CN111266404A - Preparation method of titanium substrate for coated titanium anode plate - Google Patents
Preparation method of titanium substrate for coated titanium anode plate Download PDFInfo
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- CN111266404A CN111266404A CN202010107294.3A CN202010107294A CN111266404A CN 111266404 A CN111266404 A CN 111266404A CN 202010107294 A CN202010107294 A CN 202010107294A CN 111266404 A CN111266404 A CN 111266404A
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- titanium
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21B—ROLLING OF METAL
- B21B1/00—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations
- B21B1/22—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations for rolling plates, strips, bands or sheets of indefinite length
- B21B1/227—Surface roughening or texturing
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/16—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
- C22F1/18—High-melting or refractory metals or alloys based thereon
- C22F1/183—High-melting or refractory metals or alloys based thereon of titanium or alloys based thereon
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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
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
- C23C8/08—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases only one element being applied
- C23C8/10—Oxidising
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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
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F1/00—Etching metallic material by chemical means
- C23F1/10—Etching compositions
- C23F1/14—Aqueous compositions
- C23F1/16—Acidic compositions
- C23F1/26—Acidic compositions for etching refractory metals
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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
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
- C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions
- C23G1/10—Other heavy metals
- C23G1/106—Other heavy metals refractory metals
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
Abstract
The invention relates to a preparation method of a titanium substrate for a coated titanium anode plate, which solves the problems of small effective area of the titanium substrate, insufficient binding force between a coating and the substrate and the like, and belongs to the field of electrode materials in the electrochemical industry. The method comprises the following steps: (1) preparing a titanium substrate; (2) rolling and roughening the titanium base material, namely performing single-pass rolling by adopting a laser roughening roller to form countless bosses and pits on the surface of the plate; (3) annealing and oxidizing the titanium substrate, machining the titanium substrate into a size required by the product, and then putting the product in a hornet furnace at 800-900 ℃ for annealing for 30-60min to obtain a completely recrystallized structure and form an oxide layer with a certain thickness on the surface; (4) removing oxide skin on the surface of the titanium substrate, pickling for more than 1h in boiling oxalic acid solution to remove the oxide skin, sequentially cleaning with tap water, deionized water and alcohol, and drying to obtain the rough titanium substrate. The invention can increase the effective area by more than 30 percent, and improve the adhesive force of the coating and the matrix, thereby prolonging the service life of the final product.
Description
Technical Field
The invention belongs to the field of electrode materials in the electrochemical industry, and particularly relates to a pretreatment method of a titanium plate for a coated titanium anode plate.
Background
The metal coating anode is formed by coating metal oxide on a titanium substrate, and has been widely used in a plurality of electrochemical industries such as water treatment, cathode protection, preparation of metal foil, surface treatment of metal, electroplating, electrolysis, chlor-alkali and the like due to stable performance and environmental friendliness.
In order to increase the effective area of the titanium substrate and enhance the bonding force of the coating and the titanium substrate, the effective area is generally treated by sand blasting or shot blasting texturing, then 10% -15% of alkali or washing powder is used for boiling and degreasing, and finally 10% -15% of oxalic acid is used for boiling and etching, but the following problems exist: (1) the pits and the bosses on the surface subjected to sand blasting or shot blasting texturing are not uniformly distributed, and the sizes of the pits and the bosses are large, so that the effective area is increased to a certain extent, but the effect is limited. (2) The pits and the bosses are in a hemispherical state and are not greatly different from a flat state, and although the pits and the bosses are etched by oxalic acid, the pits and the bosses have a limited effect on increasing the bonding force between the coating and the substrate.
Therefore, the preparation method of the titanium substrate for the coated titanium anode is urgently found, which can increase the effective area of the coated anode plate and increase the bonding force between the coating and the substrate.
Disclosure of Invention
The technical problem to be solved by the invention is as follows:
aiming at the defects and improvement needs in the prior art, the invention provides a pretreatment method of a titanium substrate for a coated titanium anode, which solves the problems of small effective area of the titanium substrate and insufficient binding force between the coating and the substrate.
The technical scheme of the invention is as follows:
a preparation method of a titanium plate for a coated titanium anode plate comprises the following steps:
(1) preparing a titanium base material, wherein the titanium base material is prepared by a rolling method by using a TA1 plate, and the thickness of the plate is 5-10% thicker than that of a finished product;
(2) rolling and roughening the titanium base material, namely performing single-pass rolling on the titanium plate prepared in the step (1) by adopting a laser roughening roller, and performing primary rolling to the size of a finished product, wherein countless bosses and pits are formed on the surface of the plate;
(3) annealing and oxidizing the titanium substrate, namely machining the titanium substrate prepared in the step (2) into the size required by the product, then placing the product in a hornet furnace at 800-;
(4) and (3) descaling the surface of the titanium substrate, namely pickling the titanium substrate annealed and oxidized in the step (3) in a boiling 10-15% oxalic acid solution for more than 1h to remove oxide scale and etch the surface, sequentially washing the titanium substrate by using tap water, deionized water and alcohol, and drying to obtain the titanium substrate with high specific surface area.
The invention has the beneficial effects that:
the titanium polar plate prepared by the invention has a higher effective area, the effective area is increased by more than 30% compared with a flat plate, all surfaces form uniform corrosion pits through roughening rolling, oxidation treatment and etching treatment of a titanium substrate, and the bonding force of a coating and a substrate is increased while the effective area of the titanium polar plate is increased. It is worth mentioning that the periphery of the pit is basically in a vertical state, and after etching, a corrosion pit parallel to the surface is formed, so that the adhesive force of the coating and the substrate is greatly improved. The preparation method has the advantages of stable process, simple production process, no limitation of product size and easy realization of batch production.
Detailed Description
The preparation method of the titanium substrate for the coated titanium anode plate comprises the following steps:
(1) preparing an original plate.
(2) And (5) performing roughing rolling on the titanium substrate.
(3) And (4) carrying out oxidation treatment on the titanium substrate.
(4) And (5) etching the titanium substrate.
An embodiment of the present invention will be described in detail below, but the present invention is not limited thereto
(1) A roll of TA1 plate with the width of 50cm m and the thickness of 1.5mm is selected as an original strip, the original strip is subjected to surface treatment and then is subjected to cold rolling to 1.05mm, and in order to meet the plate type requirement of the strip, the tension of the front strip and the rear strip is required in the rolling process.
(2) And (3) replacing the roller of the rolling mill or transferring the rolling mill to another special rolling mill, wherein the roller surface of the final rolling mill is a laser roughened roller surface, and the plate with the thickness of 1.05mm is rolled by 1.00mm in one step.
(3) Cutting 50cm wide strip into 48cm wide strips, flattening and straightening the cut strip without cracking, and cutting into small blocks of 48cm × 50 cm.
(4) And (3) placing the cut small blocks in a hornet furnace at 850 ℃ for annealing and oxidation treatment for 45min, and cooling along with the furnace.
(5) And (3) soaking and boiling the titanium substrate subjected to oxidation annealing treatment in a 10% oxalic acid solution for 1h to further form a rough and uneven linen surface layer on the surface of the titanium substrate, finally washing the titanium substrate with tap water, deionized water and alcohol in sequence, and drying to obtain the titanium substrate with high specific surface area.
Claims (4)
1. A preparation method of a titanium plate for a coated titanium anode plate is characterized by comprising the following steps:
(1) preparing a titanium base material, wherein the titanium base material is prepared by a rolling method, and the thickness of the plate is 5-10% thicker than that of a finished product;
(2) rolling and roughening the titanium base material, namely performing single-pass rolling on the titanium plate prepared in the step (1) by adopting a laser roughening roller, and performing primary rolling to the size of a finished product, wherein countless bosses and pits are formed on the surface of the plate;
(3) annealing and oxidizing the titanium substrate, namely machining the titanium substrate prepared in the step (2) into the size required by the product, then placing the product in a hornet furnace at 800-;
(4) and (3) descaling the surface of the titanium substrate, namely pickling the titanium substrate annealed and oxidized in the step (3) in a boiling oxalic acid solution for more than 1h to remove the scale, sequentially cleaning the titanium substrate by using tap water, deionized water and alcohol, and drying the titanium substrate.
2. The method for preparing the titanium plate for the coated titanium anode plate according to claim 1, which is characterized in that:
and (4) annealing and oxidizing the hornet furnace in the step (3) for 45min at the temperature of 850 ℃.
3. The method for preparing the titanium plate for the coated titanium anode plate according to claim 1, which is characterized in that:
the concentration of the oxalic acid solution in the step (4) is 10-15%.
4. The method for preparing a titanium plate for a coated titanium anode plate according to any one of claims 1 to 3, wherein: the titanium substrate used was TA 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010107294.3A CN111266404B (en) | 2020-02-21 | 2020-02-21 | Preparation method of titanium substrate for coated titanium anode plate |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010107294.3A CN111266404B (en) | 2020-02-21 | 2020-02-21 | Preparation method of titanium substrate for coated titanium anode plate |
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| CN111266404A true CN111266404A (en) | 2020-06-12 |
| CN111266404B CN111266404B (en) | 2021-05-18 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112588823A (en) * | 2020-12-21 | 2021-04-02 | 江苏时代华宜电子科技有限公司 | Surface roughness forming process for cold-rolled thin molybdenum sheet |
| CN112620346A (en) * | 2020-11-13 | 2021-04-09 | 江苏甬金金属科技有限公司 | Production method of wide-width precise cold-rolled titanium material |
| CN114959766A (en) * | 2022-04-14 | 2022-08-30 | 西安泰金工业电化学技术有限公司 | Pretreatment process capable of increasing binding force between titanium electrode coating and base material |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112620346A (en) * | 2020-11-13 | 2021-04-09 | 江苏甬金金属科技有限公司 | Production method of wide-width precise cold-rolled titanium material |
| CN112588823A (en) * | 2020-12-21 | 2021-04-02 | 江苏时代华宜电子科技有限公司 | Surface roughness forming process for cold-rolled thin molybdenum sheet |
| CN112588823B (en) * | 2020-12-21 | 2024-05-17 | 江苏时代华宜电子科技有限公司 | Surface roughness forming process for cold-rolled thin molybdenum sheet |
| CN114959766A (en) * | 2022-04-14 | 2022-08-30 | 西安泰金工业电化学技术有限公司 | Pretreatment process capable of increasing binding force between titanium electrode coating and base material |
| CN114959766B (en) * | 2022-04-14 | 2023-09-01 | 西安泰金新能科技股份有限公司 | Pretreatment process capable of increasing binding force between titanium electrode coating and substrate |
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| CN111266404B (en) | 2021-05-18 |
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Effective date of registration: 20230619 Address after: No. 988, Keji Road, high tech Industrial Development Zone, Kunming, Yunnan 650000 Patentee after: Yunnan Precious Metals Laboratory Co.,Ltd. Address before: No. 988, Keji Road, high tech Development Zone, Wuhua District, Kunming, Yunnan 650000 (Kunming Precious Metals Research Institute) Patentee before: Sino-Platinum Metals Co.,Ltd. |
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