preparation original foils, former foil surface treated
Machine, through a series of plating bath plates various metals films, using drying, cuts into different width using copper foil as cathode after winding
The finished product of width.
Embodiment 2
Metal copper simple substance is added in the pot for smelted copper containing sulfuric acid, high temperature air is blasted with screw rod blower, by copper dissolution system
The standby main electrolyte of acid copper sulfate, main electrolyte are mixed to get electrolyte, gained electrolysis after multistage filtering with additive solution
In liquid, the composition of copper ion concentration 85g/L, acid content 100g/L, other additives are:
2-mercaptobenzimidazole: 2mg/L；
Sodium polydithio-dipropyl sulfonate: 17mg/L；
Collagen (number-average molecular weight 3000-5000): 22mg/L；
Polyethyleneimine (category molecular weight 3000): 15mg/L；
Chloride ion: 30mg/L；
Above-mentioned electrolyte exchanges heat through heat exchanger to 50 DEG C, squeezes into electrolytic cell.Electric tank cathode is seamless roller formula titanium roller, sun
Extremely size limits anode.In 60A/dm2Current density under, in 50 DEG C of progress electrolytic preparation original foils, former foil surface treated
Machine, through a series of plating bath plates various metals films, using drying, cuts into different width using copper foil as cathode after winding
The finished product of width.
Embodiment 3
Metal copper simple substance is added in the pot for smelted copper containing sulfuric acid, high temperature air is blasted with screw rod blower, by copper dissolution system
The standby main electrolyte of acid copper sulfate, main electrolyte are mixed to get electrolyte, gained electrolysis after multistage filtering with additive solution
In liquid, the composition of copper ion concentration 85g/L, acid content 100g/L, other additives are:
2- sulfydryl -5- benzimidazole sulfonic acid: 1mg/L；
Sodium polydithio-dipropyl sulfonate: 17mg/L；
Collagen (number-average molecular weight 3000-5000): 25mg/L；
Polyethyleneimine (category molecular weight 3000): 20mg/L；
Chloride ion: 35mg/L；
Above-mentioned electrolyte exchanges heat through heat exchanger to 50 DEG C, squeezes into electrolytic cell.Electric tank cathode is seamless roller formula titanium roller, sun
Extremely size limits anode.In 60A/dm2Current density under, in 50 DEG C of progress electrolytic preparation original foils, former foil surface treated
Machine, through a series of plating bath plates various metals films, using drying, cuts into different width using copper foil as cathode after winding
The finished product of width.
Embodiment 4
Metal copper simple substance is added in the pot for smelted copper containing sulfuric acid, high temperature air is blasted with screw rod blower, by copper dissolution system
The standby main electrolyte of acid copper sulfate, main electrolyte are mixed to get electrolyte, gained electrolysis after multistage filtering with additive solution
In liquid, the composition of copper ion concentration 85g/L, acid content 100g/L, other additives are:
2-mercaptobenzothiazole: 2mg/L；
Sodium polydithio-dipropyl sulfonate: 20mg/L；
Collagen (number-average molecular weight 3000-5000): 25mg/L；
Polyethyleneimine (category molecular weight 3000): 20mg/L；
Chloride ion: 35mg/L；
Above-mentioned electrolyte exchanges heat through heat exchanger to 50 DEG C, squeezes into electrolytic cell.Electric tank cathode is seamless roller formula titanium roller, sun
Extremely size limits anode.In 60A/dm2Current density under, in 50 DEG C of progress electrolytic preparation original foils, former foil surface treated
Machine, through a series of plating bath plates various metals films, using drying, cuts into different width using copper foil as cathode after winding
The finished product of width.
Embodiment 5
Metal copper simple substance is added in the pot for smelted copper containing sulfuric acid, high temperature air is blasted with screw rod blower, by copper dissolution system
The standby main electrolyte of acid copper sulfate, main electrolyte are mixed to get electrolyte, gained electrolysis after multistage filtering with additive solution
In liquid, the composition of copper ion concentration 85g/L, acid content 100g/L, other additives are:
2- mercaptobenzoxazole: 2mg/L；
Sodium polydithio-dipropyl sulfonate: 20mg/L；
Collagen (number-average molecular weight 3000-5000): 25mg/L；
Polyethyleneimine (category molecular weight 3000): 20mg/L；
Chloride ion: 35mg/L；
Above-mentioned electrolyte exchanges heat through heat exchanger to 50 DEG C, squeezes into electrolytic cell.Electric tank cathode is seamless roller formula titanium roller, sun
Extremely size limits anode.In 60A/dm2Current density under, in 50 DEG C of progress electrolytic preparation original foils, former foil surface treated
Machine, through a series of plating bath plates various metals films, using drying, cuts into different width using copper foil as cathode after winding
The finished product of width.
The following are the reference examples of above-described embodiment.
Reference examples 1
Electrolytic copper foil is prepared using method same as Example 2, in addition to changing collagen into hydroxyethyl cellulose,
His parameter constant.
Reference examples 2
Electrolytic copper foil is prepared using method same as Example 3, in addition to changing collagen into hydroxyethyl cellulose,
His parameter constant.
Reference examples 3
Electrolytic copper foil is prepared using method same as Example 4, in addition to changing collagen into hydroxyethyl cellulose,
His parameter constant.
Embodiment 6
Embodiment 6 is tested the Fundamental Physical Properties of the embodiment 1-5 and reference examples 1-3 electrolytic copper foil prepared,
Fundamental Physical Properties test method is as follows:
Glossiness test: it according to test method GB/T 13891, is manufactured using Ke Shida photoelectric instrument Co., Ltd
WGG60-EJ vancometer measures the glossiness of the face copper foil M length direction under the conditions of 60 ° of angle of light.
Tensile strength and elongation percentage test: according to test method GB/T29847-2013, Shanghai weighing apparatus wing precision instrument is used
The HY-0230 universal testing machine of Co., Ltd's manufacture is tested the tensile strength of copper foil under the conditions of room temperature (about 25 DEG C) and is prolonged
Stretch rate.
Roughness test (Rz, 10 roughness averages): according to test method GB/T29847-2013, when using Beijing
The TR200 roughmeter of Dai Ruida Science and Technology Ltd. manufacture, tests the roughness Rz value in the face copper foil M.
After tested, the Fundamental Physical Properties test result of the electrolytic copper foil of embodiment 1-5 and reference examples 1-3 preparation is shown in Table 1:
Table 1: the performance test results of electrolytic copper foil
As shown in table 1, the flexible electrolytic copper foil of the technical matters preparation provided according to the present invention has good physical
Can, both tensile strength and elongation percentage can control in the reasonable scope.Meanwhile hair side roughness and glossiness also can reach and answer
Use demand.Comparative example 2-4 and reference examples 1-3 is it is found that A class additive and the compatible use of C class additive are raw to control nucleus
Long, the performance for taking into account tensile strength and elongation percentage is most important, has preferable adjustment effect to the copper foil obtained compared with low profile.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Within mind and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of for flexibility coat copper plate, the electrolytic copper foil of flexible printed-circuit board, which is characterized in that the electrolytic copper foil room temperature
Tensile strength is 350MPa or more, room temperature elongation percentage >=6%, and tensile strength is greater than 300MPa, heating after the electrolytic copper foil heating
Elongation percentage >=10% afterwards, electrolytic copper foil hair side roughness Rz≤2.0 μm, the electrolytic copper foil glossiness are 100-500.
2. according to claim 1 a kind of for flexibility coat copper plate, the electrolytic copper foil of flexible printed-circuit board, feature exists
In the condition of the heating is 150oC, 30 minutes.
3. a kind of preparation method for flexibility coat copper plate, the electrolytic copper foil of flexible printed-circuit board as described in claim 1,
Characterized by comprising the following steps:
S1, the pot for smelted copper containing sulfuric acid is added in copper, prepares main electrolyte；
S2, main electrolyte are mixed to get electrolyte after multistage filtering with additive, the additive include A agent, B agent, C agent,
Chloride ion, the A agent are nitrogen-containing heterocycle compound containing sulfydryl, and the B agent is organic divalent sulfur compound, and the C agent is containing containing
The natural or synthetic high-molecular compound of nitrogen, copper ion in the electrolyte, sulfuric acid, chloride ion, A agent, B agent, C agent concentration difference
For 50-100 g/L, 80-140 g/L, 20-100 mg/L, 1-50 mg/L, 3-70 mg/L, 5-70 mg/L；
S3, electrolyte is squeezed into electrolytic cell after heat exchanger exchanges heat to certain temperature；
S4, temperature be 30-70oC, current density is 30-85 A/dm2In the environment of carry out electrolytic preparation original foil；
S5, post-processing is carried out to former foil, obtains finished product.
4. a kind of preparation side for flexibility coat copper plate, the electrolytic copper foil of flexible printed-circuit board according to claim 3
Method, which is characterized in that this method is the production method of 9-20 μm of electrolytic copper foil.
5. a kind of preparation side for flexibility coat copper plate, the electrolytic copper foil of flexible printed-circuit board according to claim 3
Method, which is characterized in that in S3 step, electrolysis cathode is seamless roller formula titanium roller, and anode electrolytic cell is dimensionally stable anode.
6. a kind of preparation side for flexibility coat copper plate, the electrolytic copper foil of flexible printed-circuit board according to claim 3
Method, which is characterized in that the A agent be 2- mercaptobenzoxazole, 2-mercaptobenzimidazole, 2- sulfydryl -5- benzimidazole sulfonic acid or
One or more mixtures of person its salt, 2-mercaptobenzothiazole.
7. a kind of preparation side for flexibility coat copper plate, the electrolytic copper foil of flexible printed-circuit board according to claim 3
Method, which is characterized in that the B agent is 3-sulfydryl-1-propane sulfonic acid sodium, sodium polydithio-dipropyl sulfonate, mercapto propane sulfonic acid
The mixture of one or more of sodium.
8. a kind of preparation side for flexibility coat copper plate, the electrolytic copper foil of flexible printed-circuit board according to claim 3
Method, which is characterized in that the C agent is one or more mixtures of collagen, polyethyleneimine, polyethers ammonia.
9. a kind of preparation side for flexibility coat copper plate, the electrolytic copper foil of flexible printed-circuit board according to claim 3
Method, which is characterized in that the content of A agent is 1-15 mg/L in the electrolyte.
10. a kind of preparation side for flexibility coat copper plate, the electrolytic copper foil of flexible printed-circuit board according to claim 3
Method, which is characterized in that the S5 step specifically: after the former foil surface treated of preparation, using copper foil as cathode, through a system
Column plating bath plates various metals film cuts into the finished product of different wide cuts using drying after winding.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110453252A (en) * | 2019-08-27 | 2019-11-15 | 安徽铜冠铜箔有限公司 | A kind of manufacturing method of high-frequency high-speed copper-clad plate HVLP copper foil |
| CN111235605A (en) * | 2020-02-24 | 2020-06-05 | 江西铜业集团有限公司 | Additive for ultralow-profile electrolytic copper foil and process for preparing electrolytic copper foil |
| CN111270273A (en) * | 2020-02-24 | 2020-06-12 | 江西铜业集团有限公司 | Additive for high-tensile electrolytic copper foil and process for preparing high-tensile electrolytic copper foil |
| CN112195487A (en) * | 2020-09-18 | 2021-01-08 | 九江德福科技股份有限公司 | Manufacturing method for improving tensile strength of light and thin copper foil |
| CN112323102A (en) * | 2020-11-04 | 2021-02-05 | 湖南龙智新材料科技有限公司 | Electrolytic copper foil for FPC and preparation method thereof |
| CN112553659A (en) * | 2020-11-09 | 2021-03-26 | 九江德福科技股份有限公司 | Manufacturing method of high-modulus copper foil |
| CN113337856A (en) * | 2021-05-24 | 2021-09-03 | 中国恩菲工程技术有限公司 | Additive for double-sided photoelectric copper foil and preparation method of copper foil |
| CN113652718A (en) * | 2021-08-27 | 2021-11-16 | 安徽华威铜箔科技有限公司 | Preparation method of 3-micron electrolytic copper foil additive, product and application thereof |
| CN114318428A (en) * | 2021-12-16 | 2022-04-12 | 九江德福科技股份有限公司 | Preparation method of flexible electrolytic copper foil |
| CN114703515A (en) * | 2022-04-14 | 2022-07-05 | 中国科学院金属研究所 | Copper foil and preparation method thereof, and circuit board and current collector |
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| CN110453252A (en) * | 2019-08-27 | 2019-11-15 | 安徽铜冠铜箔有限公司 | A kind of manufacturing method of high-frequency high-speed copper-clad plate HVLP copper foil |
| CN111235605A (en) * | 2020-02-24 | 2020-06-05 | 江西铜业集团有限公司 | Additive for ultralow-profile electrolytic copper foil and process for preparing electrolytic copper foil |
| CN111270273A (en) * | 2020-02-24 | 2020-06-12 | 江西铜业集团有限公司 | Additive for high-tensile electrolytic copper foil and process for preparing high-tensile electrolytic copper foil |
| CN112195487A (en) * | 2020-09-18 | 2021-01-08 | 九江德福科技股份有限公司 | Manufacturing method for improving tensile strength of light and thin copper foil |
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| CN112323102A (en) * | 2020-11-04 | 2021-02-05 | 湖南龙智新材料科技有限公司 | Electrolytic copper foil for FPC and preparation method thereof |
| CN112553659A (en) * | 2020-11-09 | 2021-03-26 | 九江德福科技股份有限公司 | Manufacturing method of high-modulus copper foil |
| CN113337856B (en) * | 2021-05-24 | 2024-02-06 | 中国恩菲工程技术有限公司 | Additive for double-sided photoelectrolysis copper foil and preparation method of copper foil |
| CN113337856A (en) * | 2021-05-24 | 2021-09-03 | 中国恩菲工程技术有限公司 | Additive for double-sided photoelectric copper foil and preparation method of copper foil |
| CN113652718A (en) * | 2021-08-27 | 2021-11-16 | 安徽华威铜箔科技有限公司 | Preparation method of 3-micron electrolytic copper foil additive, product and application thereof |
| CN113652718B (en) * | 2021-08-27 | 2024-05-17 | 安徽华威铜箔科技有限公司 | Preparation method of 3-micrometer electrolytic copper foil additive, product and application thereof |
| CN114318428B (en) * | 2021-12-16 | 2024-01-26 | 九江德福科技股份有限公司 | Preparation method of flexible electrolytic copper foil |
| CN114318428A (en) * | 2021-12-16 | 2022-04-12 | 九江德福科技股份有限公司 | Preparation method of flexible electrolytic copper foil |
| CN114703515A (en) * | 2022-04-14 | 2022-07-05 | 中国科学院金属研究所 | Copper foil and preparation method thereof, and circuit board and current collector |
| CN114703515B (en) * | 2022-04-14 | 2024-05-03 | 中国科学院金属研究所 | Copper foil, preparation method thereof, circuit board and current collector |
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