CN109234773A - A kind of preparation method of Mg alloy surface composite coating - Google Patents
A kind of preparation method of Mg alloy surface composite coating Download PDFInfo
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- CN109234773A CN109234773A CN201811238261.1A CN201811238261A CN109234773A CN 109234773 A CN109234773 A CN 109234773A CN 201811238261 A CN201811238261 A CN 201811238261A CN 109234773 A CN109234773 A CN 109234773A
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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
- C25D11/026—Anodisation with spark discharge
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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
- C25D11/04—Anodisation of aluminium or alloys based thereon
- C25D11/06—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used
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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
- C25D3/00—Electroplating: Baths therefor
- C25D3/66—Electroplating: Baths therefor from melts
- C25D3/665—Electroplating: Baths therefor from melts from ionic liquids
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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
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/34—Pretreatment of metallic surfaces to be electroplated
- C25D5/42—Pretreatment of metallic surfaces to be electroplated of light metals
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Abstract
A kind of preparation method of Mg alloy surface composite coating, it is successively to aluminize including pretreatment, ionic liquid, differential arc oxidation step using fine aluminium electrode, magnesium alloy component, sodium hydroxide solution, phosphoric acid solution, deionized water, dehydrated alcohol, ionic liquid, electrolyte as raw material.The ceramic layer that present invention differential arc oxidation more direct than Mg alloy surface obtains is finer and close, layer porosity of aluminizing approach 0, porosity after differential arc oxidation can be improved, hardness is higher, up to 1200 ~ 1800 HV, have better corrosion resisting property, and resistance to neutral salt spray may be up to 330 ~ 480h, the non-sealing of hole in surface, product coating uniformity are good.The present invention realizes the metallurgical bonding between aluminium coated and magnesium alloy substrate, so that bond strength is far longer than the bond strength of traditional coating and matrix, is firmly combined not easily to fall off.The present invention is applied widely, is not limited by Components Shape, the use of unharmful substance in coating preparation process, no pollution to the environment, and no toxic wastewater, non-stimulated smell generate.
Description
Technical field
The invention belongs to field of surface technology, and in particular to a kind of preparation method of Mg alloy surface composite coating.
Background technique
Magnesium alloy is due to the performances such as its resource, high specific strength, damping shock absorption, Cutting free processing and dimensionally stable abundant
It receives significant attention, but its corrosion resistance difference greatly limits its larger range of popularization and application.Surface treatment is to mention
The effective means of high Mg alloy surface corrosion resistance, current main process of surface treatment have differential arc oxidation, anodic oxidation, change
Learn oxidation, plating and chemical plating etc..Wherein, the differential arc oxidization technique advantages such as efficient, environmentally friendly, practical and simple process success with it
Applied to the preparation of surface protective coating for magnesium alloy, and effectively improve the corrosion resistance and wearability of magnesium alloy product
Energy.
But magnesium alloy micro-arc oxidization ceramic coating is loose porous, corrosive medium is easily directly contacted with matrix, not resistance to when sealing of hole
Only 70h or so, anti-corrosion effect are poor for neutral salt spray；In addition, magnesium alloy micro-arc oxidization ceramic coating is mainly by MgO, Mg2SiO4、
MgAl2O4Composition, hardness are only 500HV or so, and wear-resisting property improves limited.Relative to magnesium alloy, the differential arc oxidation layer of aluminium alloy
Surface compact, ceramic layer is mainly by α-Al2O3、γ-Al2O3Composition, hardness is high, and wear and corrosion behavior is superior.
Magnesium alloy is active, can not prepare aluminium coat in aqueous solution.Ionic liquid plating aluminum technology has following advantages: first is that
The non-aqueous solution being all made of ion；Second is that anhydrous and oxygen-free, can completely cut off water oxygen removal oxidation film；Third is that quality of coating is high, it is thick
Degree is controllable.It is very suitable for preparing aluminium coat on magnesium alloy.In addition, electroplating technology is not limited by base shape, it can be in complicated structure
Part surface prepares uniform aluminium coat.The methods of current Mg alloy surface aluminium layer technology of preparing, be such as vapor-deposited and spray, exist
The problems such as binding force is insufficient, complex component surface uniformity is poor.
In conclusion differential arc oxidization technique can improve the performance of matrix in Mg alloy surface in-situ preparation ceramic layer, but
Its surface ceramii layer is loose porous and hardness is lower, causes wear and corrosion behavior limited.Existed using ionic liquid plating aluminum technology
Then aluminium coat is completely converted into Al using differential arc oxidization technique by the previously prepared aluminium coat of Mg alloy surface2O3Ceramic layer, and
And be integrated it with magnesium alloy substrate sintering, metallurgical bonding is formed, to realize magnesium alloy wear and corrosion behavior significantly
It is promoted.
The much more domestic differential arc oxidization technique that directlys adopt in Mg alloy surface prepares ceramic layer to improve its wear and corrosion behavior,
Not yet discovery aluminized using ionic liquid+differential arc oxidation method in Mg alloy surface prepares the high anti-corrosion Al-Al of high abrasion2O3It is compound
The report of coating.
To sum up, just at present apparently, it is poor that the aluminum oxide coating of Mg alloy surface still remains product compactness, difference of hardness
And cause to wear no resistance, corrosion resistance is poor, and complex component surface coating uniformity is bad, and binding force is inadequate, in conjunction with not secured enough
The technical problems urgent need to resolve such as lead to be easy to fall off.
Summary of the invention
It is an object of that present invention to provide a kind of preparation methods of Mg alloy surface composite coating.
The object of the invention is achieved through the following technical solutions:
A kind of preparation method of Mg alloy surface composite coating, which is characterized in that it is with fine aluminium electrode, magnesium alloy component, hydrogen
Sodium hydroxide solution, phosphoric acid solution, deionized water, dehydrated alcohol, ionic liquid, electrolyte be raw material, successively include pretreatment, from
Sub- liquid aluminizes, differential arc oxidation.
Composite coating of the present invention is by aluminium coated and aluminum oxide layer is compound forms.
Further, using anhydrous aluminum chloride and chlorination alkyl imidazole as raw material, after stirring evenly dissolution, i.e., above-mentioned ionic liquid is
Obtain ionic liquid；The electrolyte is NaOH, Na2SiO3、Na2WO4、NaB4O7The composite electrolyte of composition, the concentration of each component according to
Secondary be NaOH is 4~8g/L, Na2SiO3For 10~20g/L, Na2WO4For 6~10g/L, NaB4O7For 5~9g/L.
Further, the molar ratio of above-mentioned anhydrous aluminum chloride and chlorination alkyl imidazole is 1.5 ~ 2:1.
Further, above-mentioned chlorination alkyl imidazole is chlorination 1- ethyl-3-methylimidazole.
Further, above-mentioned pretreatment carries out oil removing, deoxidation film process to fine aluminium electrode and magnesium alloy component respectively, completes
Pretreatment, it is spare.
In order to enable the binding force of Mg alloy surface composite coating of the present invention is more preferable, specifically, above-mentioned pretreatment be by
Fine aluminium electrode use concentration for 30 ~ 40g/L sodium hydroxide solution, mass fraction be 30% ~ 50% phosphoric acid solution and deionized water according to
It is secondary to be cleaned, to remove the greasy dirt and oxidation film layer on surface, residual moisture is then removed using dehydrated alcohol, last cold wind is blown
It is dry；The mixed base for the sodium phosphate composition that concentration is 8 ~ 12g/L for 15 ~ 60g/L sodium hydroxide and concentration is used to magnesium alloy component
Property degreasing fluid cleaned, finally cleaned with deionized water to remove the greasy dirt on surface and oxidation film layer, then use nothing
Water-ethanol removes residual moisture, and then cold wind dries up；Finally by the magnesium alloy component and fine aluminium electrode immersion ionic liquid after cleaning
It is activated in body, using magnesium alloy component as anode, fine aluminium is cathode, carries out the processing of constant current anode activation, removes magnesium alloy
Surface film oxide persistently shakes anode and cathode in activation process.
Further, 15 ~ 25mA/cm of activation current in above-mentioned activation process2, 10 ~ 20min of time is handled, it is described to activate
Journey need to carry out under inert atmosphere protection.
In order to further increase the binding force of Mg alloy surface composite coating, so that product compactness is good, uniformity is more
Excellent, it is using the fine aluminium after cleaning as anode that above-mentioned ionic liquid, which is aluminized, and pretreated magnesium alloy is cathode, using ionic liquid
Body galvanoplastic carry out constant current plating, and the cathode after plating is cleaned with deionized water, obtains aluminium coated, aluminum layer thickness
It is 1 ~ 30 μm；The current density of the constant current plating is 5 ~ 25mA/cm2, 10 ~ 120min of electroplating time；Entire electroplating process
It is both needed to be stirred ionic liquid, mixing speed is 300 ~ 500r/min；The ionic liquid is with anhydrous aluminum chloride and chlorine
Change alkyl imidazole is raw material, is stirred evenly after dissolving to get ionic liquid electroplate liquid；The anhydrous aluminum chloride and chlorination alkyl miaow
The molar ratio of azoles is 1.5 ~ 2:1；The chlorination alkyl imidazole is chlorination 1- ethyl-3-methylimidazole；The process of aluminizing is lazy
It is carried out under property atmosphere protection.
Further, above-mentioned differential arc oxidation is to carry out ceramic layer preparation to plating almag using micro-arc oxidation process, specifically
For, the magnesium alloy for being prepared with aluminium coated is connected with microarc oxidation equipment provided positive pole first, is then immersed in electricity
Solve in liquid, finally power on and complete ceramic layer preparation, ceramic layer thickness control at 5 ~ 50 μm, the electrolyte be NaOH,
Na2SiO3、Na2WO4、NaB4O7The composite electrolyte of composition, it is 4~8g/L, Na that the concentration of each component, which is followed successively by NaOH,2SiO3For
10~20g/L, Na2WO4For 6~10g/L, NaB4O7For 5~9g/L；The electrical parameter is positive 1~6A/dm of current density2, negative electricity
0.5~2A/dm of current density2, 500~2000Hz of frequency, duty ratio 10%~30%, 10~120min of oxidization time.
Further, above-mentioned inert gas is high-purity argon gas or nitrogen, purity 99.999%.
The present invention have it is following the utility model has the advantages that
The ceramic layer that composite coating of the present invention differential arc oxidation more direct than Mg alloy surface obtains is finer and close, layer porosity of aluminizing approach
In 0, porosity after can improving differential arc oxidation, hardness is higher, up to 1200 ~ 1800HV, has better corrosion resisting property, resistance to
Neutral salt spray may be up to 330 ~ 480h, the non-sealing of hole in surface, and product coating uniformity is good.The present invention is realized using differential arc oxidization technique
Metallurgical bonding between aluminium coated and magnesium alloy substrate, so that bond strength is far longer than traditional coating and the combination of matrix is strong
Degree, is firmly combined not easily to fall off.The present invention is applied widely, is not limited by Components Shape, there is nothing in composite coating preparation process
The use of evil substance, no pollution to the environment, no toxic wastewater, non-stimulated smell generate.
Detailed description of the invention
Fig. 1 is that the SEM of Mg alloy surface composite coating produced by the present invention schemes.
Specific embodiment
The present invention is specifically described below by embodiment, it is necessary to which indicated herein is that following embodiment is only used
In invention is further explained, it should not be understood as limiting the scope of the invention, person skilled in art can
To make some nonessential modifications and adaptations to the present invention according to aforementioned present invention content.
Embodiment one
A kind of preparation method of Mg alloy surface composite coating carries out as follows:
Material: AZ91 magnesium alloy
(1) two pieces fine aluminium electrode is immersed concentration is alkali cleaning in 35g/L sodium hydroxide solution；With the tap water rinse of flowing；So
Pickling in the phosphoric acid solution that mass fraction is 40% is immersed afterwards；With the tap water rinse of flowing；It immerses in deionized water and rinses；Leaching
Enter in dehydrated alcohol and rinses；Suspension, cold wind drying are spare.
(2) magnesium alloy sample successively immerses to concentration is 30g/L sodium hydroxide and concentration is 10g/L sodium phosphate mixed solution
Cleaned under ultrasonic wave and deoil, then with the tap water rinse of flowing；It is rinsed with deionized water；It is rinsed with dehydrated alcohol；It is outstanding
It hangs, cold wind drying is spare.
(3) magnesium alloy sample and a fine aluminium electrode are immersed in ionic liquid and is activated, anhydrous chlorine in ionic liquid
The molar ratio for changing aluminium and chlorination 1- ethyl-3-methylimidazole is 1.6:1；Magnesium alloy sample connects positive pole, and it is negative that fine aluminium connects power supply
Pole, electric current are set as 16 mA/cm2, time 18min persistently shakes magnesium alloy sample in treatment process；This step is in argon gas
It is carried out in the glove box of protective atmosphere, purity of argon 99.999%.
(4) it will aluminize in the magnesium alloy sample and another another slot ionic liquid of fine aluminium electrode immersion after activation,
The molar ratio of anhydrous aluminum chloride and chlorination 1- ethyl-3-methylimidazole is 1.6:1 in ionic liquid；It is negative that magnesium alloy sample connects power supply
Pole, fine aluminium connect positive pole, and electric current is set as 6 mA/cm2, time 60min, ionic liquid mixing speed 300r/min；Electricity
It is carried out in the glove box of argon atmosphere during plating；It after plating, is rinsed through tap water, deionized water rinsing is blown
It is dry, obtain the aluminium coat with a thickness of 7 ~ 8 μm.
(5) the magnesium alloy sample after aluminizing is immersed in electrolyte after securely connecting with microarc oxidation equipment provided positive pole
In；The electrolyte is NaOH, Na2SiO3、Na2WO4、NaB4O7The concentration of the composite electrolyte of composition, each component is followed successively by
NaOH is 6g/L, Na2SiO3For 15g/L, Na2WO4For 8g/L, NaB4O7For 7g/L.
(6) start microarc oxidation equipment provided, technological parameter are as follows: positive electricity current density 1.5A/dm2, negative electricity current density 0.5A/dm2,
Frequency 700Hz, duty ratio 10%, oxidization time 40min.Using 10~15 μm of micro-arc oxidation ceramic layer thickness made from this technique.
(7) sample after differential arc oxidation, which is directly immersed in the cold water of flowing, cleans, baking oven of the sample after cleaning at 80 DEG C
Middle drying is to get finished product.
During the preparation process, if controlling bad product, to be easy to appear compactness poor, and product uniformity also poor phenomenon passes through
The ceramic layer that the differential arc oxidation more direct than Mg alloy surface of composite coating made from the method for the present invention obtains is finer and close, aluminium coated hole
Rate levels off to 0, and the porosity after can improving differential arc oxidation, the non-sealing of hole in surface, product coating uniformity is more preferable, is specifically shown in attached drawing 1.
The result shows that by Al-Al manufactured in the present embodiment2O3Composite coating appearance gray, reference standard GB/T 4340.1-2009,
Surface micro-vickers hardness is not less than 1700HV, reference standard GB/T 10125-2012, the 330h of resistance to neutral salt spray.
Embodiment two
A kind of preparation method of Mg alloy surface composite coating carries out as follows:
Material: AM60 magnesium alloy
(1) two pieces fine aluminium electrode is immersed concentration is alkali cleaning in 30g/L sodium hydroxide solution；With the tap water rinse of flowing；So
Pickling in the phosphoric acid solution that mass fraction is 30% is immersed afterwards；With the tap water rinse of flowing；It immerses in deionized water and rinses；Leaching
Enter in dehydrated alcohol and rinses；Suspension, cold wind drying are spare.
(2) magnesium alloy sample successively immerses to concentration is 15g/L sodium hydroxide and concentration is the mixed of 12g/L sodium phosphate composition
It closes to clean under solution progress ultrasonic wave and deoil, then with the tap water rinse of flowing；It is rinsed with deionized water；It is floated with dehydrated alcohol
It washes；Suspension, cold wind drying are spare.
(3) magnesium alloy sample and a fine aluminium electrode are immersed in ionic liquid and is activated, anhydrous chlorine in ionic liquid
The molar ratio for changing aluminium and chlorination 1- ethyl-3-methylimidazole is 2:1；Magnesium alloy sample connects positive pole, and fine aluminium connects power cathode,
Electric current is set as 25 mA/cm2, time 10min persistently shakes magnesium alloy sample in treatment process；This step is in nitrogen protection
It is carried out in the glove box of atmosphere, nitrogen gas purity 99.999%.
(4) it will aluminize in the magnesium alloy sample and another another slot ionic liquid of fine aluminium electrode immersion after activation,
The molar ratio of anhydrous aluminum chloride and chlorination 1- ethyl-3-methylimidazole is 2:1 in ionic liquid；It is negative that magnesium alloy sample connects power supply
Pole, fine aluminium connect positive pole, and electric current is set as 23 mA/cm2, time 50min, ionic liquid mixing speed 500r/min；Electricity
It is carried out in the glove box of nitrogen protection atmosphere during plating；It after plating, is rinsed through tap water, deionized water rinsing is blown
It is dry, obtain the aluminium coat with a thickness of 26 ~ 30 μm.
(5) the magnesium alloy sample after aluminizing is immersed in electrolyte after securely connecting with microarc oxidation equipment provided positive pole
In.The electrolyte is NaOH, Na2SiO3、Na2WO4、NaB4O7The concentration of the composite electrolyte of composition, each component is followed successively by
NaOH is 4g/L, Na2SiO3For 10g/L, Na2WO4For 6g/L, NaB4O7For 5g/L.
(6) start microarc oxidation equipment provided, technological parameter are as follows: positive electricity current density 6A/dm2, negative electricity current density 2A/dm2, frequency
1500Hz, duty ratio 25%, oxidization time 90min.Using 40~50 μm of micro-arc oxidation ceramic layer thickness made from this technique.
(7) sample after differential arc oxidation, which is directly immersed in the cold water of flowing, cleans, baking oven of the sample after cleaning at 80 DEG C
Middle drying.
The ceramic layer that composite coating of the present invention differential arc oxidation more direct than Mg alloy surface obtains is finer and close, layer porosity of aluminizing
Level off to 0, the porosity after can improving differential arc oxidation, the non-sealing of hole in surface, product coating uniformity is more preferable.
The result shows that by Al-Al manufactured in the present embodiment2O3Composite coating appearance gray, reference standard GB/T
4340.1-2009, surface micro-vickers hardness are not less than 1200HV, reference standard GB/T 10125-2012, resistance to neutral salt spray
480h。
Embodiment three
A kind of preparation method of Mg alloy surface composite coating carries out as follows:
Material: AZ91 magnesium alloy
(1) two pieces fine aluminium electrode is immersed concentration is alkali cleaning in 40g/L sodium hydroxide solution；With the tap water rinse of flowing；So
Pickling in the phosphoric acid solution that mass fraction is 50% is immersed afterwards；With the tap water rinse of flowing；It immerses in deionized water and rinses；Leaching
Enter in dehydrated alcohol and rinses；Suspension, cold wind drying are spare.
(2) magnesium alloy sample successively immerses to concentration is 60g/L sodium hydroxide and concentration is 12g/L sodium phosphate mixed solution
Cleaned under ultrasonic wave and deoil, then with the tap water rinse of flowing；It is rinsed with deionized water；It is rinsed with dehydrated alcohol；It is outstanding
It hangs, cold wind drying is spare.
(3) magnesium alloy sample and a fine aluminium electrode are immersed in ionic liquid and is activated, anhydrous chlorine in ionic liquid
The molar ratio for changing aluminium and chlorination 1- ethyl-3-methylimidazole is 1.8:1；Magnesium alloy sample connects positive pole, and it is negative that fine aluminium connects power supply
Pole, electric current are set as 20mA/cm2, time 15min persistently shakes magnesium alloy sample in treatment process；This step is protected in argon gas
It protects in the glove box of atmosphere and carries out, purity of argon 99.999%.
(4) it will aluminize in the magnesium alloy sample and another another slot ionic liquid of fine aluminium electrode immersion after activation,
The molar ratio of anhydrous aluminum chloride and chlorination 1- ethyl-3-methylimidazole is 1.8:1 in ionic liquid；It is negative that magnesium alloy sample connects power supply
Pole, fine aluminium connect positive pole, and electric current is set as 15mA/cm2, time 50min, ionic liquid mixing speed 400r/min；Electricity
It is carried out in the glove box of argon atmosphere during plating；It after plating, is rinsed through tap water, deionized water rinsing is blown
It is dry, obtain the aluminium coat with a thickness of 15 ~ 17 μm.
(5) the magnesium alloy sample after aluminizing is immersed in electrolyte after securely connecting with microarc oxidation equipment provided positive pole
In.The electrolyte is NaOH, Na2SiO3、Na2WO4、NaB4O7The concentration of the composite electrolyte of composition, each component is followed successively by
NaOH is 8g/L, Na2SiO3For 20g/L, Na2WO4For 10g/L, NaB4O7For 9g/L.
(6) start microarc oxidation equipment provided, technological parameter are as follows: positive electricity current density 4A/dm2, negative electricity current density 1A/dm2, frequency
800Hz, duty ratio 20%, oxidization time 60min.Using 20~25 μm of micro-arc oxidation ceramic layer thickness made from this technique.
(7) sample after differential arc oxidation, which is directly immersed in the cold water of flowing, cleans, baking oven of the sample after cleaning at 80 DEG C
Middle drying.
The ceramic layer that composite coating of the present invention differential arc oxidation more direct than Mg alloy surface obtains is finer and close, layer porosity of aluminizing
Level off to 0, the porosity after can improving differential arc oxidation, the non-sealing of hole in surface, product coating uniformity is more preferable.
The result shows that by Al-Al manufactured in the present embodiment2O3Composite coating appearance gray, reference standard GB/T
4340.1-2009, surface micro-vickers hardness are not less than 1500HV, reference standard GB/T 10125-2012, resistance to neutral salt spray
400h。
Claims (10)
1. a kind of preparation method of Mg alloy surface composite coating, which is characterized in that it be with fine aluminium electrode, magnesium alloy component,
Sodium hydroxide solution, phosphoric acid solution, deionized water, dehydrated alcohol, ionic liquid, electrolyte be raw material, successively include pretreatment,
Ionic liquid aluminizes, differential arc oxidation.
2. the preparation method of Mg alloy surface composite coating as described in claim 1, which is characterized in that the ionic liquid be with
Anhydrous aluminum chloride and chlorination alkyl imidazole are raw material, are stirred evenly after dissolving to get ionic liquid；The electrolyte be NaOH,
Na2SiO3、Na2WO4、NaB4O7The composite electrolyte of composition, it is 4~8g/L, Na that the concentration of each component, which is followed successively by NaOH,2SiO3For
10~20g/L, Na2WO4For 6~10g/L, NaB4O7For 5~9g/L.
3. the preparation method of Mg alloy surface composite coating as claimed in claim 2, which is characterized in that the anhydrous aluminum chloride
Molar ratio with chlorination alkyl imidazole is 1.5 ~ 2:1.
4. the preparation method of Mg alloy surface composite coating as claimed in claim 3, which is characterized in that the chlorination alkyl miaow
Azoles is chlorination 1- ethyl-3-methylimidazole.
5. the preparation method of Mg alloy surface composite coating as claimed in claim 4, which is characterized in that the pretreatment is to pure
Aluminium electrode and magnesium alloy component carry out oil removing, deoxidation film process respectively, complete pretreatment, spare.
6. the preparation method of Mg alloy surface composite coating as claimed in claim 5, which is characterized in that it is described pretreatment be by
Fine aluminium electrode use concentration for 30 ~ 40g/L sodium hydroxide solution, mass fraction be 30% ~ 50% phosphoric acid solution and deionized water according to
It is secondary to be cleaned, to remove the greasy dirt and oxidation film layer on surface, residual moisture is then removed using dehydrated alcohol, last cold wind is blown
It is dry；The mixed base for the sodium phosphate composition that concentration is 8 ~ 12g/L for 15 ~ 60g/L sodium hydroxide and concentration is used to magnesium alloy component
Property degreasing fluid cleaned, finally cleaned with deionized water to remove the greasy dirt on surface and oxidation film layer, then use nothing
Water-ethanol removes residual moisture, and then cold wind dries up；Finally by the magnesium alloy component and fine aluminium electrode immersion ionic liquid after cleaning
It is activated in body, using magnesium alloy component as anode, fine aluminium is cathode, carries out the processing of constant current anode activation, removes magnesium alloy
Surface film oxide persistently shakes anode and cathode in activation process.
7. the preparation method of Mg alloy surface composite coating as claimed in claim 6, which is characterized in that in the activation process
15 ~ 25mA/cm of activation current2, 10 ~ 20min of time is handled, the activation process need to carry out under inert atmosphere protection.
8. the preparation method of Mg alloy surface composite coating as claimed in claim 7, which is characterized in that the ionic liquid plating
Aluminium is using the fine aluminium after cleaning as anode, and pretreated magnesium alloy is cathode, carries out constant current using ionic liquid galvanoplastic
Plating, the cathode after plating is cleaned with deionized water, obtains aluminium coated, and aluminum layer thickness is 1 ~ 30 μm；The permanent electricity
The current density of galvanic electricity plating is 5 ~ 25mA/cm2, 10 ~ 120min of electroplating time；Entire electroplating process is both needed to carry out ionic liquid
Stirring, mixing speed are 300 ~ 500r/min；The ionic liquid is stirred using anhydrous aluminum chloride and chlorination alkyl imidazole as raw material
It mixes after uniform dissolution to get ionic liquid electroplate liquid；The molar ratio of the anhydrous aluminum chloride and chlorination alkyl imidazole is 1.5 ~ 2:
1；The chlorination alkyl imidazole is chlorination 1- ethyl-3-methylimidazole；The process of aluminizing carries out under inert atmosphere protection.
9. the preparation method of Mg alloy surface composite coating as claimed in claim 8, which is characterized in that the differential arc oxidation is
Ceramic layer preparation is carried out to plating almag using micro-arc oxidation process, specifically, is first closed the magnesium for being prepared with aluminium coated
It is golden to be connected with microarc oxidation equipment provided positive pole, it is then immersed in electrolyte, finally powers on and complete ceramic layer
Preparation, at 5 ~ 50 μm, the electrolyte is NaOH, Na for ceramic layer thickness control2SiO3、Na2WO4、NaB4O7The compound electric of composition
Liquid is solved, it is 4~8g/L, Na that the concentration of each component, which is followed successively by NaOH,2SiO3For 10~20g/L, Na2WO4For 6~10g/L, NaB4O7
For 5~9g/L；The electrical parameter is positive 1~6A/dm of current density2, 0.5~2A/dm of negative electricity current density2, frequency 500~
2000Hz, duty ratio 10%~30%, 10~120min of oxidization time.
10. the preparation method of Mg alloy surface composite coating as claimed in claim 9, which is characterized in that the inert gas
For high-purity argon gas or nitrogen, purity 99.999%.
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| WO2022165961A1 (en) * | 2021-02-02 | 2022-08-11 | 山东省科学院新材料研究所 | Magnesium alloy ultrahigh-porosity micro-arc oxidation coating, preparation method therefor and use thereof |
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- 2018-10-23 CN CN201811238261.1A patent/CN109234773A/en active Pending
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