CN115012014A - Preparation method of metal workpiece surface oxidation film layer under multiphase condition - Google Patents

Preparation method of metal workpiece surface oxidation film layer under multiphase condition Download PDF

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CN115012014A
CN115012014A CN202210734779.4A CN202210734779A CN115012014A CN 115012014 A CN115012014 A CN 115012014A CN 202210734779 A CN202210734779 A CN 202210734779A CN 115012014 A CN115012014 A CN 115012014A
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metal workpiece
oxidation
film layer
oxide film
water mist
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高广睿
呼丹
屈静
徐海龙
白新房
翁特
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Xi'an Surface Material Protection Co ltd
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Xi'an Surface Material Protection Co ltd
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Priority to PCT/CN2022/114486 priority patent/WO2024000767A1/en
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    • 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
    • C25D11/005Apparatus specially adapted for electrolytic conversion coating

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  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
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  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Treatment Of Metals (AREA)
  • Other Surface Treatments For Metallic Materials (AREA)

Abstract

The invention discloses a preparation method of an oxide film layer on the surface of a metal workpiece under a multiphase condition, which comprises the following steps: firstly, treating the surface of a metal workpiece; secondly, preparing an atomized solution; and thirdly, spraying the atomized solution to form water mist by taking the metal workpiece after surface treatment as an anode substrate and a stainless steel substrate as a cathode substrate, so that micro-arc points are generated between the metal workpiece and the stainless steel substrate to be oxidized, and an oxide film layer is formed on the surface of the metal workpiece. The method and the device have the advantages that the voltage is applied to the metal element in the double-phase closed environment in which the water mist and the air are mixed, the atomized solution and the air are promoted to be subjected to breakdown discharge to generate an oxidation film layer with the metal workpiece, the oxidation film layer is prepared on the surface of the metal workpiece under the multiphase condition of liquid phase, gas phase and solid phase, the preparation efficiency is improved, the local oxidation of the metal workpiece is realized, the limitation of the shape of the metal workpiece on the preparation method is broken through, and the method and the device are suitable for the metal workpiece with an irregular structure or a complex structure.

Description

Preparation method of metal workpiece surface oxidation film layer under multiphase condition
Technical Field
The invention belongs to the technical field of films, and particularly relates to a preparation method of an oxide film on the surface of a metal workpiece under a multiphase condition.
Background
The integrity of the metal oxide film is a necessary condition for protection, and the integrity is a necessary condition for the P-B value gamma (gamma-V) of the oxide film OX /V M In which V is OX Represents the volume of oxide film formed during oxidation, V M Representing the volume of metal consumed to form the oxide film) is greater than 1. The P-B value gamma of the metal oxide oxidation film generated on the surface of Al, Mg, Ti and the alloy thereof is between 1 and 2, and the film layer is complete and compact and can play a role in protection. Therefore, the metals are often prepared into dense oxide films by a surface oxidation passivation method so as to achieve the effects of wear resistance, corrosion resistance and other functions. Common oxidation techniques include atmospheric oxidation, anodic oxidation, and micro-arc oxidation.
The atmospheric oxidation refers to the protection of a substrate by heating to generate an oxide film with a certain thickness on the surface of the metal in an atmospheric environment. The process is simple and easy to implement, but the film layer is thin and has limited protection effect.
The anodic oxidation technology is that metal is put into electrolyte (such as sulfuric acid, chromic acid, oxalic acid, etc.) as anode, and oxide film is formed on the surface of the metal under the action of applied current, and the film can change the state and performance of the metal surface, such as surface coloring, corrosion resistance improvement, wear resistance enhancement, hardness enhancement, etc. The anodizing techniques for alloys of aluminum, titanium, magnesium, etc. are well established and there are standards that may be implemented.
The micro-arc oxidation technology is a surface treatment technology developed on the basis of conventional anodic oxidation, a working area is led into a high-voltage spark discharge area from a Faraday area of common anodic oxidation, an oxide film on the surface of a metal is broken down by using high voltage, arc discharge is generated on the surface, and a ceramic film layer mainly comprising matrix metal oxide grows in situ when an electrolyte enters a discharge channel and is cooled. The ceramic film and the substrate are in a metallurgical bonding mode, and have good bonding strength, high hardness, biological performance, corrosion resistance, thermal conductivity and the like. The micro-arc oxidation technology is characterized in that element components in the electrolyte can participate in reaction in the film forming process of arc discharge, and an oxide film layer with higher performance and function can be prepared by adjusting the components of the solution. However, the anodic oxidation and the micro-arc oxidation need to be carried out in an oxidation tank, and certain requirements are made on the size and shape of a power supply and a workpiece in the production process.
The study of metal surface oxidation technology at home and abroad is many, and most scholars complete the design and preparation of microstructure and phase composition of ceramic film layers by regulating and optimizing electric parameters (positive and negative voltage, current density, duty ratio, frequency, oxidation time and the like) and electrolyte (components, concentration and the like), and improve the service performance of the ceramic film layers to a certain extent. The formation process of the micro-arc oxidation ceramic membrane comprises electrochemical, thermochemical and plasma electrochemical processes, the reaction process is very complex, and theoretical explanation of the micro-arc oxidation mechanism currently comprises an electron avalanche mechanism, a volcano hole discharge model and a micro-bridge discharge model, but all experimental phenomena and film forming processes cannot be explained fully and quantitatively. According to the current mechanism explanation, at the moment of micro-arc discharge, a gas phase capable of generating electric breakdown should exist between a solid phase and a liquid phase, so that a gas dielectric electrode breakdown discharge is considered to simulate the micro-arc oxidation process, and a new oxidation method is expected to be obtained.
Disclosure of Invention
The technical problem to be solved by the present invention is to provide a method for preparing an oxide film layer on the surface of a metal workpiece under a multiphase condition, in order to overcome the defects of the prior art. The method applies voltage to a metal element in a two-phase closed environment in which water mist and air are mixed, promotes atomized solution and air to be subjected to breakdown discharge by utilizing a gas medium breakdown discharge principle, and generates an oxidation film layer by carrying out oxidation reaction with a metal workpiece, so that the oxidation film layer is prepared on the surface of the metal workpiece under the multiphase condition of liquid phase, gas phase and solid phase.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows: a preparation method of an oxide film layer on the surface of a metal workpiece under a multiphase condition is characterized by comprising the following steps:
step one, surface treatment: sequentially adopting 800#, 1000#, 1500# and 2000# sandpaper to polish the metal workpiece until the surface is smooth and clean, and then sequentially ultrasonically cleaning the metal workpiece in absolute ethyl alcohol and deionized water for 10-15 min to obtain the surface-treated metal workpiece;
step two, preparing an atomized solution: preparing an acidic solution or an alkaline solution as an atomized solution;
step three, water mist oxidation: and (2) taking the metal workpiece subjected to surface treatment in the step one as an anode substrate, taking a stainless steel substrate as a cathode substrate, placing the metal workpiece into a closed reaction chamber of water mist oxidation equipment, placing the atomized solution prepared in the step two into a water mist sprayer, opening a control valve, spraying water mist into the closed reaction chamber through a water mist spray nozzle, starting an oxidation power supply and adjusting output voltage to enable micro-arc points to be generated between the metal workpiece and the stainless steel substrate to be oxidized, forming an oxidation film layer on the surface of the metal workpiece, taking out the metal workpiece, cleaning and drying the metal workpiece to obtain the metal workpiece with the oxidation film layer.
The invention provides a new valve metal surface oxidation method which is different from the method of anodic oxidation and micro-arc oxidation, and concretely provides a method for generating an oxidation film layer on the surface of a metal workpiece, wherein the metal workpiece is used as an anode substrate and is placed in a closed reaction chamber, a gap is formed between the metal workpiece and a cathode substrate, namely a stainless steel substrate, water mist is sprayed into the closed reaction chamber, so that the metal workpiece is in a two-phase environment of mixing water mist environment and air in the closed reaction chamber, forward voltage is applied to a metal element, the gas medium breakdown discharge principle is utilized, so that atomized solution and air between the anode and the cathode, namely the metal workpiece and the stainless steel substrate are broken down to generate discharge, micro-arc points are generated in the gap between the metal workpiece and the stainless steel substrate, the oxidation reaction of electrolyte components in the atomized solution, oxygen ions in the air and the metal workpiece in the discharge process is promoted, and an oxidation film layer is generated on the surface of the metal workpiece, the preparation of the oxide film on the surface of the metal workpiece is realized under the multiphase condition of liquid phase, gas phase and solid phase. Meanwhile, in the oxidation process, the uniformity of the surface arcing of the metal workpiece in the oxidation process is effectively controlled by adjusting the composition of the atomized solution, the pressure of introduced water mist and the parameters of an oxidation power supply, so that the quality and the thickness of an oxidation film layer on the surface of the metal workpiece are controlled, and different use requirements are met. In addition, the invention can realize local area protection by processing on the metal workpiece, thereby oxidizing the local surface of the metal workpiece according to the use requirement.
The preparation method of the metal workpiece surface oxidation film layer under the multiphase condition is characterized in that in the second step, the acid solution is one or a mixture of sulfuric acid, phosphoric acid, oxalic acid and chromic acid, the addition amount of the sulfuric acid in the acid solution is 20 g/L-400 g/L, the addition amount of the phosphoric acid is 10 g/L-80 g/L, and the addition amounts of the oxalic acid and the chromic acid are 10 g/L-100 g/L.
The preparation method of the metal workpiece surface oxidation film layer under the multiphase condition is characterized in that in the second step, the alkaline solution is a mixed solution of one or more of silicate, phosphate, aluminate, a conductive agent and a stabilizing agent, the conductive agent is sodium hydroxide or potassium hydroxide, the stabilizing agent is glycerol, sodium fluoride, ethylene glycol or glycerol, the adding amount of the silicate in the alkaline solution is 10 g/L-60 g/L, the adding amount of the phosphate is 5 g/L-50 g/L, the adding amount of the aluminate is 5 g/L-40 g/L, the adding amount of the conductive agent is 1 g/L-10 g/L, and the adding amount of the stabilizing agent is 1 g/L-10 g/L.
The preparation method of the oxide film layer on the surface of the metal workpiece under the multiphase condition is characterized in that the diffusion angle of the sprayed and introduced water mist is 10-150 degrees in the third step, and the introduction flow is 1 L.min -1 ~50L·min -1 The average range is more than 5m, the fineness of the formed fog beads is not more than 100 mu m, and the pressure in the closed reaction chamber in the spraying process is 0.5 MPa-1 MPa. The optimized spraying parameters ensure that the atomized solution is sprayed to form uniformly dispersed water mist, are favorable for the oxidation process, and improve the uniformity of the oxide film layer on the surface of the metal workpiece.
The preparation method of the metal workpiece surface oxidation film layer under the multiphase condition is characterized in that in the third step, the power frequency adopted by the oxidation is 1 Hz-1000 Hz, the duty ratio is 5% -90%, the oxidation voltage is 300V-700V, and the oxidation time is 10 min-150 min.
The preparation method of the oxide film layer on the surface of the metal workpiece under the multiphase condition is characterized in that the thickness of the oxide film layer on the surface of the metal workpiece with the oxide film layer in the step three is 1-80 μm, and the surface roughness is 0.5-5 μm.
Compared with the prior art, the invention has the following advantages:
1. according to the invention, voltage is applied to the metal element in a two-phase closed environment in which water mist and air are mixed, the breakdown discharge principle of a gas medium is utilized, the breakdown discharge of atomized solution and air is promoted, and the atomized solution and the air are subjected to oxidation reaction with the metal workpiece to generate an oxidation film layer, so that the oxidation film layer is prepared on the surface of the metal workpiece under the multiphase conditions of liquid phase, gas phase and solid phase.
2. The method effectively controls the surface arcing uniformity of the metal workpiece in the oxidation process by controlling the composition of the atomized solution, the pressure of introduced water mist and the oxidation power supply parameters, further controls the quality and the thickness of an oxidation film layer on the surface of the metal workpiece, is simple and easy to realize, and meets different use requirements.
3. The method of the invention not only enables the atomized solution to participate in the oxidation reaction, but also promotes the oxygen in the air to participate in the oxidation reaction, improves the preparation efficiency of the oxidation film layer, and simultaneously can promote the nitrogen and the carbon dioxide in the air to participate in the reaction by adjusting the parameters of the oxidation power supply, so as to form the oxidation film layers with different composition contents on the surface of the metal workpiece, expand the range of the oxidation film layers and widen the application field of the method of the invention.
4. The preparation method of the invention adopts simple water mist oxidation equipment, the sprayed atomized solution and air are easy to contact with the metal workpiece, the local oxidation of the metal workpiece can be realized, the metal workpiece does not need to be arranged in an electrolytic bath, the limitation of the shape of the metal workpiece on the preparation method is broken through, the preparation method is suitable for the metal workpiece with irregular structure or complex structure and the metal workpiece needing partial oxidation, and the application field of the preparation method is further widened.
The technical solution of the present invention is further described in detail by the accompanying drawings and examples.
Drawings
FIG. 1 is a schematic view of a water mist oxidation apparatus according to the present invention.
Description of reference numerals:
1-an oxidation power supply; 2-anode base body; 3-water mist spray head.
4-control valve; 5-water mist sprayer; 6-cathode substrate;
7-sealing the reaction chamber.
Detailed Description
As shown in fig. 1, the water mist oxidation apparatus of the present embodiment includes a closed reaction chamber 7 and an oxidation power supply 1 connected to the closed reaction chamber 7 through an electric wire, a positive electrode of the oxidation power supply 1 is connected to an anode substrate 2 in the closed reaction chamber 7, a negative electrode of the oxidation power supply 1 is connected to a cathode substrate 6 in the closed reaction chamber 7, a gap is formed between the anode substrate 2 and the cathode substrate 6, the closed reaction chamber 7 is provided with an opening and is connected to a water mist nozzle 3 through the opening, the water mist nozzle 3 is connected to a water mist sprayer 5 through a pipe, and a control valve 4 is provided on the connected pipe.
Example 1
The embodiment comprises the following steps:
step one, surface treatment: sequentially adopting 800#, 1000#, 1500# and 2000# sandpaper to polish the valve metal workpiece until the surface is smooth and clean, and then sequentially ultrasonically cleaning the valve metal workpiece in absolute ethyl alcohol and deionized water for 10min to obtain the valve metal workpiece after surface treatment;
step two, preparing an atomized solution: preparing an acidic solution as an atomized solution; the acid solution is a mixed solution of sulfuric acid and phosphoric acid, the addition amount of the sulfuric acid in the acid solution is 200g/L, and the addition amount of the phosphoric acid is 20 g/L;
step three, water mist oxidation: placing the valve metal workpiece subjected to surface treatment in the step one as an anode substrate 2 and a stainless steel substrate as a cathode substrate 6 in a closed reaction chamber 7 of water mist oxidation equipment, placing the atomized solution prepared in the step two in a water mist sprayer 5, and opening a control valve 4 to pass throughThe water mist nozzle 3 sprays and introduces water mist into the closed reaction chamber 7, the diffusion angle of the sprayed and introduced water mist is 10-90 degrees, and the introduction flow is 1 L.min -1 The average range is 5m, the fineness of the formed fog beads is not more than 100 mu m, and the pressure in the closed reaction chamber 7 in the spraying process is 0.5 MPa; the method comprises the steps of adopting a direct-current pulse oxidation power supply as an oxidation power supply 1, starting the oxidation power supply 1 and adjusting output voltage to enable micro-arc points to be generated between a valve metal workpiece and a stainless steel substrate to be oxidized, forming an oxidation film layer on the surface of the valve metal workpiece when the power supply frequency adopted by oxidation is 1Hz, the duty ratio is 5%, the oxidation voltage is 300V, and the oxidation time is 10min, and cleaning and drying after the valve metal workpiece is taken out to obtain the valve metal workpiece with the oxidation film layer.
Through detection, the thickness of the oxide film layer on the surface of the metal workpiece with the oxide film layer is 1 μm, and the surface roughness is 0.5 μm.
In the embodiment, the acid solution may also be a mixed solution of one or more of sulfuric acid, phosphoric acid, oxalic acid and chromic acid, except a mixed solution of sulfuric acid and phosphoric acid, wherein the addition amount of sulfuric acid in the acid solution is 20 g/L-400 g/L, the addition amount of phosphoric acid is 10 g/L-80 g/L, and the addition amounts of oxalic acid and chromic acid are 10 g/L-100 g/L.
Example 2
The embodiment comprises the following steps:
step one, surface treatment: sequentially adopting 800#, 1000#, 1500# and 2000# sandpaper to polish the valve metal workpiece until the surface is smooth and clean, and then sequentially ultrasonically cleaning the valve metal workpiece in absolute ethyl alcohol and deionized water for 15min to obtain the valve metal workpiece after surface treatment;
step two, preparing an atomized solution: preparing an alkaline solution as an atomized solution; the alkaline solution is a mixed solution of sodium silicate, sodium phosphate, sodium hydroxide and sodium fluoride, the addition amount of the sodium silicate in the alkaline solution is 25g/L, the addition amount of the sodium phosphate is 10g/L, the addition amount of the sodium hydroxide is 2g/L, and the addition amount of the sodium fluoride is 1 g/L;
step three, water mist oxidation: placing the valve metal workpiece subjected to surface treatment in the step one as an anode substrate 2 and a stainless steel substrate as a cathode substrate 6 in water mistPutting the atomized solution prepared in the step two into a water mist sprayer 5 in a closed reaction chamber 7 of the oxidation equipment, then opening a control valve 4, spraying and introducing water mist into the closed reaction chamber 7 through a water mist spray head 3, wherein the diffusion angle of the sprayed and introduced water mist is 30-100 degrees, and the introduction flow is 20 L.min -1 The average range is 10m, the fineness of the formed fog beads is not more than 100 mu m, and the pressure in the closed reaction chamber 7 in the spraying process is 0.8 MPa; the method comprises the steps of adopting a direct-current pulse oxidation power supply as an oxidation power supply 1, starting the oxidation power supply 1 and adjusting output voltage to enable micro-arc points to be generated between a valve metal workpiece and a stainless steel substrate to be oxidized, forming an oxidation film layer on the surface of the valve metal workpiece when the power supply frequency adopted by oxidation is 800Hz, the duty ratio is 20%, the oxidation voltage is 80-500V, and the oxidation time is 50min, taking out the valve metal workpiece, cleaning and drying the valve metal workpiece after the valve metal workpiece is taken out, and obtaining the valve metal workpiece with the oxidation film layer.
Through detection, the thickness of the oxide film layer on the surface of the metal workpiece with the oxide film layer is 50 μm, and the surface roughness is 2 μm.
The alkaline solution in this embodiment may be replaced with a solution mixed with one or more of silicate, phosphate, aluminate, conductive agent and stabilizer other than a solution mixed with sodium silicate, sodium phosphate, sodium hydroxide and sodium fluoride, the conductive agent is sodium hydroxide or potassium hydroxide, the stabilizer is glycerol, sodium fluoride, ethylene glycol or glycerol, the addition amount of the silicate in the alkaline solution is 10g/L to 60g/L, the addition amount of the phosphate is 5g/L to 50g/L, the addition amount of the aluminate is 5g/L to 40g/L, the addition amount of the conductive agent is 1g/L to 10g/L, and the addition amount of the stabilizer is 1g/L to 10 g/L.
Example 3
The embodiment comprises the following steps:
step one, surface treatment: sequentially adopting 800#, 1000#, 1500# and 2000# sandpaper to polish the valve metal workpiece until the surface is smooth and clean, and then sequentially ultrasonically cleaning the valve metal workpiece in absolute ethyl alcohol and deionized water for 10min to obtain the valve metal workpiece after surface treatment;
step two, preparing an atomized solution: preparing an alkaline solution as an atomized solution; the alkaline solution is a mixed solution of sodium aluminate and sodium hydroxide, the addition amount of the sodium aluminate in the alkaline solution is 20g/L, and the addition amount of the sodium hydroxide is 10 g/L;
step three, water mist oxidation: placing the valve metal workpiece subjected to surface treatment in the first step as an anode base body 2 and a stainless steel base plate as a cathode base plate 6 in a closed reaction chamber 7 of water mist oxidation equipment, placing the atomized solution prepared in the second step in a water mist sprayer 5, opening a control valve 4, spraying and introducing water mist into the closed reaction chamber 7 through a water mist nozzle 3, wherein the diffusion angle of the sprayed and introduced water mist is 90-150 degrees, and the introduction flow is 50 L.min -1 The average range is 18m, the fineness of the formed fog beads is not more than 100 mu m, and the pressure in the closed reaction chamber 7 in the spraying process is 1 MPa; the method comprises the steps of adopting a direct-current pulse oxidation power supply as an oxidation power supply 1, starting the oxidation power supply 1 and adjusting output voltage to enable micro-arc points to be generated between a valve metal workpiece and a stainless steel substrate to be oxidized, forming an oxidation film layer on the surface of the valve metal workpiece when the power supply frequency adopted by oxidation is 1000Hz, the duty ratio is 90%, the oxidation voltage is 700V, and the oxidation time is 150min, taking out the valve metal workpiece, cleaning and drying the valve metal workpiece after the valve metal workpiece is taken out to obtain the valve metal workpiece with the oxidation film layer.
Through detection, the thickness of the oxide film layer on the surface of the metal workpiece with the oxide film layer is 80 μm, and the surface roughness is 5 μm.
The above description is only for the preferred embodiment of the present invention, and is not intended to limit the present invention in any way. Any simple modification, change and equivalent changes of the above embodiments according to the technical essence of the invention are still within the protection scope of the technical solution of the invention.

Claims (6)

1. A preparation method of an oxide film layer on the surface of a metal workpiece under a multiphase condition is characterized by comprising the following steps:
step one, surface treatment: sequentially adopting 800#, 1000#, 1500# and 2000# sandpaper to polish the metal workpiece until the surface is smooth and clean, and then sequentially ultrasonically cleaning the metal workpiece in absolute ethyl alcohol and deionized water for 10-15 min to obtain the surface-treated metal workpiece;
step two, preparing an atomized solution: preparing an acidic solution or an alkaline solution as an atomized solution;
step three, water mist oxidation: taking the metal workpiece subjected to surface treatment in the first step as an anode substrate (2), taking a stainless steel substrate as a cathode substrate (6), placing the stainless steel substrate in a closed reaction chamber (7) of water mist oxidation equipment, placing the atomized solution prepared in the second step in a water mist sprayer (5), opening a control valve (4), spraying water mist into the closed reaction chamber (7) through a water mist spray nozzle (3), starting an oxidation power supply (1) and adjusting output voltage to generate micro arc points between the metal workpiece and the stainless steel substrate for oxidation, forming an oxidation film layer on the surface of the metal workpiece, taking out the metal workpiece, cleaning and drying the metal workpiece by blowing to obtain the metal workpiece with the oxidation film layer.
2. The method for preparing the oxide film layer on the surface of the metal workpiece under the multiphase condition according to claim 1, wherein the acidic solution in the second step is a mixed solution of one or more of sulfuric acid, phosphoric acid, oxalic acid and chromic acid, the addition amount of the sulfuric acid in the acidic solution is 20 g/L-400 g/L, the addition amount of the phosphoric acid is 10 g/L-80 g/L, and the addition amounts of the oxalic acid and the chromic acid are 10 g/L-100 g/L.
3. The method for preparing the oxide film layer on the surface of the metal workpiece under the multiphase condition according to claim 1, wherein in the second step, the alkaline solution is a mixed solution of one or more of silicate, phosphate, aluminate, a conductive agent and a stabilizer, the conductive agent is sodium hydroxide or potassium hydroxide, the stabilizer is glycerol, sodium fluoride, ethylene glycol or glycerol, the addition amount of the silicate in the alkaline solution is 10 g/L-60 g/L, the addition amount of the phosphate is 5 g/L-50 g/L, the addition amount of the aluminate is 5 g/L-40 g/L, the addition amount of the conductive agent is 1 g/L-10 g/L, and the addition amount of the stabilizer is 1 g/L-10 g/L.
4. The method for preparing the oxide film layer on the surface of the metal workpiece under the multiphase condition according to claim 1, wherein the diffusion angle of the sprayed and introduced water mist in the step three is 10-150 degree, and the inlet flow is 1 L.min -1 ~50L·min -1 The average range is more than 5m, the fineness of the formed fog beads is not more than 100 mu m, and the pressure in the closed reaction chamber (7) in the spraying process is 0.5 MPa-1 MPa.
5. The method for preparing the oxide film layer on the surface of the metal workpiece under the multiphase condition according to claim 1, wherein the power frequency adopted by the oxidation in the step three is 1 Hz-1000 Hz, the duty ratio is 5% -90%, the oxidation voltage is 300V-700V, and the oxidation time is 10 min-150 min.
6. The method for preparing the oxide film layer on the surface of the metal workpiece under the multiphase condition according to claim 1, wherein the thickness of the oxide film layer on the surface of the metal workpiece with the oxide film layer in the third step is 1-80 μm, and the surface roughness is 0.5-5 μm.
CN202210734779.4A 2022-06-27 2022-06-27 Preparation method of metal workpiece surface oxidation film layer under multiphase condition Pending CN115012014A (en)

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