CN107236973A - Preparation method, product and its application of flexibility coat copper plate additive for electrolytic copper foil - Google Patents
Preparation method, product and its application of flexibility coat copper plate additive for electrolytic copper foil Download PDFInfo
- Publication number
- CN107236973A CN107236973A CN201710293810.4A CN201710293810A CN107236973A CN 107236973 A CN107236973 A CN 107236973A CN 201710293810 A CN201710293810 A CN 201710293810A CN 107236973 A CN107236973 A CN 107236973A
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- Prior art keywords
- additive
- solution
- copper foil
- electrolyte
- electrolytic
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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
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/38—Electroplating: Baths therefor from solutions of copper
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D7/00—Electroplating characterised by the article coated
- C25D7/06—Wires; Strips; Foils
- C25D7/0614—Strips or foils
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Laminated Bodies (AREA)
- Manufacturing Of Printed Wiring (AREA)
- Electroplating And Plating Baths Therefor (AREA)
Abstract
The present invention discloses preparation method, product and its application of flexibility coat copper plate additive for electrolytic copper foil, flexibility coat copper plate additive for electrolytic copper foil, including following raw material：3 mercaptopropanesulfonic acid sodium, sodium polydithio-dipropyl sulfonate, thiocarbamide, alcohol mercapto propyl-sulfonate, polyethylene glycol 12000#, hydroxyethyl cellulose 6000#.It is used to use electrodeposition technology, prepares the flexible electrolytic copper foils of 5 um;Electrolyte DC electrodeposition technique, in electrolytic process additive is added in the net liquid of copper sulphate, in the presence of electric field, metallic copper is deposited on the titanium cathode roller of cycle rotation, after the stripper roll of unit is peeled off, wound after anti-oxidation processing, the 120g/L of electrolyte copper content 80 wherein in electrolytic process, the 130g/L of sulfuric acid content 90, temperature control is at 45 60 degree, flexible additive for electrolytic copper foil is added into electrolyte, it is 60 90m to make flow of electrolyte3/ H, the 12000A/M of current density 45002Under the conditions of carry out DC electrodeposition；Strengthen tensile strength and peel strength, improve the reliability of fitting with the base material such as polyimide base film.
Description
Technical field
The present invention relates to electrolytic copper foil manufacturing technology field, and in particular to production 5um flexibility coat copper plate electrolytic copper foils
With the preparation method of additive, product and its application.
Background technology
The characteristics of flexibility coat copper plate (FCCL) has thin, light and pliability.Used extensively with the FPC that FCCL is baseplate material
In electronic products such as mobile phone, digital camera, DV, vehicle satellite direction positioning device, LCD TV, notebook computers
In.
FCCL is in addition to having the advantages that thin, light and pliability, with the FCCL of polyimide base film, also with electrical property, heat
The characteristics of performance, excellent heat resistance.Its relatively low-k (Dk) property so that electric signal is quickly transmitted.Good
Hot property, may be such that component is easy to cooling.Higher glass transition temperature (Tg) may be such that component is well transported at higher temperatures
OK.It is to be continuously supplied to user into web-like form, therefore, using FCCL production printing electricity due to the most products of FCCL
Install on road plate, the successional surface that component is carried out beneficial to the automatic continuous production for realizing FPC and on FPC.
The conductor material of flexibility coat copper plate, the overwhelming majority is to use copper foil, its own comprehensive feature, as main conductive
The copper foil of transport vehicle must have a high temperature resistant, the performance such as high-transmission, high ductibility, high antistripping, only even property low profile,
High-tensile, high-elongation, height put close, and the strong cathode copper foil of stickup property can be met simultaneously.
International aspect is faced with the existing practical challenges of both shortage of resources and emission reduction environmental protection, the rise of new science and technology simultaneously
And development, multi-functional high density electronic digital product enhancing digital product and the involvement of common people's daily life；Convenient daily life
It is living to add fun atmosphere simultaneously.Multi-functional high density electronic digital product；It can only develop to fine, high density set.This hair
The 5um flexibility coat copper plate electrolytic copper foils of open-birth output belong to the flexibility coat copper plate prepared by extra thin copper foil, and itself performance is full
Outside sufficient electronic digital product electrical property, unit usage amount is compared with conventional flex copper-clad plate, and relative reduction is more；Reduce into
This, is while subtract the input into resource, indirect protection environment.
The content of the invention
In view of the above-mentioned problems, a kind of it is an object of the present invention to provide system of flexibility coat copper plate additive for electrolytic copper foil
Preparation Method, its step is easy, and condition is easily controllable, and cost is low.
The present invention also aims to there is provided using the above method prepare flexibility coat copper plate additive for electrolytic copper foil,
Its application is prepared into flexibility coat copper plate electrolytic copper foil, in particular for production 5um electrolytic copper foils
To achieve the above object, the technical solution adopted by the present invention is：
A kind of preparation method of flexibility coat copper plate additive for electrolytic copper foil, comprises the following steps：
(1) following raw material is prepared：
3- mercaptopropanesulfonic acids sodium (ZPS)
Sodium polydithio-dipropyl sulfonate (SPS)
Thiocarbamide (N)
Alcohol mercapto propyl-sulfonate (HP)
Polyethylene glycol 12000# (PEG)
Hydroxyethyl cellulose 6000# (HEC)
Its mass ratio is：1：1.5：1：1.5：1：2；
(2) respectively by 3- mercaptopropanesulfonic acids sodium (ZPS), sodium polydithio-dipropyl sulfonate (SPS), thiocarbamide (N), alcohol sulfenyl
Propane sulfonic acid sodium (HP), polyethylene glycol 12000# (PEG), polyethylene glycol 12000# (PEG), hydroxyethyl cellulose 6000# (HEC)
It is dissolved in 250mL deionization pure water, respectively obtains solution A, solution B, solution C, solution D, solution E, solution F；
(3) solution A, solution B, solution C, solution D, solution E, solution F made from step (2) are added to the stirring of 5L constant temperature
In cup, add deionized water 2L and stirred 30 minutes under the degree environment of constant temperature 55 to 60, obtain mixed liquor；
(4) mixed liquor made from step (3) is quantitatively diluted to 10L with deionized water, completes additive and prepare.
A kind of flexibility coat copper plate additive for electrolytic copper foil, it includes following raw material：3- mercaptopropanesulfonic acid sodium, poly- two sulphur
Two propane sulfonic acid sodium, thiocarbamide, alcohol mercapto propyl-sulfonate, polyethylene glycol 12000#, hydroxyethyl cellulose 6000#, its mass ratio
Example be：1：1.5：1：1.5：1：2.
A kind of application of flexibility coat copper plate additive for electrolytic copper foil, it is used to prepare the flexible electrolytic copper foils of 5um.
The application of the flexibility coat copper plate additive for electrolytic copper foil, it is used to use electrodeposition technology, prepares 5um flexible
Electrolytic copper paper tinsel；Flexible additive for electrolytic copper foil is added in the net liquid of copper sulphate in electrolyte DC electrodeposition technique, electrolytic process, is led to
Cross in the presence of electric field, metallic copper is deposited on the titanium cathode roller of cycle rotation, after the stripper roll of unit is peeled off, through oxygen
Wound after change processing, electrolyte copper content 80-120g/L wherein in electrolytic process, sulfuric acid content 90-130g/L, temperature control exists
45-60 degree, flexible additive for electrolytic copper foil is added into electrolyte, and it is 60-90m to make flow of electrolyte3/ H, current density
4500-12000A/M2Under the conditions of carry out DC electrodeposition；The additive package of electrolyte addition includes 3- mercaptopropanesulfonic acids
Sodium, sodium polydithio-dipropyl sulfonate, thiocarbamide, alcohol mercapto propyl-sulfonate, polyethylene glycol 12000#, hydroxyethyl cellulose 6000#,
Additive flow is 100-300mL/Min.
Have the advantage that compared with prior art：
By the way that the electrolytic copper foil surface crystal grain of Additive Production of the present invention is smooth, profile is low, tensile strength, high-elongation,
Have and the preferable sticking effect of polyimide base film and characteristic simultaneously.Available for high-end flexibility coat copper plate (FCCL) circuit board base
Body material.Additive cost of the present invention is low, and the technique scope of application is wide, is easy to technology controlling and process, it is ensured that product quality and benefit.
Embodiment
The preparation method for the flexibility coat copper plate additive for electrolytic copper foil that the present embodiment is provided, comprises the following steps：
(1) following raw material is prepared：
(2) respectively by 3- mercaptopropanesulfonic acids sodium (ZPS), sodium polydithio-dipropyl sulfonate (SPS), thiocarbamide (N), alcohol sulfenyl
Propane sulfonic acid sodium (HP), polyethylene glycol 12000# (PEG), polyethylene glycol 12000# (PEG), hydroxyethyl cellulose 6000# (HEC)
It is dissolved in 250mL deionization pure water, respectively obtains solution A, solution B, solution C, solution D, solution E, solution F；
(3) solution A, solution B, solution C, solution D, solution E, solution F made from step (2) are added to the stirring of 5L constant temperature
In cup, add deionized water 2L and stirred 30 minutes under the degree environment of constant temperature 55 to 60, obtain mixed liquor；
(4) mixed liquor made from step (3) is quantitatively diluted to 10L with deionized water, completes additive and prepare.
A kind of flexibility coat copper plate additive for electrolytic copper foil, it includes following raw material：3- mercaptopropanesulfonic acid sodium, poly- two sulphur
Two propane sulfonic acid sodium, thiocarbamide, alcohol mercapto propyl-sulfonate, polyethylene glycol 12000#, hydroxyethyl cellulose 6000#, its mass ratio
Example be：1：1.5：1：1.5：1：2.
A kind of application of flexibility coat copper plate additive for electrolytic copper foil, it is used to prepare the flexible electrolytic copper foils of 5um.Flexibility is covered
The application of copper coin additive for electrolytic copper foil, it is used to use electrodeposition technology, prepares 5um flexible electrical copper foils；Electrolyte direct current
Flexible additive for electrolytic copper foil is added in the net liquid of copper sulphate in electrodeposition technology, electrolytic process, in the presence of electric field,
Metallic copper is deposited on the titanium cathode roller of cycle rotation, after the stripper roll of unit is peeled off, is wound after anti-oxidation processing, wherein
Electrolyte copper content 80-120g/L in electrolytic process, sulfuric acid content 90-130g/L, temperature control is in 45-60 degree, to electrolyte
The middle flexible additive for electrolytic copper foil of addition, it is 60-90m to make flow of electrolyte3/ H, current density 4500-12000A/M2Condition
Lower carry out DC electrodeposition；The additive package of electrolyte addition includes 3- mercaptopropanesulfonic acid sodium, polydithio-dipropyl sulfonic acid
Sodium, thiocarbamide, alcohol mercapto propyl-sulfonate, polyethylene glycol 12000#, hydroxyethyl cellulose 6000#, additive flow is 100-
300mL/Min。
Following instance is in anode reaction groove, under the technique that the net liquid recycle stream of copper sulphate is mended, by turning in continuous constant speed
Electro-deposition is carried out on dynamic cathode titanium roller, different electrolytic copper foils are obtained.
Embodiment 1：
Resulting copper foil parameter is as follows：
Embodiment 2：
Resulting copper foil parameter is as follows：
Embodiment 3：
Resulting copper foil parameter is as follows：
The present invention is not limited to above-described embodiment, all to use technical scheme same as the previously described embodiments or similar, reaches
To other schemes of the object of the invention, within the scope of the present invention.
Claims (4)
1. a kind of preparation method of flexibility coat copper plate additive for electrolytic copper foil, it is characterised in that comprise the following steps：
（1）Prepare following raw material：
3- mercaptopropanesulfonic acid sodium（ZPS）
Sodium polydithio-dipropyl sulfonate（SPS）
Thiocarbamide（N）
Alcohol mercapto propyl-sulfonate（HP）
Polyethylene glycol 12000#（PEG）
Hydroxyethyl cellulose 6000#（HEC)
Its mass ratio is：1：1.5：1：1.5：1：2；
（2）Respectively by 3- mercaptopropanesulfonic acid sodium（ZPS）, sodium polydithio-dipropyl sulfonate（SPS）, thiocarbamide（N）, alcohol sulfenyl propane
Sodium sulfonate（HP）, polyethylene glycol 12000#（PEG）, polyethylene glycol 12000#（PEG）, hydroxyethyl cellulose 6000#（HEC it is) molten
In 250mL deionization pure water, solution A, solution B, solution C, solution D, solution E, solution F are respectively obtained；
（3）By step（2）Obtained solution A, solution B, solution C, solution D, solution E, solution F are added to 5L constant temperature stirring cup
In, add deionized water 2L and stirred 30 minutes under the degree environment of constant temperature 55 to 60, obtain mixed liquor；
（4）By step（3）Obtained mixed liquor is quantitatively diluted to 10L with deionized water, completes additive and prepares.
2. the flexibility coat copper plate additive for electrolytic copper foil that a kind of method according to claim 1 is prepared from, it include with
Lower raw material：3- mercaptopropanesulfonic acid sodium, sodium polydithio-dipropyl sulfonate, thiocarbamide, alcohol mercapto propyl-sulfonate, polyethylene glycol
12000#, hydroxyethyl cellulose 6000#, its mass ratio is：1：1.5：1：1.5：1：2.
3. a kind of application of the additive for electrolytic copper foil of flexibility coat copper plate according to claim 2, it is characterised in that it is used for
Prepare the flexible electrolytic copper foils of 5 um.
4. the application of flexibility coat copper plate additive for electrolytic copper foil according to claim 3, it is characterised in that it uses electricity heavy
Product technique, prepares flexible electrical copper foil；In electrolyte DC electrodeposition technique, electrolytic process flexible electrolysis is added in the net liquid of copper sulphate
Copper foil additive, in the presence of electric field, metallic copper is deposited on the titanium cathode roller of cycle rotation, by the stripping of unit
After roller is peeled off, wound after anti-oxidation processing, electrolyte copper content 80-120g/L, sulfuric acid content 90- wherein in electrolytic process
130g/L, temperature control adds flexible additive for electrolytic copper foil into electrolyte in 45-60 degree, and it is 60- to make flow of electrolyte
90m3/ H, current density 4500-12000A/M2Under the conditions of carry out DC electrodeposition；The additive package of electrolyte addition includes 3-
Mercaptopropanesulfonic acid sodium, sodium polydithio-dipropyl sulfonate, thiocarbamide, alcohol mercapto propyl-sulfonate, polyethylene glycol 12000#, ethoxy
Cellulose 6000#, additive flow is 100-300mL/Min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710293810.4A CN107236973A (en) | 2017-04-28 | 2017-04-28 | Preparation method, product and its application of flexibility coat copper plate additive for electrolytic copper foil |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710293810.4A CN107236973A (en) | 2017-04-28 | 2017-04-28 | Preparation method, product and its application of flexibility coat copper plate additive for electrolytic copper foil |
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| CN201710293810.4A Pending CN107236973A (en) | 2017-04-28 | 2017-04-28 | Preparation method, product and its application of flexibility coat copper plate additive for electrolytic copper foil |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108560025A (en) * | 2018-06-14 | 2018-09-21 | 九江德福科技股份有限公司 | A kind of preparation method of electrolytic copper foil |
| CN108677222A (en) * | 2018-06-14 | 2018-10-19 | 九江德福科技股份有限公司 | A kind of electrolyte and production technology being used to prepare lithium electrolytic copper foil |
| CN111850620A (en) * | 2020-08-28 | 2020-10-30 | 江东电子材料有限公司 | Preparation method and preparation system of 4.5-micrometer ultrathin copper foil for lithium battery |
| CN113416985A (en) * | 2021-07-06 | 2021-09-21 | 铜陵市华创新材料有限公司 | Additive adding method for preventing edge tearing of 4.5-micron copper foil |
| CN113445081A (en) * | 2021-05-21 | 2021-09-28 | 江西理工大学 | Additive for electrolytic copper foil, electrolyte for electrolytic copper foil, copper foil and method for producing the same |
| CN114059105A (en) * | 2021-11-08 | 2022-02-18 | 灵宝华鑫铜箔有限责任公司 | Copper-nickel-cobalt alloy foil process |
| CN114351190A (en) * | 2021-12-27 | 2022-04-15 | 安徽华威铜箔科技有限公司 | Preparation method of additive for flexible copper clad laminate electrolytic copper foil, product and application thereof |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108560025A (en) * | 2018-06-14 | 2018-09-21 | 九江德福科技股份有限公司 | A kind of preparation method of electrolytic copper foil |
| CN108677222A (en) * | 2018-06-14 | 2018-10-19 | 九江德福科技股份有限公司 | A kind of electrolyte and production technology being used to prepare lithium electrolytic copper foil |
| CN108560025B (en) * | 2018-06-14 | 2020-01-21 | 九江德福科技股份有限公司 | Preparation method of electrolytic copper foil |
| CN111850620A (en) * | 2020-08-28 | 2020-10-30 | 江东电子材料有限公司 | Preparation method and preparation system of 4.5-micrometer ultrathin copper foil for lithium battery |
| CN111850620B (en) * | 2020-08-28 | 2022-04-05 | 江东电子材料有限公司 | Preparation method and preparation system of 4.5-micrometer ultrathin copper foil for lithium battery |
| CN113445081A (en) * | 2021-05-21 | 2021-09-28 | 江西理工大学 | Additive for electrolytic copper foil, electrolyte for electrolytic copper foil, copper foil and method for producing the same |
| CN113416985A (en) * | 2021-07-06 | 2021-09-21 | 铜陵市华创新材料有限公司 | Additive adding method for preventing edge tearing of 4.5-micron copper foil |
| CN114059105A (en) * | 2021-11-08 | 2022-02-18 | 灵宝华鑫铜箔有限责任公司 | Copper-nickel-cobalt alloy foil process |
| CN114351190A (en) * | 2021-12-27 | 2022-04-15 | 安徽华威铜箔科技有限公司 | Preparation method of additive for flexible copper clad laminate electrolytic copper foil, product and application thereof |
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Application publication date: 20171010 |