CN102995086A - Additive for producing low-profile electrolytic copper foil and production process - Google Patents
Additive for producing low-profile electrolytic copper foil and production process Download PDFInfo
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- CN102995086A CN102995086A CN2012105308537A CN201210530853A CN102995086A CN 102995086 A CN102995086 A CN 102995086A CN 2012105308537 A CN2012105308537 A CN 2012105308537A CN 201210530853 A CN201210530853 A CN 201210530853A CN 102995086 A CN102995086 A CN 102995086A
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- copper foil
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- electrolytic copper
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- profile
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 61
- 239000011889 copper foil Substances 0.000 title claims abstract description 48
- 239000000654 additive Substances 0.000 title claims abstract description 38
- 230000000996 additive effect Effects 0.000 title claims abstract description 38
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- CNLHIRFQKMVKPX-UHFFFAOYSA-N 1,1-diethylthiourea Chemical compound CCN(CC)C(N)=S CNLHIRFQKMVKPX-UHFFFAOYSA-N 0.000 claims abstract description 5
- 125000000217 alkyl group Chemical group 0.000 claims abstract description 5
- 239000010949 copper Substances 0.000 claims description 21
- 239000008151 electrolyte solution Substances 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 15
- OBDVFOBWBHMJDG-UHFFFAOYSA-N 3-mercapto-1-propanesulfonic acid Chemical compound OS(=O)(=O)CCCS OBDVFOBWBHMJDG-UHFFFAOYSA-N 0.000 claims description 4
- 230000032696 parturition Effects 0.000 claims description 2
- 239000004353 Polyethylene glycol 8000 Substances 0.000 abstract 1
- 229920002873 Polyethylenimine Polymers 0.000 abstract 1
- 229940085678 polyethylene glycol 8000 Drugs 0.000 abstract 1
- 235000019446 polyethylene glycol 8000 Nutrition 0.000 abstract 1
- FRTIVUOKBXDGPD-UHFFFAOYSA-M sodium;3-sulfanylpropane-1-sulfonate Chemical compound [Na+].[O-]S(=O)(=O)CCCS FRTIVUOKBXDGPD-UHFFFAOYSA-M 0.000 abstract 1
- 229920002554 vinyl polymer Polymers 0.000 abstract 1
- 229910052802 copper Inorganic materials 0.000 description 13
- 238000000576 coating method Methods 0.000 description 10
- 239000007788 liquid Substances 0.000 description 10
- 230000000704 physical effect Effects 0.000 description 10
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 9
- 239000011248 coating agent Substances 0.000 description 8
- 239000000203 mixture Substances 0.000 description 8
- 238000009472 formulation Methods 0.000 description 7
- 238000002360 preparation method Methods 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 238000005868 electrolysis reaction Methods 0.000 description 4
- 229910001416 lithium ion Inorganic materials 0.000 description 4
- 238000002425 crystallisation Methods 0.000 description 3
- 230000008025 crystallization Effects 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 238000004381 surface treatment Methods 0.000 description 3
- 239000010936 titanium Substances 0.000 description 3
- 229910052719 titanium Inorganic materials 0.000 description 3
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 2
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 2
- 108010010803 Gelatin Proteins 0.000 description 2
- 241000784732 Lycaena phlaeas Species 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229920000159 gelatin Polymers 0.000 description 2
- 239000008273 gelatin Substances 0.000 description 2
- 235000019322 gelatine Nutrition 0.000 description 2
- 235000011852 gelatine desserts Nutrition 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000012856 packing Methods 0.000 description 2
- 238000004062 sedimentation Methods 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 1
- 229920002594 Polyethylene Glycol 8000 Polymers 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 229910000365 copper sulfate Inorganic materials 0.000 description 1
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 description 1
- 229960004643 cupric oxide Drugs 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 229910052741 iridium Inorganic materials 0.000 description 1
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- -1 polyoxyethylene Polymers 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 238000007581 slurry coating method Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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Abstract
The invention relates to low-profile electrolytic copper foil, particularly relates to an additive for producing the low-profile electrolytic copper foil, and also relates to a production process. The additive for producing the low-profile electrolytic copper foil is mixed by the following components: 0.2-0.4 part of sodium 3-mercapto-1-propanesulfonate; 0.8-1.2 part of polyvinyl alkylimine or polyethyleneimine alkyl compounds; 1.0-2.0 parts of polyethylene glycol 8000; 0.08-0.12 part of N,N-diethyl thiourea; and 20 parts of pure water. Electrolytic copper foil produced by the additive and the production process of the invention can not only maintain a low profile tolerance and low impedance, but also maintain high peel strength, and also is suitable for the manufacture of interior and exterior lines.
Description
Technical field
The present invention relates to a kind of low profile electrolytic copper foil, particularly produce the additive that the low profile electrolytic copper foil is used, also relate to its production technique.
Background technology
Various dissimilar electrolytic copper foils, anode surface (being commonly called as hair side) structure to Copper Foil has different requirements, in process of production, Copper Foil anode surface structure is mainly by additive control, by adjusting prescription or the proportioning of additive, form a complete production network with suitable production technique, can obtain the Copper Foil of different crystallization modes and hair side structure.
CCL, PCB has strict demand with the anode surface profile tolerance of high-grade electrolytic copper foil, 3～5 μ m are comparatively suitable for Rz value general requirement, and to guarantee higher peel strength, if with low profile electrolytic copper foil explained hereafter very, although profile tolerance very low (about Rz value 1～3 μ m), but peel strength meeting decrease, when making outer-layer circuit, the circuit obscission can occur, thus be not suitable for the application of outer-layer circuit, and produce with ordinary process, although peel strength is higher, but profile tolerance too high (about Rz value＞6 μ m), make circuit after, the impedance of circuit is higher under identical condition.This is because the high-frequency signals energy that RCA transmits concentrates in the thin layer of conductive line surfaces mostly, Here it is so-called " surface action ", be the most Copper Foil crest line zones (anode surface) of concentrating online root of electric current of plate upper thread road signal, so the roughness of line root can not be too high, so could under lower resistance, reduce the loss of transmitting energy.
The lithium ion battery negative carrier has strict demand equally to electrolytic copper foil anode surface profile tolerance, when profile tolerance is too high, the anode surface that is the mountain peak shape, can cause producing the space between negative pole coating and peak valley, because coating is that certain granularity is arranged, general peak valley shape all is " V " font, so negative pole coating can't arrive the lowermost end of peak valley, form the space, thereby increase the internal resistance of cell; When profile tolerance is excessively low, when anode surface is mirror shape, the sticking power between coating and Copper Foil is declined to a great extent, coating can not occur in the coating process, or behind the coating Paint Falling phenomenon occurs.So lithium ion battery must be controlled at certain limit with the anode surface profile tolerance of electrolytic copper foil.
Summary of the invention
Technical problem to be solved by this invention provides a kind of additive that low profile degree electrolytic copper foil is used of producing, its production technique also is provided, electrolytic copper foil with this additive and production technique production, not only can keep low profile degree and low resistance, simultaneously higher peel strength can also be guaranteed, the making of ectonexine circuit can be applicable to simultaneously.
The technical scheme that the present invention solves the problems of the technologies described above is:
A kind of production low profile additive for electrolytic copper foil is mixed by the component of following mass fraction:
3-sulfydryl-1-propanesulfonate (code name MPS), 0.2～0.4 part;
Polymine alkyl salt or polymine alkylate (code name P), 0.8～1.2 part;
PEG 8000) (code name PN), 1.0～2.0 parts;
N, N-diethyl thiourea (code name N), 0.08～0.12 part;
Pure water, 20 parts.
Above-mentioned each component acting as at electrolytic process:
MPS-as grain-refining agent, make the copper crystallization careful and fine and close, and be improved the effect of current density; Its molecular formula is as follows:
PN-enhancing cathodic polarization improves the copper crystallization profile tolerance in low current density district, makes the copper foil surface uniform crystal particles;
P-nonionic surface active agent can make coating more even, avoids producing the mass defects such as pin hole, pit;
N-leveling agent, the whole profile tolerance that reduces Copper Foil crystal grain reaches the low profile effect.
Further, the mass fraction of each component is preferably:
3-sulfydryl-1-propanesulfonate, 0.3 part;
Polymine alkyl salt or polymine alkylate, 1 part;
PEG 8000,1.5 parts;
N, N-diethyl thiourea, 0.1 part;
Pure water, 20 parts.
The production technique of above-mentioned Additive Production low profile electrolytic copper foil is: described additive is added in the electrolytic solution, and the additive add-on is 0.5ml/L electrolytic solution; In the described electrolytic solution, Cu=70～100g/L, H
2SO
4=80～110g/L, Cl
-=30～60mg/L; Temperature is 50～60 ℃; Giving birth to the paper tinsel current density is 60～80A/dm
2
The present invention has following beneficial effect:
The low profile electrolytic copper foil that uses this additive formulations and production technique to produce, the anode surface profile tolerance is low, not surface treated Copper Foil anode surface roughness Rz value is about 2～4 μ m, crystal grain is more careful, and use gelatin and hydroxylated cellulose are as the ordinary student production art of additive, the electrolytic copper foil product anode surface crystalline-granular texture that produces is the mountain peak shape, and its Rz value is generally more than 5 μ m.
Amplifying 3000 times of pictures by microscope can find out, use patent production Copper Foil anode surface profile tolerance of the present invention more smooth, the peak valley degree of depth is more shallow and round and smooth, without " V " font peak and valley structure of common Copper Foil, the former paper tinsel of this kind structure is after surface treatment, can keep low profile degree and higher peel strength, can be applicable to simultaneously multiple-plate ectonexine circuit and make, and after making circuit, the impedance of circuit is low; And as the negative pole carrier of lithium ion battery, slurry and Copper Foil bounding force are large, after coating process or the coating, obscission can not occur.And the Copper Foil hair side profile tolerance that ordinary process is produced is high, and the peak valley degree of depth is darker, and the lowest point forms very tiny slit, and after the Copper Foil of these structures was made into circuit, although peel strength is high, impedance was large, was unfavorable for the making of HF link plate; During as the negative pole carrier of lithium ion battery, produce easily the space after the slurry coating between Copper Foil and slurry, increase the internal resistance of cell.
Utilize above-mentioned additive and production technique to produce former paper tinsel, its physical property can reach such as the following table scope:
Description of drawings
Fig. 1 is 3000 times of enlarged photographs of the electrolytic copper foil of embodiment 1 production.
Fig. 2 is 3000 times of enlarged photographs of the electrolytic copper foil of embodiment 2 productions.
Fig. 3 is 3000 times of enlarged photographs of the electrolytic copper foil of embodiment 3 productions.
Fig. 4 is 3000 times of enlarged photographs of the electrolytic copper foil of embodiment 4 productions.
Fig. 5 is 3000 times of enlarged photographs of the electrolytic copper foil of embodiment 5 productions.
Fig. 6 is 3000 times of enlarged photographs of the electrolytic copper foil of Comparative Examples example 1 production.
Embodiment
The production of electrolytic copper foil is given birth to paper tinsel, surface treatment, is cut packing department and form by molten copper liquid, electrolysis, and the present invention mainly uses at molten copper liquid and electrolysis and gives birth to paper tinsel workshop section, surface treatment with cut packing department and do not relate to.
Molten copper liquid: the idiographic flow of molten copper liquid is:
In copper dissolving tank, stack a certain amount of high-purity copper cash, vitriolated solution is arranged in the container for storing liquid, by heat exchanger solution temperature is adjusted to 50 ~ 60 ℃, with pump delivery to the copper dissolving tank shower, shower with vitriolated solution spraying to copper line surface, and the temperature of utilizing spray liquid constantly oxidation in air, the cupric oxide of its generation is constantly dissolved, generate copper-bath, be back in the container for storing liquid.Copper sulfate electrolyte in the container for storing liquid is regulated temperature (50 ~ 60 ℃) and twice filtration through over-heat-exchanger, is delivered in the clean liquid bath, adds additive of the present invention in clean liquid bath, is delivered to living paper tinsel machine after stirring.
Paper tinsel is given birth in electrolysis: it namely is a kind of electrolytic process that the paper tinsel process is given birth in electrolysis, and it is finished in electrolyzer.The general titanium matter surface roller of being made by special-purpose titanium material that adopts is as cathode roller, and the titanium material that is coated with iridium, tantalum mixture take the surface is anode, and the copper-bath that contains additive is delivered between the anode and cathode, is 60A～80A/dm in current density
2Under the direct current effect, just there is metallic copper to separate out on the cathode roller, additive in the electrolytic solution begins to have an effect at this moment, as control nucleus formation speed, grain growing speed, reduce the sedimentation velocity of high current density region, accelerate the sedimentation velocity in low current density district etc., make the anode surface structure of Copper Foil reach the low profile effect.Along with the continuous rotation of cathode roller, copper is constantly separated out at roll surface, and constantly the metallic copper of separating out is peeled off from roll surface, through washing, oven dry, twines rolling again, and this has just formed former paper tinsel.Regulate the different rotating speeds of cathode roller, just produce the former paper tinsel of different thickness.
The present invention will be described in detail below in conjunction with drawings and Examples.
Embodiment one
1, additive formulations: additive is in the mass fraction ratio preparation of MPS:PN:P:N: water=0.3:1:1.5:0.1:20, and add-on is 0.5ml/L electrolytic solution.
2, electrolytic solution technic index: Cu=70～100g/L, H
2SO
4=80～110g/L, Cl
-=30～60mg/L, temperature=50～60 ℃.
3, give birth to paper tinsel current density: 75A/dm
2
4, test-results:
A, physicals
B, surface tissue (3000X) are as shown in Figure 1.
C, interpretation of result: the physicals of Copper Foil reaches set quota, and anode surface Rz value is between 2 ~ 4 μ m, and the profile height is suitable, and the peak valley degree of depth is more shallow and round and smooth, without " V " font peak and valley structure of common Copper Foil, is optimum structure of the present invention.
Embodiment two:
1, additive formulations: additive is in the mass fraction ratio preparation of MPS:PN:N: water=0.1:1:0.05:20, and add-on is 0.5ml/L electrolytic solution.
2, electrolytic solution technic index: Cu=70～100g/L, H
2SO
4=80～110g/L, Cl
-=30～60mg/L, temperature=50～60 ℃.
3, give birth to paper tinsel current density: 75A/dm
2
4, test-results:
A, physicals
B, surface tissue (3000X) are as shown in Figure 2.
C, interpretation of result: since in the additive without P (polyoxyethylene glycol), and MPS, N add-on are less, little space appears in the Copper Foil anode surface, the surface profile degree is larger, Testing Tensile Strength at Elevated Temperature and unit elongation are on the low side.
Embodiment three:
1, additive formulations: additive is in the mass fraction ratio preparation of MPS:PN:P:N: water=0.3:1:1.5:0.05:20, and add-on is 0.5ml/L electrolytic solution.
2, electrolytic solution technic index: Cu=70～100g/L, H
2SO
4=80～110g/L, Cl
-=30～60mg/L, temperature=50～60 ℃.
3, give birth to paper tinsel current density: 75A/dm
2
4, test-results:
A, physicals
B, surface tissue (3000X) are as shown in Figure 3.
C, interpretation of result: the N addition is less, and the anode surface profile tolerance is higher, and the Rz value is larger.
Embodiment four:
1, additive formulations: additive is in the mass fraction ratio preparation of MPS:PN:P:N: water=0.2:1:1.5:0.1:20, and add-on is 0.5ml/L.
2, electrolytic solution technic index: Cu=70～100g/L, H
2SO
4=80～110g/L, Cl
-=30～60mg/L, temperature=50～60 ℃.
3, give birth to paper tinsel current density: 75A/dm
2
4, test-results:
A, physicals
B, surface tissue (3000x) are as shown in Figure 4.
C, interpretation of result: the physicals of Copper Foil reaches set quota, and anode surface Rz value is between 2 ~ 4 μ m, and the profile height is suitable, and sample result is basic consistent with " embodiment one ".
Embodiment five:
1, additive formulations: additive is in the mass fraction ratio preparation of MPS:PN:P:N: water=0.3:0.5:1.5:0.1:20, and add-on is 0.5ml/L electrolytic solution.
2, electrolytic solution technic index: Cu=70～100g/L, H
2SO
4=80～110g/L, Cl
-=30～60mg/L, temperature=50～60 ℃.
3, give birth to paper tinsel current density: 75A/dm
2
4, test-results:
A, physicals
B, surface tissue (3000x) are as shown in Figure 5.
C, interpretation of result: the PN add-on is less, and the anode surface crystalline-granular texture is inhomogeneous, and it is larger part crystal grain to occur, causes whole Rz value bigger than normal.
Comparative Examples one:
1, additive formulations: additive is in gelatin: the mass fraction ratio preparation of Natvosol: water=1:0.1:10, add-on is 0.5ml/L electrolytic solution.
2, electrolytic solution technic index: Cu=70～100g/L, H
2SO
4=80～110g/L, Cl
-=30～60mg/L, temperature=50～60 ℃.
3, give birth to paper tinsel current density: 75A/dm
2
4, test-results:
A, physicals
B, surface tissue (3000x) are as shown in Figure 6.
C, interpretation of result: the physicals aspect, Testing Tensile Strength at Elevated Temperature and the unit elongation range of decrease are large, and roughness Rz value is higher, the anode surface coarse grains, profile tolerance is high, and intergranule has darker slit.
Claims (3)
1. produce the low profile additive for electrolytic copper foil for one kind, it is characterized in that, mixed by the component of following mass fraction:
3-sulfydryl-1-propanesulfonate, 0.2～0.4 part;
Polymine alkyl salt or polymine alkylate, 0.8～1.2 part;
PEG 8000,1.0～2.0 parts;
N, N-diethyl thiourea, 0.08～0.12 part;
Pure water, 20 parts.
2. production low profile additive for electrolytic copper foil according to claim 1 is characterized in that the mass fraction of each component is preferably:
3-sulfydryl-1-propanesulfonate, 0.3 part;
Polymine alkyl salt or polymine alkylate, 1 part;
PEG 8000,1.5 parts;
N, N-diethyl thiourea, 0.1 part;
Pure water, 20 parts.
3. a right to use requires the production technique of 1 or 2 described Additive Production low profile electrolytic copper foils, and it is characterized in that: described additive is added in the electrolytic solution, and the additive add-on is 0.5ml/L electrolytic solution; In the described electrolytic solution, Cu=70～100g/L, H
2SO
4=80～110g/L, Cl
-=30～60mg/L; Temperature is 50～60 ℃; Giving birth to the paper tinsel current density is 60～80A/dm
2
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| CN2012105308537A CN102995086A (en) | 2012-12-11 | 2012-12-11 | Additive for producing low-profile electrolytic copper foil and production process |
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| CN104313653A (en) * | 2014-09-22 | 2015-01-28 | 梅县金象铜箔有限公司 | Method for preparing electrolyte for copper foil electrolysis by using regenerated copper oxide |
| 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 |
| CN109267111A (en) * | 2018-12-06 | 2019-01-25 | 湖北工程学院 | Additive for electrolytic copper foil and its application, electrolytic copper foil and its preparation method and application, lithium ion battery |
| CN106480479B (en) * | 2016-10-12 | 2019-02-15 | 东莞华威铜箔科技有限公司 | Preparation method, product and its application of flexible additive for electrolytic copper foil |
| CN110016697A (en) * | 2019-05-22 | 2019-07-16 | 青海电子材料产业发展有限公司 | A kind of method and its additive preparing high temperature high-elongation power battery electrolytic copper foil |
| CN110042438A (en) * | 2019-04-24 | 2019-07-23 | 福建清景铜箔有限公司 | The preparation method of electrolytic copper foil |
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| CN111850620A (en) * | 2020-08-28 | 2020-10-30 | 江东电子材料有限公司 | A preparation method and preparation system of 4.5μm ultra-thin copper foil for lithium battery |
| CN115491729A (en) * | 2022-09-21 | 2022-12-20 | 九江德福科技股份有限公司 | Method for reducing pinholes of 4.5um lithium battery foil |
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Effective date of registration: 20151216 Address after: Town Guangdong city of Huizhou province Boluo County 516139 Luo Shun Applicant after: Huizhou Lianhe copper foil Electronic Material Co., Ltd. Address before: 516139 Guangdong city of Huizhou Province town Boluo County Shun cuff Management District Applicant before: United Copper Foils (Huizhou) Ltd. |