CN113061895B - Micro-arc oxidation treatment method for surface of titanium alloy fastener - Google Patents

Micro-arc oxidation treatment method for surface of titanium alloy fastener Download PDF

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CN113061895B
CN113061895B CN202110238716.5A CN202110238716A CN113061895B CN 113061895 B CN113061895 B CN 113061895B CN 202110238716 A CN202110238716 A CN 202110238716A CN 113061895 B CN113061895 B CN 113061895B
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micro
arc oxidation
fastener
electrolyte
treatment method
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CN113061895A (en
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陈刚
杨晓禹
王红杰
钱坤明
张立君
吴瑜
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Ningbo Surface Engineering Research Institute Co ltd
China Weapon Science Academy Ningbo Branch
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Ningbo Surface Engineering Research Institute Co ltd
China Weapon Science Academy Ningbo Branch
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    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23FNON-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
    • C23F17/00Multi-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
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23GCLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G1/00Cleaning or pickling metallic material with solutions or molten salts
    • C23G1/02Cleaning or pickling metallic material with solutions or molten salts with acid solutions
    • C23G1/10Other heavy metals
    • C23G1/106Other heavy metals refractory metals
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02Anodisation
    • C25D11/026Anodisation with spark discharge
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02Anodisation
    • C25D11/26Anodisation of refractory metals or alloys based thereon
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
    • F16BDEVICES FOR FASTENING OR SECURING CONSTRUCTIONAL ELEMENTS OR MACHINE PARTS TOGETHER, e.g. NAILS, BOLTS, CIRCLIPS, CLAMPS, CLIPS OR WEDGES; JOINTS OR JOINTING
    • F16B33/00Features common to bolt and nut
    • F16B33/008Corrosion preventing means
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
    • F16BDEVICES FOR FASTENING OR SECURING CONSTRUCTIONAL ELEMENTS OR MACHINE PARTS TOGETHER, e.g. NAILS, BOLTS, CIRCLIPS, CLAMPS, CLIPS OR WEDGES; JOINTS OR JOINTING
    • F16B33/00Features common to bolt and nut
    • F16B33/06Surface treatment of parts furnished with screw-thread, e.g. for preventing seizure or fretting

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

Abstract

The invention relates to a micro-arc oxidation treatment method for the surface of a titanium alloy fastener, which sequentially comprises the following steps: 1) Washing and pickling the fastener; 2) Performing sand blasting on the outer surface of the fastener; 3) The preparation of a first micro-arc oxidation electrolyte and a second micro-arc oxidation electrolyte; 4) Micro-arc oxidation treatment: placing the thread section of the fastener in a first oxidation micro-arc electrolyte for micro-arc oxidation; placing the non-threaded section and the head of the fastener in a second micro-arc oxidation electrolyte for micro-arc oxidation; 5) And (3) soaking the fastener treated in the step (4) in boiling water. Micro-arc oxidation is carried out on the thread sections and the non-thread sections in sequence, so that the thread sections and the non-thread sections of the fastener obtain different performances, the lubrication and wear resistance of the thread sections are enhanced, and the corrosion resistance of the whole fastener is increased.

Description

Micro-arc oxidation treatment method for surface of titanium alloy fastener
Technical Field
The invention belongs to the technical field of surface treatment, and particularly relates to a micro-arc oxidation treatment method for the surface of a titanium alloy fastener.
Background
Titanium and titanium alloy have high specific strength, excellent corrosion resistance, good high temperature resistance and the like, and are widely applied to national defense industries such as aviation, aerospace, ships, ground weaponry and the like. Titanium alloy fastener connectors are typical structural members on aircraft and ground weaponry, and their failure includes fatigue of the fastener itself, fatigue and corrosion fatigue at the fastening holes of the connecting plates, and the like. In general, in order to prevent corrosion, a dense oxide film is generally formed on the surface of titanium and titanium alloy, but in a severe environment such as (ocean or humid) or in the case that the oxide film breaks and crevice corrosion occurs, the corrosion resistance of titanium alloy is greatly reduced. When titanium alloy contacts with dissimilar metals such as structural steel, aluminum alloy and the like, galvanic corrosion often accelerates corrosion of other metals and the metals themselves, and cracks are generated around the fasteners and the fastening holes.
In order to solve the technical problems, the surface of a titanium alloy fastener is treated, such as cadmium plating, anodic oxidation, surface alloying, organic coating and the like, but cadmium plating causes pollution to the environment, the organic coating process is complex, special custom-made equipment is needed for surface alloying and the like, in order to solve the technical problems, a micro-arc oxidation treatment method gradually appears, such as a preparation method of a corrosion-resistant and wear-resistant ceramic coating on the surface of a titanium alloy in China patent application No. CN200810064369.3 (application publication No. CN 101260558A), the TA15 titanium alloy subjected to surface polishing and ultrasonic cleaning is placed in a stainless steel tank body filled with alkaline electrolyte, the TA15 titanium alloy is used as an anode, the stainless steel tank body is used as a cathode, and the micro-arc oxidation is carried out under the conditions of 400-600V pulse voltage, 400-800 Hz frequency, 4-20% duty ratio and 0-50 ℃. The micro-arc oxidation surface treatment method improves the corrosion resistance and the wear resistance of the titanium alloy surface, but the micro-arc oxidation surface treatment method is adopted for the fastener with the threaded section and the non-threaded section on the stud, the friction force is usually larger at the threaded position, and the lubrication and the wear resistance requirements of the threaded position of the fastener can not be met.
Accordingly, there is a need for further improvements in the methods of micro-arc oxidation treatment of existing titanium alloy fastener surfaces.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a micro-arc oxidation treatment method for the surface of a titanium alloy fastener, which aims at the current state of the art and is used for improving corrosion resistance and wear resistance and improving the lubricity of a thread section.
The technical scheme adopted for solving the technical problems is as follows: the utility model provides a micro-arc oxidation treatment method on titanium alloy fastener surface, the longitudinal section of fastener is T shape, including the double-screw bolt of vertical setting and set up the head at the double-screw bolt top, the lower part of double-screw bolt peripheral wall has the external screw thread, thereby makes the double-screw bolt is screw thread section and non-screw thread section from down upwards in proper order, its characterized in that: the micro-arc oxidation treatment method sequentially comprises the following steps:
1) Washing and pickling the fastener;
2) Sand blasting: performing sand blasting on the outer surface of the fastener;
3) Preparing a micro-arc oxidation electrolyte:
the first micro-arc oxidation electrolyte is prepared from sodium silicate, borax, disodium ethylenediamine tetraacetate and sodium hydroxide, wherein the concentration of the sodium silicate is 10-40 g/L, the concentration of the borax is 0.5-3 g/L, the concentration of the disodium ethylenediamine tetraacetate is 0.5-3 g/L, and the PH of the sodium hydroxide is 8-11;
the second micro-arc oxidation electrolyte is prepared from sodium silicate, borax, nickel acetate, copper sulfate, glycerol and sodium hydroxide, wherein the concentration of the sodium silicate is 10-40 g/L, the concentration of the borax is 0.5-3 g/L, the concentration of the nickel acetate is 0.1-1 g/L, the concentration of the copper sulfate is 0.5-1.5 g/L, the concentration of the glycerol is 1-5 ml/L, and the PH of the sodium hydroxide is 8-11;
4) Micro-arc oxidation treatment: placing the thread section of the fastener in a first oxidation micro-arc electrolyte for micro-arc oxidation; placing the non-threaded section and the head of the fastener in a second micro-arc oxidation electrolyte for micro-arc oxidation;
5) And (3) soaking the fastener treated in the step (4) in boiling water.
Preferably, in step 1), the fastener is subjected to ultrasonic washing for a period of 5 to 30 minutes, and then the fastener is placed in HF-HNO 3 Pickling is carried out for 3-5 s in pickling solution. Thus, the oil stain and the scraps on the surface are removed better.
Preferably, HF-HNO 3 The concentration of HF in the pickling solution is 1-5%, HNO 3 5 to 30 percent. Thus, the surface reaction layer can be removed rapidly and completely without generating pollution of other elements on the surface
Preferably, in step 2), the injection pressure is between 0.1 and 0.45MPa and the injection time is between 5 and 30 seconds. When the sand blasting pressure is too high, the sand grains impact the titanium surface to generate intense sparks, the temperature rise can react with the titanium surface to form secondary pollution, and the surface quality is affected, so that the sand blasting pressure and the injection time are adopted.
In order to obtain a lubricating wear-resistant layer on the outer surface of the thread segment, in step 4), the temperature of the first micro-arc oxidation electrolyte is kept at 15-40 ℃, and the micro-arc oxidation electrical parameters of the thread segment are set: positive voltage 300-550V, negative voltage 50-250V, current density 1-5A/dm 2 The positive and negative frequency ratio is 11-17, the frequency is 400-1000 Hz, the duty ratio is 5-20%, and the micro-arc oxidation time is 3-5 min.
In order to obtain higher hardness and thickness of the micro-arc oxidation film layer under the same time, a direct current power supply is externally applied to the first electrolyte, and a magnetic field is applied, wherein the magnetic field strength is 50-350 Gs.
In order to obtain the corrosion-resistant and wear-resistant micro-arc oxidation film layer on the surfaces of the non-threaded section and the head part, the second micro-arc oxidation film layer is formed byThe temperature of the arc oxidation electrolyte is kept between 15 and 40 ℃, and in the step 4), the micro-arc oxidation electric parameters of the non-threaded section and the head are set: positive voltage of 350-550V, negative voltage of 150-250V and current density of 3-8A/dm 2 The positive and negative frequency ratio is 14-17, the frequency is 800-1000 Hz, the duty ratio is 5-20%, and the micro-arc oxidation time is 5-10 min.
Preferably, the fastener treated in the step 4) is placed in a second micro-arc oxidation electrolyte for micro-arc oxidation, the temperature of the second micro-arc oxidation electrolyte is kept at 15-40 ℃, and the micro-arc oxidation time is 1-1.5 min. In this way, the overall fastener is made more resistant to wear and corrosion.
Preferably, the temperature in the soaking process in the step 5) is kept at 60-100 ℃ and the soaking time is 1-5 min. The micro-arc oxidized micropores can be subjected to preliminary hole sealing by adopting boiling water hole sealing treatment.
Further preferably, the fastener treated in the step 5) is sealed by paraffin wax. The paraffin has lubricating effect and can be used for sealing the holes by micro-arc oxidation, so that the paraffin can be used for sealing the holes, thereby improving the corrosion resistance and reducing the friction coefficient.
Compared with the prior art, the invention has the advantages that: the titanium alloy fastener is subjected to regional micro-arc oxidation, namely, the micro-arc oxidation is carried out according to the sequence of the threaded section and the non-threaded section, so that the threaded section and the non-threaded section of the fastener obtain different performances: the components of the electrolyte in the first electrolyte can effectively inhibit the rapid growth of the micro-arc oxidation film, and a more uniform and smoother film can be obtained in the same time; the nickel acetate, copper sulfate and the like in the second electrolyte composition can not only improve the corrosion resistance of the film layer, but also properly improve the wear resistance, and the whole fastener can be invaded subsequently, so that the overall wear resistance and corrosion resistance are enhanced. In addition, as the micro-arc oxidation time is shorter, the lubricity of the thread section is not affected, and the subsequent lubrication performance can be further enhanced through paraffin hole sealing, namely, the lubrication and wear resistance of the thread section are enhanced, the corrosion resistance of the whole fastener is enhanced, the titanium alloy fastener is protected, and the problems of wear resistance, galvanic corrosion and large friction force at the thread of the titanium alloy fastener are effectively solved.
Drawings
FIG. 1 is a schematic view of the structure of a fastener of the present embodiment;
FIG. 2 is a flow chart of a micro-arc oxidation process for a titanium alloy fastener.
Detailed Description
The invention is described in further detail below with reference to the embodiments of the drawings.
Example 1
As shown in fig. 1, the longitudinal section of the titanium alloy fastener of this embodiment is T-shaped, and the fastener includes a vertically arranged stud 2 and a head 1 disposed at the top of the stud, the stud is located at a position adjacent to the center of the head 1, and an external thread is provided on the peripheral wall of the lower portion of the stud 2, so that the stud is sequentially provided with a thread section 21 and a non-thread section 22 from bottom to top, as shown in fig. 2, the micro-arc oxidation treatment method of the titanium alloy fastener sequentially includes the following steps:
1) Washing and pickling the fastener: ultrasonic washing the fastener for 5min, and placing the fastener in HF-HNO 3 Pickling for 3s in pickling solution, wherein HF-HNO 3 The pickling solution comprises the following components: HF concentration of 1%, HNO 3 Is 5%;
2) Sand blasting: carrying out sand blasting on the outer surface of the fastener, wherein the spraying pressure is 0.1MPa, and the spraying time is 5s;
3) Preparing a micro-arc oxidation electrolyte:
the first micro-arc oxidation electrolyte is prepared from sodium silicate, borax, disodium ethylenediamine tetraacetate and sodium hydroxide, wherein the concentration of the sodium silicate is 10g/L, the concentration of the borax is 0.5g/L, the concentration of the disodium ethylenediamine tetraacetate is 0.5g/L, and the PH of the sodium hydroxide is 8;
the second micro-arc oxidation electrolyte is prepared from sodium silicate, borax, nickel acetate, copper sulfate, glycerol and sodium hydroxide, wherein the concentration of the sodium silicate is 10g/L, the concentration of the borax is 0.5g/L, the concentration of the nickel acetate is 0.1g/L, the concentration of the copper sulfate is 0.5g/L, the concentration of the glycerol is 1ml/L, and the PH of the sodium hydroxide is 8;
4) Micro-arc oxidation treatment:in order to obtain a self-lubricating wear-resistant film layer on the outer surface of the threaded section 21 of the fastener, after the fastener subjected to sand blasting is cleaned, the threaded section 21 of the fastener is placed in a first micro-arc oxidation electrolyte for micro-arc oxidation, the temperature of the first micro-arc oxidation electrolyte is kept at 15 ℃, and the micro-arc oxidation electrical parameters of the threaded section 21 are set: a positive voltage of 300V, a negative voltage of 50V and a current density of 1A/dm 2 The positive and negative frequency ratio is 11, the frequency is 400Hz, the duty ratio is 5%, the micro-arc oxidation time is 3min, in the whole process, the first micro-arc oxidation electrolyte is externally added with a direct current power supply and a magnetic field is applied, and the magnetic field strength is 50Gs.
In order to obtain a corrosion-resistant and wear-resistant micro-arc oxidation film layer on the non-threaded section 22 and the head 1 of the fastener, after the fastener with the threaded section 21 subjected to micro-arc oxidation treatment is cleaned, the non-threaded section 22 and the head 1 of the fastener are placed in a second micro-arc oxidation electrolyte for micro-arc oxidation, the temperature of the second micro-arc oxidation electrolyte is kept at 15 ℃, and the micro-arc oxidation electrical parameters of the non-threaded section 22 and the head 1 are set: a positive voltage of 350V, a negative voltage of 150V and a current density of 3A/dm 2 The positive and negative frequency ratio is 14, the frequency is 800Hz, the duty ratio is 5%, and the micro-arc oxidation time t1 is 5min. Setting micro-arc oxidation parameters of the non-threaded section and the head, placing the whole fastener in a second micro-arc oxidation electric solution for micro-arc oxidation again, wherein the temperature of the second micro-arc oxidation electric solution is kept at 15-40 ℃, and the time t2 of the micro-arc oxidation is 1-1.5 min;
5) And (3) soaking the fastener subjected to the micro-arc oxidation treatment in boiled water, keeping the temperature at 60 ℃ in the soaking process for 1min, taking out the fastener, and sealing the hole by adopting paraffin.
In the description and claims of the present invention, terms indicating directions, such as "upper", "lower", "top", etc., are used to describe various example structural parts and elements of the present invention, but these terms are used herein for convenience of description only and are determined based on the example orientations shown in the drawings. Because the disclosed embodiments of the invention may be arranged in a variety of orientations, the directional terminology is used for purposes of illustration and is in no way limiting, such as "upper" and "lower" are not necessarily limited to being in a direction opposite or coincident with the direction of gravity.
The micro-arc oxidation treatment method for the titanium alloy fastener surfaces of example 2 and example 3 is the same as that of example 1, except that: the technological parameters of water washing, acid washing and sand blasting treatment are selected, the configuration of the first micro-arc oxidation electrolyte is selected, the configuration of the second micro-arc oxidation electrolyte is selected, the electrical parameters of the self-lubricating wear-resistant micro-arc oxidation film layer are selected, the electrical parameters of the corrosion-resistant wear-resistant micro-arc oxidation film layer are selected, and the parameters of the magnetic field strength and the soaking treatment parameters are selected differently.
The process parameters of the water washing, acid washing and sand blasting treatment of the three embodiments are shown in the following table 1; the configuration of the first micro-arc oxidation electrolyte of the above three examples is shown with reference to table 2 below; the configuration of the second micro-arc oxidation electrolyte of the above three examples is shown with reference to table 3 below; the electrical parameter process of the self-lubricating wear-resistant micro-arc oxidation film layer of the three embodiments is shown in the following table 4, the parameters of the magnetic field strength of the three embodiments are shown in the following table 5, the electrical parameter process of the corrosion-resistant wear-resistant micro-arc oxidation film layer of the three embodiments is shown in the following table 6, and the soaking treatment parameters of the three embodiments are shown in the following table 7. The friction coefficient and hardness of the above three examples are specifically shown with reference to table 8 below.
TABLE 1 Water washing, acid washing and sand blasting treatment process
Figure GDA0003071632270000051
Table 2 first micro-arc oxidation electrolyte configuration for preparing self-lubricating wear-resistant micro-arc oxidation film
Numbering device Sodium silicate g/L Borax g/L Ethylene diamine tetraacetic acid disodium g/L PH (NaOH adjusting)
Example 1 10 0.5 0.5 8
Example 2 25 1 1 9
Example 3 40 3 3 11
TABLE 3 second micro-arc oxidation electrolyte configuration of corrosion and wear resistant micro-arc oxidation film
Figure GDA0003071632270000052
Table 4 self-lubricating wear-resistant micro-arc oxide film layer electrical parameters
Figure GDA0003071632270000053
TABLE 5 magnetic field strength parameter table
Numbering device Magnetic field strength/Gs
Example 1 50
Example 2 150
Example 3 350
Table 6 corrosion and wear resistant micro-arc oxide film electrical parameters
Figure GDA0003071632270000061
Table 7 soaking treatment parameter table
Numbering device Temperature/. Degree.C Soaking time/min
Example 1 60 1
Example 2 80 3
Example 3 100 5
Table 8 is a table of the friction coefficient and hardness of the thread segments and the hardness properties of the non-thread segments in 3 examples and comparative examples
Figure GDA0003071632270000062
Comparative example 1 is a titanium alloy fastener which has not undergone micro-arc oxidation treatment, and the titanium alloy fastener is the same as the original titanium alloy fastener of the present embodiment.
The friction coefficient was measured throughout the thread segments of the fastener according to standard ISO16047-2005, and as can be seen from table 8 above, the friction coefficient was lower throughout the thread segments of the 3 examples than that of comparative example 1. As is clear from table 8 above, the hardness of the thread segments and the non-thread segments in examples 1 to 3 was greatly improved compared with the comparative examples, in which the hardness of the non-thread segment in example 3 was 1340HV at the maximum, by testing the vickers hardness (using the same loading force and dwell time) with a microhardness meter in each of 3 examples and comparative examples in table 8 above, and the loading force was 0.98N and the dwell time was 5s.
According to the test of salt spray test of artificial atmosphere corrosion test of standard GB/T10125-1997, the corrosion resistance is tested, and the table shows that the corrosion resistance of 3 examples is greatly improved compared with that of the comparative example, and the highest salt spray resistance time of the example 2 is 168 hours.

Claims (10)

1. The utility model provides a micro-arc oxidation treatment method on titanium alloy fastener surface, the longitudinal section of fastener is T shape, including the double-screw bolt of vertical setting and set up the head at the double-screw bolt top, the lower part of double-screw bolt peripheral wall has the external screw thread, thereby makes the double-screw bolt is screw thread section and non-screw thread section from down upwards in proper order, its characterized in that: the micro-arc oxidation treatment method sequentially comprises the following steps:
1) Washing and pickling the fastener;
2) Sand blasting: performing sand blasting on the outer surface of the fastener;
3) Preparing a micro-arc oxidation electrolyte:
the first micro-arc oxidation electrolyte is prepared from sodium silicate, borax, disodium ethylenediamine tetraacetate and sodium hydroxide, wherein the concentration of the sodium silicate is 10-40 g/L, the concentration of the borax is 0.5-3 g/L, the concentration of the disodium ethylenediamine tetraacetate is 0.5-3 g/L, and the PH of the sodium hydroxide is 8-11;
the second micro-arc oxidation electrolyte is prepared from sodium silicate, borax, nickel acetate, copper sulfate, glycerol and sodium hydroxide, wherein the concentration of the sodium silicate is 10-40 g/L, the concentration of the borax is 0.5-3 g/L, the concentration of the nickel acetate is 0.1-1 g/L, the concentration of the copper sulfate is 0.5-1.5 g/L, the concentration of the glycerol is 1-5 ml/L, and the PH of the sodium hydroxide is 8-11;
4) Micro-arc oxidation treatment: placing the thread section of the fastener in a first oxidation micro-arc electrolyte for micro-arc oxidation; placing the non-threaded section and the head of the fastener in a second micro-arc oxidation electrolyte for micro-arc oxidation;
5) And (3) soaking the fastener treated in the step (4) in boiling water.
2. The micro-arc oxidation treatment method according to claim 1, wherein: in the step 1), the fastening piece is subjected to ultrasonic washing for 5-30 min, and then the fastening piece is placed in HF-HNO 3 Pickling is carried out for 3-5 s in pickling solution.
3. The micro-arc oxidation treatment method according to claim 2, wherein: HF-HNO 3 The concentration of HF in the pickling solution is 1-5%, HNO 3 The concentration is 5-30%.
4. The micro-arc oxidation treatment method according to claim 1, wherein: in step 2), the injection pressure is 0.1-0.45 MPa and the injection time is 5-30 s.
5. The micro-arc oxidation treatment method according to claim 1, wherein: in the step 4), the temperature of the first micro-arc oxidation electrolyte is kept at 15-40 ℃, and the micro-arc oxidation electrical parameters of the thread section are set: positive voltage 300-550V, negative voltage 50-250V, current density 1-5A/dm 2 The positive and negative frequency ratio is 11-17, the frequency is 400-1000 Hz, the duty ratio is 5-20%, and the micro-arc oxidation time is 3-5 min.
6. The micro-arc oxidation treatment method according to claim 5, wherein: and applying a direct current power supply to the first electrolyte and applying a magnetic field, wherein the magnetic field strength is 50-350 Gs.
7. The micro-arc oxidation treatment method according to claim 5, wherein: the temperature of the second micro-arc oxidation electrolyte is kept at 15-40 ℃, and in the step 4), the micro-arc oxidation electric parameters of the non-threaded section and the head are set: positive voltage of 350-550V, negative voltage of 150-250V and current density of 3-8A/dm 2 The positive and negative frequency ratio is 14-17, the frequency is 800-1000 Hz, the duty ratio is 5-20%, and the micro-arc oxidation time is 5-10 min.
8. The micro-arc oxidation treatment method according to claim 7, wherein: placing the fastener treated in the step 4) into a second micro-arc oxidation electrolyte for micro-arc oxidation, wherein the temperature of the second micro-arc oxidation electrolyte is kept at 15-40 ℃, and the micro-arc oxidation time is 1-1.5 min.
9. The micro-arc oxidation treatment method according to claim 1, wherein: the temperature in the soaking process in the step 5) is kept at 60-100 ℃ and the soaking time is 1-5 min.
10. The micro-arc oxidation treatment method according to claim 9, wherein: and (3) sealing the fastener treated in the step (5) by adopting paraffin.
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