CN103132110B - A kind of preparation method of high performance electrolytic copper foil - Google Patents
A kind of preparation method of high performance electrolytic copper foil Download PDFInfo
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Abstract
The invention discloses a kind of preparation method of high performance electrolytic copper foil, it is characterized in that comprising the steps and processing condition: second step, cathode roller starts to rotate, and the rotating speed of cathode roller is 2 ~ 10 ms/min, and current density is 3500 ~ 8000A/m
2, electrolyte temperature is 50 ~ 70 DEG C, generates continuous print electrolytic copper foil, then peeled off from cathode roller by the electrolytic copper foil of generation under Electric and magnetic fields acting in conjunction at the surface crystallization of cathode roller.Electrolytic copper foil surface roughness prepared by the present invention is low, improves the electrical property of Copper Foil; The improvement of crystal structure improves the resistance to bending performance of Copper Foil; Present invention saves the huge facility investment of producing needed for rolled copper foil, low-profile electrolytic copper foil and ultrathin electrolytic copper foil, simplify production technique, reduce production cost.
Description
Technical field
The present invention relates to electronic material preparing technical field, specifically refer to a kind of preparation method of high performance electrolytic copper foil.
Background technology
Copper Foil is the critical material of printed circuit board playing support, interconnection components and parts effect in electronic product, is called " neural network " of electronic product signal and power transmission.Since the nineties in last century, the development of IT product technology, facilitate printed circuit board towards multiple stratification, slimming, densification, high speed future development, the performance of electrolytic copper foil, quality, reliability are had higher requirement, has greatly promoted the development of Productive Technology of Electronlytical Copper-foil.
Copper Foil is the important materials manufacturing rigidity copper-clad plate, flexibility printed circuit board (FPC), high-frequency circuit board and cathode of lithium battery collector.Global printed-wiring board (PWB) (PCB) the industry output value about 37,700,000,000 dollars in 2010, the wherein flexible sheet output value about 6,100,000,000, copper clad laminate market reaches 73.7 hundred million dollars.Copper-clad plate is the direct material of PCB, and Copper Foil accounts for the maximum starting material of cost proportion during copper-clad plate is produced, and accounts for 50% of copper-clad plate cost.According to the statistical information of the Industrial Technology Research Institute of Taiwan IEK, within 2010, the global Copper Foil output value for the manufacture of copper-clad plate is about 3,700,000,000 dollars, and the Copper Foil output value wherein for the manufacture of flexible sheet is about 3,000,000,000 dollars, mainly uses rolled copper foil and a small amount of high performance electrolytic copper foil.Whole world electrolytic copper foil 2010 annual value of production is about 2,300,000,000 dollars, except certain applications are except copper coated foil plate, are mainly used in and make lithium ion battery negative collector.As can be seen from the statistic data of 2010, in copper-clad plate Application Areas, rolled copper foil and the market share shared by high performance electrolytic copper foil are far above standard electrolytic Copper Foil.
The mode of production of rolled copper foil determines its surface and has homogeneous smoothness, and therefore the surfaceness of rolled copper foil is starkly lower than electrolytic copper foil.In general, the surfaceness (Rz) of the raw paper tinsel of rolled copper foil can reach 1 μm, is 1/5th of the raw paper tinsel surfaceness of standard electrolytic Copper Foil.With electronic product to high performance, multifunction future development, require that electronic component can carry out fast transport and process to the signal comprising bulk information in a short period of time, electronic component uses high frequency circuit more and more.Because high frequency circuit exists " surface action ", the surfaceness of Copper Foil is less, and the distance of Signal transmissions is shorter, is more not easy generation and delays with slow, is conducive to forming fine-line.Rolled copper foil surface uniform, during making wire, each several part etch-rate difference is very little, is conducive to the impedance characteristic improving wire, thus ensures the correct transmission of signal.Therefore, in high frequency charge transfer process, the electrical property of the rolled copper foil that roughness is little is much better than electrolytic copper foil.
For being used as the Copper Foil of lithium ion battery negative collector, its surfaceness has considerable influence to battery electrode manufacture craft and battery performance, the contact of the negative electrode active materials such as the electrolytic copper foil that surfaceness is large and graphite is poor, cause the negative electrode active materials such as graphite loss of adhesion at copper foil surface, easy generation applies coming off of active substance, directly affects the cycle life of battery.Therefore, high to reliability requirement high performance lithium ion battery still needs to select rolled copper foil as negative current collector.
Compared with rolled copper foil, the resistance to deflection of electrolytic copper foil is poor.Electrolytic copper foil is generated by galvanic deposit mode, and the growth of crystal through-thickness forms column crystal, when bending, easily produces cracking along column crystallization tissue.The crystal structure of rolled copper foil is the sheet tissue along rolling direction arrangement, and such crystal structure does not propagate the crackle of particle interface when Copper Foil bends, have very high bending resistance folding endurance, is about 5 times of same thickness standard electrolytic Copper Foil.
In sum, the problems such as the resistance to bending performance difference existed due to standard electrolytic Copper Foil and surfaceness height, make its application on flexible sheet and HF link plate and high performance lithium ion battery be extremely restricted.High-speed high frequency wideband and high density interconnect pcb board, flexible sheet and the roughness requirements of IC substrate to Copper Foil high, rolled copper foil has obvious advantage.
The investment of production of rolled copper foil is large, technical process is complicated, affects the many factors of quality product and yield rate, and production difficulty is large, production cost is high.The production capacity of whole world rolled copper foil more than 90% rests in Japanese manufacturer's hand, and the production capacity of more than 80% concentrates on Japanese native country.Because facility investment is large, production technology is complicated, in addition the external blockade to crucial production technology, the development of China's rolled copper foil industry is subject to great restriction, high-precision calendering electronics Copper Foil is produced and is substantially in space state, and the domestic high-precision rolled copper foil for the manufacture of flexible sheet mainly relies on external import.Because production technology, market and price all rest in external Ji Jia manufacturer hand, the production capacity of rolled copper foil is too concentrated, causes imported product price higher, and output and price uncertainty are comparatively large, seriously govern the development of China's electronic information downstream industry.
For reducing costs and evading raw material supply risk, current most of printed circuit board (PCB) and lithium cell production industry all are actively being sought to utilize electrolytic copper foil to substitute rolled copper foil, have promoted the exploitation upsurge of electrolytic copper foil manufacturer to special high performance electrolytic copper foils such as high ductibility electrolytic copper foil and low-profile electrolytic copper foil thus.
Be described as follows for making electrolytic copper foil of flexible sheet and other fine circuitries and preparation method thereof so far.Along with the raising of electrolytic copper foil production technology, Japan, U.S. part Copper Foil producer have developed the low-profile electrolytic copper foil and ultrathin electrolytic copper foil that meet flexible sheet requirement.Low profile high performance electrolytic copper foil mainly utilizes special mixed additive to control surface profile and the mechanical property of Copper Foil, strengthens cathodic polarization by adding and suppresses metal misgrowth thus improve elasticity, intensity, the hardness of Copper Foil and smoothly feel containing the inorganic additives of arsenic containing antimony.By using organic additives such as can improving the hydrolyzed animal protein (gelatin) of Copper Foil hair side peak valley shape and PEG, prepare the extremely low low profile of surfaceness and ultra-low profile Copper Foil.The hair side of this Copper Foil is after special processing, and roughness Rz drops to 1.5 μm, and its overall mechanical property maintains certain level.Low-profile electrolytic copper foil has excellent bending resistance folding endurance and etching, is applicable to make flexible sheet and other fine circuitries.Employing has certain thickness foils and makes negative electrode, acid copper thereon, then the foils of the extra thin copper foil plated together with negative electrode is compressed on dielectric panel through hot pressing, solidification, then is peeled off by the metallic support paper tinsel as negative electrode, can be made into ultrathin electrolytic copper foil.The key mainly problem that is separated with extra thin copper foil of resolved vector paper tinsel that extra thin copper foil is produced, the peel ply used at present mainly includes machine layer, inorganic layer and inorganic and organic peel ply.The existing thickness of Japan is that the ultrathin electrolytic copper foil of 5 μm, 3 μm puts into production.
Prior art exists following not enough: the investment of production of (1) rolled copper foil is large, technical process is complicated, and production difficulty is large, production cost is high.The production capacity of whole world rolled copper foil more than 90% rests in Japanese manufacturer's hand, and China's high-precision calendering electronics Copper Foil is produced and is substantially in space state.(2) investment of production equipment of low-profile electrolytic copper foil and ultrathin electrolytic copper foil is large, Technology is complicated, realizes difficulty very big, cause the technology barriers entering high-grade electrolytic copper foil industry high for general Copper Foil manufacturer.The production technology of current low-profile electrolytic copper foil and ultrathin electrolytic copper foil control by national minority Copper Foil companies such as Japan and the United States.
Summary of the invention
In order to overcome above-mentioned deficiency, the object of the present invention is to provide a kind of preparation method of high performance electrolytic copper foil, the method is on existing installation basis, being solved the problems such as the resistance to bending performance difference of electrolytic copper foil and surfaceness height by scrap build and technological innovation, is the economic means that preparation is organized, performance is similar to the high performance electrolytic copper foil of rolled copper foil.
The present invention is achieved through the following technical solutions: a kind of preparation method of high performance electrolytic copper foil, it is characterized in that comprising the steps and processing condition:
The first step, electrolyte level, between cathode roller and positive plate, the cathode roller and positive plate of raw paper tinsel machine arranges magnetic pole, between cathode roller and positive plate, forms complementary field;
Second step, cathode roller starts to rotate, and the rotating speed of cathode roller is 2 ~ 10 ms/min, and current density is 3500 ~ 8000A/m
2, electrolyte temperature is 50 ~ 70 DEG C, generates continuous print electrolytic copper foil, then peeled off from cathode roller by the electrolytic copper foil of generation under Electric and magnetic fields acting in conjunction at the surface crystallization of cathode roller.
Further, the rotating speed of described cathode roller is 6 ms/min, and described current density is 5500A/m
2, described electrolyte temperature is 60 DEG C.
Described complementary field acts on Copper Foil and starts crystallization to the whole deposition process peeled off.
Described complementary field intensity is adjustable from 0T to 1.4T.
Described complementary field direction is adjustable to 80 ° from 0 ° with deposition direction of an electric field relative orientation angle.
Ultimate principle of the present invention: add high-intensity magnetic field in the raw paper tinsel process of electrolytic deposition, utilize complementary field to change the tissue of electrolytic copper foil to the impact of electrolyting precipitation process.In electrolyting precipitation process, can be subject to the effect of lorentz's force when ionic current cutting magnetic line, its apparent effect is exactly that electrolytic solution is stirred.The stirring action of complementary field makes the dispersive ability of electrolytic solution significantly improve, improve the homogeneity of cupric ion distribution, make that electrode surface diffusion layer is thinning, limit current density increases, sedimentation effect improves, and promotes the mass transfer of ate electrode, thus impel settled layer surface more smooth, careful.The bubble hydrogen produced in electrodeposition process is adsorbed on coating surface and does not depart from time, is the reason causing surface hole defect.Apply behind magnetic field, to be stirred and the promoter action of magnetic field to diamagnetism hydrogen molecule De contamination makes bubble hydrogen depart from from coating surface in time due to electrolytic solution, therefore hole disappears, and obtains fine and close deposition layer.The stirring action of complementary field produces souring in the frictional belt of cathode surface, the crystal grain tip of cathode surface is smashed, suppresses its vertical surface forward growth, thus make surface grain refinement, and settled layer surface finish improves.Therefore, utilize magnetic field assisted electrolysis deposition technique section to enlarge markedly the compactness of Copper Foil, improve the planarization of copper foil surface, reduce the roughness of Copper Foil.
The magnetizing force of externally-applied magnetic field can also affect the crystalline orientation of deposition layer, and because crystal exists magneticanisotropy, the magnetizing force that crystal is subject in different directions there are differences.Under the action of a magnetic field, crystal can rotate and separate out towards the direction that the energy of magnetization is stable.Utilize magnetic field assisted electrolysis deposition technique can improve the crystal structure of Copper Foil.
The present invention compared with prior art, tool has the following advantages and beneficial effect: 1, the present invention adopts magnetic field assisted electrolysis deposition technique, existing equipment basis is prepared through scrap build and technological innovation organize, high performance electrolytic copper foil that performance is similar to rolled copper foil, save the huge facility investment of producing needed for rolled copper foil, break away from and produced the technical controlling and monopolization that rolled copper foil faces, simplify production technique, reduce production cost; 2, the present invention adopts magnetic field assisted electrolysis deposition technique, the effect of lorentz's force and magnetizing force is utilized to improve the density of Copper Foil, reduce surfaceness, the surfaceness of electrolytic copper foil and mechanical property is made to reach the level of low-profile electrolytic copper foil and ultrathin electrolytic copper foil phase, save and produce low profile copper foil and the huge facility investment needed for extra thin copper foil, overcome and enter the high technology barriers of high-grade electrolytic copper foil industry;
3, magnetic field assisted electrolysis depositing operation is utilized, obtained have the crystal structure of raw paper tinsel direction, edge layered arrangement and the continuous electrolysis Copper Foil of low surface roughness, saves huge facility investment, simplify manufacturing process, reducing production cost, is the economical route manufacturing high performance electrolytic copper foil.
Accompanying drawing explanation
Below in conjunction with the drawings and specific embodiments, the present invention is described in further detail:
Fig. 1 is the structural representation of the raw paper tinsel machine with magnetic field after repacking.
In figure: 1, cathode roller; 2, positive plate; 3, electrolytic solution; 4, magnetic pole.
Embodiment
Embodiment one
A preparation method for high performance electrolytic copper foil, is characterized in that comprising the steps and processing condition:
The first step, electrolytic solution 3, between cathode roller 1 and positive plate 2, the cathode roller and positive plate of raw paper tinsel machine arranges magnetic pole 4, as shown in Figure 1, forms the complementary field that magneticstrength is 0T between cathode roller and anode;
Second step, cathode roller starts to rotate, and adopt roll-type continuous electrolysis method to generate continuous electrolysis Copper Foil under Electric and magnetic fields acting in conjunction, the rotating speed of cathode roller is 10 ms/min, and current density is 8000A/m
2, electrolyte temperature is 50 DEG C, and preparing thickness is 7 microns, hair side roughness R
zit is the electrolytic copper foil of 4.
Embodiment two
A preparation method for high performance electrolytic copper foil, is characterized in that comprising the steps and processing condition:
The first step, electrolyte level is between cathode roller and positive plate, cathode roller of foil manufacturing machine cylinder and positive plate arrange magnetic pole, forms the complementary field that magneticstrength is 1.4T between cathode roller and anode, magnetic field is 80 ° with deposition direction of an electric field relative orientation angle;
Second step, cathode roller starts to rotate, and adopt roll-type continuous electrolysis method to generate continuous electrolysis Copper Foil under Electric and magnetic fields acting in conjunction, drum rotational speed is 2 ms/min, and current density is 3500A/m
2, electrolyte temperature 70 DEG C, preparing thickness is 18 microns, hair side roughness R
zit is the electrolytic copper foil of 2.
Embodiment three
A preparation method for high performance electrolytic copper foil, is characterized in that comprising the steps and processing condition:
The first step, electrolyte level, between cathode roller and positive plate, cathode roller of foil manufacturing machine cylinder and positive plate arranges magnetic pole, forms the complementary field that magneticstrength is 1T between cathode roller and anode; Magnetic field is 0 ° with deposition direction of an electric field relative orientation angle;
Second step, cathode roller starts to rotate, and adopt roll-type continuous electrolysis method to generate continuous electrolysis Copper Foil under Electric and magnetic fields acting in conjunction, drum rotational speed is 8 ms/min, and current density is 5000A/m
2, electrolyte temperature is 60 DEG C, and preparing thickness is 9 microns, hair side roughness R
zit is the electrolytic copper foil of 4.
Embodiment four
A preparation method for high performance electrolytic copper foil, is characterized in that comprising the steps and processing condition:
The first step, electrolyte level, between cathode roller and positive plate, cathode roller of foil manufacturing machine cylinder and positive plate arranges magnetic pole, forms the complementary field that magneticstrength is 0.8T between cathode roller and anode; Magnetic field is 45 ° with deposition direction of an electric field relative orientation angle;
Second step, cathode roller starts to rotate, and adopt roll-type continuous electrolysis method to generate continuous electrolysis Copper Foil under Electric and magnetic fields acting in conjunction, drum rotational speed is 5 ms/min, and current density is 4000A/m
2, electrolyte temperature is 70 DEG C, and preparing thickness is 12 microns, hair side roughness R
zit is the electrolytic copper foil of 3.5.
Embodiment five
A preparation method for high performance electrolytic copper foil, is characterized in that comprising the steps and processing condition:
The first step, electrolyte level, between cathode roller and positive plate, cathode roller of foil manufacturing machine cylinder and positive plate arranges magnetic pole, forms the complementary field that magneticstrength is 1.2T between cathode roller and anode; Magnetic field is 60 ° with deposition direction of an electric field relative orientation angle;
Second step, cathode roller starts to rotate, and adopts roll-type continuous electrolysis method under Electric and magnetic fields acting in conjunction, to generate continuous electrolysis Copper Foil, drum rotational speed 3 ms/min, current density 7000A/m
2, electrolyte temperature is 50 DEG C, and preparing thickness is 12 microns, hair side roughness R
zit is the electrolytic copper foil of 3.
Embodiment six
A preparation method for high performance electrolytic copper foil, is characterized in that comprising the steps and processing condition:
The first step, electrolyte level, between cathode roller and positive plate, cathode roller of foil manufacturing machine cylinder and positive plate arranges magnetic pole, forms the complementary field that magneticstrength is 1.0T between cathode roller and anode; Magnetic field is 20 ° with deposition direction of an electric field relative orientation angle;
Second step, cathode roller starts to rotate, and adopts roll-type continuous electrolysis method under Electric and magnetic fields acting in conjunction, to generate continuous electrolysis Copper Foil, drum rotational speed 7 ms/min, current density 5500A/m
2, electrolyte temperature 60 DEG C, preparing thickness is 10 microns, hair side roughness R
zit is the electrolytic copper foil of 3.5.
Embodiment seven
A preparation method for high performance electrolytic copper foil, is characterized in that comprising the steps and processing condition:
The first step, electrolyte level, between cathode roller and positive plate, cathode roller of foil manufacturing machine cylinder and positive plate arranges magnetic pole, forms the complementary field that magneticstrength is 1.3T between cathode roller and anode; Magnetic field is 70 ° with deposition direction of an electric field relative orientation angle;
Second step, cathode roller starts to rotate, and adopts roll-type continuous electrolysis method under Electric and magnetic fields acting in conjunction, to generate continuous electrolysis Copper Foil, drum rotational speed 9 ms/min, current density 6000A/m
2, electrolyte temperature 70 DEG C, preparing thickness is 9 microns, hair side roughness R
zit is the electrolytic copper foil of 2.5.
Embodiment eight
A preparation method for high performance electrolytic copper foil, is characterized in that comprising the steps and processing condition:
The first step, electrolyte level, between cathode roller and positive plate, cathode roller of foil manufacturing machine cylinder and positive plate arranges magnetic pole, forms the complementary field that magneticstrength is 0.6T between cathode roller and anode; Magnetic field is 70 ° with deposition direction of an electric field relative orientation angle;
Second step, cathode roller starts to rotate, and adopts roll-type continuous electrolysis method under Electric and magnetic fields acting in conjunction, to generate continuous electrolysis Copper Foil, drum rotational speed 4 ms/min, current density 6500A/m
2, electrolyte temperature is 50 DEG C, and preparing thickness is 7 microns, hair side roughness R
zit is the electrolytic copper foil of 3.5.
Embodiment nine
A preparation method for high performance electrolytic copper foil, is characterized in that comprising the steps and processing condition:
The first step, electrolyte level, between cathode roller and positive plate, cathode roller of foil manufacturing machine cylinder and positive plate arranges magnetic pole, forms the complementary field that magneticstrength is 1.3T between cathode roller and anode; Magnetic field is 30 ° with deposition direction of an electric field relative orientation angle;
Second step, cathode roller starts to rotate, and adopts roll-type continuous electrolysis method under Electric and magnetic fields acting in conjunction, to generate continuous electrolysis Copper Foil, drum rotational speed 6 ms/min, current density 4500A/m
2, electrolyte temperature 60 DEG C, preparing thickness is 9 microns, hair side roughness R
zit is the electrolytic copper foil of 3.
Embodiment ten
A preparation method for high performance electrolytic copper foil, is characterized in that comprising the steps and processing condition:
The first step, electrolyte level, between cathode roller and positive plate, cathode roller of foil manufacturing machine cylinder and positive plate arranges magnetic pole, forms the complementary field that magneticstrength is 1.4T between cathode roller and anode; Magnetic field is 75 ° with deposition direction of an electric field relative orientation angle;
Second step, cathode roller starts to rotate, and adopts roll-type continuous electrolysis method under Electric and magnetic fields acting in conjunction, to generate continuous electrolysis Copper Foil, drum rotational speed 10 ms/min, current density 7500A/m
2, electrolyte temperature is 50 DEG C, and preparing thickness is 7 microns, hair side roughness R
zit is the electrolytic copper foil of 2.
In a word; those skilled in the art although the present invention lists above-mentioned preferred implementation, should illustrate, although can carry out various change and remodeling; unless such change and remodeling deviate from scope of the present invention, otherwise all should be included in protection scope of the present invention.
Claims (4)
1. a preparation method for high performance electrolytic copper foil, is characterized in that comprising the steps and processing condition:
The first step, electrolyte level is between cathode roller and positive plate, the cathode roller and positive plate of raw paper tinsel machine arrange magnetic pole, complementary field is formed between cathode roller and positive plate, described complementary field acts on Copper Foil and starts crystallization to the whole deposition process peeled off, described complementary field intensity is adjustable from 0T to 1.4T, and described complementary field direction is adjustable to 80 ° from 0 ° with deposition direction of an electric field relative orientation angle;
Second step, cathode roller starts to rotate, and the rotating speed of cathode roller is 2 ~ 10 ms/min, and current density is 3500 ~ 8000A/m
2, electrolyte temperature is 50 ~ 70 DEG C, generates continuous print electrolytic copper foil, then peeled off from cathode roller by the electrolytic copper foil of generation under Electric and magnetic fields acting in conjunction at the surface crystallization of cathode roller.
2. the preparation method of high performance electrolytic copper foil according to claim 1, is characterized in that: described cathode roller rotating speed is 6 ms/min.
3. the preparation method of high performance electrolytic copper foil according to claim 2, is characterized in that: described current density is 5500A/m
2.
4. the preparation method of high performance electrolytic copper foil according to claim 3, is characterized in that: described electrolyte temperature is 60 DEG C.
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Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103397342B (en) * | 2013-08-19 | 2016-03-30 | 湖北中科铜箔科技有限公司 | A kind of high heat-resisting electrolytic copper foil and preparation method thereof |
| CN104485459B (en) * | 2014-11-13 | 2017-05-10 | 昆明理工大学 | Method for preparing copper foil for lithium ion battery through low eutectic type ionic liquid electro-deposition |
| CN105256331B (en) * | 2015-11-06 | 2017-10-31 | 清华大学 | A kind of electrolysis unit using magneto-electric coupled control oxygen bubbles motion |
| CN106245077B (en) * | 2016-07-18 | 2018-06-26 | 江苏大学 | A kind of taper magnetic field and the compound localization deposition process device of electric field |
| CN108425135B (en) * | 2017-02-15 | 2020-02-07 | 金居开发股份有限公司 | Production equipment of electrolytic copper foil and current adjusting and controlling device thereof |
| CN108251827A (en) * | 2018-01-25 | 2018-07-06 | 胡旭日 | A kind of anti-oxidation liquid of Chrome-free of lithium ion battery electrolytic copper foil and anti-oxidation technique |
| CN109208040B (en) * | 2018-11-02 | 2021-03-30 | 山东金盛源电子材料有限公司 | Composite additive for preparing low-roughness electrolytic copper foil |
| CN110205656A (en) * | 2019-06-06 | 2019-09-06 | 贵州中鼎高精铜箔制造有限公司 | A kind of fine roughening treatment technique of electrolytic copper foil surface |
| CN112695351A (en) * | 2020-12-18 | 2021-04-23 | 苏州天承化工有限公司 | Through hole electroplating method of printed circuit board |
| CN116607183B (en) * | 2023-06-07 | 2023-11-24 | 湖南龙智新材料科技有限公司 | Automatic control method and device for electrolytic copper foil |
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| CN101122035A (en) * | 2006-08-11 | 2008-02-13 | 财团法人工业技术研究院 | Method for manufacturing copper foil |
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