CN104878415A - Preparation method of ultra-thin high-tenacity copper foil - Google Patents
Preparation method of ultra-thin high-tenacity copper foil Download PDFInfo
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Abstract
The invention relates to the technical field of the preparation of a copper foil, and in particular relates to a preparation method of an ultra-thin high-tenacity copper foil. According to the preparation method of the ultra-thin high-tenacity copper foil disclosed by the invention, 1, a high-performance copper foil which is similar to a rolled copper foil in performance can be prepared from an electrolytic copper foil by virtue of a technology combining electrolysis and rolling through the process disclosed by the invention, so as to save huge equipment investment required by the preparation of the rolled copper foil, simplify the production process and reduce production cost; 2, by virtue of the technology combining electrolysis and rolling, the surface roughness of the copper foil is reduced, so that the surface of the copper foil is low in profile tolerance; and the copper foil is thinned; therefore, the copper foil is excellent in electric conductivity, high-frequency signal shielding effect and tenacity; and 3, through a heat treatment process, the copper foil releases residual stress at high temperature and is recrystallized, so that the copper foil is better in bending resistance.
Description
Technical field
The present invention relates to Copper Foil preparing technical field, refer in particular to a kind of preparation method of ultra-thin high tenacity Copper Foil.
Background technology
Copper Foil has low surperficial oxygen species, can be attached to various different substrate materials, and as metal, insulating material etc., have wider temperature use range.Be mainly used in electromagnetic shielding and antistatic, copper-foil conducting electricity be placed in substrate surface, metal substrate combining, there is excellent conduction, and the effect of electromagnetic shielding is provided.(purity more than 99.7%, thickness (1 μm-105 μm) is one of base mateiral of electronic industry to electronic-grade Copper Foil.Along with electronics and information industry is fast-developing, the usage quantity of electronic-grade Copper Foil is increasing, product is widely used in industrial counter, communication equipment, lithium-ions battery, commercial television machine, duplicating machine, phone, air conditioner, automobile electrical subassembly, game machine etc.Along with the development of technology, require Copper Foil to thinner, gentlier develop, suitable toughness to be possessed simultaneously.Current production Copper Foil has two kinds of methods: rolling process and electrolytic process.Generally speaking, thickness is 8 μm and the preparation of above Copper Foil employing rolling process, and the Copper Foil that thickness is less than 8 μm adopts electrolytic process preparation, and the thickness that electrolytic process is produced in recent years has the trend of increase.Rolling process is generally do starting material by copper ingot, through hot pressing, tempering malleableize, cuts the operations such as dirt, cold rolling, continuous malleableize, pickling, calendering and degreaser drying and makes Copper Foil; Electrolytic process is deposited on smooth rotation stainless steel plate (or titanium plate) circular cathode cylinder by the cupric ion in electrolytic solution to form Copper Foil.Copper Foil prepared by rolling process has good electricity, mechanical property, toughness is better, the resistance to deflection of high-precision rolled copper foil (gauge is generally below 20 μm) can reach tens thousand of times even more than one hundred million times, surfaceness can reach 0.1 μm even lower, but equipment investment is large, complex process, production cost is higher; Electrolytic process cost is lower, technique comparatively simplifies, but copper foil surface roughness is high, and uneven surface surface profile value is minimum is 5 μm, and electrical signal shield effectiveness is poor, and also comparatively rolling process is low for mechanical property.In high-frequency signal transmission, due to skin effect effect, signal can accumulate in conductive surface, and therefore the impact of copper foil surface roughness on signal transmission loss is very important.In high-frequency situation, surfaceness is higher, and signal transmits the transmission loss that loss more greatly reduces high-frequency signal, needs to adopt low profile or even surface Copper Foil.
Summary of the invention
The deficiency that the invention reside in that rolling process cost when preparing for current ultra-thin high tenacity Copper Foil is high, the deficiency of complex process and electrolytic process poor-performing exists, and provide a kind of proof strength, the conductivity that overcome the above problems, the preparation method of a kind of ultra-thin high tenacity Copper Foil that operational path is two-in-one.
For achieving the above object, the present invention adopts following technical scheme:
A preparation method for ultra-thin high tenacity Copper Foil, is characterized in that: described preparation method comprises following processing step:
(1) electrolytic copper foil is prepared: generally adopt copper sulfate, sulfuric acid to fill a prescription liquid as electrolysis; Wherein containing concentration is the cupric ion of 30 ~ 90g/L and the sulfuric acid of 150g/L;
In general, electrowinning process is by following process implementation: fine copper is heated to 50 ~ 60 DEG C by (1), passes to oxygen and sulphuric acid soln, makes it occur to react 2Cu+O as follows
2+ 2H
2sO
4=2CuSO
4+ 2H
2o obtains electrolytic solution; (2) apply electric field, formation density is 6000-8000A/m
2electric current, there is electrochemical reaction and obtain continuous print electrolytic copper foil in cupric ion, the Copper Foil obtained is peeled off rolling from cathode roller on cathode roller.
(2) electrolytic copper foil is carried out roll-in in roll squeezer, copper thickness≤12 μm after roll-in; Generally, the Copper Foil obtained by electrolysis process carries out roll-in through twin rollers, and the pressure adjusting between the roller of roll squeezer is 50t-850t, and the spacing between roller adjusted, generally between 0-10 μm according to the thick end of processing number of times and demand.
(3) thermal treatment, under vacuum environment, keeps 1-240 minute through the temperature spots of 380 DEG C and under the environment of 500-800 DEG C; Heat up gradually under the environment of vacuum, effectively can eliminate through the temperature spots of 380 DEG C the stress that roll-in produces, under the environment of 500-800 DEG C, keep 1-240 minute, make intermolecular recrystallization.
Preferably, the speed of roller is crossed in described Copper Foil roll-in is 1-100m/min.
Preferably, after described step 1 completes, step 2,3 is carried out 2-4 cyclical operation, obtains thinner Copper Foil.
The preparation method of ultra-thin high tenacity Copper Foil of the present invention: by the internal organizational structure of the method affect electrolytic copper foil of roll-in, make the gap produced in electrolytic process become less by high pressure, crystal grain becomes more closely knit, and the thickness of Copper Foil reduces; The high pressure of roll-in makes the coarse surface of the Copper Foil formed in electrolytic process become more smooth simultaneously, and roughness reduces, and electroconductibility strengthens; By heat treated mode, the unrelieved stress of Copper Foil inside is released, simultaneously recrystallization, adds ductility and the toughness of Copper Foil, obtain high tenacity Copper Foil flex endurant be not less than 5 × 10 fatigue lifetime
3secondary; Tool beneficial effect of the present invention is: 1, the present invention adopts electrolysis to add rolling techniques, utilize electrolytic copper foil high-performance Copper Foil with rolled copper foil similar to performance obtained after technique of the present invention, save the huge facility investment prepared needed for rolled copper foil, simplify production technique, reduce production cost; 2, the present invention adopts electrolysis in conjunction with the technology of roll-in, reduces the surfaceness of Copper Foil, makes copper foil surface reach low profile degree, and copper thickness reduces, and has higher electroconductibility, high-frequency signal shield effectiveness and toughness; 3, have employed thermal treatment process, make Copper Foil at high temperature discharge unrelieved stress and recrystallize, Copper Foil obtains better resistance to bending ability.
Embodiment
Below in conjunction with embodiment, the present invention is further elaborated:
Embodiment 1:
A preparation method for ultra-thin high tenacity Copper Foil, comprises following processing step:
(1) electrolysis: fine copper is put into copper dissolving tank, passes into oxygen and dilute sulphuric acid, heating copper dissolving tank to 60 DEG C temperature, obtain the electrolytic solution of the sulfuric acid of cupric ion containing 70g/L and 150g/L, put into positive plate and cathode roller in the electrolytic solution, apply electric field, make current density reach 7500A/m
2, there is electrochemical reaction and obtain continuous print electrolytic copper foil in cupric ion, peeled off by the Copper Foil obtained can obtain the electrolytic copper foil that thickness is 8 μm from cathode roller on cathode roller.
(2) roll-in: electrolytic copper foil is inserted in roll squeezer and carry out roll-in, pressuring method is hydraulic pressurization, and roller pressure is set to 50t, Copper Foil through roller speed be 1m/min.
(3) thermal treatment: the thermal chamber individual layer Copper Foil through roll-in being put into vacuum environment, temperature raises gradually and through 380 DEG C, keeps 1min at 500 DEG C, cooling recrystallization; Obtain that thickness is 7 μ, surface roughness Ra 0.3 μm, flex endurant fatigue lifetime be 5 × 10
3secondary high tenacity Copper Foil.
Embodiment 2:
The present embodiment provides the preparation method of another kind of ultra-thin high tenacity Copper Foil, comprises following processing step:
(1) electrolysis: fine copper is put into copper dissolving tank, passes into oxygen and dilute sulphuric acid, heating copper dissolving tank to 60 DEG C temperature, obtain the electrolytic solution of the sulfuric acid of cupric ion containing 75g/L and 150g/L, put into positive plate and cathode roller in the electrolytic solution, apply electric field, make current density reach 6500A/m
2, there is electrochemical reaction and obtain continuous print electrolytic copper foil in cupric ion, peeled off by the Copper Foil obtained can obtain the electrolytic copper foil that thickness is 7 μm from cathode roller on cathode roller.
(2) roll-in: electrolytic copper foil is carried out roll-in in roll squeezer, pressuring method is hydraulic pressurization, and the pressure adjusting between the roller of roll squeezer is 850t, Copper Foil through roller speed be 100m/min.
(3) thermal treatment: the thermal chamber Copper Foil coiled strip through roll-in being put into vacuum environment, heating up gradually keeps 240 minutes under the environment of 800 DEG C through the temperature spot of 380 DEG C, cooling recrystallization.Roll-in and heat treatment process circulation carry out 2 times, obtain that thickness is 6 μ, surface roughness Ra 0.25 μm, flex endurant fatigue lifetime be 6.5 × 10
3secondary high tenacity Copper Foil.
Embodiment 3:
The present embodiment also provides a kind of preparation method of ultra-thin high tenacity Copper Foil, comprises following processing step:
(1) electrolysis: fine copper is put into copper dissolving tank, passes into oxygen and dilute sulphuric acid, heating copper dissolving tank to 60 DEG C temperature, obtain the electrolytic solution of the sulfuric acid of cupric ion containing 80g/L and 160g/L, put into positive plate and cathode roller in the electrolytic solution, apply electric field, make current density reach 8500A/m
2, there is electrochemical reaction and obtain continuous print electrolytic copper foil in cupric ion, peeled off by the Copper Foil obtained can obtain the electrolytic copper foil that thickness is 7.5 μm from cathode roller on cathode roller.
(2) roll-in: electrolytic copper foil is carried out roll-in in roll squeezer, pressuring method is hydraulic pressurization, and the pressure adjusting between the roller of roll squeezer is 650t, Copper Foil through roller speed be 100m/min.
(3) thermal treatment: the thermal chamber Copper Foil coiled strip through roll-in being put into vacuum environment, keeps 200 minutes under the environment of 650 DEG C through the temperature spots of 380 DEG C; , cooling recrystallization.Roll-in and heat treatment process circulation carry out 4 times, obtain that thickness is 5.5 μ, surface roughness Ra 0.20 μm, flex endurant fatigue lifetime be 7.2 × 10
3secondary high tenacity Copper Foil.
The Copper Foil that present invention process is produced, carries out follow-up being processed into gold-plated Copper Foil, silver-plated Copper Foil and nickel plating Copper Foil, has good surface effect, effectively reduces the thickness of coating, save the consumption of coated metal, promote the electric property of coating Copper Foil.
The above embodiment, just preferred embodiments of the present invention, be not limit the scope of the present invention, therefore all equivalences done according to structure, feature and the principle described in the present patent application the scope of the claims change or modify, and all should be included in patent claim of the present invention.
Claims (4)
1. a preparation method for ultra-thin high tenacity Copper Foil, is characterized in that: described preparation method comprises following processing step:
(1) electrolytic copper foil is prepared;
(2) electrolytic copper foil is carried out roll-in in roll squeezer, copper thickness≤12 μm after roll-in;
(3) thermal treatment, under vacuum environment, keeps 1-240 minute through the temperature spots of 380 DEG C and under the environment of 500-800 DEG C.
2. the preparation method of a kind of ultra-thin high tenacity Copper Foil according to claim 1, is characterized by: in described step 2 roll squeezer roller between pressure adjusting be 50t-850t.
3. a kind of method preparing ultra-thin high tenacity Copper Foil according to claim 1, is characterized by: the speed that roller is crossed in described Copper Foil roll-in is 1-100m/min.
4. a kind of method preparing ultra-thin high tenacity Copper Foil according to claim 1, is characterized by: after described step 1 completes, step 2,3 is carried out 2-4 cyclical operation.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109778246A (en) * | 2019-02-22 | 2019-05-21 | 圣达电气有限公司 | A kind of electrolytic copper foil manufacturing equipment |
| CN110644022A (en) * | 2019-09-16 | 2020-01-03 | 铜陵市华创新材料有限公司 | Ultrathin copper foil for producing lithium ion battery by electrolytic calendering and preparation method thereof |
| CN111607810A (en) * | 2020-07-14 | 2020-09-01 | 安徽铜冠铜箔集团股份有限公司 | Efficient production method of ultrathin electrolytic copper foil |
| CN112064071A (en) * | 2020-09-09 | 2020-12-11 | 松山湖材料实验室 | Bending-resistant copper foil, preparation method thereof and FPC (flexible printed circuit) flexible circuit board |
| CN113026061A (en) * | 2021-03-02 | 2021-06-25 | 赣州逸豪新材料股份有限公司 | Continuous discharging foil-generating device for copper foil processing and processing method thereof |
| CN113275379A (en) * | 2021-06-02 | 2021-08-20 | 清远市进田企业有限公司 | Preparation process of high-ductility electrolytic copper |
| CN113444990A (en) * | 2021-06-02 | 2021-09-28 | 清远市进田企业有限公司 | Electrolytic copper recrystallization heat treatment process |
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| CN1709596A (en) * | 2004-06-17 | 2005-12-21 | 上海兴一金属材料有限公司 | Method for preparing rolled copper foil |
| CN102716908A (en) * | 2012-07-04 | 2012-10-10 | 北京科技大学 | Forming method of high-flexibility ultrathin rolled copper foil |
| CN102732917A (en) * | 2011-04-12 | 2012-10-17 | 佛冈建滔实业有限公司 | Preparation method of double-sided photoelectrolytic copper foil |
| CN103071678A (en) * | 2012-11-20 | 2013-05-01 | 无锡常安通用金属制品有限公司 | Calendaring method of copper foil |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1709596A (en) * | 2004-06-17 | 2005-12-21 | 上海兴一金属材料有限公司 | Method for preparing rolled copper foil |
| CN102732917A (en) * | 2011-04-12 | 2012-10-17 | 佛冈建滔实业有限公司 | Preparation method of double-sided photoelectrolytic copper foil |
| CN102716908A (en) * | 2012-07-04 | 2012-10-10 | 北京科技大学 | Forming method of high-flexibility ultrathin rolled copper foil |
| CN103071678A (en) * | 2012-11-20 | 2013-05-01 | 无锡常安通用金属制品有限公司 | Calendaring method of copper foil |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109778246A (en) * | 2019-02-22 | 2019-05-21 | 圣达电气有限公司 | A kind of electrolytic copper foil manufacturing equipment |
| CN109778246B (en) * | 2019-02-22 | 2021-09-03 | 圣达电气有限公司 | Electrolytic copper foil manufacturing equipment |
| CN110644022A (en) * | 2019-09-16 | 2020-01-03 | 铜陵市华创新材料有限公司 | Ultrathin copper foil for producing lithium ion battery by electrolytic calendering and preparation method thereof |
| CN111607810A (en) * | 2020-07-14 | 2020-09-01 | 安徽铜冠铜箔集团股份有限公司 | Efficient production method of ultrathin electrolytic copper foil |
| CN112064071A (en) * | 2020-09-09 | 2020-12-11 | 松山湖材料实验室 | Bending-resistant copper foil, preparation method thereof and FPC (flexible printed circuit) flexible circuit board |
| CN112064071B (en) * | 2020-09-09 | 2021-08-03 | 松山湖材料实验室 | Bending-resistant copper foil, preparation method thereof and FPC (flexible printed circuit) flexible circuit board |
| CN113026061A (en) * | 2021-03-02 | 2021-06-25 | 赣州逸豪新材料股份有限公司 | Continuous discharging foil-generating device for copper foil processing and processing method thereof |
| CN113275379A (en) * | 2021-06-02 | 2021-08-20 | 清远市进田企业有限公司 | Preparation process of high-ductility electrolytic copper |
| CN113444990A (en) * | 2021-06-02 | 2021-09-28 | 清远市进田企业有限公司 | Electrolytic copper recrystallization heat treatment process |
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Application publication date: 20150902 |
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