CN111020671A - Method for forming oxide film on surface of titanium product - Google Patents
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- CN111020671A CN111020671A CN202010049615.9A CN202010049615A CN111020671A CN 111020671 A CN111020671 A CN 111020671A CN 202010049615 A CN202010049615 A CN 202010049615A CN 111020671 A CN111020671 A CN 111020671A
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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
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/26—Anodisation of refractory metals or alloys based thereon
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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
- 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
- C23G1/14—Cleaning or pickling metallic material with solutions or molten salts with alkaline solutions
- C23G1/20—Other heavy metals
- C23G1/205—Other heavy metals refractory metals
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Abstract
The invention provides a method for forming an oxide film on the surface of a titanium product, which comprises the following steps: firstly, cleaning oil stains; step two, heat treatment; step three, polishing the surface of the titanium product; step four, carrying out anodic oxidation treatment for the first time; step five, washing with deionized water and performing ultrasonic treatment; step six, carrying out anodic oxidation treatment for the second time; step seven, washing with deionized water and performing ultrasonic treatment; and step eight, carrying out mechanical polishing treatment on the surface of the titanium product. The process for forming the oxide film on the surface of the titanium product is stable and reliable, the operation is convenient, the control is easy, and the equipment is simple. After the treatment of the invention, the oxide film layer generated on the surface of the titanium product has good stability and is not easy to fall off, and simultaneously, the situations that handprints are adhered on the titanium product, the product is scratched, and the titanium product is damaged and the appearance of the titanium product is influenced can be avoided, so that the color of the surface of the titanium product is uniform and has no color difference, the surface is smooth and beautiful, the surface hardness of the titanium product is enhanced, and the overall performance of the titanium product is improved.
Description
Technical Field
The invention relates to the technical field of titanium product surface treatment, in particular to a method for forming an oxide film on the surface of a titanium product.
Background
The titanium and the titanium alloy have many excellent characteristics, such as high corrosion resistance, high strength, good high-temperature and low-temperature strength performance, good human body adaptability, low density and the like, and are widely applied to the national defense industry fields of nuclear power aviation, aerospace, ships and the like. Also applied to civil and chemical industry fields such as shipbuilding, petrochemical equipment, offshore platforms, electric power equipment, medical treatment, high-grade consumer goods and the like, and is called as strategic metal. With the continuous research on titanium and titanium metal, titanium products also slowly permeate into the field of daily necessities, such as vacuum cups, ornaments, furniture and the like of the titanium products.
The titanium product is more and more widely applied, but no matter in the field of national defense industry, civil and chemical industry or in the field of daily necessities, the surface of the titanium product needs to be retreated after the titanium product is manufactured, so that the performances of the titanium product in various aspects such as durability, economy, beauty and the like are improved, the surface engineering technology of the titanium product is separate from various technologies, and great attention is paid to the titanium product.
At present, a titanium oxide film is generated on the surface of a titanium product by a surface treatment technology of the titanium product so as to improve the surface quality of the titanium product. The surface treatment technology of the titanium product mainly comprises electroplating, anodic oxidation, micro-arc oxidation, ion implantation, nitridation, electron beam and laser surface modification, thermal spraying, carburization, Physical Vapor Deposition (PVD) and the like. The problems of obvious polishing lines, non-uniform color, color difference and the like are often caused after the surface of the titanium product is treated at present.
Therefore, there is a need for an improvement of the existing surface treatment method of titanium products to improve the surface quality of the titanium products.
Disclosure of Invention
The invention aims to improve the surface quality of a titanium product and provides a method for forming an oxide film on the surface of the titanium product. The surface quality of the surface of the titanium product is improved by forming the oxide film layer on the surface of the titanium product, and the titanium product surface treatment method is suitable for surface treatment of the titanium product in various industries, so that the titanium product is more durable, economic, beautiful, safe and reliable.
The technical scheme for realizing the purpose of the invention is as follows: a method for forming an oxide film layer on the surface of a titanium product comprises the following steps:
step one, oil stain cleaning: cleaning oil stains on the surface of the titanium product;
step two, heat treatment: the titanium product in the step one is at 4 multiplied by 10-5~6×10-5Pa, raising the temperature of the treatment device to 500-600 ℃ at a speed of 5-10 ℃ per second, keeping the temperature for 30-60 min, raising the temperature of the treatment device to 800-900 ℃ at a speed of 10-20 ℃ per second, preserving the heat for 120min, filling inert gas into the device in the heat treatment process, reducing the temperature of the titanium product to normal temperature at a speed of 10 ℃ per second after the heat treatment, and taking out the titanium product for later use;
step three, polishing the surface of the titanium product: polishing the surface of the titanium product in the step two;
step four, first anodic oxidation treatment: placing the titanium product in the third step as an anode and one of a lead plate, a graphite plate and a stainless steel plate as a cathode in primary electrolyte for primary electrolysis;
step five, washing the titanium product in the step four with deionized water to remove primary electrolyte, and then carrying out ultrasonic treatment to remove an oxidation layer which is not firmly attached to the surface of the titanium product and is easy to fall off;
step six, second anodic oxidation treatment: placing the titanium product in the fifth step into secondary electrolyte for second electrolysis by taking the titanium product as an anode and one of a lead plate, a graphite plate and a stainless steel plate as a cathode;
step seven, washing the titanium product obtained in the step six with deionized water to remove secondary electrolyte, and then carrying out ultrasonic treatment to remove an oxidation layer which is not firmly attached to the surface of the titanium product and is easy to fall off;
step eight, mechanical polishing treatment of the surface of the titanium product: and F, washing the titanium product in the step seven by using deionized water to remove secondary electrolyte, drying the titanium product under a vacuum condition, and performing mechanical polishing treatment on the surface of the titanium product.
The heat treatment can eliminate the component segregation in the titanium product, reduce the residual stress in the titanium product, remove the impurities such as hydrogen in the titanium product and improve the quality of the titanium product. When the titanium product is subjected to heat treatment, the temperature is raised step by step and slowly, and in the process of temperature rise, the titanium product can be heated more uniformly due to the adoption of uniform and slow temperature rise at a certain speed, so that cracks on the surface of the titanium product are avoided.
Carrying out anodic oxidation on the surface of the titanium product twice to form an oxide film layer, wherein the anodic oxidation for the first time generates a layer of oxide film layer on the surface of the polished titanium product, the oxide film layer at part of the part can be firmly attached to the surface of the titanium product, and the oxide film which is not firmly attached is removed by an ultrasonic method. According to the invention, as the components of the titanium oxide film layer change to titanium → titanium monoxide → titanium trioxide → titanium dioxide in sequence along with the difference of electrolysis time, electrolyte composition and electrolysis pressure, if the electrolysis reaction is complete, the components of the generated oxide film layer are all titanium dioxide, if the electrolysis reaction is incomplete, a mixture of titanium monoxide, titanium trioxide and titanium dioxide is generated, the property of the oxide film layer is unstable, the thicknesses of the oxide film layers are different, and the uniformity of the oxide film layer is poor, therefore, the titanium product is subjected to the second anodic oxidation treatment after the first anodic oxidation treatment, on one hand, the titanium oxide film layer reacts completely, the titanium dioxide final product is generated, and meanwhile, the stable oxide film layer is generated on the exposed surface of the titanium product after ultrasonic treatment.
Because of two times of anodic oxidation treatment and two times of ultrasonic treatment, the thickness of the oxide film layer on the surface of the titanium product is uneven, and the quality problem that the smoothness does not reach the standard possibly exists, therefore, the surface of the titanium product is treated by mechanical polishing to improve the surface smoothness of the titanium product, and the problems that the color of the titanium product is disordered and the appearance quality is poor under the action of light reflection and refraction are avoided.
In a preferred embodiment of the invention, in the step one, the titanium product is treated by soaking in acetone solution, rinsing with deionized water, soaking in sodium hydroxide solution and rinsing with deionized water.
In a preferred embodiment of the invention, in the third step, the surface roughness of the titanium product is 30-120 μm.
In a preferred embodiment of the present invention, in the fourth step, the primary electrolyte is a mixed solution of phosphoric acid and sodium gluconate, the electrolysis temperature of the first anodic oxidation treatment is 30 ± 3 ℃, the first electrolysis time is 20-30 min, and the electrolysis voltage is 45-50V.
In the sixth step, the secondary electrolyte is a mixed solution of absolute ethyl alcohol, perchloric acid and hydrofluoric acid, the electrolysis temperature of the second anodic oxidation treatment is 25 +/-3 ℃, the time of the second electrolysis is 60-120 min, and the electrolysis voltage is 30-45V.
In a preferred embodiment of the present invention, in the fourth and sixth steps, the primary electrolyte and the secondary electrolyte are stirred every 5min for 30s in the first electrolysis and the second electrolysis.
In a preferred embodiment of the invention, in the fifth step and the seventh step, the ultrasonic time is 3-10 min, the ultrasonic power is 20-30 kHz, and the ultrasonic liquid is deionized water.
Compared with the prior art, the beneficial effects of the invention are as follows:
1. the primary electrolytic solution and the second electrolytic solution adopted by the invention are both environment-friendly electrolytic solutions, and meet the requirement of environment-friendly discharge.
2. The method adopts a new surface treatment process, and comprises the steps of carrying out surface treatment on a titanium product, removing impurities in the titanium product during the heat treatment, slightly polishing the surface of the titanium product, and generating an oxide film on the surface of the titanium product through two different electrolytic reactions. After the treatment of the invention, the oxide film layer generated on the surface of the titanium product has good stability and is not easy to fall off, and simultaneously, the situations that handprints are adhered on the titanium product, the product is scratched, and the titanium product is damaged and the appearance of the titanium product is influenced can be avoided, so that the color of the surface of the titanium product is uniform and has no color difference, the surface is smooth and beautiful, the surface hardness of the titanium product is enhanced, and the overall performance of the titanium product is improved.
Drawings
FIG. 1 is a flow chart of a method for forming an oxide film on the surface of a titanium product according to the present invention.
Detailed Description
The present invention is described in detail with reference to the embodiments shown in the drawings, but it should be understood that these embodiments are not intended to limit the present invention, and those skilled in the art should understand that functional, methodological, or structural equivalents or substitutions made by these embodiments are within the scope of the present invention.
Furthermore, the terms "first," "second," "third," and the like are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicit to a number of indicated technical features. Thus, a feature defined as "first," "second," etc. may explicitly or implicitly include one or more of that feature. In the description of the invention, the meaning of "a plurality" is two or more unless otherwise specified.
The terms "mounted," "connected," and "coupled" are to be construed broadly and may, for example, be fixedly coupled, detachably coupled, or integrally coupled; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meaning of the above terms in the creation of the present invention can be understood by those of ordinary skill in the art through specific situations.
A method for forming an oxide film layer on the surface of a titanium product comprises the following steps:
step one, oil stain cleaning: cleaning oil stains on the surface of the titanium product;
step two, heat treatment: the titanium product in the step one is at 4 multiplied by 10-5~6×10-5Pa, raising the temperature of the processing device to 500-600 ℃ at a speed of 5-10 ℃ per second, maintaining the temperature for 30-60 min, and raising the temperature of the processing device to 10-20 ℃ per secondPerforming heat treatment at 800-900 ℃, preserving heat for 120min, filling inert gas into the device in the heat treatment process, cooling the temperature of the titanium product to normal temperature at the speed of 10 ℃ per second after the heat treatment, and taking out for later use;
step three, polishing the surface of the titanium product: polishing the surface of the titanium product in the step two;
step four, first anodic oxidation treatment: placing the titanium product in the third step as an anode and one of a lead plate, a graphite plate and a stainless steel plate as a cathode in primary electrolyte for primary electrolysis;
step five, washing the titanium product in the step four with deionized water to remove primary electrolyte, and then carrying out ultrasonic treatment to remove an oxidation layer which is not firmly attached to the surface of the titanium product and is easy to fall off;
step six, second anodic oxidation treatment: placing the titanium product in the fifth step into secondary electrolyte for second electrolysis by taking the titanium product as an anode and one of a lead plate, a graphite plate and a stainless steel plate as a cathode;
step seven, washing the titanium product obtained in the step six with deionized water to remove secondary electrolyte, and then carrying out ultrasonic treatment to remove an oxidation layer which is not firmly attached to the surface of the titanium product and is easy to fall off;
step eight, mechanical polishing treatment of the surface of the titanium product: and F, washing the titanium product in the step seven by using deionized water to remove secondary electrolyte, drying the titanium product under a vacuum condition, and performing mechanical polishing treatment on the surface of the titanium product.
In the invention, the heat treatment 1 can eliminate the component segregation in the titanium product, reduce the residual stress in the titanium product, remove the impurities such as hydrogen in the titanium product and improve the quality of the titanium product. When the titanium product is subjected to heat treatment, the temperature is raised step by step and slowly, and in the process of temperature rise, the titanium product can be heated more uniformly due to the adoption of uniform and slow temperature rise at a certain speed, so that cracks on the surface of the titanium product are avoided. 2. And (3) anodizing for the first time to generate an oxide film layer on the surface of the polished titanium product, wherein the oxide film layer on part of the part can be firmly attached to the surface of the titanium product, and the oxide film which is not firmly attached is removed by an ultrasonic method. 3. According to the invention, as the components of the titanium oxide film layer change to titanium → titanium monoxide → titanium trioxide → titanium dioxide in sequence along with the difference of electrolysis time, electrolyte composition and electrolysis pressure, if the electrolysis reaction is complete, the components of the generated oxide film layer are all titanium dioxide, if the electrolysis reaction is incomplete, a mixture of titanium monoxide, titanium trioxide and titanium dioxide is generated, the property of the oxide film layer is unstable, the thicknesses of the oxide film layers are different, and the uniformity of the oxide film layer is poor, therefore, the titanium product is subjected to the second anodic oxidation treatment after the first anodic oxidation treatment, on one hand, the titanium oxide film layer reacts completely, the titanium dioxide final product is generated, and meanwhile, the stable oxide film layer is generated on the exposed surface of the titanium product after ultrasonic treatment.
The method for forming an oxide film layer on the surface of a titanium product according to the present invention will be described in detail below with reference to specific examples.
Example 1:
referring to fig. 1, fig. 1 is a flow chart illustrating a method for forming an oxide film on a surface of a titanium product according to the present invention.
In this embodiment, the method for forming an oxide film on the surface of a titanium gasket, in which the titanium product is a titanium gasket having different sizes, includes the steps of:
step one, oil stain cleaning: soaking the titanium gasket by using an acetone solution, washing the titanium gasket by using deionized water, soaking the titanium gasket by using a sodium hydroxide solution and washing the titanium gasket by using deionized water to remove oil stains on the surface of the titanium gasket;
step two, heat treatment: the titanium gasket in the step one is in a range of (4.5 +/-0.5) multiplied by 10-5And Pa, raising the temperature of the treatment device to 550 ℃ at a speed of 5 ℃ per second, keeping the temperature for 45min, raising the temperature of the treatment device to 900 ℃ at a speed of 15 ℃ per second, preserving the temperature for 120min, filling inert gas into the device in the heat treatment process, reducing the temperature of the titanium gasket to normal temperature at a speed of 10 ℃ per second after the heat treatment, and taking out the titanium gasket for later use.
Step three, polishing the surface of the titanium gasket: polishing the surface of the titanium gasket in the second step to ensure that the surface roughness of the titanium gasket is 50 +/-20 microns;
step four, first anodic oxidation treatment: and (3) placing the titanium gasket in primary electrolyte to carry out primary electrolysis by taking the titanium gasket in the third step as an anode and taking one of a lead plate, a graphite plate and a stainless steel plate as a cathode. During the first anodizing treatment, the primary electrolyte is a mixed solution of phosphoric acid and sodium gluconate, the electrolysis temperature is 30 +/-3 ℃, the first electrolysis time is 20-30 min, and the electrolysis voltage is 45-50V;
step five, washing the titanium gasket in the step four with deionized water to remove primary electrolyte, and then carrying out ultrasonic treatment, wherein the ultrasonic time is 5min, the ultrasonic power is 25kHz, and an oxidation layer which is not firm and is easy to fall off is removed from the surface of the titanium gasket;
step six, second anodic oxidation treatment: and D, taking the titanium gasket in the step five as an anode, taking one of a lead plate, a graphite plate and a stainless steel plate as a cathode, and putting the titanium gasket in secondary electrolyte for secondary electrolysis. During the second anodizing treatment, the secondary electrolyte is a mixed solution of absolute ethyl alcohol, perchloric acid and hydrofluoric acid, the electrolysis temperature of the second anodizing treatment is 25 +/-3 ℃, the time of the second electrolysis is 60-120 min, and the electrolysis voltage is 30-45V;
step seven, washing the titanium gasket in the step six with deionized water to remove secondary electrolyte, performing ultrasonic treatment for 3min at the ultrasonic power of 20kHz, and removing an oxidation layer which is attached to the surface of the titanium gasket and is not firm and easy to fall off;
step eight, mechanical polishing treatment of the surface of the titanium gasket: and washing the titanium gasket obtained in the step seven by using deionized water to remove secondary electrolyte, drying the titanium gasket under a vacuum condition, and then carrying out mechanical polishing treatment on the surface of the titanium gasket.
Example 2:
referring to fig. 1, fig. 1 is a flow chart illustrating a method for forming an oxide film on a surface of a titanium product according to the present invention.
In this embodiment, the method for forming an oxide film on the surface of a titanium vacuum cup, in which the titanium product is a titanium vacuum cup, includes the steps of:
step one, oil stain cleaning: soaking the titanium vacuum cup by using an acetone solution, washing the titanium vacuum cup by using deionized water, soaking the titanium vacuum cup by using a sodium hydroxide solution and washing the titanium vacuum cup by using the deionized water to remove oil stains on the surface of the titanium vacuum cup;
step two, heat treatment: the titanium vacuum cup in the step one is placed at (5.5 +/-0.5) multiplied by 10-5Pa, raising the temperature of the processing device to 500 ℃ at a speed of 10 ℃ per second, keeping the temperature for 30min, raising the temperature of the processing device to 800 ℃ at a speed of 20 ℃ per second, preserving the heat for 120min, filling inert gas into the device during the heat treatment, reducing the temperature of the titanium vacuum cup to normal temperature at a speed of 10 ℃ per second after the heat treatment, and taking out the titanium vacuum cup for later use.
Step three, polishing the surface of the titanium vacuum cup: polishing the surface of the titanium vacuum cup in the step two to ensure that the surface roughness of the titanium vacuum cup is 100 +/-10 microns;
step four, first anodic oxidation treatment: and (3) placing the titanium vacuum cup in primary electrolyte for first electrolysis by taking the titanium vacuum cup in the third step as an anode and one of a lead plate, a graphite plate and a stainless steel plate as a cathode. During the first anodizing treatment, the primary electrolyte is a mixed solution of phosphoric acid and sodium gluconate, the electrolysis temperature is 30 +/-3 ℃, the first electrolysis time is 20-30 min, and the electrolysis voltage is 45-50V. During first electrolysis, stirring the first electrolyte every 5min for 30 s;
step five, washing the titanium vacuum cup in the step four with deionized water to remove primary electrolyte, and then carrying out ultrasonic treatment, wherein the ultrasonic time is 5min, the ultrasonic power is 25kHz, and an oxidation layer which is not firm and is easy to fall off is removed from the surface of the titanium vacuum cup;
step six, second anodic oxidation treatment: and D, placing the titanium vacuum cup in secondary electrolyte for secondary electrolysis by taking the titanium vacuum cup in the step five as an anode and one of a lead plate, a graphite plate and a stainless steel plate as a cathode. During the second anodizing treatment, the secondary electrolyte is a mixed solution of absolute ethyl alcohol, perchloric acid and hydrofluoric acid, the electrolysis temperature of the second anodizing treatment is 25 +/-3 ℃, the time of the second electrolysis is 60-120 min, the electrolysis voltage is 30-45V, and during the second electrolysis, the secondary electrolyte is stirred every 5min, and the stirring time is 30 s;
step seven, washing the titanium vacuum cup in the step six with deionized water to remove secondary electrolyte, performing ultrasonic treatment for 10min at the ultrasonic power of 30kHz, and removing an oxidation layer which is attached to the surface of the titanium vacuum cup and is not firm and is easy to fall off;
step eight, mechanical polishing treatment of the surface of the titanium gasket: and (5) washing the titanium vacuum cup in the seventh step with deionized water to remove secondary electrolyte, drying under a vacuum condition, and then carrying out mechanical polishing treatment on the surface of the titanium vacuum cup.
The titanium products treated in examples 1 and 2 were tested:
a. scratch resistance test: the titanium articles were subjected to a surface scratch test, specifically a scratch depth at constant force and a critical scratch force at increasing force.
b. And (3) hardness test: and performing a small force value Vickers hardness test on the titanium product, wherein the average hardness value is higher than the hardness of the matrix.
The above-listed detailed description is only a specific description of a possible embodiment of the present invention, and they are not intended to limit the scope of the present invention, and equivalent embodiments or modifications made without departing from the technical spirit of the present invention should be included in the scope of the present invention.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (6)
1. A method for forming an oxide film layer on the surface of a titanium product is characterized by comprising the following steps:
step one, oil stain cleaning: cleaning oil stains on the surface of the titanium product;
step two, heat treatment: the titanium product in the step one is at 4 multiplied by 10-5~6×10-5Pa, raising the temperature of the treatment device to 500-600 ℃ at a speed of 5-10 ℃ per second, keeping the temperature for 30-60 min, raising the temperature of the treatment device to 800-900 ℃ at a speed of 10-20 ℃ per second, preserving the heat for 120min, filling inert gas into the device in the heat treatment process, reducing the temperature of the titanium product to normal temperature at a speed of 10 ℃ per second after the heat treatment, and taking out the titanium product for later use;
step three, polishing the surface of the titanium product: polishing the surface of the titanium product in the step two;
step four, first anodic oxidation treatment: placing the titanium product in the third step as an anode and one of a lead plate, a graphite plate and a stainless steel plate as a cathode in primary electrolyte for primary electrolysis;
step five, washing the titanium product in the step four with deionized water to remove primary electrolyte, and then carrying out ultrasonic treatment to remove an oxidation layer which is not firmly attached to the surface of the titanium product and is easy to fall off;
step six, second anodic oxidation treatment: placing the titanium product in the fifth step into secondary electrolyte for second electrolysis by taking the titanium product as an anode and one of a lead plate, a graphite plate and a stainless steel plate as a cathode;
step seven, washing the titanium product obtained in the step six with deionized water to remove secondary electrolyte, and then carrying out ultrasonic treatment to remove an oxidation layer which is not firmly attached to the surface of the titanium product and is easy to fall off;
step eight, mechanical polishing treatment of the surface of the titanium product: and F, washing the titanium product in the step seven by using deionized water to remove secondary electrolyte, drying the titanium product under a vacuum condition, and performing mechanical polishing treatment on the surface of the titanium product.
2. The method of claim 1, wherein in the first step, the titanium product is treated by soaking in acetone solution, rinsing with deionized water, soaking in sodium hydroxide solution, and rinsing with deionized water.
3. The method of claim 1, wherein in the third step, the surface roughness of the titanium product is 30-120 μm.
4. The method for forming an oxide film on the surface of a titanium product according to claim 1, wherein in the fourth step, the primary electrolyte is a mixed solution of phosphoric acid and sodium gluconate, the electrolysis temperature of the first anodic oxidation treatment is 30 ± 3 ℃, the first electrolysis time is 20-30 min, and the electrolysis voltage is 45-50V;
in the sixth step, the secondary electrolyte is a mixed solution of absolute ethyl alcohol, perchloric acid and hydrofluoric acid, the electrolysis temperature of the second anodic oxidation treatment is 25 +/-3 ℃, the time of the second electrolysis is 60-120 min, and the electrolysis voltage is 30-45V.
5. The method according to claim 1, wherein in the fourth and sixth steps, the first and second electrolytes are stirred every 5min for 30s during the first and second electrolyzations.
6. The method of claim 1, wherein in the fifth step and the seventh step, the ultrasonic time is 3-10 min, the ultrasonic power is 20-30 kHz, and the ultrasonic liquid is deionized water.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111663165A (en) * | 2020-06-18 | 2020-09-15 | 西北有色金属研究院 | Phosphoric acid system-based secondary anodic oxidation method for industrial pure titanium |
| CN114855105A (en) * | 2022-02-09 | 2022-08-05 | 宝鸡钛普锐斯钛阳极科技有限公司 | Pretreatment method of titanium anode base material |
| CN115074712A (en) * | 2022-07-29 | 2022-09-20 | 四川大学 | Surface modification treatment method for titanium metal implant material |
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| CN115074712A (en) * | 2022-07-29 | 2022-09-20 | 四川大学 | Surface modification treatment method for titanium metal implant material |
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