CN115433930A - Phosphorus-free blackening solution for copper metal grid conductive film and preparation and use methods thereof - Google Patents
Phosphorus-free blackening solution for copper metal grid conductive film and preparation and use methods thereof Download PDFInfo
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- CN115433930A CN115433930A CN202210787275.9A CN202210787275A CN115433930A CN 115433930 A CN115433930 A CN 115433930A CN 202210787275 A CN202210787275 A CN 202210787275A CN 115433930 A CN115433930 A CN 115433930A
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- blackening
- conductive film
- phosphorus
- copper metal
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 34
- 239000010949 copper Substances 0.000 title claims abstract description 34
- 239000002184 metal Substances 0.000 title claims abstract description 29
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 29
- 238000000034 method Methods 0.000 title claims abstract description 15
- 238000002360 preparation method Methods 0.000 title abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000000654 additive Substances 0.000 claims abstract description 19
- 230000000996 additive effect Effects 0.000 claims abstract description 18
- 239000003513 alkali Substances 0.000 claims abstract description 18
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 18
- 239000002270 dispersing agent Substances 0.000 claims abstract description 13
- 239000007788 liquid Substances 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims description 18
- 238000001035 drying Methods 0.000 claims description 12
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 claims description 8
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 8
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 claims description 6
- 238000002791 soaking Methods 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 6
- 239000002202 Polyethylene glycol Substances 0.000 claims description 5
- 229920002873 Polyethylenimine Polymers 0.000 claims description 5
- 229920001223 polyethylene glycol Polymers 0.000 claims description 5
- 239000005725 8-Hydroxyquinoline Substances 0.000 claims description 4
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 4
- 229960003540 oxyquinoline Drugs 0.000 claims description 4
- MCJGNVYPOGVAJF-UHFFFAOYSA-N quinolin-8-ol Chemical compound C1=CN=C2C(O)=CC=CC2=C1 MCJGNVYPOGVAJF-UHFFFAOYSA-N 0.000 claims description 4
- -1 sodium alkyl sulfonate Chemical class 0.000 claims description 4
- QRUDEWIWKLJBPS-UHFFFAOYSA-N benzotriazole Chemical compound C1=CC=C2N[N][N]C2=C1 QRUDEWIWKLJBPS-UHFFFAOYSA-N 0.000 claims description 3
- 239000012964 benzotriazole Substances 0.000 claims description 3
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims description 3
- 229910052708 sodium Inorganic materials 0.000 claims description 3
- 239000011734 sodium Substances 0.000 claims description 3
- FBPFZTCFMRRESA-FSIIMWSLSA-N D-Glucitol Natural products OC[C@H](O)[C@H](O)[C@@H](O)[C@H](O)CO FBPFZTCFMRRESA-FSIIMWSLSA-N 0.000 claims description 2
- FBPFZTCFMRRESA-JGWLITMVSA-N D-glucitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-JGWLITMVSA-N 0.000 claims description 2
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 2
- 229910017464 nitrogen compound Inorganic materials 0.000 claims description 2
- 150000002989 phenols Chemical group 0.000 claims description 2
- 239000000600 sorbitol Substances 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 4
- 238000002310 reflectometry Methods 0.000 abstract description 4
- 230000008030 elimination Effects 0.000 abstract description 2
- 238000003379 elimination reaction Methods 0.000 abstract description 2
- YCIMNLLNPGFGHC-UHFFFAOYSA-N catechol Chemical compound OC1=CC=CC=C1O YCIMNLLNPGFGHC-UHFFFAOYSA-N 0.000 description 6
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 5
- 229910052698 phosphorus Inorganic materials 0.000 description 5
- 239000011574 phosphorus Substances 0.000 description 5
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 229910001111 Fine metal Inorganic materials 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000012851 eutrophication Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 239000002346 layers by function Substances 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
- C23C22/60—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using alkaline aqueous solutions with pH greater than 8
- C23C22/63—Treatment of copper or alloys based thereon
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/73—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals characterised by the process
Landscapes
- Chemical & Material Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Paints Or Removers (AREA)
Abstract
The invention relates to a phosphorus-free blackening solution for a copper metal grid conductive film and a preparation and use method thereof, wherein the phosphorus-free blackening solution comprises the following components in parts by weight: 0.1-5 parts of a blackening agent, 0.5-20 parts of alkali, 0.1-1 part of a dispersing agent, 0.1-1 part of a blackening accelerator, 0.1-1 part of an additive and 72-98.6 parts of water. The invention has the advantages that: the blackening liquid has the advantages of high blackening speed, blackening temperature close to room temperature, obvious reduction of the reflectivity and brightness of copper, shadow elimination effect, no damage to grid lines, no influence on electric conductivity and the like.
Description
Technical Field
The invention relates to a phosphorus-free blackening solution for a copper grid conductive film and a preparation method and a use method thereof, belonging to the field of blackening solutions.
Background
A Metal-Mesh-Film (Metal-Mesh-Film) is a transparent conductive Film composed of a substrate and fine Metal wires densely distributed on the substrate. The transparent conduction is realized by taking an ultrafine metal grid as a conductive functional layer; the touch sensor manufactured by the touch sensor has the characteristics of low power consumption, sensitive touch, long service life and the like, and has the characteristics of flexibility, water resistance, explosion resistance, no pollution and the like, so that the touch sensor is widely applied to the technical field of touch. In consideration of the price, performance and other factors, the metal in the metal grid conductive film is generally copper. However, these processes generally form copper films having high visibility of metallic luster and high reflectivity, and the copper films are easily perceived by the naked eye when the circuits are formed, thereby affecting the visual effect of the user. Meanwhile, the line width of the copper grid on the touch screen is generally 2-5 μm, generally less than 5 μm, which is not easy to see by naked eyes, but is bright and has strong light reflection, so that the copper needs to be blackened to make the surface of the copper dark, and the reflectivity and brightness of the metal are reduced, so as to achieve the effect of being invisible by naked eyes.
With the progress of society and the enhancement of environmental awareness of people, phosphorus pollution has attracted much attention. Phosphorus emissions will cause eutrophication of the surrounding waters and may cause "red tides". In some countries such as Europe and America, japan, etc., phosphorus inhibition measures have been proposed, such as Germany requiring phosphorus emission of 1 mg.l-1 or less. Therefore, the application of the phosphorus-free blackening solution is a development direction in the future.
The problems that blackening degree is uneven and lines are damaged easily due to the use of blackening liquid medicine are common in the industry at present; in addition, the blackening solution disclosed in the patent, CN103898498B and CN 113161044A have the problems of high blackening temperature, long blackening time and the like; CN 111748810A has the problems of waste liquid discharge, phosphorus pollution and the like.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides a phosphorus-free blackening solution for a copper metal grid conductive film and a preparation and use method thereof, and the technical scheme of the invention is as follows:
a phosphorus-free blackening solution for a copper metal grid conductive film comprises the following components in parts by weight: 0.1-5 parts of a blackening agent, 0.5-20 parts of alkali, 0.1-1 part of a dispersing agent, 0.1-1 part of a blackening accelerator, 0.1-1 part of an additive and 72-98.6 parts of water.
3 parts of a blackening agent, 15 parts of alkali, 0.5 part of a dispersing agent, 0.5 part of a blackening accelerator, 0.5 part of an additive and 80 parts of water.
The blackening agent is used for blackening and comprises one or more of thiourea, 8-hydroxyquinoline and sorbitol which are mixed according to any proportion.
The alkali comprises one or a mixture of more of ethanolamine, diethanolamine, triethanolamine, KOH and NaOH according to any proportion.
The dispersing agent comprises one or a mixture of two of polyethylene glycol or alkyl sodium sulfonate according to any proportion.
The blackening accelerator is a phenolic compound.
The additive is an amine nitrogen compound, and comprises a mixture of one or more of imidazole, benzotriazole and polyethyleneimine according to any proportion.
A method for preparing a phosphorus-free blackening solution for a copper metal grid conductive film is characterized by comprising the following steps of:
(1) Weighing the blackening agent and the alkali according to the specific weight of each part by weight, dissolving the blackening agent and the alkali by using half of the total weight of water, heating to 20-60 ℃, and stirring for 1-60min;
(2) And then adding the additive, the dispersant and the accelerator in sequence, and performing constant volume by using the remaining half of water to obtain the blackening solution.
A method for using a phosphorus-free blackening solution for a copper metal grid conductive film comprises the following steps: and soaking the copper metal grid conductive film in blackening liquid for blackening, washing with water, and drying to obtain the blackened conductive film, wherein the blackening temperature is 20-50 ℃, the blackening time is 20s-2min, the washing temperature is 20-40 ℃, the washing time is 30-60s, the sponge is wiped, and the drying temperature is 20-40 ℃. The invention has the advantages that: the blackening liquid has the advantages of high blackening speed, blackening temperature close to room temperature, obvious reduction of the reflectivity and brightness of copper, shadow elimination effect, no damage to grid lines, no influence on electric conductivity and the like.
Detailed Description
The invention will be further described with reference to specific embodiments, and the advantages and features of the invention will become apparent as the description proceeds. These examples are illustrative only and do not limit the scope of the present invention in any way. It will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention, and that such changes and substitutions are intended to be within the scope of the invention.
Example 1: a phosphorus-free blackening solution for a copper metal grid conductive film comprises 2 parts of thiourea, 0.1 part of KOH, 0.05 part of ethanolamine and 1000 parts of polyethylene glycol: 0.8 part, 0.2 part of catechol, 0.1 part of polyethyleneimine, 0.05 part of benzotriazole and 96.7 parts of water.
The preparation method of the blackening solution comprises the following steps:
(1) Weighing the blackening agent and the alkali according to the specific weight of each part by weight, dissolving the blackening agent and the alkali by using half of the total weight of water, heating to 50 ℃, and stirring for 30min.
(2) Then adding the additive, the dispersant, the accelerator and the additive, and fixing the volume by using the rest water to obtain the blackening solution.
The using method comprises the following steps:
and soaking the copper metal grid conductive film in the blackening solution for blackening, and washing and drying to obtain the blackened conductive film. The blackening temperature is 30 ℃, and the blackening time is 60s. The washing temperature is 30 ℃, the washing time is 30s, the sponge is wiped, and the drying temperature is 30 ℃.
Example 2: a phosphorus-free blackening solution for a copper metal grid conductive film comprises 4 parts of 8-hydroxyquinoline, 0.1 part of KOH, 0.05 part of ethanolamine and 1000 parts of polyethylene glycol: 0.8 part, 0.2 part of polyethyleneimine, 0.1 part of phenol and 94.75 parts of water;
the preparation method of the blackening solution comprises the following steps:
(1) Weighing the blackening agent and the alkali according to the specific weight of each part by weight, dissolving the blackening agent and the alkali by using half of the total weight of water, heating to 50 ℃, and stirring for 30min.
(2) Then adding the additive, the dispersant, the accelerator and the additive, and fixing the volume by using the rest water to obtain the blackening solution.
The using method comprises the following steps:
(1) And soaking the copper metal grid conductive film in the blackening solution for blackening, and washing and drying to obtain the blackened conductive film. The blackening temperature is 40 ℃, and the blackening time is 100s. The washing temperature is 30 ℃, the washing time is 30s, the sponge wiping is carried out, and the drying temperature is 30 ℃.
Example 3: a phosphorus-free blackening solution for a copper metal grid conductive film comprises 5 parts of 8-hydroxyquinoline, 20 parts of KOH, 1 part of diethanolamine and sodium alkyl sulfonate: 1 part of polyethyleneimine, 1 part of phenol and 98.6 parts of water;
the preparation method of the blackening solution comprises the following steps:
(1) Weighing the blackening agent and the alkali according to the specific weight of each part by weight, dissolving the blackening agent and the alkali by using half of the total weight of water, heating to 50 ℃, and stirring for 30min.
(2) Then adding the additive, the dispersant, the accelerator and the additive, and fixing the volume with water to obtain the blackening solution. The using method comprises the following steps:
(1) And soaking the copper metal grid conductive film in the blackening solution for blackening, and washing and drying to obtain the blackened conductive film. The blackening temperature is 40 ℃, and the blackening time is 100s. The washing temperature is 30 ℃, the washing time is 30s, the sponge wiping is carried out, and the drying temperature is 30 ℃.
Example 4: as a comparative example, additives were reduced compared to the formulations of the present invention.
The method comprises the following specific steps: the blackening solution comprises 2 parts of thiourea, 0.1 part of KOH, 0.05 part of MEA, 1000 parts of polyethylene glycol: 0.8 part of pyrocatechol, 0.2 part of catechol, no additive and 96.85 parts of water.
The preparation method of the blackening solution comprises the following steps:
(1) Weighing the blackening agent and the alkali according to the specific weight of each part by weight, dissolving the blackening agent and the alkali by using half of the total weight of water, heating to 50 ℃, and stirring for 30min.
(2) Then adding the additive, the dispersant, the accelerator and the additive, and fixing the volume with water to obtain the blackening solution. The using method comprises the following steps:
and soaking the copper metal grid conductive film in the blackening solution for blackening, and washing and drying to obtain the blackened conductive film. The blackening temperature is 35 ℃, and the blackening time is 30s. The washing temperature is 30 ℃, the washing time is 30s, the sponge is wiped, and the drying temperature is 25 ℃.
The blackening effect picture is shot by a Canon camera EOS 90D, the grid picture is shot by a Leica microscope, and the experimental result is shown in Table 1.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (9)
1. A phosphorus-free blackening solution for a copper metal grid conductive film is characterized by comprising the following components in parts by weight: 0.1-5 parts of a blackening agent, 0.5-20 parts of alkali, 0.1-1 part of a dispersing agent, 0.1-1 part of a blackening accelerator, 0.1-1 part of an additive and 72-98.6 parts of water.
2. The phosphorus-free blackening solution for the copper metal grid conductive film as claimed in claim 1, wherein the blackening agent is 3 parts, the alkali is 15 parts, the dispersing agent is 0.5 part, the blackening accelerator is 0.5 part, the additive is 0.5 part, and the water is 80 parts.
3. The phosphorus-free blackening solution for the conductive film of the copper metal grid as claimed in claim 1 or 2, wherein the blackening agent is used for blackening and comprises a mixture of one or more of thiourea, 8-hydroxyquinoline and sorbitol in any proportion.
4. The phosphorus-free blackening solution for the copper metal mesh conductive film as claimed in claim 1 or 2, wherein the alkali comprises one or more of ethanolamine, diethanolamine, triethanolamine, KOH and NaOH in any proportion.
5. The phosphorus-free blackening solution for the copper metal mesh conductive film as claimed in claim 1 or 2, wherein the dispersing agent comprises one or a mixture of two of polyethylene glycol and sodium alkyl sulfonate in any proportion.
6. The phosphorus-free blackening solution for the copper metal mesh conductive film as claimed in claim 1 or 2, wherein the blackening accelerator is a phenolic compound.
7. The phosphorus-free blackening solution for the copper metal grid conductive film as claimed in claim 1 or 2, wherein the additive is an amine nitrogen compound comprising a mixture of one or more of imidazole, benzotriazole and polyethyleneimine in any proportion.
8. A method for preparing the phosphorus-free blackening solution for the conductive film of the copper metal grid as defined in any one of claims 1 to 7, which is characterized by comprising the following steps:
(1) Weighing a blackening agent and alkali according to the specific weight of each part by weight, dissolving by using half of the total weight of water, heating to 20-60 ℃, and stirring for 1-60min;
(2) And then adding the additive, the dispersant and the accelerator in sequence, and performing constant volume by using the remaining half of water to obtain the blackening solution.
9. A use method of a phosphorus-free blackening solution for a copper metal grid conductive film is characterized by comprising the following steps: and soaking the copper metal grid conductive film in blackening liquid for blackening, washing with water, and drying to obtain the blackened conductive film, wherein the blackening temperature is 20-50 ℃, the blackening time is 20s-2min, the washing temperature is 20-40 ℃, the washing time is 30-60s, the sponge is wiped, and the drying temperature is 20-40 ℃.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN116970934A (en) * | 2023-08-03 | 2023-10-31 | 广东盈华电子科技有限公司 | Double-sided blackening surface treatment process for electrolytic copper foil |
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JPH04136186A (en) * | 1990-09-25 | 1992-05-11 | Pentel Kk | Blackening treatment of copper or copper alloy and blackening treatment liquid |
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