CN110983387B - Method for prolonging service life of anode plate for electrolytic copper foil - Google Patents
Method for prolonging service life of anode plate for electrolytic copper foil Download PDFInfo
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- CN110983387B CN110983387B CN201911390168.7A CN201911390168A CN110983387B CN 110983387 B CN110983387 B CN 110983387B CN 201911390168 A CN201911390168 A CN 201911390168A CN 110983387 B CN110983387 B CN 110983387B
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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
- C25D1/00—Electroforming
- C25D1/04—Wires; Strips; Foils
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- 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
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/08—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of metallic material
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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
- C25D17/10—Electrodes, e.g. composition, counter electrode
- C25D17/12—Shape or form
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Abstract
The invention discloses a method for prolonging the service life of an anode plate for electrolytic copper foil, which comprises the steps of selecting a titanium substrate, and punching a plurality of quincuncial holes on the surface of the titanium substrate; preparing a titanium tantalum iridium solution according to a certain proportion, coating the titanium tantalum iridium solution on the back of a titanium substrate for 1 to 3 times, and sintering the titanium tantalum iridium solution at the temperature of 450-550 ℃ for 10 to 60min to form a titanium tantalum iridium coating; preparing an iridium tantalum solution according to a certain proportion, coating the iridium tantalum solution on the back of a titanium substrate for 1-2 times, and sintering the titanium substrate for 10-60min at the temperature of 450-550 ℃ to form a first iridium tantalum coating; coating iridium tantalum solution at the plum blossom holes for 3-5 times, and sintering at the temperature of 450-550 ℃ for 10-60min to form a second iridium tantalum coating; the invention has the beneficial technical effects of innovating the preparation process technology of the anode plate by the thermal decomposition method and effectively prolonging the service life of the anode plate for the electrolytic copper foil.
Description
Technical Field
The invention belongs to the field of preparation processes of anode plates by thermal decomposition methods, and particularly relates to a method for prolonging the service life of an anode plate for electrolytic copper foil.
Background
The anode plate prepared by the traditional thermal decomposition method is widely applied to various anode plate manufacturers at present, has the advantages of simple process and good product stability, but has a great defect, and the back of the anode plate is easily and continuously oxidized at high temperature during sintering, so that the oxide layer on the back of the anode plate is thicker and has larger resistance, and the service life of the anode plate is finally influenced.
Patent publication No. CN109763149A proposes a preparation method of an anode plate, which coats titanium tantalum and iridium tantalum coatings with the same thickness on the front and back surfaces of the anode plate, so that although the anode plate is prevented from being continuously oxidized in production and the service life of the anode plate is prolonged, the back surface of a titanium substrate does not contact with electrolyte in the use process, thereby greatly causing the waste of the titanium tantalum and iridium tantalum coatings and simultaneously increasing the production cost.
In the aspect of electrolytic copper foil, along with the requirement of thinner and thinner electrolytic copper foil, the current density of the anode plate is continuously increased, the requirement on the anode plate for the electrolytic copper foil is higher and higher, and the condition that the service life of the anode plate is reduced due to oxidation of the back surface of the titanium substrate when the anode plate for the electrolytic copper foil is prepared by the traditional thermal decomposition method is more and more obvious.
Disclosure of Invention
The invention aims to provide a method for prolonging the service life of an anode plate for an electrolytic copper foil, which solves the problem that the service life of the anode plate is reduced due to oxidation of the back surface of a titanium substrate when the anode plate for the electrolytic copper foil is prepared by a traditional thermal decomposition method.
The purpose of the invention is realized by the following technical scheme:
a method for prolonging the service life of an anode plate for electrolytic copper foil specifically comprises the following steps:
s1: selecting a titanium base material, and punching a plurality of quincuncial holes in the back of the titanium base plate;
s2: preparing a titanium tantalum iridium solution, uniformly coating the titanium tantalum iridium solution on the back of a titanium substrate, and sintering to form a titanium tantalum iridium coating;
s3: preparing an iridium tantalum solution, uniformly coating the iridium tantalum solution on the back of the titanium substrate, and sintering to form a first iridium tantalum coating;
s4: preparing the same iridium-tantalum solution in the step S3, uniformly coating the iridium-tantalum solution on the plum blossom holes, and sintering to form a second iridium-tantalum coating;
s5: after high-temperature sintering, the titanium substrate, the titanium-tantalum-iridium coating, the first iridium-tantalum coating and the second iridium-tantalum coating are firmly combined into a whole.
Further: the preparation of the titanium-tantalum-iridium solution in the S2 specifically comprises the following steps:
s21: titanium tetrachloride, tantalum pentachloride and chloroiridic acid are selected as solutes;
s22: according to the mass ratio of titanium, tantalum and iridium (5-50): (50-45): (5-10) adding;
s23: one or two of isopropanol and n-butanol are used as solvents;
s24: preparing titanium tantalum iridium solution.
Further: and in the step S2, the coating times of the titanium tantalum iridium solution on the back surface of the titanium substrate are 1-3.
Further: the sintering temperature in the S2 is 450-550 ℃.
Further: and the sintering time in the S2 is 10-60 min.
Further: the total thickness of the titanium tantalum iridium coating formed in the S2 after sintering is 200nm-500 nm.
Further: the preparation of the iridium tantalum solution in the step S3 specifically comprises the following steps:
s31: tantalum pentachloride, chloroiridic acid and cobalt chloride are selected as solutes;
s32: according to the mass ratio of tantalum, iridium and cobalt (60-90): (30-10): (5-10) adding;
s33: one or two of isopropanol and n-butanol are used as solvents;
s34: preparing iridium-tantalum solution.
Further: and in the step S3, the coating times of the iridium tantalum solution on the back surface of the titanium substrate are 1-2 times.
Further: and in the S3, the sintering temperature is 450-550 ℃, the sintering time is 10-60min, and the total thickness of the first iridium-tantalum coating formed after sintering is 200-500 nm.
Further: the coating times of coating the iridium tantalum solution on the back of the plum blossom hole in the S4 are 3-5, the sintering temperature is 450-550 ℃, the sintering time is 10-60min, and the total thickness of the second iridium tantalum coating formed after sintering is 600-1200 nm.
Compared with the prior art, the invention has the following beneficial technical effects:
1) coating a titanium tantalum iridium coating with a certain thickness on the back of an anode plate for electrolytic copper foil, so that the anode plate is prevented from being oxidized in the production process;
2) coating an iridium tantalum coating with a certain thickness on the back of the anode plate for the electrolytic copper foil, so that the surface current distribution is more uniform in the use process of the anode plate;
3) an iridium tantalum coating with a certain thickness is additionally coated on a quincuncial hole on the back of an anode plate for the electrolytic copper foil, so that the conductivity of the anode plate is increased, and the current can be more uniformly distributed;
4) the anode plate for the electrolytic copper foil prepared by the technology has excellent comprehensive performance, greatly prolongs the service life of the anode for the electrolytic copper foil, and can be widely popularized and applied to the process of preparing the anode by various thermal decomposition methods.
Drawings
FIG. 1 is a schematic structural view of the present invention;
FIG. 2 is a schematic structural view of a quincuncial hole of the present invention.
Wherein: 1. a titanium substrate; 2. a titanium tantalum iridium coating; 3. a first iridium tantalum coating; 4. plum blossom holes; 5. a second iridium tantalum coating.
Detailed Description
The invention is described in further detail below with reference to the accompanying drawings:
as shown in fig. 1 and 2, the anode plate for the electrolytic copper foil comprises a titanium substrate 1, wherein a titanium tantalum iridium solution and an iridium tantalum solution are sequentially coated on the back of the titanium substrate 1 to form a titanium tantalum iridium coating 2 and a first iridium tantalum coating 3, a plurality of quincunx holes 4 punched on the back of the titanium substrate 1 are sintered at high temperature, and the titanium substrate 1, the titanium tantalum iridium coating 2 and the first iridium tantalum coating 3 are firmly combined together.
The titanium substrate 1 is made of TA1 or TA2, has a thickness of 1-3mm, and has 6 grooves and a quincuncial hole 4 with a hole diameter of 16-18 mm.
A method for prolonging the service life of an anode plate for electrolytic copper foil specifically comprises the following steps:
s1: selecting a titanium substrate 1, and punching a plurality of quincuncial holes 4 on the back of the titanium substrate.
S2: and preparing a titanium-tantalum-iridium solution.
S21: titanium tetrachloride, tantalum pentachloride and chloroiridic acid are selected as solutes;
s22: according to the mass ratio of titanium, tantalum and iridium (5-50): (50-45): (5-10) adding;
s23: one or two of isopropanol and n-butanol are used as solvents;
s24: preparing titanium tantalum iridium solution.
The titanium tantalum iridium solution is prepared and then is evenly coated on the back of the titanium substrate 1, the coating frequency of the titanium tantalum iridium solution coated on the back of the titanium substrate 1 is 1-3 times, the sintering temperature is 450-550 ℃, the sintering time is 10-60min, and the total thickness of the coating formed after sintering is 200-500 nm to form the titanium tantalum iridium coating 2.
S3: preparing iridium-tantalum solution.
S31: tantalum pentachloride, chloroiridic acid and cobalt chloride are selected as solutes;
s32: according to the mass ratio of tantalum, iridium and cobalt (60-90): (30-10): (5-10) adding;
s33: one or two of isopropanol and n-butanol are used as solvents;
s34: preparing iridium-tantalum solution.
The iridium-tantalum solution is uniformly coated on the back surface of the titanium substrate 1, the coating times of the iridium-tantalum solution coated on the back surface of the titanium substrate 1 are 1-2 times, the sintering temperature is 450-550 ℃, the sintering time is 10-60min, and the total thickness of the coating formed after sintering is 200-500 nm, so that the first iridium-tantalum coating 3 is formed.
S4: preparing the same iridium-tantalum solution in the step S3, uniformly coating the iridium-tantalum solution on the plum blossom holes 4, wherein the coating times of coating the iridium-tantalum solution on the back surfaces of the plum blossom holes 4 are 3-5, the sintering temperature is 450-550 ℃, the sintering time is 10-60min, and the total thickness of the coating formed after sintering is 600-1200 nm, and sintering to form the second iridium-tantalum coating 5.
S5: after high-temperature sintering, the titanium substrate 1, the titanium-tantalum-iridium coating 2, the first iridium-tantalum coating and the second iridium-tantalum coating 5 are firmly combined into a whole.
Example 1
The titanium substrate 1 was selected as TA1, and a number of quincunx holes 4 were punched in the surface thereof, followed by surface treatment.
Titanium tetrachloride, tantalum pentachloride and chloroiridic acid are selected as solutes, and the mass ratio of titanium to tantalum to iridium is 20: 75: 5, preparing a titanium tantalum iridium solution by using an isopropanol solvent, uniformly coating the titanium tantalum iridium solution on the back surface of the titanium substrate 1 for 2 times, sintering at 500 ℃ for 15min, and forming the titanium tantalum iridium coating layer 2.
Tantalum pentachloride, chloroiridic acid and cobalt chloride are selected as solutes, and the mass ratio of tantalum, iridium and cobalt elements is 20: 75: 5, preparing an iridium tantalum solution by using isopropanol as a solvent, uniformly coating the iridium tantalum solution on the back surface of the titanium substrate 1 for 1 time, sintering at 500 ℃ for 15min, and forming the first iridium tantalum coating layer 3.
And (3) coating an iridium tantalum coating on the positions of the plum blossom holes 4 according to the proportion, wherein the coating times are 3 times, the sintering temperature is 500 ℃, and the time is 15min, so that a second iridium tantalum coating 5 is formed.
Example 2
The titanium substrate 1 was selected as TA1, and a number of quincunx holes 4 were punched in the surface thereof, followed by surface treatment.
Titanium tetrachloride, tantalum pentachloride and chloroiridic acid are selected as solutes, and the mass ratio of titanium to tantalum to iridium is 25: 70: 5, preparing a titanium tantalum iridium solution by using an isopropanol solvent, uniformly coating the titanium tantalum iridium solution on the back surface of the titanium substrate 1 for 1 time, sintering at 520 ℃ for 10min, and forming the titanium tantalum iridium coating layer 2.
Tantalum pentachloride, chloroiridic acid and cobalt chloride are selected as solutes, and the mass ratio of tantalum, iridium and cobalt elements is 20: 75: 5, preparing an iridium tantalum solution by using isopropanol as a solvent, uniformly coating the iridium tantalum solution on the back surface of the titanium substrate 1 for 2 times, sintering at 500 ℃ for 15min, and forming the first iridium tantalum coating layer 3.
And (3) coating an iridium tantalum coating on the positions of the plum blossom holes 4 according to the proportion, wherein the coating times are 3 times, the sintering temperature is 500 ℃, and the time is 15min, so that a second iridium tantalum coating 5 is formed.
Example 3
The titanium substrate 1 was selected as TA2, and a number of quincunx holes 4 were punched in the surface thereof, followed by surface treatment.
Titanium tetrachloride, tantalum pentachloride and chloroiridic acid are selected as solutes, and the mass ratio of titanium to tantalum to iridium is 20: 75: 5, preparing a titanium tantalum iridium solution by using an isopropanol solvent, uniformly coating the titanium tantalum iridium solution on the back surface of the titanium substrate 1 for 1 time, sintering at 520 ℃, and keeping the time for 15min to form the titanium tantalum iridium coating layer 2.
Tantalum pentachloride, chloroiridic acid and cobalt chloride are selected as solutes, and the mass ratio of tantalum, iridium and cobalt elements is 25: 70: 5, preparing an iridium tantalum solution by using isopropanol as a solvent, uniformly coating the iridium tantalum solution on the back surface of the titanium substrate 1 for 2 times, sintering at 500 ℃ for 15min, and forming the first iridium tantalum coating layer 3.
And (3) coating an iridium tantalum coating on the positions of the plum blossom holes 4 according to the proportion, wherein the coating times are 3 times, the sintering temperature is 500 ℃, and the time is 15min, so that a second iridium tantalum coating 5 is formed.
It is noted that relational terms such as "first" and "second," and the like, may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that an 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.
The above description is merely exemplary of the present application and is presented to enable those skilled in the art to understand and practice the present application. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the application. Thus, the present application is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
It is to be understood that the present application is not limited to what has been described above, and that various modifications and changes may be made without departing from the scope thereof. The scope of the application is limited only by the appended claims.
Claims (8)
1. A method for prolonging the service life of an anode plate for electrolytic copper foil is characterized by comprising the following steps:
s1: selecting a titanium base material (1), and punching a plurality of plum blossom holes (4) on the back of a titanium substrate;
s2: preparing a titanium-tantalum-iridium solution, uniformly coating the titanium-tantalum-iridium solution on the back of a titanium base material (1), and sintering to form a titanium-tantalum-iridium coating (2);
s3: preparing an iridium tantalum solution, uniformly coating the iridium tantalum solution on the back of the titanium substrate (1), and sintering to form a first iridium tantalum coating (3);
s4: preparing the same iridium-tantalum solution in the step S3, uniformly coating the iridium-tantalum solution on the plum blossom holes (4), and sintering to form a second iridium-tantalum coating (5);
s5: after high-temperature sintering, the titanium substrate (1), the titanium-tantalum-iridium coating (2), the first iridium-tantalum coating (3) and the second iridium-tantalum coating (5) are firmly combined into a whole;
the preparation of the titanium-tantalum-iridium solution in the S2 specifically comprises the following steps:
s21: titanium tetrachloride, tantalum pentachloride and chloroiridic acid are selected as solutes;
s22: according to the mass ratio of titanium, tantalum and iridium (5-50): (50-45): (5-10) adding;
s23: one or two of isopropanol and n-butanol are used as solvents;
s24: preparing a titanium-tantalum-iridium solution;
the preparation of the iridium tantalum solution in the step S3 specifically comprises the following steps:
s31: tantalum pentachloride, chloroiridic acid and cobalt chloride are selected as solutes;
s32: according to the mass ratio of tantalum, iridium and cobalt (60-90): (30-10): (5-10) adding;
s33: one or two of isopropanol and n-butanol are used as solvents;
s34: preparing iridium-tantalum solution.
2. The method for improving the lifetime of an anode plate for an electrodeposited copper foil according to claim 1, wherein the number of coating times of the titanium tantalum iridium solution on the back surface of the titanium substrate (1) in S2 is 1 to 3.
3. The method as claimed in claim 1, wherein the sintering temperature in S2 is 450-550 ℃.
4. The method for improving the lifetime of an anode plate for an electrolytic copper foil as claimed in claim 1, wherein the sintering time in S2 is 10-60 min.
5. The method for improving the lifetime of an anode plate for an electrodeposited copper foil according to claim 1, wherein the total thickness of the titanium tantalum iridium coating (2) formed after sintering in S2 is 200nm to 500 nm.
6. The method for improving the lifetime of the anode plate for electrolytic copper foil as claimed in claim 1, wherein the number of coating times of the iridium tantalum solution on the back surface of the titanium substrate (1) in S3 is 1-2.
7. The method as claimed in claim 1, wherein the sintering temperature of S3 is 450-.
8. The method for prolonging the service life of the anode plate for the electrolytic copper foil as claimed in claim 1, wherein the coating times of the iridium tantalum solution on the back of the quincunx holes (4) in S4 is 3-5, the sintering temperature is 450-550 ℃, the sintering time is 10-60min, and the total thickness of the second iridium tantalum coating (5) formed after sintering is 600-1200 nm.
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| CN113355705B (en) * | 2021-06-02 | 2022-05-03 | 建滔（连州）铜箔有限公司 | Titanium anode plate for electrolytic copper foil and back treatment process |
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| CN207918974U (en) * | 2018-01-23 | 2018-09-28 | 福建清景铜箔有限公司 | A kind of foil machine anode plate structure for improving the copper foil thickness uniformity and adjusting |
| CN108642479A (en) * | 2018-05-29 | 2018-10-12 | 江阴安诺电极有限公司 | The preparation method of the electrode coating of efficient high activity |
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| CN109763149A (en) * | 2019-03-12 | 2019-05-17 | 江阴安诺电极有限公司 | Iridium tantalum coated anode plate |
| CN109989075A (en) * | 2019-05-10 | 2019-07-09 | 建滔（连州）铜箔有限公司 | A kind of back coating technique producing electrolytic copper foil titanium anode plate |
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| CN207918974U (en) * | 2018-01-23 | 2018-09-28 | 福建清景铜箔有限公司 | A kind of foil machine anode plate structure for improving the copper foil thickness uniformity and adjusting |
| CN108642479A (en) * | 2018-05-29 | 2018-10-12 | 江阴安诺电极有限公司 | The preparation method of the electrode coating of efficient high activity |
| CN109457270A (en) * | 2018-12-29 | 2019-03-12 | 西安泰金工业电化学技术有限公司 | A kind of preparation method of ti-based coating Ni―Ti anode |
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Address after: 710299 No. 15, west section of Xijin Road, Jingwei Industrial Park, Xi'an Economic and Technological Development Zone, Xi'an City, Shaanxi Province Patentee after: Xi'an Taijin Xinneng Technology Co.,Ltd. Address before: No.15, west section of Xijin Road, Jingwei Industrial Park, Xi'an Economic and Technological Development Zone, Xi'an City, Shaanxi Province 710201 Patentee before: XI'AN TAIJIN INDUSTRIAL ELECTROCHEMICAL TECHNOLOGY Co.,Ltd. |