CN1995469A - High temperature high ductibility electrolytic copper foil production process - Google Patents
High temperature high ductibility electrolytic copper foil production process Download PDFInfo
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- CN1995469A CN1995469A CN 200610070550 CN200610070550A CN1995469A CN 1995469 A CN1995469 A CN 1995469A CN 200610070550 CN200610070550 CN 200610070550 CN 200610070550 A CN200610070550 A CN 200610070550A CN 1995469 A CN1995469 A CN 1995469A
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Abstract
The invention discloses a making technique of high-temperature high-extending electrolytic copper foil, which is characterized by the following: (1) (1) selecting the technical scale of electrolytic liquid; (2) affirming additive; (3) purifying electrolytic liquid; (4) selecting current density and polar distance.
Description
Technical field
The present invention relates to a kind of high temperature high ductibility electrolytic copper foil production process, belong to electrolytic copper foil manufacturing technology field.
Background technology
Electrolytic copper foil is the important materials of making printed circuit board (pcb).PCB is mainly used in fields such as robot calculator, Industry Control, aerospace and all consumer electrical equipment, and the high speed development of printed circuit board (pcb) industry technology and demand growing is to the electrolytic copper foil demands for higher performance.Particularly high-end multilayer circuit board industry development is swift and violent, because it is with high content of technology, the added value height is subjected to domestic and international board production producer and payes attention to, and will produce emphasis and begin to transfer to multilayer circuit board production, and multilayer circuit board market is understood increasing.
Though good market outlook and opportunity to develop are arranged, but multilayer circuit board is very high to the performance requriements of electrolytic copper foil, particularly the high temperature extension property to multilayer circuit inner cord electrolytic copper foil has proposed very high requirement, if the high temperature extension property is bad, the internal layer Copper Foil will occur and heat up or welding process generation copper foil circuit phenomenon of rupture, have a strong impact on the quality of circuit card through pressing plate repeatedly.The electrolytic copper foil that existing multilayer circuit board manufacturer uses is mostly from Copper Foil manufacturing enterprise imports such as Japan, Taiwan, and cost is higher.
Production method and additive that present domestic Copper Foil manufacturer adopts have nothing in common with each other, mostly adopt simple additive such as gelatin, hydrochloric acid, the high temperature unit elongation is generally less than 3%, such high temperature unit elongation can't satisfy the multilayer circuit board needs, is instant so develop a kind of new production high temperature high ductibility electrolytic copper foil technology.
Summary of the invention
The object of the invention is to provide a kind of can solve the low problem of high temperature ductility, can guarantee that also every performance of electrolytic copper foil is in the manufacturing process of the high temperature high ductibility electrolytic copper foil of steady state.
The manufacturing process of a kind of high temperature high ductibility electrolytic copper foil of the present invention, this technology are to adopt different technology and additive in the electrolytic copper foil manufacturing processed, and the high temperature extension performance of electrolytic copper foil is significantly improved.
High temperature high ductibility electrolytic copper foil production process of the present invention
One, electrolytic solution processing range: the production process of electrolytic copper foil is earlier cathode copper, the vitriol oil, soft water, vapor mixing to be dissolved, and generates copper-bath, enters and carries out electrolysis in the electrolyzer, generates Copper Foil, wherein, and Cu
2+: 90-140g/l, H
2SO
4: 140-200g/l, t:45-70 ℃, optimised process scope: Cu
2+: 100-130g/l, H
2SO
4: 150-180g/l, t:60-70 ℃;
Two, the selection of additive: in electrolytic solution, add additive continuously, can obtain the electrolytic copper foil of stable performance; Described additive is that one or more mixing among gelatin, Natvosol, Sodium dodecylbenzene sulfonate, propenyl thiocarbamide, polyacrylamide, the mixture A are used, wherein mixture A is a polyoxyethylene glycol PEG (ethylene oxide condensate, molecular weight 400-6000), the percentage mix of any two kinds or three kinds in the polyethers (vinyl carbinol polyoxy alkyl oxide), asccharin (o-benzoic sulfimide), polydithio-dipropyl sulfonic acid, casein food grade, direct water of the use of additive or electrolytic solution dissolving;
Three, electrolyte purification: total impurities is no more than 0.1% in the electrolytic solution, and electrolytic solution requires filtering accuracy to reach 0.1um, and the electrolytic solution activated carbon dosage is 1-3g/L days;
Four, electrolytic copper foil production current density is at 40-90A/dm
2, pole span in the 10-30mm scope, optimum current density at 50-80A/dm2, pole span at 15-25mm.
The composition of described additive and content are: gelatin 0.01～0.1g/L and mixture A 0.01～0.05g/L;
The composition of described additive and content are: propenyl thiocarbamide 0.01～0.1g/L, Sodium dodecylbenzene sulfonate 0.005～0.03g/L and mixture A 0.02～0.06g/L;
The composition of described additive and content are: gelatin 0.01～0.1g/L, Natvosol 0.01～0.05g/L and mixture A 0.01～0.05g/L;
The composition of described additive and content are: gelatin 0.01～0.1g/L, polyacrylamide 0.01～0.05g/L and mixture A 0.01～0.05g/L;
The composition of described additive and content are: mixture A 0.03～0.08g/L.
The present invention has following advantage:
1, this electrolytic copper foil production process, solution compolision: Cu
2+: 90-140g/L, H
2SO
4: 140-200g/L, current density 50-80A/dm
2All can produce qualified product;
2, this electrolytic copper foil production process adopts the method for adding continuously with additive, can obtain the electrolytic copper foil of stable performance;
3, this electrolytic copper foil production process is simple with the using method of additive, directly water or electrolytic solution dissolving;
4, the electrolytic copper foil Rz value of this electrolytic copper foil production process production is even, and aftertreatment lays the foundation to electrolytic copper foil;
5, electrolytic copper foil high temperature unit elongation＞6% of this electrolytic copper foil production process production, technology and additive control stabilization can reach more than 8%, high temperature unit elongation＞10% behind the employing composite additive.
The electrolytic copper foil that high temperature high ductibility electrolytic copper foil production process of the present invention is produced uses a kind of additive, high temperature unit elongation＞6%, use two kinds of additives, high temperature unit elongation＞8% uses three kinds of additives, wherein comprise a kind of in the composite additive of independent research and development, high temperature unit elongation＞10%; In the electrolytic copper foil manufacturing processed, adopt different technology and additive, the high temperature extension performance of electrolytic copper foil is significantly improved, not only solved the low problem of high temperature ductility, can guarantee that also other performances of electrolytic copper foil are in steady state.
Description of drawings
Fig. 1 is 2000 times of shape appearance figures of 18um electrolytic copper foil that this electrolytic copper foil manufacturing technology is produced;
Fig. 2 is 2000 times of shape appearance figures of 35um electrolytic copper foil that this electrolytic copper foil manufacturing technology is produced.
Embodiment
Embodiment one
The high temperature high ductibility electrolytic copper foil production process of present embodiment is as follows:
One, electrolytic solution technology: the production process of electrolytic copper foil is earlier cathode copper, the vitriol oil, soft water, vapor mixing to be dissolved, and generates copper-bath, enters and carries out electrolysis in the electrolyzer, generates Copper Foil, wherein, and Cu
2+: 90g/l, H
2SO
4: 200g/l, t:45 ℃;
Two, the selection of additive: in electrolytic solution, add additive continuously, can obtain the electrolytic copper foil of stable performance; Described additive is that one or more mixing among gelatin, Natvosol, Sodium dodecylbenzene sulfonate, propenyl thiocarbamide, polyacrylamide, the mixture A are used, wherein mixture A is a polyoxyethylene glycol PEG (ethylene oxide condensate, molecular weight 400-6000), the percentage mix of any two kinds or three kinds in the polyethers (vinyl carbinol polyoxy alkyl oxide), asccharin (o-benzoic sulfimide), polydithio-dipropyl sulfonic acid, casein food grade, direct water of the use of additive or electrolytic solution dissolving;
Three, electrolyte purification: total impurities is no more than 0.1% in the electrolytic solution, and electrolytic solution requires filtering accuracy to reach 0.1um, and the electrolytic solution activated carbon dosage is 1-3g/L days;
Four, electrolytic copper foil production current density 40A/dm
2, pole span 30mm.
The present embodiment electrolytic copper foil production process, electrolytic copper foil high temperature unit elongation＞6% of production.
Embodiment two
Present embodiment and embodiment one different being
One, electrolytic solution technology: Cu
2+: 140g/l, H
2SO
4: 140g/l, t:70 ℃;
Two, the selection of additive: in electrolytic solution, add additive continuously, can obtain the electrolytic copper foil of stable performance; Described additive is that 2 kinds of mixing of gelatin, Natvosol, Sodium dodecylbenzene sulfonate, propenyl thiocarbamide, polyacrylamide, mixture A are used, and the use of additive is directly dissolved with electrolytic solution;
Four, electrolytic copper foil production current density 90A/dm
2, pole span 15mm.
Electrolytic copper foil high temperature unit elongation＞8% of producing.
Embodiment three
Present embodiment and embodiment one different being
One, electrolytic solution technology: Cu
2+: 100g/l, H
2SO
4: 150g/l, t:60-70 ℃;
Two, the selection of additive: additive is that three kinds among gelatin, Natvosol, Sodium dodecylbenzene sulfonate, propenyl thiocarbamide, polyacrylamide, the mixture A mix use, and water dissolution is directly used in the use of additive;
Four, electrolytic copper foil production current density 50A/dm
2, pole span 20mm.
Electrolytic copper foil high temperature unit elongation＞10% of producing.
Embodiment four
Additive is formed: adding gelatin 0.01～0.1g/L and mixture A 0.01～0.05g/L can make electrolytic copper foil hair side crystallization refinement in electrolytic solution.
High temperature unit elongation test result mean value 9.5%.
Embodiment five
Additive is formed: add propenyl thiocarbamide 0.01～0.1g/L, Sodium dodecylbenzene sulfonate 0.005～0.03g/L and mixture A 0.02～0.06g/L and can make electrolytic copper foil hair side compact crystallization in electrolytic solution.
High temperature unit elongation test result mean value 12.8%.
Embodiment six
Additive is formed: add gelatin 0.01～0.1g/L, Natvosol 0.01～0.05g/L and mixture A 0.01～0.05g/L and can make the crystallization of electrolytic copper foil hair side fine and close more in electrolytic solution.
High temperature unit elongation test result mean value 13.2%.
Embodiment seven
Additive is formed: add gelatin 0.01～0.1g/L, polyacrylamide 0.01～0.05g/L and mixture A 0.01～0.05g/L and can make the crystallization of electrolytic copper foil hair side fine and close more in electrolytic solution.
High temperature unit elongation test result mean value 12.2%.
Embodiment eight
Additive is formed: add mixture A 0.03～0.08g/L and can make the crystallization of electrolytic copper foil hair side fine and close more in electrolytic solution.
High temperature unit elongation test result mean value 10.8%.
Because electrolytic copper foil is produced the equipment difference of each producer, used production technology also has nothing in common with each other, as long as adopt the electrolytic copper foil production technique of the art of this patent scheme, high temperature extension performance all can improve a lot.
The technology of the present invention has solved Copper Foil high temperature extension performance issue, but needs auxiliary infrared and ultra-violet analysis instrument in the control of the concentration analysis of additive.
Claims (7)
1, high temperature high ductibility electrolytic copper foil production process is characterized in that
(1), the electrolytic solution processing range: the production process of electrolytic copper foil is earlier with cathode copper, the vitriol oil, soft water, vapor mixing dissolving, generates copper-bath, enters and carries out electrolysis in the electrolyzer, generates Copper Foil, wherein, Cu
2+: 90-140g/l, H
2So
4: 140-200g/l, t:45-70 ℃;
(2), the selection of additive: in electrolytic solution, add additive continuously, can obtain the electrolytic copper foil of stable performance; Described additive is that one or more mixing among gelatin, Natvosol, Sodium dodecylbenzene sulfonate, propenyl thiocarbamide, polyacrylamide, the mixture A are used, wherein mixture A is a polyoxyethylene glycol PEG (ethylene oxide condensate, molecular weight 400-6000), the percentage mix of any two kinds or three kinds in the polyethers (vinyl carbinol polyoxy alkyl oxide), asccharin (o-benzoic sulfimide), polydithio-dipropyl sulfonic acid, casein food grade, the use of additive is directly with soft water or electrolytic solution dissolving;
(3), electrolyte purification: total impurities is no more than 0.1% in the electrolytic solution, and electrolytic solution requires filtering accuracy to reach 0.1um, and the electrolytic solution activated carbon dosage is 1-3g/L days;
(4), electrolytic copper foil production current density is at 40-90A/dm
2, pole span is in the 10-30mm scope.
2, the described high temperature high ductibility electrolytic copper foil production process of claim 1 is characterized in that
(1), electrolytic solution processing range: optimised process scope: Cu
2+: 100-130g/l, H
2So
4: 150-180g/l, t:60-70 ℃;
(4), electrolytic copper foil produce optimum current density at 50-80A/dm2, pole span at 15-25mm.
3, the described high temperature high ductibility electrolytic copper foil production process of claim 1 is characterized in that the composition of described additive and content are: gelatin 0.01～0.1g/L and mixture A 0.01～0.05g/L.
4, the described high temperature high ductibility electrolytic copper foil production process of claim 1 is characterized in that the composition of described additive and content are: propenyl thiocarbamide 0.01～0.1g/L, Sodium dodecylbenzene sulfonate 0.005～0.03g/L and mixture A 0.02～0.06g/L
5, the described high temperature high ductibility electrolysis of claim 1.The Copper Foil manufacturing process is characterized in that the composition of described additive and content are: gelatin 0.01～0.1g/L, Natvosol 0.01～0.05g/L and mixture A0.01～0.05g/L.
6, the described high temperature high ductibility electrolytic copper foil production process of claim 1 is characterized in that the composition of described additive and content are: gelatin 0.01～0.1g/L, polyacrylamide 0.01～0.05g/L and mixture A0.01～0.05g/L.
7, the described high temperature high ductibility electrolytic copper foil production process of claim 1 is characterized in that the composition of described additive and content are: mixture A 0.03～0.08g/L.
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| CN1995469B CN1995469B (en) | 2011-06-15 |
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| CN102181889A (en) * | 2011-04-08 | 2011-09-14 | 联合铜箔(惠州)有限公司 | Additive for electrolytic copper foil, electrolytic copper foil manufacturing process and electrolytic copper foil |
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