CN112501658A - Production process of high-modulus copper foil - Google Patents
Production process of high-modulus copper foil Download PDFInfo
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- CN112501658A CN112501658A CN202011422027.1A CN202011422027A CN112501658A CN 112501658 A CN112501658 A CN 112501658A CN 202011422027 A CN202011422027 A CN 202011422027A CN 112501658 A CN112501658 A CN 112501658A
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- main electrolyte
- copper foil
- copper
- foil
- modulus
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 79
- 239000011889 copper foil Substances 0.000 title claims abstract description 50
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 19
- 239000003792 electrolyte Substances 0.000 claims abstract description 67
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 38
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims abstract description 34
- 239000000654 additive Substances 0.000 claims abstract description 30
- 230000000996 additive effect Effects 0.000 claims abstract description 30
- 239000000956 alloy Substances 0.000 claims abstract description 27
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 27
- 239000011888 foil Substances 0.000 claims abstract description 20
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims abstract description 19
- 108010010803 Gelatin Proteins 0.000 claims abstract description 19
- 229910052802 copper Inorganic materials 0.000 claims abstract description 19
- 239000010949 copper Substances 0.000 claims abstract description 19
- 229920000159 gelatin Polymers 0.000 claims abstract description 19
- 239000008273 gelatin Substances 0.000 claims abstract description 19
- 235000019322 gelatine Nutrition 0.000 claims abstract description 19
- 235000011852 gelatine desserts Nutrition 0.000 claims abstract description 19
- 238000005868 electrolysis reaction Methods 0.000 claims abstract description 18
- 229960005070 ascorbic acid Drugs 0.000 claims abstract description 17
- 235000010323 ascorbic acid Nutrition 0.000 claims abstract description 17
- 239000011668 ascorbic acid Substances 0.000 claims abstract description 17
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000004381 surface treatment Methods 0.000 claims abstract description 11
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000007864 aqueous solution Substances 0.000 claims abstract description 10
- 229910000365 copper sulfate Inorganic materials 0.000 claims abstract description 10
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims abstract description 10
- 238000001914 filtration Methods 0.000 claims abstract description 10
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 10
- 239000011733 molybdenum Substances 0.000 claims abstract description 10
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 10
- 239000010937 tungsten Substances 0.000 claims abstract description 10
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910052700 potassium Inorganic materials 0.000 claims abstract description 9
- 239000011591 potassium Substances 0.000 claims abstract description 9
- 238000000034 method Methods 0.000 claims description 11
- 238000005275 alloying Methods 0.000 claims description 8
- LJCNRYVRMXRIQR-OLXYHTOASA-L potassium sodium L-tartrate Chemical compound [Na+].[K+].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O LJCNRYVRMXRIQR-OLXYHTOASA-L 0.000 claims description 8
- 229940074439 potassium sodium tartrate Drugs 0.000 claims description 8
- 235000011006 sodium potassium tartrate Nutrition 0.000 claims description 8
- XMVONEAAOPAGAO-UHFFFAOYSA-N sodium tungstate Chemical compound [Na+].[Na+].[O-][W]([O-])(=O)=O XMVONEAAOPAGAO-UHFFFAOYSA-N 0.000 claims description 8
- 235000015393 sodium molybdate Nutrition 0.000 claims description 2
- 239000011684 sodium molybdate Substances 0.000 claims description 2
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims description 2
- 239000000463 material Substances 0.000 description 3
- 230000014759 maintenance of location Effects 0.000 description 2
- 241000784732 Lycaena phlaeas Species 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 150000003071 polychlorinated biphenyls Chemical class 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D1/00—Electroforming
- C25D1/04—Wires; Strips; Foils
Abstract
The invention discloses a production process of a high modulus copper foil, which comprises the following steps: step S1: dissolving a copper rod and a copper wire into a high-purity copper sulfate aqueous solution serving as a main electrolyte by using sulfuric acid; step S2: adding an alloy element into the main electrolyte, wherein the alloy element at least contains one of tungsten, molybdenum and potassium; step S3: filtering the main electrolyte added with the alloy elements; step S4: adding an additive into the filtered main electrolyte; the additive comprises gelatin, ascorbic acid and chloride ions; step S5: feeding the main electrolyte added with the additive into an electrolytic cell for electrolysis to obtain a rough foil; step S6: and carrying out surface treatment on the rough foil to obtain the high-modulus copper foil. The invention provides a production process of a high-modulus copper foil, which can produce the high-modulus copper foil and can greatly improve the smoothness and reliability of a subsequently processed plate.
Description
Technical Field
The invention relates to the technical field of metal materials, in particular to a high-modulus copper foil production process.
Background
Copper foil is used as a conductive material for printed wiring boards (PCBs). With the development of technology, electronic products tend to be multifunctional, light and thin integrated. Due to the thinning of the PCB, in order to ensure the reliability of IC assembly, the PCB is especially important to keep certain rigidity for the high-temperature performance of materials, and once phenomena such as plate bending, plate warping and the like occur, the original device can not be assembled finally.
Modulus, is a physical quantity that describes the ability of a solid material to resist deformation. High modulus materials are rigid and not easily bent or stretched. The invention develops a high modulus copper foil based on shear modulus. Shear modulus refers to the ratio of shear stress to shear strain. The common electrolytic copper foil has an elastic modulus of 105GPa and a shear modulus of 38GPa at 20 ℃, and is generally related to the components of the material and has little relation with the structure.
The high-modulus copper foil is adopted, the modulus retention rate of the PCB board at high temperature reaches more than 80%, the smoothness and the reliability of the board in subsequent processing are greatly improved, and the modulus retention rate of the PCB pressed by the common copper foil at high temperature is only 25%.
Disclosure of Invention
Aiming at the problems in the related art, the invention provides a high modulus copper foil production process, which solves the problem that the modulus of a copper foil produced by the existing production process is low.
In order to achieve the technical purpose, the technical scheme of the invention is as follows:
the production process of the high modulus copper foil comprises the following steps:
step S1: dissolving a copper rod and a copper wire into a high-purity copper sulfate aqueous solution serving as a main electrolyte by using sulfuric acid;
step S2: adding an alloy element into the main electrolyte, wherein the alloy element at least contains one of tungsten, molybdenum and potassium;
step S3: filtering the main electrolyte added with the alloy elements;
step S4: adding an additive into the filtered main electrolyte; the additive comprises gelatin, ascorbic acid and chloride ions;
step S5: feeding the main electrolyte added with the additive into an electrolytic cell for electrolysis to obtain a rough foil;
step S6: and carrying out surface treatment on the rough foil to obtain the high-modulus copper foil.
Further, in the step S1, the concentrations of copper and sulfuric acid in the main electrolyte are 35-50 g/L and 60-90 g/L, respectively.
Further, in step S2, the alloying element includes at least one of: sodium tungstate, ammonium tungstate, sodium molybdate and potassium sodium tartrate, and the concentration is 1.5-25g/l, 1.0-20 g/l, 2.5-25 g/l and 20-40g/l respectively.
Further, in the step S4, the concentrations of gelatin, ascorbic acid and chloride ion are 3-15ppm, 35-125 ppm and 10-30 ppm, respectively.
Further, in the step S5, the main electrolyte electrolysis temperature is 45-60 ℃, and the current density is 800-2。
Further, in the step S6, the content of tungsten and molybdenum in the high-modulus copper foil is 0.01% to 0.05%.
Further, in the step S6, the electrodeposited thickness of the copper foil is 9 to 105 um.
The invention has the beneficial effects that: the copper foil production process can produce high-modulus copper foil, and improves the production quality of the copper foil.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments that can be derived by one of ordinary skill in the art from the embodiments given herein are intended to be within the scope of the present invention.
The first embodiment is as follows:
the production process of the high modulus copper foil provided by the embodiment of the invention comprises the following steps:
step S1: dissolving a copper rod and a copper wire into a high-purity copper sulfate aqueous solution serving as a main electrolyte by using sulfuric acid;
step S2: adding an alloy element into the main electrolyte, wherein the alloy element at least contains one of tungsten, molybdenum and potassium;
step S3: filtering the main electrolyte added with the alloy elements;
step S4: adding an additive into the filtered main electrolyte; the additive comprises gelatin, ascorbic acid and chloride ions;
step S5: feeding the main electrolyte added with the additive into an electrolytic cell for electrolysis to obtain a rough foil;
step S6: and carrying out surface treatment on the rough foil to obtain the high-modulus copper foil.
In this embodiment, in step S1, the concentrations of copper and sulfuric acid in the main electrolyte are 50 g/L and 90 g/L, respectively.
In this embodiment, in step S2, the alloying elements include: sodium tungstate, potassium sodium tartrate, and the concentration is 21.3g/l and 40g/l respectively.
In this example, the concentrations of gelatin, ascorbic acid and chloride ion were 15ppm, 75 ppm and 15ppm, respectively, in the step S4.
In this embodiment, in the step S5, the main electrolyte electrolysis temperature is 60 ℃ and the current density is 1500A/m2。
In this embodiment, in step S6, the electrodeposited thickness of the copper foil is 35 um.
Example two:
the production process of the high modulus copper foil provided by the embodiment of the invention comprises the following steps:
step S1: dissolving a copper rod and a copper wire into a high-purity copper sulfate aqueous solution serving as a main electrolyte by using sulfuric acid;
step S2: adding an alloy element into the main electrolyte, wherein the alloy element at least contains one of tungsten, molybdenum and potassium;
step S3: filtering the main electrolyte added with the alloy elements;
step S4: adding an additive into the filtered main electrolyte; the additive comprises gelatin, ascorbic acid and chloride ions;
step S5: feeding the main electrolyte added with the additive into an electrolytic cell for electrolysis to obtain a rough foil;
step S6: and carrying out surface treatment on the rough foil to obtain the high-modulus copper foil.
In this embodiment, in step S1, the concentrations of copper and sulfuric acid in the main electrolyte are 50 g/L and 90 g/L, respectively.
In this embodiment, in step S2, the alloying elements include: sodium tungstate, potassium sodium tartrate, and the concentration is 10.65g/l and 30g/l respectively.
In this example, the concentrations of gelatin, ascorbic acid and chloride ion were 15ppm, 50 ppm and 15ppm, respectively, in the step S4.
In this embodiment, in the step S5, the main electrolyte electrolysis temperature is 60 ℃ and the current density is 1500A/m2。
In this embodiment, in step S6, the electrodeposited thickness of the copper foil is 35 um.
Example three:
the production process of the high modulus copper foil provided by the embodiment of the invention comprises the following steps:
step S1: dissolving a copper rod and a copper wire into a high-purity copper sulfate aqueous solution serving as a main electrolyte by using sulfuric acid;
step S2: adding an alloy element into the main electrolyte, wherein the alloy element at least contains one of tungsten, molybdenum and potassium;
step S3: filtering the main electrolyte added with the alloy elements;
step S4: adding an additive into the filtered main electrolyte; the additive comprises gelatin, ascorbic acid and chloride ions;
step S5: feeding the main electrolyte added with the additive into an electrolytic cell for electrolysis to obtain a rough foil;
step S6: and carrying out surface treatment on the rough foil to obtain the high-modulus copper foil.
In this embodiment, in step S1, the concentrations of copper and sulfuric acid in the main electrolyte are 50 g/L and 90 g/L, respectively.
In this embodiment, in step S2, the alloying elements include: sodium tungstate, potassium sodium tartrate, and the concentration is 4.25g/l and 25g/l respectively.
In this example, the concentrations of gelatin, ascorbic acid and chloride ion were 15ppm, 30 ppm and 15ppm, respectively, in the step S4.
In this embodiment, the step S5The main electrolyte has an electrolysis temperature of 60 ℃ and a current density of 1750A/m2。
In this embodiment, in step S6, the electrodeposited thickness of the copper foil is 35 um.
Example four:
the production process of the high modulus copper foil provided by the embodiment of the invention comprises the following steps:
step S1: dissolving a copper rod and a copper wire into a high-purity copper sulfate aqueous solution serving as a main electrolyte by using sulfuric acid;
step S2: adding an alloy element into the main electrolyte, wherein the alloy element at least contains one of tungsten, molybdenum and potassium;
step S3: filtering the main electrolyte added with the alloy elements;
step S4: adding an additive into the filtered main electrolyte; the additive comprises gelatin, ascorbic acid and chloride ions;
step S5: feeding the main electrolyte added with the additive into an electrolytic cell for electrolysis to obtain a rough foil;
step S6: and carrying out surface treatment on the rough foil to obtain the high-modulus copper foil.
In this embodiment, in step S1, the concentrations of copper and sulfuric acid in the main electrolyte are 50 g/L and 90 g/L, respectively.
In this embodiment, in step S2, the alloying elements include: sodium tungstate, potassium sodium tartrate, and the concentration is 10.5g/l and 40g/l respectively.
In this example, the concentrations of gelatin, ascorbic acid and chloride ion were 15ppm, 50 ppm and 15ppm, respectively, in the step S4.
In this embodiment, in the step S5, the main electrolyte electrolysis temperature is 55 ℃ and the current density is 1200A/m2。
In this embodiment, in step S6, the electrodeposited thickness of the copper foil is 18 um.
Example five:
the production process of the high modulus copper foil provided by the embodiment of the invention comprises the following steps:
step S1: dissolving a copper rod and a copper wire into a high-purity copper sulfate aqueous solution serving as a main electrolyte by using sulfuric acid;
step S2: adding an alloy element into the main electrolyte, wherein the alloy element at least contains one of tungsten, molybdenum and potassium;
step S3: filtering the main electrolyte added with the alloy elements;
step S4: adding an additive into the filtered main electrolyte; the additive comprises gelatin, ascorbic acid and chloride ions;
step S5: feeding the main electrolyte added with the additive into an electrolytic cell for electrolysis to obtain a rough foil;
step S6: and carrying out surface treatment on the rough foil to obtain the high-modulus copper foil.
In this embodiment, in step S1, the concentrations of copper and sulfuric acid in the main electrolyte are 50 g/L and 90 g/L, respectively.
In this embodiment, in step S2, the alloying elements include: sodium tungstate, potassium sodium tartrate, and the concentration is 15g/l and 20g/l respectively.
In this example, the concentrations of gelatin, ascorbic acid and chloride ion were 12ppm, 24 ppm and 18ppm, respectively, in the step S4.
In this embodiment, in the step S5, the main electrolyte electrolysis temperature is 55 ℃ and the current density is 1000A/m2。
In this embodiment, in step S6, the electrodeposited thickness of the copper foil is 18 um.
Example six:
the production process of the high modulus copper foil provided by the embodiment of the invention comprises the following steps:
step S1: dissolving a copper rod and a copper wire into a high-purity copper sulfate aqueous solution serving as a main electrolyte by using sulfuric acid;
step S2: adding an alloy element into the main electrolyte, wherein the alloy element at least contains one of tungsten, molybdenum and potassium;
step S3: filtering the main electrolyte added with the alloy elements;
step S4: adding an additive into the filtered main electrolyte; the additive comprises gelatin, ascorbic acid and chloride ions;
step S5: feeding the main electrolyte added with the additive into an electrolytic cell for electrolysis to obtain a rough foil;
step S6: and carrying out surface treatment on the rough foil to obtain the high-modulus copper foil.
In this embodiment, in step S1, the concentrations of copper and sulfuric acid in the main electrolyte are 50 g/L and 90 g/L, respectively.
In this embodiment, in step S2, the alloying elements include: sodium tungstate and potassium sodium tartrate, and the concentration is 5g/l and 20g/l respectively.
In this example, the concentrations of gelatin, ascorbic acid and chloride ion were 15ppm, 30 ppm and 15ppm, respectively, in the step S4.
In this embodiment, in the step S5, the main electrolyte electrolysis temperature is 55 ℃ and the current density is 800A/m2。
In this embodiment, in step S6, the electrodeposited thickness of the copper foil is 18 um.
Example seven (comparative):
the production process of the high modulus copper foil provided by the embodiment of the invention comprises the following steps:
step S1: dissolving a copper rod and a copper wire into a high-purity copper sulfate aqueous solution serving as a main electrolyte by using sulfuric acid;
step S2: filtering the main electrolyte;
step S3: adding an additive into the filtered main electrolyte; the additive comprises gelatin, and chloride ions;
step S4: feeding the main electrolyte added with the additive into an electrolytic cell for electrolysis to obtain a rough foil;
step S5: and carrying out surface treatment on the rough foil to obtain the copper foil.
In this embodiment, in step S1, the concentrations of copper and sulfuric acid in the main electrolyte are respectively 80 g/L and 90 g/L.
In this embodiment, in step S3, the concentrations of gelatin and chloride ion were 15ppm and 25ppm, respectively.
In this embodiment, in the step S4, the main electrolyte is electrolyzedThe temperature is 55 ℃, and the current density is 2500A/m2。
In this embodiment, in step S5, the electrodeposited thickness of the copper foil is 18 um.
The shear modulus under the different production conditions in the above examples was determined as follows:
in summary, the high modulus copper foil manufactured in the examples can be made into a high modulus electronic circuit copper foil by any one of the known surface treatment processes of peel strength enhancement and oxidation resistance.
It should be noted that, in this document, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other identical elements in a process, method, article, or apparatus that comprises the element.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (5)
1. The production process of the high modulus copper foil is characterized by comprising the following steps of:
step S1: dissolving a copper rod and a copper wire into a high-purity copper sulfate aqueous solution serving as a main electrolyte by using sulfuric acid;
step S2: adding an alloy element into the main electrolyte, wherein the alloy element at least contains one of tungsten, molybdenum and potassium;
step S3: filtering the main electrolyte added with the alloy elements;
step S4: adding an additive into the filtered main electrolyte; the additive comprises gelatin, ascorbic acid and chloride ions;
step S5: feeding the main electrolyte added with the additive into an electrolytic cell for electrolysis to obtain a rough foil;
step S6: and carrying out surface treatment on the rough foil to obtain the high-modulus copper foil.
2. The process for producing a high modulus copper foil as claimed in claim 1, wherein in step S1, the concentrations of copper and sulfuric acid in the main electrolyte are 35-50 g/L and 60-90 g/L, respectively.
3. The process for producing a high modulus copper foil according to claim 1, wherein in step S2, the alloying element comprises at least one of: sodium tungstate, ammonium tungstate, sodium molybdate and potassium sodium tartrate, and the concentration is 1.5-25g/l, 1.0-20 g/l, 2.5-25 g/l and 20-40g/l respectively.
4. The process for producing a high modulus copper foil as claimed in claim 1, wherein the concentrations of gelatin, ascorbic acid and chloride ions in step S4 are 3-15ppm, 35-125 ppm and 10-30 ppm respectively.
5. The process for producing a high modulus copper foil as claimed in claim 1, wherein in step S5, the main electrolyte electrolysis temperature is 45-60 ℃, the current density is 800-3000A/m2。
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Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1053818A (en) * | 1989-09-13 | 1991-08-14 | 古尔德有限公司 | The processing method and the electrolytic solution that are used for the controlled paillon foil of printed circuit board (PCB) and its character and produce this paillon foil |
JPH0967693A (en) * | 1995-08-29 | 1997-03-11 | Nikko Gould Foil Kk | Production of electrolytic copper foil |
CN103827358A (en) * | 2011-10-31 | 2014-05-28 | 古河电气工业株式会社 | High strength, high heat-resistance electrolytic copper foil, and manufacturing method for same |
CN104903495A (en) * | 2013-01-24 | 2015-09-09 | 古河电气工业株式会社 | Electrolytic copper foil and method for producing same |
-
2020
- 2020-12-08 CN CN202011422027.1A patent/CN112501658A/en active Pending
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1053818A (en) * | 1989-09-13 | 1991-08-14 | 古尔德有限公司 | The processing method and the electrolytic solution that are used for the controlled paillon foil of printed circuit board (PCB) and its character and produce this paillon foil |
JPH0967693A (en) * | 1995-08-29 | 1997-03-11 | Nikko Gould Foil Kk | Production of electrolytic copper foil |
CN103827358A (en) * | 2011-10-31 | 2014-05-28 | 古河电气工业株式会社 | High strength, high heat-resistance electrolytic copper foil, and manufacturing method for same |
CN104903495A (en) * | 2013-01-24 | 2015-09-09 | 古河电气工业株式会社 | Electrolytic copper foil and method for producing same |
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