CN114686952A - Preparation method of transparent oxide film on surface of plastic deformation magnesium alloy workpiece - Google Patents

Preparation method of transparent oxide film on surface of plastic deformation magnesium alloy workpiece Download PDF

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CN114686952A
CN114686952A CN202210491662.8A CN202210491662A CN114686952A CN 114686952 A CN114686952 A CN 114686952A CN 202210491662 A CN202210491662 A CN 202210491662A CN 114686952 A CN114686952 A CN 114686952A
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magnesium alloy
micro
arc oxidation
alloy workpiece
oxide film
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CN114686952B (en
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赵李斌
高亚楠
赵灏琳
冯霖
李红
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SHANXI YINGUANG HUASHENG MAGNESIUM INDUSTRY 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
    • C25D11/30—Anodisation of magnesium 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
    • C23F3/00—Brightening metals by chemical means
    • C23F3/02—Light metals
    • 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
    • C23G1/025—Cleaning or pickling metallic material with solutions or molten salts with acid solutions acidic pickling pastes
    • 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
    • C23G1/12—Light metals
    • 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
    • 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

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

Abstract

The invention provides a preparation method of a transparent oxide film on the surface of a plastically deformed magnesium alloy workpiece, belonging to the technical field of surface treatment of magnesium alloy products; the method comprises the following specific steps: performing natural color micro-arc oxidation and natural color sealing; the micro-arc oxidation electrolyte comprises NH with the concentration of 13-16 g/L4HF28 to 12g/L of (NaPO)3)60.25-0.35 g/L EDTA-2 Na, 0.25-0.35 g/L trisodium citrate, 0.2-0.4 g/L titanium potassium oxalate and 0.25-0.45 g/L glucose; the temperature of the micro-arc oxidation electrolyte is 60-90 ℃, and the pH = 4-5.5; the micro-arc oxidation is simultaneously controlled by adopting a forward constant voltage and a reverse constant voltage; the invention forms a transparent film layer on the surface of the magnesium alloy, and the oxide film is hardBut also has certain self-cleaning function.

Description

Preparation method of transparent oxide film on surface of plastic deformation magnesium alloy workpiece
Technical Field
The invention belongs to the technical field of surface treatment of magnesium alloy products, and relates to a preparation method of a transparent oxide film on the surface of a plastic deformation magnesium alloy workpiece.
Background
The magnesium alloy has low specific gravity and excellent electromagnetic shielding performance, is widely applied to the 3C electronic field and the rail transit field by people, and has noble brightness which is different from aluminum brightness and silver brightness, and can be stored for a short time and not be used for a long time due to the easy oxidation and corrosion of the magnesium, so the magnesium alloy is luxurious in the magnesium alloy application field for a long time.
Although the Anomag process from australia has properly solved the problem in this respect, Anomag must be electrolyzed in a low-temperature ammonia solution, which is very volatile and easily causes environmental pollution, and in addition, the domestic related patent adopts a solution added with ammonia or organic amine to form a transparent or semitransparent oxide film in an arc suppression state, but the oxide film is soft and lacks necessary scratch resistance, and cannot support the use under the condition of unnecessary appearance protection layer.
Disclosure of Invention
The invention overcomes the defects of the prior art and provides a preparation method of a transparent oxide film on the surface of a plastic deformation magnesium alloy workpiece.
In order to achieve the purpose, the invention is realized by the following technical scheme:
a preparation method of a transparent oxide film on the surface of a plastic deformation magnesium alloy workpiece comprises the following steps:
a) natural color micro-arc oxidation: placing the magnesium alloy workpiece in micro-arc oxidation electrolyte for micro-arc oxidation;
the micro-arc oxidation electrolyte comprises NH with the concentration of 13-16 g/L4HF28 to 12g/L of (NaPO)3)60.25-0.35 g/L EDTA-2 Na, 0.25-0.35 g/L trisodium citrate, 0.2-0.4 g/L titanium potassium oxalate and 0.25-0.45 g/L glucose; the temperature of the micro-arc oxidation electrolyte is 60-90 ℃, and the pH = 4-5.5.
The micro-arc oxidation is simultaneously controlled by adopting a forward constant voltage and a reverse constant voltage, the forward electricity is used for 0-90 s and the voltage is 100-200V, or the forward electricity is used for 90-900 s and the voltage is 300-450V; the time of using the reverse electricity is 0-30 s, and the voltage is 4-5V, or the time of using the reverse electricity is 30-900 s, and the voltage is 9-10V.
b) Sealing the natural color: placing the magnesium alloy workpiece subjected to the natural-color micro-arc oxidation treatment into a sealing liquid, and performing ultrasonic oscillation for 3-5 min; the confining liquid comprises KH-550 with the concentration of 8-12 mL/L and C with the concentration of 40-60 mL/L2H5OH; the pH of the confining liquid is = 6-6.5, and the temperature is 70-85 ℃.
Preferably, the time of using the forward electricity is 0-30 s, and the voltage is 100V; or the forward electrification time is 30-60 s and the voltage is 150V; or the forward electrification time is 60-90 s, and the voltage is 200V; or the forward electrification time is 90-120 s, and the voltage is 300V; or the forward power time is 120-900 s and the voltage is 450V.
Preferably, the frequency controlled by adopting the forward constant voltage is 1200 Hz; the frequency controlled with a reverse electrical constant voltage was 1000 Hz.
Preferably, before the natural color micro-arc oxidation operation, the clean waste magnesium alloy workpiece is firstly subjected to high-pressure electrolytic oxidation once in the micro-arc oxidation electrolyte according to the proportion of 0.8-1 dm2Micro-arc oxidation is carried out on waste magnesium alloy workpieces by the aid of/L working area for supplementing Mg into micro-arc oxidation electrolyte2+。
Preferably, the pH of the sealing liquid is adjusted to 6-6.5 by adopting potassium hydrogen phthalate.
Preferably, the magnesium alloy workpiece with the sealed natural color is cleaned and dried, wherein the drying temperature is 150-170 ℃, and the drying time is 10-15 min.
Preferably, the magnesium alloy workpiece is subjected to surface pretreatment and then subjected to natural-color micro-arc oxidation.
Preferably, the surface pretreatment comprises degreasing, pickling and brightening.
Preferably, the degreasing solution comprises the following concentrations: 4-6 g/L KOH, 4-6 g/L Na2CO3、4~6 g/L Na3PO4The temperature of the degreased liquid is 50-70 ℃.
Preferably, the pickling solution for pickling comprises citric acid with the concentration of 4-6 g/L, lactic acid with the concentration of 8-12 g/L and tartaric acid with the concentration of 2-3 g/L; the temperature of the pickling solution is 40-50 ℃; the treating fluid adopted by the brightening treatment comprises KOH with the concentration of 4-6 g/L and Na with the concentration of 2-3 g/L4P2O7、0.4~0.6 g/L NaNO3。
Compared with the prior art, the invention has the beneficial effects that.
The transparent natural-color micro-arc oxidation film formed by the invention is a silver gray film layer before arcing. After a slight micro-discharge, a transparent film layer is formed, the oxide film is hard and has a certain self-cleaning function, and the transparent layer can be effectively thickened and sealed by adopting necessary measures.
The magnesium alloy transparent micro-arc oxidation layer prepared by the method of the invention comprises the following steps:
1) through the component control and the electrolysis parameter control of the micro-arc oxidation electrolyte, the surface of the magnesium alloy forms a transparent ceramic film in the micro-arc oxidation process.
2) After the arc is struck, the set elements in the electrolyte form part of the transparent ceramic, but when the arc is too large, a white film layer is formed, so the formation of the transparent film layer is directly related to the striking voltage.
3) The oxide film is gradually thickened but still keeps transparent after being oxidized for a plurality of times at constant voltage within a determined liquid system and voltage range.
Detailed Description
In order to make the technical problems, technical solutions and beneficial effects to be solved by the present invention more clearly apparent, the present invention is further described in detail with reference to the embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. The technical solutions of the present invention are described in detail below with reference to examples, but the scope of protection is not limited thereto.
Example 1
A preparation method of a transparent oxide film on the surface of a plastic deformation magnesium alloy workpiece comprises the following process flows:
the method comprises the steps of degreasing → washing with water 1 → water 2 → acid washing → washing with water → sixteenth brightening treatment → washing with water → natural color micro-arc oxidation → natural color closure of self-color → washing with water → high-pressure air drying → testing with water → packaging.
Specifically, the chemical formula and the process conditions of each step are as follows:
(1) the method comprises the following steps of:
KOH 5 g/L
Na2CO3 5 g/L
Na3PO4 5 g/L
sodium dodecyl benzene sulfonate 0.2 g/L
Temperature: 50-70 ℃, time: 1-3 min. If the water cannot be cleaned at one time, the water can be repeatedly washed, and the water must be washed by hot water at the temperature of more than 50 ℃ after the water is taken out of the bath for the first time.
(2) Step four, pickling:
citric acid 5 g/L
Lactic acid 10 g/L
Tartaric acid 3 g/L
Temperature: 40-50 ℃, time: and (3) blackening the whole surface of the steel for 30-180 s, wherein the mark is a thorough pickling mark.
(3) Step sixthly, brightening
KOH 5 g/L
Na4P2O7 3 g/L
NaNO3 0.5 g/L
Temperature: 60-85 ℃, time: and (4) carrying out ultrasonic oscillation for 2-10 min, so that the surface is clean and white after washing, and the water film is uniformly attached, and repeating the fourth step to the sixth step if the effect cannot be achieved.
(4) Step and aspect of the original color micro-arc oxidation treatment
NH4HF2 15 g/L
(NaPO3)6 10 g/L
EDTA·2Na 0.25 g/L
Trisodium citrate 0.25 g/L
Titanium potassium oxalate 0.2 g/L
Glucose 0.25 g/L
Mg2+ Micro-scale
Preparing electrolyte:
1) measured NH4HF2And (NaPO)3)6Respectively adding 200 mL of pure water at the temperature of 70-90 ℃, stirring and dissolving for later use.
2) Respectively adding EDTA-2 Na, sodium citrate and glucose into 100 mL of pure water at the temperature of 70-90 ℃, and stirring and dissolving for later use.
3) Adding metered potassium titanium oxalate into the solution obtained in the step 2), stirring and melting, and heating to 90-95 ℃ on an electric furnace.
4) Adding the solution prepared in the steps 1) and 3) into an electrolytic bath, and then supplementing hot pure water at 70-90 ℃ to a certain quantity.
5) Taking a magnesium alloy clean waste workpiece to carry out high-pressure electrolytic oxidation once in the electrolyte of the step 4) according to the proportion of 0.8-1 dm2the/L working area carries out micro-arc oxidation on the waste magnesium alloy workpiece to supplement Mg2+。
Controlling the micro-arc oxidation process:
1) and opening the temperature regulating and controlling equipment to regulate the electrolyte within the range of 60-75 ℃.
2) After hanging and cutting the workpiece, the workpiece is required to be electrified and enter the groove, and the voltage range is 1-3V before entering the groove.
3) Electrical parameters: the micro-arc oxidation adopts the simultaneous control of a forward constant voltage and a reverse constant voltage, and the control parameters are shown in the following table:
Figure DEST_PATH_IMAGE002
(5) the self-color of the self-skin is sealed:
KH-550 10 mL
C2H5OH 50 mL
H2o (pure water) to 1L
The liquid is hydrolyzed at the constant temperature of 60-65 ℃ for 24 hours for use.
And (3) adding pure water into 100 mL of the hydrolysis liquid to dilute to 1L, adjusting the pH to be between 6 and 6.5 by using potassium hydrogen phthalate, heating to 70 to 85 ℃, washing the workpiece subjected to the natural color micro-arc oxidation treatment by using the pure water, then putting the workpiece into the liquid, carrying out ultrasonic oscillation for 3 to 5 min, washing by using the pure water after the workpiece is taken out of the bath, and blowing the workpiece to be dry by using high-pressure air.
(6) Step by step drying
And taking out air to cool to room temperature after drying treatment by circulating air in a drying furnace at 150-170 ℃ for 10-15 min.
(7) Detection of
And detecting the prepared magnesium alloy workpiece, wherein the detection items comprise film thickness, neutral salt spray test, acetylene flame retardant test, wear resistance and L (a + b) transmittance test.
The test methods and results are as follows:
Figure DEST_PATH_IMAGE004
while the invention has been described in further detail with reference to specific preferred embodiments thereof, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.

Claims (10)

1. A preparation method of a transparent oxide film on the surface of a plastic deformation magnesium alloy workpiece is characterized by comprising the following steps:
a) natural color micro-arc oxidation: placing the magnesium alloy workpiece in a micro-arc oxidation electrolyte for micro-arc oxidation:
the micro-arc oxidation electrolyte comprises NH with the concentration of 13-16 g/L4HF28 to 12g/L of (NaPO)3)60.25-0.35 g/L EDTA-2 Na, 0.25-0.35 g/L trisodium citrate, 0.2-0.4 g/L titanium potassium oxalate and 0.25-0.45 g/L glucose; the temperature of the micro-arc oxidation electrolyte is 60-90 ℃, and the pH = 4-5.5;
the micro-arc oxidation is simultaneously controlled by adopting a forward constant voltage and a reverse constant voltage, the forward electricity is used for 0-90 s and the voltage is 100-200V, or the forward electricity is used for 90-900 s and the voltage is 300-450V; the time of using the reverse electricity is 0-30 s, the voltage is 4-5V, or the time of using the reverse electricity is 30-900 s, and the voltage is 9-10V;
b) sealing the natural color: placing the magnesium alloy workpiece subjected to the natural-color micro-arc oxidation treatment into a sealing liquid, and performing ultrasonic oscillation for 3-5 min; the confining liquid comprises KH-550 with the concentration of 8-12 mL/L and C with the concentration of 40-60 mL/L2H5OH; the pH of the confining liquid is = 6-6.5, and the temperature is 70-85 ℃.
2. The method for preparing the transparent oxide film on the surface of the plastic deformation magnesium alloy workpiece according to claim 1, characterized in that forward electricity is used for 0-30 s at a voltage of 100V; or the forward electrification time is 30-60 s and the voltage is 150V; or the forward electrification time is 60-90 s, and the voltage is 200V; or the forward electricity time is 90-120 s, and the voltage is 300V; or the forward power time is 120-900 s and the voltage is 450V.
3. The method for preparing the transparent oxide film on the surface of the plastic deformation magnesium alloy workpiece according to the claim 1 or 2, characterized in that the frequency controlled by adopting the positive constant voltage is 1200 Hz; the frequency controlled with a reverse electrical constant voltage was 1000 Hz.
4. The method for preparing the transparent oxide film on the surface of the plastic deformation magnesium alloy workpiece according to claim 1, wherein before the natural color micro-arc oxidation operation, the magnesium alloy clean waste workpiece is firstly taken and subjected to high-pressure electrolytic oxidation once in the micro-arc oxidation electrolyte according to the proportion of 0.8-1 dm2Micro-arc oxidation is carried out on waste magnesium alloy workpieces by the aid of/L working area for supplementing Mg into micro-arc oxidation electrolyte2+。
5. The method for preparing the transparent oxide film on the surface of the plastic deformation magnesium alloy workpiece according to claim 1, characterized in that potassium hydrogen phthalate is adopted to adjust the pH value of the sealing liquid to 6-6.5.
6. The method for preparing the transparent oxide film on the surface of the plastic deformation magnesium alloy workpiece according to claim 1, wherein the magnesium alloy workpiece with the sealed natural color is cleaned and dried, and the drying temperature is 150-170 ℃ and the drying time is 10-15 min.
7. The method for preparing the transparent oxide film on the surface of the plastic deformation magnesium alloy workpiece according to claim 1, wherein the magnesium alloy workpiece is subjected to surface pretreatment and then subjected to natural-color micro-arc oxidation.
8. The method of claim 7, wherein the surface pretreatment comprises degreasing, pickling and brightening.
9. The method for preparing the transparent oxide film on the surface of the plastic deformation magnesium alloy workpiece as claimed in claim 8, wherein the degreased degreasing solution comprises the following components in concentration: 4-6 g/L KOH, 4-6 g/L Na2CO3、4~6 g/L Na3PO4The temperature of the degreased liquid is 50-70 ℃.
10. The method for preparing the transparent oxide film on the surface of the plastic deformation magnesium alloy workpiece according to claim 8, wherein the pickling solution for pickling comprises citric acid with the concentration of 4-6 g/L, lactic acid with the concentration of 8-12 g/L and tartaric acid with the concentration of 2-3 g/L; the temperature of the pickling solution is 40-50 ℃; the treating fluid adopted by the brightening treatment comprises KOH with the concentration of 4-6 g/L and Na with the concentration of 2-3 g/L4P2O7、0.4~0.6 g/L NaNO3。
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Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2002220697A (en) * 2001-01-30 2002-08-09 Chiyoda Kiki Hanbai Kk Film forming method on magnesium alloy and electrolytic solution therefor
JP2002256494A (en) * 2000-12-28 2002-09-11 Fuji Kogyo Co Ltd Method for forming anodic oxide film on magnesium alloy
JP2004018901A (en) * 2002-06-13 2004-01-22 Niigata Prefecture Surface treatment method for magnesium material product
CN101010452A (en) * 2004-06-22 2007-08-01 东洋制罐株式会社 Surface-treated metal materials, method of treating the surfaces thereof, resin-coated metal materials, cans and can lids
CN101054712A (en) * 2007-02-07 2007-10-17 北京交通大学 Method of preparing transparent film on magnesium alloy surface
TW200741038A (en) * 2006-04-21 2007-11-01 Hon Hai Prec Ind Co Ltd Electrolyte for anodizing magnesium product
CN102703892A (en) * 2012-01-14 2012-10-03 哈尔滨工程大学 Microarc-oxidized coating silylation fluid and hole sealing method thereby
CN103286909A (en) * 2012-02-24 2013-09-11 比亚迪股份有限公司 Metal resin integrated forming method and metal resin composite
CN103459677A (en) * 2011-03-29 2013-12-18 新日铁住金株式会社 Surface-treated steel sheet and method for producing same
CN107699935A (en) * 2017-10-17 2018-02-16 江西科技师范大学 A kind of Mg alloy surface prepares the micro-arc oxidation electrolyte and method of iron content coating

Patent Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2002256494A (en) * 2000-12-28 2002-09-11 Fuji Kogyo Co Ltd Method for forming anodic oxide film on magnesium alloy
JP2002220697A (en) * 2001-01-30 2002-08-09 Chiyoda Kiki Hanbai Kk Film forming method on magnesium alloy and electrolytic solution therefor
JP2004018901A (en) * 2002-06-13 2004-01-22 Niigata Prefecture Surface treatment method for magnesium material product
CN101010452A (en) * 2004-06-22 2007-08-01 东洋制罐株式会社 Surface-treated metal materials, method of treating the surfaces thereof, resin-coated metal materials, cans and can lids
TW200741038A (en) * 2006-04-21 2007-11-01 Hon Hai Prec Ind Co Ltd Electrolyte for anodizing magnesium product
CN101054712A (en) * 2007-02-07 2007-10-17 北京交通大学 Method of preparing transparent film on magnesium alloy surface
CN103459677A (en) * 2011-03-29 2013-12-18 新日铁住金株式会社 Surface-treated steel sheet and method for producing same
CN102703892A (en) * 2012-01-14 2012-10-03 哈尔滨工程大学 Microarc-oxidized coating silylation fluid and hole sealing method thereby
CN103286909A (en) * 2012-02-24 2013-09-11 比亚迪股份有限公司 Metal resin integrated forming method and metal resin composite
CN107699935A (en) * 2017-10-17 2018-02-16 江西科技师范大学 A kind of Mg alloy surface prepares the micro-arc oxidation electrolyte and method of iron content coating

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