CN102383148A - Mixed additive for electrolytic copper foil, preparation method for mixed additive, and method for preparing ultralow-profile electrolytic copper foil - Google Patents
Mixed additive for electrolytic copper foil, preparation method for mixed additive, and method for preparing ultralow-profile electrolytic copper foil Download PDFInfo
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- CN102383148A CN102383148A CN2011103660813A CN201110366081A CN102383148A CN 102383148 A CN102383148 A CN 102383148A CN 2011103660813 A CN2011103660813 A CN 2011103660813A CN 201110366081 A CN201110366081 A CN 201110366081A CN 102383148 A CN102383148 A CN 102383148A
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Abstract
The invention provides a mixed additive for an ultralow-profile (VLP) electrolytic copper foil. The invention is characterized in that: each liter of mixed additive comprises 0.3 to 2g of Arabic gum (AG), 1 to 2.5g of hydroxyethylcellulose (HEC), 0.5 to 1.6g of gelatin (Glue), 0.5 to 1.5g of sodium dithiodipropane sulfonate (SPS) and 0.01 to 0.1g of ethylene thiourea (N). In the 12-micron VLP copper foil produced by the mixed additive, the tensile strength at normal temperature (23 DEG C) is more than 380 MPa; the elongation percentage at normal temperature is more than 6 percent; the tensile strength at high temperature (180 DEG C) is more than 200 MPa; and the elongation percentage at high temperature is more than 8 percent. The roughness Rz of the crystal growth surface (M surface) is 1.5 to 2.5 mu m. The mixed additive is particularly applicable to a flexible printed circuit board (FPC) and a lithium ion battery.
Description
Technical field
The present invention relates to a kind of ultralow profile electrolytic copper foil with mixed additive and compound method thereof, belong to the high-precision electrolytic copper foil technical field of producing.
Background technology
Flexible print wiring board (Flexible Printed Circuit; FPC); Be called for short soft board; Have advantages such as softness, light, thin and deflection, fast under light, thin, short, the little trend of trend, be widely used in products such as notebook computer, digital camera, mobile phone, pick up camera, liquid-crystal display at the information electronic product.China is the second largest printed circuit board big export country that is only second to after the Japan; Degree of integration increase along with printed circuit board; Electronic circuit trends towards high meticulous and high-density; Signal transmission frequencies is increasingly high, and this Copper Foil that require to use must have excellent etching, oxidation-resistance, unit elongation, ultralow characteristics such as surface profile.At present, the production technology of domestic high-grade electrolytic copper foil is compared with the U.S., Japan and is had big gap, has caused high-grade Copper Foil mainly to rely on the situation of import.
Current FPC production technology trends towards graph thinning and slimming; The target of graph thinning is to draw close to semiconductor technology, develops to minimum 10 μ m pitches (each 5 μ m of live width/line-spacing) direction, and slimming is the FPC of thin paper type; Thinner than present 25 μ m PI, and can be fit to the high frequency performance requirement.Halogen is generally used with the matrix resin that can be recycled, nano composite material etc., and the FPC base material is had higher requirement.
Electrolytic copper foil is one of main raw material of producing of PCB, and its manufacture craft has two kinds of rolling process and electrolytic process, and rolled copper foil has bigger advantage in performances such as unit elongation, anti-bendings, makes former FPC manufacturer only use rolled copper foil.In recent years, along with the raising of electrolytic copper foil production technology, Japanese part Copper Foil producer had developed and had satisfied the electrolytic copper foil that FPC requires.Because the lifting of electrolytic copper foil manufacturing technology and advantage in price, the increasing FPC that is applied to of electrolytic copper foil, and the development trend of the rolled copper foil of alternative same specification is arranged.
FPC uses electrolytic copper foil, and its main characteristic is low profile, high-elongation and high-tensile, and this all helps improving anti-bending (MIT) performance.The surfaceness of Copper Foil is low more, and the mechanical thickness of processing FPC can reduce, and MIT property can significantly improve.Higher unit elongation, the copper in the time of can effectively solving the FPC bending splits problem.High-tensile then can improve the Copper Foil fatigue property.In general, high-end FPC is with ultralow profile electrolytic copper foil, and surfaceness Rz is below 2.5 μ m, and thickness is also many at 9-12 μ m.The technological difficulties of producing are the electrolysis hair paper tinsel and the process for treating surface of high uniformity.
For general electrolysis hair paper tinsel (like STD, HTE paper tinsel), its tensile strength and unit elongation are inversely proportional to, and FPC requires to guarantee advantages of higher tensile strength and unit elongation simultaneously with paper tinsel, must use special mixed additive to control.The surface-treated technological difficulties, what be to solve the ultra-thin ultralow profile of 9-12 μ m (VLP) Copper Foil skids problems such as foldover.
Current, domestic VLP electrolytic copper foil also mainly be lithium ion battery with two-sided smooth Copper Foil, FPC does not also have important breakthrough technically with the electrolytic copper foil of VLP.
Summary of the invention
The purpose of this invention is to provide and a kind ofly be intended to solve FPC and use mixed additive with the ultralow profile electrolytic copper foil of ultralow profile, high-tensile and the high-elongation problem of Copper Foil; The method that the compound method of this additive also is provided simultaneously and utilizes the ultralow profile electrolytic copper foil of its production, through mixed additive of the present invention can access excellent property FPC with ultralow profile electrolytic copper foil.
The present invention realizes through following technical scheme:
Electrolytic copper foil is used mixed additive, and its special character is that its raw material comprises Sudan Gum-arabic AG, Natvosol HEC, gelatin Glue, dimercapto two propane sulfonic acid sodium SPS and ethylene thiourea N.
The consumption of above-mentioned raw materials is to contain in the aqueous solution of every liter of mixed additive:
Sudan Gum-arabic 0.3~2g
Natvosol 1~2.5g
Gelatin 0.5~1.6g
Dimercapto two propane sulfonic acid sodium 0.5~1.5g
Ethylene thiourea 0.01~0.1g
Above-mentioned electrolytic copper foil is following with the compound method of mixed additive:
1,, be to stir in 50~55 ℃ the 0.25L water it fully to be dissolved in 15 minutes in temperature at first with Sudan Gum-arabic 0.3~2g, dimercapto two propane sulfonic acid sodium 0.5~1.5g, ethylene thiourea 0.01~0.1g uniform mixing;
2, be to stir in 65~70 ℃ the 0.3L water it fully to be dissolved in 15 minutes with Natvosol 1~2.5g in temperature then;
Secondly 3, gelatin 0.5~1.6g is stirred in temperature is 45~50 ℃ 0.35L water and it was fully dissolved in 30 minutes;
4, the solution that at last above-mentioned three steps is obtained mixes, and adds water to 1L, stirs 10 minutes, remain on 50~55 ℃ subsequent use.
Above-mentioned mixed additive is used to prepare the method for ultralow profile electrolytic copper foil, and its special character is to comprise the steps:
At Cu
2+85~90 g/L, H
2SO
4120~130 g/L, Cl
-20~60 ppm, flow 60~90 m
3/ h in the solution that temperature is 45~60 ℃, adds mixed additive of the present invention with the speed of 80~120 ml/min, uses the drum type titanium tube of rotation continuously to be negative electrode, uses the arc titanium to be coated with iridium (DSA) anode, is 60~75 A/dm in current density
2Electrodeposit metals copper under the condition continues to peel off and obtains the ultralow profile electrolytic copper foil of 12 μ m.
Ultralow its normal temperature of profile electrolytic copper foil (23 ℃) tensile strength that obtains is greater than 380 MPa; The normal temperature unit elongation is greater than 6 %; High temperature (180 ℃) tensile strength is greater than 200 MPa, and the high temperature unit elongation is greater than 8 %, and crystal growth face (M face) roughness Rz is at 1.5~2.5 μ m.
Advantage of the present invention is more to access the ultra-thin ultralow profile Copper Foil of the outstanding 9-12 μ m of performance, is specially adapted to FPC and lithium ion battery, in the production of reality, is easy to control.Higher unit elongation and ultralow surface profile, help to improve FPC resistance to bend(ing) can, be particularly suitable for making the winding displacement of slide phone, folding digital camera, notebook computer.
Description of drawings
The SEM photo of the ultra-thin ultralow profile electrolysis hair paper tinsel of 12 μ m of Fig. 1 Additive Production of the present invention
The ultra-thin ultralow profile FPC of 12 μ m of Fig. 2 Additive Production of the present invention is with the SEM photo of Copper Foil.
Embodiment
Below providing embodiment of the present invention is used for the present invention is further described.
Embodiment 1
Electrolytic copper foil is used mixed additive, and the raw material that comprises in the aqueous solution of every liter of mixed additive has: Sudan Gum-arabic 1.0g, Natvosol 1.5g, gelatin 0.8g, dimercapto two propane sulfonic acid sodium 0.8g, ethylene thiourea 0.02g.
Embodiment 2
Electrolytic copper foil is used mixed additive, and the raw material that comprises in the aqueous solution of every liter of mixed additive has: Sudan Gum-arabic 0.5g, Natvosol 2.5g, gelatin 1.2g, dimercapto two propane sulfonic acid sodium 1.2g, ethylene thiourea 0.05g.
Embodiment 3
Electrolytic copper foil is used mixed additive, and the raw material that comprises in the aqueous solution of every liter of mixed additive has: Sudan Gum-arabic 1.6g, Natvosol 2.0g, gelatin 1.0g, dimercapto two propane sulfonic acid sodium 1.0g, ethylene thiourea 0.03g.
Embodiment 4
Electrolytic copper foil is used mixed additive, and the raw material that comprises in the aqueous solution of every liter of mixed additive has: Sudan Gum-arabic 0.8g, Natvosol 1.2g, gelatin 1.4g, dimercapto two propane sulfonic acid sodium 0.75g, ethylene thiourea 0.06g.
Embodiment 5
Electrolytic copper foil is used mixed additive, and the raw material that comprises in the aqueous solution of every liter of mixed additive has: Sudan Gum-arabic 0.6g, Natvosol 1.0g, gelatin 0.6g, dimercapto two propane sulfonic acid sodium 1.3g, ethylene thiourea 0.04g.
Embodiment 6
Electrolytic copper foil is used mixed additive, and the raw material that comprises in the aqueous solution of every liter of mixed additive has: Sudan Gum-arabic 0.3g, Natvosol 1.0g, gelatin 0.5g, dimercapto two propane sulfonic acid sodium 0.5g, ethylene thiourea 0.01g.
Embodiment 7
Electrolytic copper foil is used mixed additive, and the raw material that comprises in the aqueous solution of every liter of mixed additive has: Sudan Gum-arabic 2g, Natvosol 2.5g, gelatin 1.6g, dimercapto two propane sulfonic acid sodium 1.5g, ethylene thiourea 0.1g.
Comparative example 1
Electrolytic copper foil is used mixed additive, and the raw material that comprises in the aqueous solution of every liter of mixed additive has: gelatin 2.5g, Natvosol 1.5g, dimercapto two propane sulfonic acid sodium 0.8g.
Comparative example 2
Electrolytic copper foil is used mixed additive, and the raw material that comprises in the aqueous solution of every liter of mixed additive has: gelatin 3.5g, Natvosol 2.0g, dimercapto two propane sulfonic acid sodium 1.2g.
Following table provides the embodiment and the performance of Additive Production 12 μ m VLP Copper Foils of the present invention, further specifies technical solution of the present invention.
The aqueous solution with preparation 100L mixed additive is example, and the compound method of mixed additive of the present invention is following:
1,, be to stir in 50~55 ℃ the 25L water it fully to be dissolved in 15 minutes in temperature at first with Sudan Gum-arabic 30~200g, dimercapto two propane sulfonic acid sodium 50~150g, ethylene thiourea 1~10g uniform mixing;
2, be to stir in 65~70 ℃ the 30L water it fully to be dissolved in 15 minutes with Natvosol 100~250g in temperature then;
Secondly 3, gelatin 50~160g is stirred in temperature is 45~50 ℃ 35L water and it was fully dissolved in 30 minutes;
4, the solution that at last above-mentioned three steps is obtained mixes, and adds water to 100L, stirs 10 minutes, remain on 50~55 ℃ subsequent use.
Above-mentioned mixed additive is used to prepare the method for ultralow profile electrolytic copper foil, comprises the steps:
At Cu
2+88g/L, H
2SO
4125 g/L, Cl
-25 ppm, flow 85 m
3/ h; In the solution that temperature is 55 ℃, add mixed additive of the present invention with the speed of 80~120 ml/min, use diameter be 2700 mm, wide be 1400 mm continuously the drum type titanium tube of rotation be negative electrode; Using the arc titanium to be coated with iridium (DSA) anode, is 60~75 A/dm in current density
2Electrodeposit metals copper under the condition continues to peel off and obtains the former paper tinsel of 12 μ m VLP (being ultralow profile electrolytic copper foil).
Its normal temperature of former paper tinsel (23 ℃) tensile strength that obtains is greater than 380 MPa, and the normal temperature unit elongation is greater than 6 %, and high temperature (180 ℃) tensile strength is greater than 200 MPa, and the high temperature unit elongation is greater than 8 %, and crystal growth face (M face) roughness Rz is at 1.5~2.5 μ m.
Mixed additive of the present invention, it consists of Sudan Gum-arabic (AG, 0.3-2 g/L), Natvosol (HEC; 1-2.5 g/L), gelatin (Glue; 0.5-1.6 g/L), dimercapto two propane sulfonic acid sodium (SPS, 0.5-1.5 g/L), ethylene thiourea (N, 0.01-0.1 g/L).Increase the concentration of Sudan Gum-arabic, help improving the unit elongation of Copper Foil, increase the copper foil surface roughness.Increase the concentration of Natvosol, can reduce the tensile strength of Copper Foil, improve the high temperature unit elongation, reduce surfaceness.Increase the concentration of dimercapto two propane sulfonic acid sodium, help improving normal temperature, the high temperature tensile strength of Copper Foil, reduce the normal temperature unit elongation, the surfaceness of Copper Foil can significantly reduce.Increase the content of ethylene thiourea, the tensile strength of the Copper Foil that can increase sharply, the too much affiliation that adds causes the normal temperature unit elongation to descend rapidly.
Additive of the present invention also is used to produce two-sided smooth lithium ion battery and uses electrolytic copper foil.
Claims (5)
1. electrolytic copper foil is used mixed additive, it is characterized in that, raw material comprises Sudan Gum-arabic AG, Natvosol HEC, gelatin Glue, dimercapto two propane sulfonic acid sodium SPS and ethylene thiourea N.
2. electrolytic copper foil is used mixed additive according to claim 1, it is characterized in that the consumption of above-mentioned raw materials does, contains in the aqueous solution of every liter of mixed additive:
Sudan Gum-arabic 0.3~2g
Natvosol 1~2.5g
Gelatin 0.5~1.6g
Dimercapto two propane sulfonic acid sodium 0.5~1.5g
Ethylene thiourea 0.01~0.1g.
3. claim 1 or 2 said electrolytic copper foils are following with the compound method of mixed additive:
1), at first with Sudan Gum-arabic 0.3~2g, dimercapto two propane sulfonic acid sodium 0.5~1.5g, ethylene thiourea 0.01~0.1g uniform mixing, be to stir in 50~55 ℃ the 0.25L water it fully to be dissolved in 15 minutes in temperature;
2) be to stir in 65~70 ℃ the 0.3L water it fully to be dissolved in 15 minutes with Natvosol 1~2.5g in temperature then;
Secondly 3), gelatin 0.5~1.6g is stirred in temperature is 45~50 ℃ 0.35L water and it was fully dissolved in 30 minutes;
4), the solution that at last above-mentioned three steps obtained mixes, and adds water to 1L, stirs 10 minutes, remain on 50~55 ℃ subsequent use.
4. claim 1 or 2 said mixed additives are used to prepare the method for ultralow profile electrolytic copper foil, it is characterized in that comprising the steps:
At Cu
2+85~90 g/L, H
2SO
4120~130 g/L, Cl
-20~60 ppm, flow 60~90 m
3/ h in the solution that temperature is 45~60 ℃, adds mixed additive of the present invention with the speed of 80~120 ml/min, uses the drum type titanium tube of rotation continuously to be negative electrode, uses the arc titanium to be coated with the iridium anode, is 60~75 A/dm in current density
2Electrodeposit metals copper under the condition continues to peel off and obtains the ultralow profile electrolytic copper foil of 12 μ m.
5. be used to prepare the method for ultralow profile electrolytic copper foil like the said mixed additive of claim 4; Ultralow its room temperature tensile strength of profile electrolytic copper foil that it is characterized in that obtaining is greater than 380 MPa; The normal temperature unit elongation is greater than 6 %; High temperature tensile strength is greater than 200 MPa, and the high temperature unit elongation is greater than 8 %, and crystal growth surface roughness Rz is at 1.5~2.5 μ m.
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CN103074657A (en) * | 2013-02-26 | 2013-05-01 | 灵宝华鑫铜箔有限责任公司 | Additive for electrolytic copper foil and production process of electrolytic copper foil for 7-mu. m double-light lithium ion battery |
CN103173812A (en) * | 2013-03-21 | 2013-06-26 | 山东金宝电子股份有限公司 | Mixed additive for removing internal stress of electrolytic copper foil and method for producing low-stress copper foil |
CN103834972A (en) * | 2014-02-10 | 2014-06-04 | 东莞华威铜箔科技有限公司 | Additive for 4-micrometre carrier-free electrolytic copper foil, preparation method and application thereof |
CN104762642A (en) * | 2015-03-31 | 2015-07-08 | 灵宝华鑫铜箔有限责任公司 | Production process of electrolytic copper foil with low warping degree |
CN106350836A (en) * | 2016-08-29 | 2017-01-25 | 灵宝华鑫铜箔有限责任公司 | Additive for electrodeposited copper foil and production technology for preparing electrodeposited copper foil for double-shiny battery |
CN106637308A (en) * | 2016-11-16 | 2017-05-10 | 山东金宝电子股份有限公司 | Mixing additive for electrolytic profile-free copper foil and method thereof for preparing electrolytic copper foil |
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CN103074657B (en) * | 2013-02-26 | 2015-07-29 | 灵宝华鑫铜箔有限责任公司 | A kind of additive for electrolytic copper foil and 7 μm of two light lithium ion battery electrolytic copper foil production technique |
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CN103834972A (en) * | 2014-02-10 | 2014-06-04 | 东莞华威铜箔科技有限公司 | Additive for 4-micrometre carrier-free electrolytic copper foil, preparation method and application thereof |
CN104762642A (en) * | 2015-03-31 | 2015-07-08 | 灵宝华鑫铜箔有限责任公司 | Production process of electrolytic copper foil with low warping degree |
CN106350836A (en) * | 2016-08-29 | 2017-01-25 | 灵宝华鑫铜箔有限责任公司 | Additive for electrodeposited copper foil and production technology for preparing electrodeposited copper foil for double-shiny battery |
CN106637308A (en) * | 2016-11-16 | 2017-05-10 | 山东金宝电子股份有限公司 | Mixing additive for electrolytic profile-free copper foil and method thereof for preparing electrolytic copper foil |
CN106637308B (en) * | 2016-11-16 | 2019-07-09 | 山东金宝电子股份有限公司 | Electrolysis is without profile copper foil additive package and the method for preparing electrolytic copper foil with it |
CN109750334A (en) * | 2019-02-28 | 2019-05-14 | 灵宝华鑫铜箔有限责任公司 | A kind of production technology of 6 μm of double light high tensile additive for electrolytic copper foil and the electrolytic copper foil |
CN112301382A (en) * | 2020-09-07 | 2021-02-02 | 浙江大学 | Preparation method of high-ductility low-profile electrolytic copper foil |
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Application publication date: 20120321 |