CN112981494A - Titanium alloy micro-arc oxidation process with high light absorption rate - Google Patents

Titanium alloy micro-arc oxidation process with high light absorption rate Download PDF

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CN112981494A
CN112981494A CN202110180673.XA CN202110180673A CN112981494A CN 112981494 A CN112981494 A CN 112981494A CN 202110180673 A CN202110180673 A CN 202110180673A CN 112981494 A CN112981494 A CN 112981494A
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titanium alloy
concentration
micro
arc oxidation
light absorption
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张邦清
赵李斌
付国龙
赵灏琳
程李靖
张纬栋
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Shenzhen Juncheng Precision Manufacturing Co ltd
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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
    • 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
    • C23F17/00—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
    • 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
    • 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
    • C25D11/026—Anodisation with spark discharge
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/34—Pretreatment of metallic surfaces to be electroplated
    • C25D5/38—Pretreatment of metallic surfaces to be electroplated of refractory metals or nickel
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/48—After-treatment of electroplated surfaces

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Mechanical Engineering (AREA)
  • General Chemical & Material Sciences (AREA)
  • Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)

Abstract

The invention discloses a titanium alloy micro-arc oxidation process with high light absorption rate, wherein electrolyte used for micro-arc oxidation is Na3PO4Phytic acid, sodium oxalate, potassium cobalt cyanide and Na2CO3And Na6TeO6An aqueous solution of (a). By adopting the technical scheme of the invention, the oxide film with high blackness, uniform color and high light absorption rate can be obtained on the surface of the titanium alloy in a short time. The film layer has good combination with the matrix, high density, wear resistance and hardness, and oxygen with different blackness degrees can be obtained by adjusting the concentration of the electrolyte and the related electrical parametersAnd (5) film layer formation. Therefore, the titanium alloy surface oxidation film layer with high light absorption rate expands the application range of the titanium alloy to a certain extent and can meet the requirements of practical application.

Description

Titanium alloy micro-arc oxidation process with high light absorption rate
Technical Field
The invention belongs to the technical field of electrolytic oxidation, and particularly relates to a titanium alloy micro-arc oxidation process with high light absorption rate.
Background
Titanium alloy is widely applied to optical instruments due to corrosion resistance, lower density and smaller thermal expansion coefficient, and particularly, in recent years, high-end optical instruments made of titanium alloy are developed rapidly along with the development of aerospace and navigation industries in China. However, the inner surface of the optical instrument needs to be provided with an anti-reflection coating with extremely high absorptivity. The current means needed include painting/electrophoresis matte paint, black micro-arc oxidation, black anodic oxidation and the like. However, the coating/electrophoresis matte paint cannot meet the strict requirements of high-precision instruments on the size, and the black micro-arc oxidation always has an absorbance of about 75% at present and cannot meet the requirement of high absorbance.
Black anodic oxidation is an old process of former Soviet Union, and Cr is not separated from the black anodic oxidation although the black anodic oxidation has adjustment changes in the aspects of additives, electrical parameters, the proportion of medicaments and the like6+And (3) an oxidation system. Except that the environmental protection can not be ensured in the manufacturing process, the material passes through K2Cr2O7/(NH4)2SO4/Na2SO4The wear resistance, hardness and adhesion of the film formed by the system are poor. Therefore, it is critical to develop a hard and wear-resistant oxide layer having high absorptivity and capable of ensuring precise size to satisfy the development of the field.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a titanium alloy micro-arc oxidation process with high light absorption rate.
The micro-arc oxidation process comprises the following steps:
step 1: the area of the handle is 30 multiplied by 100m2The titanium alloy sample is put into pickling solution at room temperature, and the surface of the sample is washed for 3 times by deionized water after being washed for 2-5 min;
step 2: step 1 is obtainedPlacing the obtained titanium alloy sample into electrolyte, and controlling current density at 1.5-3.5A/dm at 20-30 deg.C and duty ratio of 15%2Performing constant-current micro-arc oxidation, stopping oxidation after the required color is achieved, taking out a titanium alloy sample wafer, washing with deionized water for 3 minutes, and finally drying the surface with high-pressure air for later use;
and step 3: and (3) putting the titanium alloy sample wafer obtained in the step (2) into a sealing agent, sealing for 3min under ultrasonic waves, taking out the titanium alloy sample wafer, washing with deionized water for 3 times, and drying with high-pressure air to obtain the titanium alloy micro-arc oxidation product with high light absorption rate.
In the step 1, the pickling solution takes water as a solvent and NH4HF2And nitric acid as solute, wherein NH4HF2The concentration is 10ml/L, and the solute nitric acid is a nitric acid solution with the mass fraction of 68%.
The electrolyte in the step 2 is Na3PO4Phytic acid, sodium oxalate, potassium cobalt cyanide and Na2CO3And Na6TeO6In which Na is present3PO4The concentration is 30-50g/L, the phytic acid concentration is 1-10ml/L, the sodium oxalate concentration is 75-200g/L, and the potassium cobalt cyanide concentration is 3-5g/L, Na2CO3The concentration is 5-9g/L, Na6TeO6The concentration is 5-14 g/L;
the sealing agent in the step 3 is nano graphene powder, KH-550 and C2H5OH, hard film antirust oil and Tianna water, wherein the Tianna water is used as a solvent, the concentration of the nano graphene powder is 10g/L, KH-550, and the concentration is 10ml/L, C2H5The OH concentration is 20ml/L and the hard film rust preventive oil concentration is 50 ml/L.
By adopting the technical scheme of the invention, the oxide film with high blackness, uniform color and high light absorption rate can be obtained on the surface of the titanium alloy in a short time. The film layer is well combined with a matrix, the film layer has high density, wear resistance and hardness, and the oxide film layers with different blackness degrees can be obtained by adjusting the concentration of the electrolyte and related electrical parameters. Therefore, the titanium alloy surface oxidation film layer with high light absorption rate expands the application range of the titanium alloy to a certain extent and can meet the requirements of practical application.
Detailed Description
For a further understanding of the invention, reference will now be made to the preferred embodiments of the invention by way of example, and it is to be understood that the description is intended to further illustrate features and advantages of the invention, and not to limit the scope of the claims.
Example 1
A micro-arc oxidation process of titanium alloy with high light absorption rate comprises the following steps:
step 1: the area of the handle is 30 multiplied by 100m2The titanium alloy sample is put into pickling solution at room temperature, and the surface of the sample is washed for 3 times by deionized water after being washed for 2 min;
step 2: putting the titanium alloy sample obtained in the step 1 into electrolyte, and controlling the current density to be 1.5A/dm under the conditions of 20 ℃ and duty ratio of 15 percent2Performing constant-current micro-arc oxidation, stopping oxidation after the required color is achieved, taking out a titanium alloy sample wafer, washing with deionized water for 3 minutes, and finally drying the surface with high-pressure air for later use;
and step 3: and (3) putting the titanium alloy sample wafer obtained in the step (2) into a sealing agent, sealing for 3min under ultrasonic waves, taking out the titanium alloy sample wafer, washing with deionized water for 3 times, and drying with high-pressure air to obtain the titanium alloy micro-arc oxidation product with high light absorption rate.
In the step 1, the pickling solution takes water as a solvent and NH4HF2And nitric acid as solute, wherein NH4HF2The concentration is 10ml/L, and the solute nitric acid is a nitric acid solution with the mass fraction of 68%.
The electrolyte in the step 2 is Na3PO4Phytic acid, sodium oxalate, potassium cobalt cyanide and Na2CO3And an aqueous solution of Na6TeO6, wherein Na3PO4The concentration is 30g/L, the phytic acid concentration is 1ml/L, the sodium oxalate concentration is 75g/L, and the potassium cobalt cyanide concentration is 3g/L, Na2CO3The concentration is 5g/L, Na6TeO6The concentration is 5 g/L;
the sealing agent in the step 3 is nano graphene powder, KH-550 and C2H5OH, dura mater preventionThe mixture of the rust oil and the Tiana water, wherein the Tiana water is used as a solvent, the concentration of the nano graphene powder is 10g/L, KH-550, and the concentration is 10ml/L, C2H5The OH concentration is 20ml/L and the hard film rust preventive oil concentration is 50 ml/L.
Example 2
A micro-arc oxidation process of titanium alloy with high light absorption rate comprises the following steps:
step 1: the area of the handle is 30 multiplied by 100m2The titanium alloy sample is put into pickling solution at room temperature, and the surface of the sample is washed for 3 times by deionized water after being washed for 3.5min for standby;
step 2: putting the titanium alloy sample obtained in the step 1 into electrolyte, and controlling the current density to be 2.5A/dm under the conditions of 25 ℃ and duty ratio of 15 percent2Performing constant-current micro-arc oxidation, stopping oxidation after the required color is achieved, taking out a titanium alloy sample wafer, washing with deionized water for 3 minutes, and finally drying the surface with high-pressure air for later use;
and step 3: and (3) putting the titanium alloy sample wafer obtained in the step (2) into a sealing agent, sealing for 3min under ultrasonic waves, taking out the titanium alloy sample wafer, washing with deionized water for 3 times, and drying with high-pressure air to obtain the titanium alloy micro-arc oxidation product with high light absorption rate.
In the step 1, the pickling solution takes water as a solvent and NH4HF2And nitric acid as solute, wherein NH4HF2The concentration is 10ml/L, and the solute nitric acid is a nitric acid solution with the mass fraction of 68%.
The electrolyte in the step 2 is Na3PO4, phytic acid, sodium oxalate, potassium cobalt cyanide and Na2CO3And Na6TeO6In which Na is present3PO4The concentration is 40g/L, the phytic acid concentration is 5ml/L, the sodium oxalate concentration is 135g/L, and the potassium cobalt cyanide concentration is 4g/L, Na2CO3The concentration is 7g/L, Na6TeO6The concentration is 9 g/L;
the sealing agent in the step 3 is nano graphene powder, KH-550 and C2H5OH, hard film antirust oil and Tianna water, wherein the Tianna water is used as a solvent, the concentration of the nano graphene powder is 10g/L, KH-550, and the concentration is 10ml/L, C2H5The OH concentration is 20ml/L and the hard film rust preventive oil concentration is 50 ml/L.
Example 3
The invention provides a titanium alloy micro-arc oxidation process with high light absorption rate, which comprises the following steps:
step 1: the area of the handle is 30 multiplied by 100m2The titanium alloy sample is put into pickling solution at room temperature, and the surface of the sample is washed for 3 times by deionized water after 5min of cleaning;
step 2: putting the titanium alloy sample obtained in the step 1 into electrolyte, and controlling the current density to be 3.5A/dm under the conditions of 30 ℃ and 15% duty ratio2Performing constant-current micro-arc oxidation, stopping oxidation after the required color is achieved, taking out a titanium alloy sample wafer, washing with deionized water for 3 minutes, and finally drying the surface with high-pressure air for later use;
and step 3: and (3) putting the titanium alloy sample wafer obtained in the step (2) into a sealing agent, sealing for 3min under ultrasonic waves, taking out the titanium alloy sample wafer, washing with deionized water for 3 times, and drying with high-pressure air to obtain the titanium alloy micro-arc oxidation product with high light absorption rate.
In the step 1, the pickling solution takes water as a solvent and NH4HF2And nitric acid as solute, wherein NH4HF2The concentration is 10ml/L, and the solute nitric acid is a nitric acid solution with the mass fraction of 68%.
The electrolyte in the step 2 is Na3PO4Phytic acid, sodium oxalate, potassium cobalt cyanide and Na2CO3And an aqueous solution of Na6TeO6, wherein Na3PO4The concentration is 50g/L, the phytic acid concentration is 10ml/L, the sodium oxalate concentration is 200g/L, and the potassium cobalt cyanide concentration is 5g/L, Na2CO3The concentration is 9g/L, Na6TeO6The concentration is 14 g/L;
the sealing agent in the step 3 is nano graphene powder, KH-550 and C2H5OH, hard film antirust oil and Tianna water, wherein the Tianna water is used as a solvent, the concentration of the nano graphene powder is 10g/L, KH-550, and the concentration is 10ml/L, C2H5The OH concentration is 20ml/L and the hard film rust preventive oil concentration is 50 ml/L.
Comparative example 1
The invention provides a titanium alloy micro-arc oxidation process with high light absorption rate, which comprises the following steps:
step 1: the area of the handle is 30 multiplied by 100m2The titanium alloy sample is put into pickling solution at room temperature, and the surface of the sample is washed for 3 times by deionized water after 5min of cleaning;
step 2: putting the titanium alloy sample obtained in the step 1 into electrolyte, and controlling the current density to be 3.5A/dm under the conditions of 30 ℃ and 15% duty ratio2Performing constant-current micro-arc oxidation, stopping oxidation after the required color is achieved, taking out a titanium alloy sample wafer, washing with deionized water for 3 minutes, and finally drying the surface with high-pressure air for later use;
and step 3: and (3) putting the titanium alloy sample wafer obtained in the step (2) into a sealing agent, sealing for 3min under ultrasonic waves, taking out the titanium alloy sample wafer, washing with deionized water for 3 times, and drying with high-pressure air to obtain the titanium alloy micro-arc oxidation product with high light absorption rate.
In the step 1, the pickling solution takes water as a solvent and NH4HF2And nitric acid as solute, wherein NH4HF2The concentration is 10ml/L, and the solute nitric acid is a nitric acid solution with the mass fraction of 68%.
The electrolyte in the step 2 is Na3PO4, phytic acid, sodium oxalate, potassium cobalt cyanide and Na2CO3Aqueous solution of Na in3PO4The concentration is 50g/L, the phytic acid concentration is 10ml/L, the sodium oxalate concentration is 200g/L, and the potassium cobalt cyanide concentration is 5g/L, Na2CO3The concentration is 9 g/L;
the sealing agent in the step 3 is nano graphene powder, KH-550 and C2H5OH, hard film antirust oil and Tianna water, wherein the Tianna water is used as a solvent, the concentration of the nano graphene powder is 10g/L, KH-550, and the concentration is 10ml/L, C2H5The OH concentration is 20ml/L and the hard film rust preventive oil concentration is 50 ml/L.
Comparative example 2
The invention provides a titanium alloy micro-arc oxidation process with high light absorption rate, which comprises the following steps:
step 1: area of handleIs 30 x 100m2The titanium alloy sample is put into pickling solution at room temperature, and the surface of the sample is washed for 3 times by deionized water after 5min of cleaning;
step 2: putting the titanium alloy sample obtained in the step 1 into electrolyte, and controlling the current density to be 3.5A/dm under the conditions of 30 ℃ and 15% duty ratio2Performing constant-current micro-arc oxidation, stopping oxidation after the required color is achieved, taking out a titanium alloy sample wafer, washing with deionized water for 3 minutes, and finally drying the surface with high-pressure air for later use;
and step 3: and (3) putting the titanium alloy sample wafer obtained in the step (2) into a sealing agent, sealing for 3min under ultrasonic waves, taking out the titanium alloy sample wafer, washing with deionized water for 3 times, and drying with high-pressure air to obtain the titanium alloy micro-arc oxidation product with high light absorption rate.
The pickling solution in the step 1 is prepared by taking water as a solvent and NH4HF2And nitric acid as solute, wherein NH4HF2The concentration is 10ml/L, and the solute nitric acid is a nitric acid solution with the mass fraction of 68%.
The electrolyte in the step 2 is Na3PO4, phytic acid, sodium oxalate and Na2CO3And an aqueous solution of Na6TeO6, wherein Na3PO4The concentration is 50g/L, the phytic acid concentration is 10ml/L, and the sodium oxalate concentration is 200g/L, Na2CO3The concentration is 9g/L, Na6TeO6The concentration is 14 g/L;
the sealing agent in the step 3 is nano graphene powder, KH-550 and C2H5OH, hard film antirust oil and Tianna water, wherein the Tianna water is used as a solvent, the concentration of the nano graphene powder is 10g/L, KH-550, and the concentration is 10ml/L, C2H5The OH concentration is 20ml/L and the hard film rust preventive oil concentration is 50 ml/L.
The sample absorbance, abrasion resistance and hardness in each embodiment were measured, and 5 samples obtained in each embodiment were measured and averaged.
1. Absorbance test
The spectrophotometer with double beams and double monochromators is used in Lambda 950 of Perkin Elmer, and during instrument test, iodine tungsten lamp and protium lamp are used as light source and high sensitivity photomultiplier is used as detector in ultraviolet/visible region. To accurately collect the reflectance spectrum of the sample piece, a 150mm integrating sphere was used for the test. Testing in the wavelength region of 200-2500 nm.
2. Surface abrasion resistance test
The surface of the sample was rubbed back and forth with No. 1000 3M sandpaper under a vertical pressure of 9.8N until the bottom titanium alloy metal was seen, and the number of rubs was recorded.
3. Surface hardness test
The test was carried out according to microhardness standard ZBY 337-85.
Performance index Example 1 Example 2 Example 3 Comparative example 1 Comparative example 2
Absorbance (%) 91.2 91.0 91.8 83.2 85.4
Surface abrasion resistance (times) 3331.4 3341.2 3337.8 2872 2916.2
Surface hardness (g. F) 843.5 842.8 845.7 632.4 636.1
As can be seen from the data in the table, the sample absorbances, surface abrasion resistances and surface hardnesses in examples 1 to 3 are significantly higher than those in the comparative example, because the components of potassium cobalt cyanide and Na6TeO6 change the physical structure and chemical composition of the oxide film during the micro-arc oxidation process, so that the properties are significantly improved.

Claims (4)

1. The micro-arc oxidation process of the titanium alloy with high light absorption rate is characterized by comprising the steps of acid washing, micro-arc oxidation and sealing, wherein electrolyte used for the micro-arc oxidation is Na3PO4Phytic acid, sodium oxalate, potassium cobalt cyanide and Na2CO3And Na6TeO6And Na3PO4The concentration is 30-50g/L, the phytic acid concentration is 1-10ml/L, the sodium oxalate concentration is 75-200g/L, and the potassium cobalt cyanide concentration is 3-5g/L, Na2CO3The concentration is 5-9g/L, Na6TeO6The concentration is 5-14 g/L.
2. The micro-arc oxidation process of titanium alloy with high absorbance as claimed in claim 1, wherein the acid washing solution used in the micro-arc oxidation process acid washing step uses water as solvent and NH4HF2And nitric acid as solute, wherein NH4HF2The concentration is 10ml/L, and the solute nitric acid is a nitric acid solution with the mass fraction of 68%.
3. The micro-arc oxidation process of titanium alloy with high absorbance according to claim 1, wherein the blocking agent used in the blocking step is nano graphene powder, KH-550, C2H5OH, hard film antirust oil and Tianna water, wherein the Tianna water is used as a solvent, the concentration of the nano graphene powder is 10g/L, KH-550, and the concentration is 10ml/L, C2H5The OH concentration is 20ml/L and the hard film rust preventive oil concentration is 50 ml/L.
4. The micro-arc oxidation process of titanium alloy with high absorptivity according to claim 1, characterized in that the micro-arc oxidation process of titanium alloy comprises the following specific steps:
step 1: the area of the handle is 30 multiplied by 100m2The titanium alloy sample is put into pickling solution at room temperature, and the surface of the sample is washed for 3 times by deionized water after being washed for 2-5 min;
step 2: putting the titanium alloy sample obtained in the step 1 into electrolyte, and controlling the current density to be 1.5-3.5A/dm under the conditions of 20-30 ℃ and duty ratio of 15%2Performing constant-current micro-arc oxidation, stopping oxidation after the required color is achieved, taking out a titanium alloy sample wafer, washing with deionized water for 3 minutes, and finally drying the surface with high-pressure air for later use;
and step 3: and (3) putting the titanium alloy sample wafer obtained in the step (2) into a sealing agent, sealing for 3min under ultrasonic waves, taking out the titanium alloy sample wafer, washing with deionized water for 3 times, and drying with high-pressure air to obtain the titanium alloy micro-arc oxidation product with high light absorption rate.
CN202110180673.XA 2021-02-08 2021-02-08 Titanium alloy micro-arc oxidation process with high light absorption rate Pending CN112981494A (en)

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US4968391A (en) * 1988-01-29 1990-11-06 Nippon Steel Corporation Process for the preparation of a black surface-treated steel sheet
US5032236A (en) * 1989-06-22 1991-07-16 Nippon Steel Corporation Process for producing a surface-blackened steel sheet
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