CN111013983B - Preparation method of anode plate applied to electrolytic copper foil - Google Patents
Preparation method of anode plate applied to electrolytic copper foil Download PDFInfo
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- CN111013983B CN111013983B CN201911146165.9A CN201911146165A CN111013983B CN 111013983 B CN111013983 B CN 111013983B CN 201911146165 A CN201911146165 A CN 201911146165A CN 111013983 B CN111013983 B CN 111013983B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
- B05D7/14—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials to metal, e.g. car bodies
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- B05D5/00—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
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- B05D5/12—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures to obtain a coating with specific electrical properties
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- 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
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D17/00—Constructional parts, or assemblies thereof, of cells for electrolytic coating
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- B05D2202/00—Metallic substrate
- B05D2202/30—Metallic substrate based on refractory metals (Ti, V, Cr, Zr, Nb, Mo, Hf, Ta, W)
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Abstract
The invention discloses a preparation method of an anode plate applied to electrolytic copper foil, which comprises the following steps: substrate pretreatment, coating liquid preparation, single-layer firing, multi-layer firing and shaping firing; the preparation steps of the coating liquid comprise: the iridium trichloride, the palladium chloride, the cobalt chloride, the manganese chloride, the hydrochloric acid and the ethanol are uniformly mixed to prepare coating liquid. According to the invention, the composite coating containing iridium, palladium, cobalt and manganese is fired on the surface of the anode substrate, so that the anode plate has stronger corrosion resistance and heat resistance, the mechanical strength of the anode plate is obviously improved, and the service life of the anode plate is prolonged; meanwhile, the current density in the electrolytic reaction process is more uniform, and the preparation of high-quality ultrathin copper foil is facilitated.
Description
Technical Field
The invention relates to the field of electrolytic copper foil, in particular to a preparation method of an anode plate applied to electrolytic copper foil.
Background
The prior electrolytic copper foil is a method for producing the copper foil by a continuous electrolytic method, is suitable for producing wide copper foil and is the most common method for producing the copper foil on a large scale at present, and good anode plates and cathode rollers often have great influence on the performance of the deposited copper foil during electrolytic preparation of the copper foil. Inert anodes are often used in industrial metallurgy, and inert anodes with good quality often have the characteristics of high conductivity, strong corrosion resistance, high mechanical strength and the like.
Lead electrodes and titanium electrodes are often adopted as anode materials in the prior art when the electrolytic copper foil is used, wherein the lead electrodes are gradually replaced by the titanium electrode plates due to the problems of weaker self conductivity and heavy metal pollution, but the existing titanium electrode plates often show the phenomenon of uneven current density in the electrolytic process, and meanwhile, the titanium electrode plates are weaker in quality and mechanical strength and larger in contact resistance, so that electric energy waste is caused, and the production of the electrolytic copper foil is influenced to a greater extent. Therefore, it is necessary to provide a new method for preparing an anode plate to solve the above problems.
Disclosure of Invention
The invention aims to provide a preparation method of an anode plate applied to electrolytic copper foil, which is used for solving the problems that a titanium substrate in the prior art is weak in mechanical strength and uneven in current density in an electrolytic reaction process.
In order to solve the technical problem, the invention provides a preparation method of an anode plate applied to electrolytic copper foil, which comprises the following steps: substrate pretreatment, coating liquid preparation, single-layer firing, multi-layer firing and shaping firing; the preparation method of the coating liquid comprises the following steps: the iridium trichloride, the palladium chloride, the cobalt chloride, the manganese chloride, the hydrochloric acid and the ethanol are uniformly mixed to prepare coating liquid.
Wherein the mass ratio of iridium trichloride, palladium chloride, cobalt chloride, manganese chloride and hydrochloric acid in the coating liquid is (30-40): (15-18): (8-10): (10-12): (60-68), wherein the volume ratio of the ethanol to the hydrochloric acid is 1: (1-1.2), the concentration of the hydrochloric acid is 15-20%.
Preferably, the mass ratio of iridium trichloride, palladium chloride, cobalt chloride, manganese chloride and hydrochloric acid in the coating liquid is 36: 17: 8: 12: 64, and the volume ratio of the ethanol to the hydrochloric acid is 1: 1, the concentration of hydrochloric acid is 15%.
The substrate pretreatment step specifically comprises the following steps: processing the substrate into an arc shape, manufacturing a mounting hole, washing with water after alkali washing, and drying to finish the pretreatment of the substrate.
Wherein, the substrate is a titanium plate or a stainless steel plate.
Wherein the single layer firing step specifically comprises: and (3) uniformly coating the coating liquid on the surface of the pretreated substrate, drying at 80-90 ℃ for 15-20 min, sintering at 550-580 ℃ for 20-30 min, and naturally cooling to room temperature.
Wherein the multilayer firing step specifically comprises: and repeating the single-layer firing step, superposing and sintering 10-12 coatings on the surface of the substrate to obtain a composite coating substrate, and cooling the temperature to 400-450 ℃ after the last sintering and performing shaping firing.
Wherein, the shaping and firing steps specifically comprise: and (3) heating the composite coated substrate from 400-450 ℃ to 550-580 ℃ again, carrying out heat preservation sintering for 30-40 min, and naturally cooling to room temperature to obtain the anode plate applied to the electrolytic copper foil.
Wherein the iridium content in the anode plate applied to the electrolytic copper foil is 0.5-5 g/m2。
The invention has the beneficial effects that: the invention provides the preparation method of the anode plate applied to the electrolytic copper foil, which is different from the situation of the prior art, and the composite coating containing iridium, palladium, cobalt and manganese is fired on the surface of the anode substrate, so that the anode plate has stronger corrosion resistance and heat resistance, the mechanical strength of the anode plate is obviously improved, and the service life of the anode plate is prolonged; meanwhile, the current density in the electrolytic reaction process is more uniform, and the preparation of high-quality ultrathin copper foil is facilitated.
Drawings
FIG. 1 is a process flow diagram of an embodiment of the method for manufacturing an anode plate applied to an electrolytic copper foil according to the present invention.
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, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
Referring to fig. 1, fig. 1 is a process flow diagram of an embodiment of a method for manufacturing an anode plate applied to an electrolytic copper foil according to the present invention. The preparation method of the anode plate applied to the electrolytic copper foil comprises the following steps: substrate pretreatment S1, coating solution preparation S2, single layer firing S3, multi-layer firing S4, and setting firing S5, each of which is described in detail below.
S1: and (4) preprocessing a substrate. The method specifically comprises the following steps: processing the substrate into an arc shape, manufacturing a mounting hole, washing with water after alkali washing, and drying to finish the pretreatment of the substrate. In the present embodiment, the substrate is a titanium plate or a stainless steel plate.
S2: and (4) preparing a coating liquid. The method specifically comprises the following steps: the iridium trichloride, the palladium chloride, the cobalt chloride, the manganese chloride, the hydrochloric acid and the ethanol are uniformly mixed to prepare coating liquid. In the embodiment, the mass ratio of iridium trichloride, palladium chloride, cobalt chloride, manganese chloride and hydrochloric acid in the coating liquid is (30-40): (15-18): (8-10): (10-12): (60-68), wherein the volume ratio of the ethanol to the hydrochloric acid is 1: (1-1.2), wherein the concentration of the hydrochloric acid is 15-20%; preferably, the mass ratio of iridium trichloride, palladium chloride, cobalt chloride, manganese chloride and hydrochloric acid in the coating liquid is 36: 17: 8: 12: 64, and the volume ratio of the ethanol to the hydrochloric acid is 1: 1, the concentration of hydrochloric acid is 15%.
S3: and (4) single-layer firing. The method specifically comprises the following steps: and (3) uniformly coating the coating liquid on the surface of the pretreated substrate, drying at 80-90 ℃ for 15-20 min, sintering at 550-580 ℃ for 20-30 min, and naturally cooling to room temperature. Here, the sintering temperature should be lower than 600 ℃ during the single layer firing process, and the sintering temperature needs to be strictly controlled in order to avoid that part of the doped metal in the coating liquid is changed into a liquid phase during the sintering process, and the fluidity of the doped metal can cause adverse effects on the final sintered structure.
S4: and (4) multi-layer firing. The method specifically comprises the following steps: and repeating the single-layer firing step, superposing and sintering 10-12 coatings on the surface of the substrate to obtain a composite coating substrate, and cooling the temperature to 400-450 ℃ after the last sintering and performing shaping firing. The purpose of multiple times of superposition sintering is to obviously enhance the strength of the anode plate through a multi-layer compact structure, facilitate the reduction of the contact resistance of the anode plate, and limit the cooling requirement after the last sintering so as to facilitate the subsequent shaping sintering of S5 and make the whole anode plate after the shaping sintering of S5 more compact.
S5: and (5) shaping and firing. The method specifically comprises the following steps: and (3) heating the composite coated substrate from 400-450 ℃ to 550-580 ℃ again, carrying out heat preservation sintering for 30-40 min, and naturally cooling to room temperature to obtain the anode plate applied to the electrolytic copper foil. In the embodiment, the iridium content in the anode plate applied to the electrolytic copper foil is 0.5-5 g/m2。
Specifically, the principle of the above method for preparing an anode plate applied to an electrolytic copper foil is explained in detail: 1): the iridium is doped in the coating liquid and is matched with the palladium, so that the corrosion resistance and the heat resistance of the surface of the substrate can be obviously improved, and the surface of the substrate is activated, so that the current density during the electrolytic reaction is more uniform, the copper foil deposited by electrolysis is more uniformly distributed, and the deposition rate is more stable; 2) the surface hardness of the substrate can be obviously improved by doping cobalt and manganese into the coating liquid, wherein the manganese chloride is adopted during preparation, so that the grain refinement is facilitated, the doped elements are uniformly dispersed, and the oxidation resistance is also improved; 3) the arrangement mode of the multilayer overlapped coating is adopted, so that the whole structure of the manufactured anode plate is more compact, and the contact resistance is favorably reduced.
Further, effects of the above-described method for manufacturing an anode plate applied to an electrolytic copper foil will be explained in detail by way of specific embodiments.
Example 1
S1: substrate pretreatment: processing the substrate into an arc shape, manufacturing a mounting hole, washing with water after alkali washing, and drying to finish pretreatment of the substrate, wherein the substrate is a stainless steel plate.
S2: preparing a coating liquid, wherein the mass ratio of iridium trichloride, palladium chloride, cobalt chloride, manganese chloride and hydrochloric acid in the coating liquid is 32: 15: 8: 10: 62, and the volume ratio of the ethanol to the hydrochloric acid is 1: 1, the concentration of hydrochloric acid is 15%.
S3: single-layer firing: and (3) uniformly coating the coating liquid on the surface of the pretreated substrate, drying at 85 ℃ for 15min, sintering at 550 ℃ for 25min, and naturally cooling to room temperature.
S4: multilayer firing: and repeating the single-layer firing step, superposing and sintering 10 coatings on the surface of the substrate to obtain the composite coating substrate, and cooling to 400 ℃ after the last sintering and carrying out shaping firing.
S5: shaping and firing: heating the composite coated substrate from 400 ℃ to 550 ℃ again, carrying out heat preservation sintering for 30min, naturally cooling to room temperature to obtain an anode plate applied to the electrolytic copper foil, and detecting the content of iridium in the anode plate to be 1.8g/m2。
Example 2
S1: substrate pretreatment: processing the substrate into an arc shape, manufacturing a mounting hole, washing with water after alkali washing, and drying to finish the pretreatment of the substrate, wherein the substrate is a titanium plate.
S2: preparing a coating liquid, wherein the mass ratio of iridium trichloride, palladium chloride, cobalt chloride, manganese chloride and hydrochloric acid in the coating liquid is 36: 17: 8: 12: 64, and the volume ratio of the ethanol to the hydrochloric acid is 1: 1, the concentration of hydrochloric acid is 15%.
S3: single-layer firing: and (3) uniformly coating the coating liquid on the surface of the pretreated substrate, drying at 85 ℃ for 15min, sintering at 560 ℃ for 25min, and naturally cooling to room temperature.
S4: multilayer firing: and repeating the single-layer firing step, superposing and sintering 10 coatings on the surface of the substrate to obtain the composite coating substrate, and cooling to 420 ℃ after the last sintering and carrying out shaping firing.
S5: shaping and firing: heating the composite coated substrate from 420 ℃ to 570 ℃ again, carrying out heat preservation sintering for 30min, naturally cooling to room temperature to obtain an anode plate applied to the electrolytic copper foil, and detecting the content of iridium in the anode plate to be 2.2g/m2。
Example 3
S1: substrate pretreatment: processing the substrate into an arc shape, manufacturing a mounting hole, washing with water after alkali washing, and drying to finish the pretreatment of the substrate, wherein the substrate is a titanium plate.
S2: preparing a coating liquid, wherein the mass ratio of iridium trichloride, palladium chloride, cobalt chloride, manganese chloride and hydrochloric acid in the coating liquid is 39: 18: 10: 12: 67, and the volume ratio of ethanol to hydrochloric acid is 1: 1.1, the concentration of hydrochloric acid is 18%.
S3: single-layer firing: and (3) uniformly coating the coating liquid on the surface of the pretreated substrate, drying at 85 ℃ for 15min, sintering at 580 ℃ for 25min, and naturally cooling to room temperature.
S4: multilayer firing: and repeating the single-layer firing step, superposing and sintering 10 coatings on the surface of the substrate to obtain the composite coating substrate, and cooling the temperature to 450 ℃ after the last sintering and carrying out shaping firing.
S5: shaping and firing: heating the composite coated substrate from 450 ℃ to 580 ℃ again, carrying out heat preservation sintering for 30min, naturally cooling to room temperature to obtain an anode plate applied to the electrolytic copper foil, and detecting the content of iridium in the anode plate to be 2.3g/m2。
The anode plates obtained in the above examples 1 to 3 are operated for a long time, the service life of the anode plates is tested, meanwhile, the conventional titanium plate is used as a comparative example 1 to be synchronously tested, the test result is shown in table 1, wherein the service life improvement rate is calculated by the difference ratio calculation of the examples 1 to 3 relative to the comparative example 1, it can be seen that the service life of the examples 1 to 3 is remarkably improved compared with that of the comparative example 1, wherein the improvement rate of the scheme of the example 2 is the best, that is, the coating preparation parameter and the firing parameter in the example 2 are considered to be the best, so that the service life of the anode plate can be remarkably improved by the scheme.
TABLE 1
| Example 1 | Example 2 | Example 3 | Comparative example 1 | |
| Service life/h | 1225 | 1245 | 1189 | 960 |
| Service life enhancement rate/%) | 27.6 | 29.7 | 23.9 | / |
The invention provides the preparation method of the anode plate applied to the electrolytic copper foil, which is different from the situation of the prior art, and the composite coating containing iridium, palladium, cobalt and manganese is fired on the surface of the anode substrate, so that the anode plate has stronger corrosion resistance and heat resistance, the mechanical strength of the anode plate is obviously improved, and the service life of the anode plate is prolonged; meanwhile, the current density in the electrolytic reaction process is more uniform, and the preparation of high-quality ultrathin copper foil is facilitated.
It should be noted that the above embodiments belong to the same inventive concept, and the description of each embodiment has a different emphasis, and reference may be made to the description in other embodiments where the description in individual embodiments is not detailed.
The above-mentioned embodiments only express the embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (8)
1. The preparation method of the anode plate applied to the electrolytic copper foil is characterized by comprising the following steps of: substrate pretreatment, coating liquid preparation, single-layer firing, multi-layer firing and shaping firing;
the preparation steps of the coating liquid comprise: uniformly mixing iridium trichloride, palladium chloride, cobalt chloride, manganese chloride, hydrochloric acid and ethanol to obtain coating liquid;
the coating liquid is characterized in that the mass ratio of iridium trichloride, palladium chloride, cobalt chloride, manganese chloride and hydrochloric acid is (30-40): (15-18): (8-10): (10-12): (60-68), wherein the volume ratio of the ethanol to the hydrochloric acid is 1: (1-1.2), the concentration of the hydrochloric acid is 15-20%.
2. The method for preparing an anode plate applied to an electrolytic copper foil according to claim 1, wherein the coating liquid contains iridium trichloride, palladium chloride, cobalt chloride, manganese chloride and hydrochloric acid in a mass ratio of 36: 17: 8: 12: 64, and the volume ratio of the ethanol to the hydrochloric acid is 1: 1, the concentration of hydrochloric acid is 15%.
3. The method for preparing an anode plate applied to an electrolytic copper foil according to claim 1, wherein the substrate pretreatment step specifically comprises: processing the substrate into an arc shape, manufacturing a mounting hole, washing with water after alkali washing, and drying to finish the pretreatment of the substrate.
4. The method for preparing an anode plate for electrolytic copper foil according to claim 3, wherein the substrate is a titanium plate or a stainless steel plate.
5. The method for preparing an anode plate applied to an electrolytic copper foil according to claim 3, wherein the single layer firing step specifically comprises: and uniformly coating the coating liquid on the surface of the pretreated substrate, drying at 80-90 ℃ for 15-20 min, sintering at 550-580 ℃ for 20-30 min, and naturally cooling to room temperature.
6. The method for preparing an anode plate for electrolytic copper foil according to claim 5, wherein the multi-firing step comprises: and repeating the single-layer firing step, superposing and sintering 10-12 coatings on the surface of the substrate to obtain a composite coating substrate, and cooling the temperature to 400-450 ℃ after the last sintering and performing the shaping firing step.
7. The method for preparing an anode plate applied to an electrolytic copper foil according to claim 6, wherein the step of setting and firing specifically comprises: and heating the composite coated substrate from 400-450 ℃ to 550-580 ℃ again, carrying out heat preservation sintering for 30-40 min, and naturally cooling to room temperature to obtain the anode plate applied to the electrolytic copper foil.
8. The method for preparing an anode plate applied to an electrolytic copper foil according to claim 7, wherein the iridium content in the anode plate applied to the electrolytic copper foil is 0.5 to 5g/m2。
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