CN116837427A - Preparation method of high-oxidation-resistance ultrathin electrolytic copper foil - Google Patents
Preparation method of high-oxidation-resistance ultrathin electrolytic copper foil Download PDFInfo
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- CN116837427A CN116837427A CN202310931796.1A CN202310931796A CN116837427A CN 116837427 A CN116837427 A CN 116837427A CN 202310931796 A CN202310931796 A CN 202310931796A CN 116837427 A CN116837427 A CN 116837427A
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- Prior art keywords
- copper foil
- electrolytic copper
- electrolyte
- oxidation resistance
- ultrathin
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 80
- 239000011889 copper foil Substances 0.000 title claims abstract description 74
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 50
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 42
- 239000003792 electrolyte Substances 0.000 claims abstract description 29
- 238000005868 electrolysis reaction Methods 0.000 claims abstract description 23
- 229910000365 copper sulfate Inorganic materials 0.000 claims abstract description 22
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims abstract description 22
- 230000003647 oxidation Effects 0.000 claims abstract description 18
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 18
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 14
- 229910017053 inorganic salt Inorganic materials 0.000 claims abstract description 13
- 229910052751 metal Inorganic materials 0.000 claims abstract description 11
- 239000002184 metal Substances 0.000 claims abstract description 11
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 22
- 239000010936 titanium Substances 0.000 claims description 22
- 229910052719 titanium Inorganic materials 0.000 claims description 22
- 238000000034 method Methods 0.000 claims description 13
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 claims description 11
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 claims description 10
- 229910052741 iridium Inorganic materials 0.000 claims description 10
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 claims description 10
- 229910052707 ruthenium Inorganic materials 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 2
- 229910000510 noble metal Inorganic materials 0.000 claims 1
- 239000013078 crystal Substances 0.000 abstract description 5
- JRBRVDCKNXZZGH-UHFFFAOYSA-N alumane;copper Chemical compound [AlH3].[Cu] JRBRVDCKNXZZGH-UHFFFAOYSA-N 0.000 abstract description 4
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 abstract description 3
- 239000000956 alloy Substances 0.000 abstract description 3
- 229910045601 alloy Inorganic materials 0.000 abstract description 3
- 229910001431 copper ion Inorganic materials 0.000 abstract description 2
- 238000001035 drying Methods 0.000 description 8
- 238000005406 washing Methods 0.000 description 8
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 230000003064 anti-oxidating effect Effects 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- -1 aluminum ions Chemical class 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 238000005254 chromizing Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000002161 passivation 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
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/38—Electroplating: Baths therefor from solutions of copper
Abstract
The application discloses a preparation method of high oxidation resistance ultrathin electrolytic copper foil, which takes copper sulfate and sulfuric acid solution as electrolyte, and adds 10-100 mg/L of metal aluminum inorganic salt and 5-20 mL/L of hydrofluoric acid into the electrolyte to carry out direct current electrolysis to obtain the electrolytic copper foil, and the electrolytic copper foil is peeled off to obtain the ultrathin electrolytic copper foil. According to the application, proper amounts of metal aluminum inorganic salt and hydrofluoric acid are added into the electrolyte, so that the crystal face of the copper foil (111) is preferentially oriented, and aluminum and copper ions are co-deposited to form the copper-aluminum micro-alloy, so that the prepared ultrathin electrolytic copper foil has good oxidation resistance and basically does not change color after being stored for 1 month in a conventional environment.
Description
Technical Field
The application relates to the technical field of copper foil production, in particular to a preparation method of a high-oxidation-resistance ultrathin electrolytic copper foil.
Background
The ultrathin electrolytic copper foil is an important base material of the lithium ion power battery, however, the ultrathin electrolytic copper foil is easily oxidized and corroded in the production and application processes, so that the internal resistance of the battery is increased, the battery capacity is reduced, and the performance and stability of the battery are affected. The traditional ultra-thin electrolytic copper foil surface passivation process generally forms a compact antioxidation layer on the surface of the copper foil through chromic anhydride treatment, so that the antioxidation performance of the copper foil is improved, however, the chromium is difficult to be introduced to meet the requirements of no chromizing and environmental protection of products, and in the present stage, a large number of workers are trying to research to coat organic matters on the surface of the copper foil or electroplate an alloy layer on the surface of the copper foil so as to replace the traditional chromic anhydride antioxidation process.
Disclosure of Invention
The purpose of the scheme is to provide a preparation method of the high-oxidation-resistance ultrathin electrolytic copper foil, which is characterized in that proper amounts of aluminum nitrate and hydrofluoric acid are added into electrolyte, so that the prepared ultrathin electrolytic copper foil has good oxidation resistance and is basically not discolored after being stored for 1 month under the conventional environmental conditions.
In order to achieve the above purpose, the application adopts the following technical scheme: a preparation method of high oxidation resistance ultrathin electrolytic copper foil takes a copper sulfate+sulfuric acid solution as electrolyte, 10-100 mg/L of metal aluminum inorganic salt and 5-20 mL/L of hydrofluoric acid are added into the electrolyte for direct current electrolysis to obtain the electrolytic copper foil, and the electrolytic copper foil is stripped to obtain the ultrathin electrolytic copper foil.
Preferably, the metal aluminum inorganic salt is one or a mixture of aluminum sulfate and aluminum nitrate.
Preferably, the electrolyte temperature is 55 ℃.
Preferably, the current density of the direct current electrolysis is 1000A/m 2 The electrolysis time was 4min.
Preferably, titanium sheets plated with ruthenium and iridium are used as anodes, and titanium sheets are used as cathodes.
Preferably, the concentration of copper sulfate in the electrolyte is 80g/L and the concentration of sulfuric acid is 0.2mol/L.
The beneficial effects of the application are as follows:
the metal aluminum inorganic salt and hydrofluoric acid are added into the electrolyte, and the hydrofluoric acid can lead the crystal face of the copper foil (111) to have preferred orientation, and aluminum and copper ions form copper-aluminum micro alloy through codeposition, so that the prepared ultrathin electrolytic copper foil has good oxidation resistance and basically does not change color after being stored for 1 month in a conventional environment.
Drawings
Fig. 1 is a photograph of an ultrathin electrolytic copper foil prepared by adding an inorganic salt of metallic aluminum and hydrofluoric acid and an ultrathin electrolytic copper foil sample of comparative example 1 after being stored for one month in a conventional environment.
Fig. 2 is an XRD pattern of an ultra-thin electrolytic copper foil prepared by adding an inorganic salt of metallic aluminum and hydrofluoric acid and an ultra-thin electrolytic copper foil sample of comparative example 1.
Detailed Description
Embodiments of the present solution are described in further detail below. It is clear that the described embodiments are only some of the embodiments of the present solution, not an exhaustive list of all embodiments.
A preparation method of high-oxidation-resistance ultrathin electrolytic copper foil comprises the following steps:
the method comprises the steps of taking a titanium sheet plated with ruthenium and iridium as an anode, taking the titanium sheet as a cathode, taking a copper sulfate and sulfuric acid solution as electrolyte, wherein the concentration of copper sulfate is 80g/L, the concentration of sulfuric acid is 0.2mol/L, adding a certain amount of metal aluminum inorganic salt and hydrofluoric acid into the electrolyte, carrying out direct current electrolysis at the temperature of 55 ℃ to obtain electrolytic copper foil, and the current density is 1000A/m 2 The electrolysis time is 4min, and after washing by deionized water and drying by cold air, the ultrathin electrolytic copper foil with the thickness of 6 mu m and high oxidation resistance is obtained by stripping.
In one embodiment, the amount of aluminum sulfate is 10mg/L and the amount of hydrofluoric acid is 5mL/L.
In one embodiment, the amount of aluminum sulfate is 10mg/L and the amount of hydrofluoric acid is 20mL/L.
In one embodiment, the amount of aluminum sulfate is 100mg/L and the amount of hydrofluoric acid is 5mL/L.
In one embodiment, the amount of aluminum sulfate is 100mg/L and the amount of hydrofluoric acid is 20mL/L.
In one embodiment, the amount of aluminum nitrate is 50mg/L and the amount of hydrofluoric acid is 10mL/L.
In one embodiment, the amount of aluminum sulfate is 20mg/L, the amount of aluminum nitrate is 30mg/L, and the amount of hydrofluoric acid is 15mL/L.
The application will be further illustrated by means of specific examples.
Example 1
Titanium sheet plated with ruthenium and iridium is used as anode, titanium sheet is used as cathode, copper sulfate and sulfuric acid solution are used as electrolyte, the concentration of copper sulfate is 80g/L, the concentration of sulfuric acid is 0.2mol/L, and 10mg of copper sulfate is added into the electrolyteAluminum sulfate/L and hydrofluoric acid 5mL/L, wherein the temperature of electrolyte is 55 ℃, and the electrolytic copper foil is obtained by direct current electrolysis, and the current density is 1000A/m 2 The electrolysis time is 4min, and after washing by deionized water and drying by cold air, the ultrathin electrolytic copper foil with the thickness of 6 mu m is obtained by stripping, and the ultrathin electrolytic copper foil is preserved for 1 month in a conventional environment.
Example 2
Taking a titanium sheet plated with ruthenium and iridium as an anode, taking the titanium sheet as a cathode, taking a copper sulfate and sulfuric acid solution as electrolyte, wherein the concentration of copper sulfate is 80g/L, the concentration of sulfuric acid is 0.2mol/L, adding 10mg/L aluminum sulfate and 20mL/L hydrofluoric acid into the electrolyte, and carrying out direct current electrolysis at the temperature of 55 ℃ to obtain an electrolytic copper foil with the current density of 1000A/m 2 The electrolysis time is 4min, and after washing by deionized water and drying by cold air, the ultrathin electrolytic copper foil with the thickness of 6 mu m is obtained by stripping, and the ultrathin electrolytic copper foil is preserved for 1 month in a conventional environment.
Example 3
Taking a titanium sheet plated with ruthenium and iridium as an anode, taking the titanium sheet as a cathode, taking a copper sulfate and sulfuric acid solution as electrolyte, wherein the concentration of copper sulfate is 80g/L, the concentration of sulfuric acid is 0.2mol/L, adding 100mg/L aluminum sulfate and 5mL/L hydrofluoric acid into the electrolyte, and carrying out direct current electrolysis at the temperature of 55 ℃ to obtain an electrolytic copper foil with the current density of 1000A/m 2 The electrolysis time is 4min, and after washing by deionized water and drying by cold air, the ultrathin electrolytic copper foil with the thickness of 6 mu m is obtained by stripping, and the ultrathin electrolytic copper foil is preserved for 1 month in a conventional environment.
Example 4
Taking a titanium sheet plated with ruthenium and iridium as an anode, taking the titanium sheet as a cathode, taking a copper sulfate and sulfuric acid solution as electrolyte, wherein the concentration of copper sulfate is 80g/L, the concentration of sulfuric acid is 0.2mol/L, adding 100mg/L aluminum sulfate and 20mL/L hydrofluoric acid into the electrolyte, and carrying out direct current electrolysis at the temperature of 55 ℃ to obtain an electrolytic copper foil with the current density of 1000A/m 2 The electrolysis time is 4min, and after washing by deionized water and drying by cold air, the ultrathin electrolytic copper foil with the thickness of 6 mu m is obtained by stripping, and the ultrathin electrolytic copper foil is preserved for 1 month in a conventional environment.
Example 5
Titanium sheet plated with ruthenium and iridium is used as anodeThe method comprises the steps of taking a titanium sheet as a cathode, taking a copper sulfate and sulfuric acid solution as an electrolyte, adding 50mg/L aluminum nitrate and 10mL/L hydrofluoric acid into the electrolyte, performing direct current electrolysis at the temperature of 55 ℃ to obtain electrolytic copper foil, wherein the concentration of copper sulfate is 80g/L, the concentration of sulfuric acid is 0.2mol/L, and the current density is 1000A/m 2 The electrolysis time is 4min, and after washing by deionized water and drying by cold air, the ultrathin electrolytic copper foil with the thickness of 6 mu m is obtained by stripping, and the ultrathin electrolytic copper foil is preserved for 1 month in a conventional environment.
Example 6
The method comprises the steps of taking a titanium sheet plated with ruthenium and iridium as an anode, taking the titanium sheet as a cathode, taking a copper sulfate and sulfuric acid solution as electrolyte, wherein the concentration of copper sulfate is 80g/L, the concentration of sulfuric acid is 0.2mol/L, adding 20mg/L of aluminum sulfate, 30mg/L of aluminum nitrate and 15mL/L of hydrofluoric acid into the electrolyte, carrying out direct current electrolysis at the temperature of 55 ℃ to obtain electrolytic copper foil, and the current density is 1000A/m 2 The electrolysis time is 4min, and after washing by deionized water and drying by cold air, the ultrathin electrolytic copper foil with the thickness of 6 mu m is obtained by stripping, and the ultrathin electrolytic copper foil is preserved for 1 month in a conventional environment.
Comparative example 1
The electrolytic copper foil is obtained by direct current electrolysis with a titanium sheet plated with ruthenium and iridium as an anode, a titanium sheet as a cathode, a copper sulfate and sulfuric acid solution as an electrolyte, wherein the concentration of copper sulfate is 80g/L, the concentration of sulfuric acid is 0.2mol/L, the temperature of the electrolyte is 55 ℃, and the current density is 1000A/m 2 The electrolysis time is 4min, and after washing by deionized water and drying by cold air, the ultrathin electrolytic copper foil with the thickness of 6 mu m is obtained by stripping, and the ultrathin electrolytic copper foil is preserved for 1 month in a conventional environment.
It is apparent from fig. 1 that the surface of the non-additive ultrathin electrolytic copper foil is obviously discolored after being stored for one month in a conventional environment, which means that the ultrathin electrolytic copper foil is easily oxidized, and the ultrathin electrolytic copper foil prepared by adding metal aluminum inorganic salt and hydrofluoric acid is basically not discolored after being stored for 1 month in the conventional environment (the ultrathin electrolytic copper foil obtained in each example is basically the same in change, so that only one picture is provided, and the color picture cannot be submitted, so that fig. 1 is a gray scale, and the color difference generated by oxidation of the comparative example and the example is obvious in physical observation), which means that the ultrathin electrolytic copper foil has good oxidation resistance. Hydrofluoric acid and metal aluminum inorganic salt addition can promote preferred orientation of copper (220) crystal faces (XRD patterns of all embodiments are similar, thus only figure 2 is provided, and as is obvious from figure 2, the (220) crystal face relative strength of the copper foil is obviously enhanced after the addition of the inorganic aluminum metal salt, the preferred orientation of the copper (220) crystal faces is beneficial to improving the oxidation resistance of the copper (Nature, 2020,586: 390-394), meanwhile, aluminum ions and copper ions can form copper-aluminum microalloy through co-deposition, and the copper-aluminum microalloy structure has the property of improving the copper foil, so that the ultrathin electrolytic copper foil prepared by adding the metal aluminum inorganic salt and the hydrofluoric acid has good oxidation resistance.
The above-described specific embodiments further illustrate the objects, technical solutions and technical effects of the present application in detail. It should be understood that the foregoing is only illustrative of the present application and is not intended to limit the scope of the application, and that all equivalent changes and modifications that may be made by those skilled in the art without departing from the spirit and principles of the application shall fall within the scope of the application.
Claims (8)
1. A preparation method of high oxidation resistance ultrathin electrolytic copper foil is characterized in that a copper sulfate+sulfuric acid solution is used as electrolyte, 10-100 mg/L of metal aluminum inorganic salt and 5-20 mL/L of hydrofluoric acid are added into the electrolyte for direct current electrolysis to obtain the electrolytic copper foil, and the electrolytic copper foil is peeled off to obtain the ultrathin electrolytic copper foil.
2. The method for preparing the high oxidation resistance ultrathin electrolytic copper foil according to claim 1, wherein the metal aluminum inorganic salt is one or a mixture of aluminum sulfate and aluminum nitrate.
3. The method for preparing a high oxidation resistance ultra-thin electrolytic copper foil according to claim 1, wherein the temperature of the electrolyte is 55 ℃.
4. The method for preparing a high oxidation resistance ultrathin electrolytic copper foil according to claim 1, wherein the electrolytic copper foil is directly manufactured byThe current density of the flow electrolysis is 1000A/m 2 The electrolysis time was 4min.
5. The method for preparing the high oxidation resistance ultrathin electrolytic copper foil according to claim 1, wherein the electrolytic copper foil is peeled off after being washed by deionized water and dried by cold air.
6. The method for preparing a high oxidation resistance ultra-thin electrolytic copper foil according to claim 1, wherein a titanium sheet plated with noble metal is used as an anode and a titanium sheet is used as a cathode.
7. The method for preparing a high oxidation resistance ultrathin electrolytic copper foil according to claim 1, wherein titanium sheets plated with ruthenium and iridium are used as anodes and titanium sheets are used as cathodes.
8. The method for preparing a high oxidation resistance ultra-thin electrolytic copper foil according to claim 1, wherein the concentration of copper sulfate in the electrolyte is 80g/L and the concentration of sulfuric acid is 0.2mol/L.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310931796.1A CN116837427A (en) | 2023-07-27 | 2023-07-27 | Preparation method of high-oxidation-resistance ultrathin electrolytic copper foil |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310931796.1A CN116837427A (en) | 2023-07-27 | 2023-07-27 | Preparation method of high-oxidation-resistance ultrathin electrolytic copper foil |
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| CN116837427A true CN116837427A (en) | 2023-10-03 |
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| CN202310931796.1A Pending CN116837427A (en) | 2023-07-27 | 2023-07-27 | Preparation method of high-oxidation-resistance ultrathin electrolytic copper foil |
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| CN (1) | CN116837427A (en) |
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- 2023-07-27 CN CN202310931796.1A patent/CN116837427A/en active Pending
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