CN102234803B - Preparation method of composite coating on magnesium alloy plasma oxide ceramic surface - Google Patents

Preparation method of composite coating on magnesium alloy plasma oxide ceramic surface Download PDF

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Publication number
CN102234803B
CN102234803B CN201010165323A CN201010165323A CN102234803B CN 102234803 B CN102234803 B CN 102234803B CN 201010165323 A CN201010165323 A CN 201010165323A CN 201010165323 A CN201010165323 A CN 201010165323A CN 102234803 B CN102234803 B CN 102234803B
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coating
varnish
magnesium alloy
chemical plating
abs resin
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CN102234803A (en
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杜克勤
张伟
王福会
严川伟
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Institute of Metal Research of CAS
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Abstract

The invention relates to a preparation method of a composite coating consisting of an organic coating and a chemical coating on a magnesium alloy plasma oxide ceramic surface, belonging to the technical field of metal surface treatment. The method mainly comprises the following steps of: performing plasma anode oxidation on a magnesium alloy to form a porous ceramic layer; spraying ABS (Acrylonitrile Butadiene Styrene) resin or varnish; and forming a nickel-phosphorus clad layer by adopting chemical plating. In the method, the porous ceramic layer formed by performing plasma anode oxidation on the magnesium alloy is taken as a substrate, the hole sealing is performed by using an organic coating, and chemical plating is performed. A multi-layer composite film layer prepared with the method has enough protective thickness, the coating has high bonding force with the substrate and high hardness, and the protective requirements of scraping resistance and corrosion resistance on a magnesium alloy are met effectively.

Description

Magnesiumalloy plasma oxidation ceramic membrane surface preparation method of composite coating
Technical field
The present invention relates to prepare the compound coating method of organic coating-chemical plating, belong to field of metal surface treatment technology at magnesiumalloy plasma sunization ceramic membrane surface.
Background technology
Magnesiumalloy has high specific tenacity and specific rigidity and good damping characteristic, is the structural metallic materials that satisfies the tool potentiality of car lightization, environmental protectionization and performance optimization development, also is 21st century one of metallic substance of application prospect to be arranged most.But because the thermodynamic stability of magnesium is poor, and oxide compound (film) short texture, cause the corrosion resistance of magnesiumalloy relatively poor, to a great extent limit its widespread use.Therefore, the Mg alloy surface processing is crucial in practical application.The method of surface-treated is a lot, like electrochemical process, chemical method, hot-work method etc.Surface treatment method that some are novel such as Laser Surface Treatment, chromium nitride coating, Mg alloy surface deposition of aluminum etc.But up to now, a kind of protective layer that is applicable to magnesium alloy substrate of resisting severe environment also can not developed in countries in the world.
For surface anticorrosion and the wear resistance that improves MAGNESIUM METAL 99; Chinese scholars has been developed numerous surface-treateds and has been coated with/plating process; As can obtain the dura mater of and anti-corrosion anti scuffing firm at magnesiumalloy microplasma electrolytic oxide film surface recombination non-crystalline state Ni-P settled layer, be a kind of effective and feasible technical thought with matrix bond.On the one hand, complete nickeling layer can play sealing process to the multilayer ceramic film, has avoided magnesium alloy substrate to contact with the direct of corrosive medium, on the other hand because the chemicalstability of metallic nickel is good, hardness is high, has good wear-resisting and corrosion stability.But the magnesiumalloy ceramic membrane has vesicular structure, directly carries out electroless plating on its surface, because coated metal is higher than magnesiumalloy current potential, and is easy to take place the bimetal galvanic corrosion after magnesiumalloy contacts.Especially be difficult to obtain even flawless coating for complex-shaped or big area plating piece.The formation of this textural defect is easy to occur local bimetallic corrosion or microcosmic galvanic corrosion phenomenon, causes the deterioration of magnesium alloy component mechanical property, can accelerate corrosion process greatly so on the contrary, causes catastrophic consequence.
Adopting organic coating to apply also is a kind of magnesiumalloy means of defence commonly used, and organic coating protection mechanism mainly is shielding effect, passivation corrosion inhibition.But coating generally relatively approaches, has not anti scuffing of hole and bad mechanical property, under strong corrosive medium and high-temp and high-strength environment, comes off easily, generally can only be used for the short duration protection metal, can not be used for doing long-term protection.
Research shows, to form protective coating technology many though be used in Mg alloy surface, and polytechnic anticorrosion and wear resisting property all is difficult to reach higher level, and coating's adhesion also often becomes restraining factors.
Summary of the invention
The invention reside in the deficiency that overcomes prior art; A kind of compound coating method for preparing organic coating-chemical plating at magnesiumalloy plasma oxidation ceramic membrane surface is provided; Improve the anticorrosion and attrition resistant over-all properties of magnesiumalloy, solved magnesiumalloy anti scuffing and corrosion resistant requirement of shelter.
The present invention implements through following technical proposal:
A kind ofly prepare the compound coating method of organic coating-chemical plating, at first magnesiumalloy is carried out the plasma anodic oxidation, form porous ceramic layer at magnesiumalloy plasma oxidation ceramic membrane surface; Carry out the coating of organic coating then, form high hard anti-corrosion nickel-phosphorus coating through electroless plating at outermost layer at last, specifically comprise the steps:
(1) Mg alloy surface plasma oxidation
After the polishing of magnesium alloy sample process, polishing, removing the wet goods pre-treatment, to remove surface scale and impurity.Then magnesium alloy sample (as anode) being put into electrolytic solution adopts the high voltage pulse mode that sample is carried out plasma spark discharge oxidation.The electrolytic solution of plasma oxidation is: sodium hydroxide 1~3g/L, and water glass 5~20g/L, sodium phosphate 5~10g/L, all the other are water, uniform mixing, temperature is 0~50 ℃; Adopt pulse mode to carry out oxidation, pulse-repetition is 100~2000Hz, and current density is 1~10A/dm 2, oxidization time is 30~120 minutes, and oxide thickness is 5~40 μ m, and this sull is a porous ceramic film, and porosity is 30%~60%, the aperture is 3~10 μ m.
(2) be coated with organic coating: ABS resin applies or varnish applies
1) ABS resin applies
Magnesium alloy sample behind the plasma oxidation is carried out the resin spraying, and spray coating liquor is formed: ABS resin 150~250g/L, solvent are DMSO 99.8MIN., uniform mixing.Spraying parameter is: powder size is 200~400 orders, and spray pressure is 1.5~2.5MPa, and spray distance is 20~40mm, and the thickness of ABS resin coating is at 1~5mm.
Among the present invention, by weight percentage, the composition of ABS resin is following: vinyl cyanide (A) accounts for 15%~35%, and divinyl (B) accounts for 5%~30%, and vinylbenzene (S) accounts for 40%~60%.
2) varnish applies
Magnesium alloy sample behind the plasma oxidation is carried out the varnish spraying, and spray coating liquor is formed: varnish 100~200g/L, solvent are ether, uniform mixing.Spraying parameter is: powder size is 200~400 orders, and spraying temperature is decided to be 150~300 ℃, and pressure is 1.5~2.5MPa, and spray distance is 10~40mm, and the thickness of varnish coating is at 1~3mm.
Among the present invention, varnish is meant acrylic varnish commonly used, and its weight is formed can be following: TEB 3K 30~50%; NSC 20956 10%~30%; Methylacrylic acid copolymer resins 10%~30%; Nitro-cotton 5%~10%.
(3) electroless plating
The magnesium alloy sample that applies ABS resin or varnish is put into chemical plating fluid carry out electroless plating.Chemical plating fluid is formed: basic nickel carbonate 10~15g/L, inferior sodium phosphate 20~30g/L, Trisodium Citrate 3~5g/L, matt salt 10~15g/L, sodium acetate 10~15g/L, thiocarbamide 2~4mg/L, oxysuccinic acid 2~6mg/L, ammoniacal liquor 10~20mL/L, uniform mixing.The nickel chemical plating technology parameter is: service temperature is 85~90 ℃, and the electroless plating time is 30~60min, and the chemical plating thickness of acquisition is 8~10 μ m.Thereby, obtain the compound coating that magnesiumalloy plasma sunization ceramic membrane surface prepares organic coating-chemical plating.
Among the present invention; Before the ABS resin spraying, can carry out sealing treatment to magnesium alloy sample, the effect of sealing treatment is; Make encapsulant can fill micropore bigger in the rete; And then obtain uniform micropore surface, guarantee disperse that ABS resin distributes at film surface and careful, and then help the even growth of chemical plating.Seal treatment technique is: chromic anhydride 400~420g/L, and all the other are water, uniform mixing; Temperature: 50~60 ℃, the time: 30~50min.After the taking-up, clean 1~3min with tap water immediately, use washed with de-ionized water 1~3min again.
Among the present invention; After adopting the varnish spraying; Can carry out etch to magnesium alloy sample and handle, its role is to that film surface is carried out activation treatment and be beneficial to adhering to of varnish, corrosion-tank finishing process is: etch 2~5 seconds (s) under the room temperature of hydrochloric acid 1~2% (weight concentration).After the taking-up, clean 1~3min with tap water immediately, use washed with de-ionized water 1~3min again.
Advantage of the present invention and beneficial effect are following:
1, the porous ceramic film surface bonding organic coating and the chemical plating that form at the magnesiumalloy plasma oxidation through the inventive method; Form multilayer proofing layer (thickness>30 μ m); Effectively isolated magnesium alloy substrate contacts with extraneous corrosive medium; Have stronger anticorrosion ability, and the compound coating bonding strength is big, hardness is high, has the performance that wear-resisting scratch-resisting is hindered.The use of the present invention's unharmful substance in the preparation process of magnesiumalloy multilayer proofing layer and energy utilization efficiency are high, have environmental friendliness and characteristic of low energy consumption.
2, the present invention is applicable to the magnesiumalloy of AZ, ZM, MB and rare earth metal: like AZ91D, AZ31B, ZM5, ZM6, MB5 and Mg-Gd-Y etc.
Embodiment
Below in conjunction with embodiment the present invention is done and to further describe.
Embodiment 1
1. material is prepared: after AZ91D magnesiumalloy cutting polishing, the polishing, in acetone soln, use the ultrasonic cleaning oil removing, then at deionized water for ultrasonic cleaning and removing organic matter removal and impurity.
2. plasma oxidation: in the electrolytic solution, sodium hydroxide 3g/L, water glass 15g/L, sodium phosphate 10g/L, all the other are water, temperature is 50 ℃; Adopt pulse mode to carry out oxidation, pulse-repetition is 1000Hz, and current density is 5A/dm 2, oxidization time is 40 minutes, and oxide thickness is 30 μ m, and this sull is a porous ceramic film, and porosity is 40%, the aperture is 5~10 μ m.
3.ABS resin spraying: the specimen surface after the article on plasma oxidation carries out the ABS resin spraying, and spray coating liquor is formed: ABS resin 150g/L, solvent are DMSO 99.8MIN..Spraying parameter is: powder size is 300 orders, and spray pressure is 2MPa, and spray distance is 20mm, the thickness 2mm of ABS resin coating.
In the present embodiment, the weight of ABS resin is formed A: B: S=20: 30: 50.
4. chemical nickel phosphorus plating
Chemical plating fluid is formed: basic nickel carbonate 10gg/L, inferior sodium phosphate 25gg/L, Trisodium Citrate 3gg/L, matt salt 15gg/L, sodium acetate 10g/L, thiocarbamide 2mg/L, oxysuccinic acid 4mg/L, ammoniacal liquor 15mL/L.The nickel chemical plating technology parameter is: service temperature is 85 ℃, and the electroless plating time is 50min, and the chemical plating thickness of acquisition is 10 μ m.
Bonding strength>the 30MPa of the compound coating that obtains by present embodiment, surperficial Vickers' hardness maximum can reach 900HV, and anti-neutral salt spray test reaches more than the 2000h.
Embodiment 2
Be with embodiment 1 difference:
1. material is prepared: after AZ31B magnesiumalloy cutting polishing, the polishing, in acetone soln, use the ultrasonic cleaning oil removing, then at deionized water for ultrasonic cleaning and removing organic matter removal and impurity.
2. plasma oxidation: in the electrolytic solution, sodium hydroxide 2g/L, water glass 10g/L, sodium phosphate 5g/L, all the other are water, temperature is a room temperature.Adopt pulse mode to carry out oxidation, pulse-repetition is 1000Hz, and current density is 2A/dm 2, oxidization time is 60min, and oxide thickness is 15 μ m, and this sull is a porous ceramic film, and porosity is 30%, the aperture is 3~8 μ m.
3. varnish spraying: the specimen surface after the article on plasma oxidation carries out the varnish spraying, and spray coating liquor is formed: varnish 200g/L, solvent are ether.Spraying parameter is: powder size is 400 orders, and spraying temperature is decided to be 300 ℃, and pressure is 2.5MPa, and spray distance is 30mm, the thickness 3mm of varnish.
In the present embodiment, varnish is meant acrylic acid varnish commonly used, and its weight is formed can be following: TEB 3K 30%; NSC 20956 30%; Methylacrylic acid copolymer resins 30%; Nitro-cotton 10%.
4. chemical nickel phosphorus plating:
Chemical plating fluid is formed: basic nickel carbonate 10g/L, inferior sodium phosphate 25g/L, Trisodium Citrate 3g/L, matt salt 15g/L, sodium acetate 15g/L, thiocarbamide 2mg/L, oxysuccinic acid 5mg/L, ammoniacal liquor 10mL/L.The nickel chemical plating technology parameter is: service temperature is 90 ℃, and the electroless plating time is 60min, and the chemical plating thickness of acquisition is 10 μ m.
Bonding strength>the 35MPa of the compound coating that obtains by present embodiment, surperficial Vickers' hardness maximum can reach 800HV, and anti-neutral salt spray test reaches more than the 1500h.
Embodiment 3
Be with embodiment 2 differences:
1. material is prepared: after ZM5 magnesiumalloy cutting polishing, the polishing, in acetone soln, use the ultrasonic cleaning oil removing, then at deionized water for ultrasonic cleaning and removing organic matter removal and impurity.
2. plasma oxidation: in the electrolytic solution, electrolytic solution contains sodium hydroxide 2g/L, water glass 15g/L, and sodium phosphate 5g/L, all the other are water, temperature is 30 ℃; Adopt pulse mode to carry out oxidation, pulse-repetition is 1500Hz, and current density is 8A/dm 2, oxidization time is 30 minutes, and oxide thickness is 20 μ m, and this sull is a porous ceramic film, and porosity is 50%, the aperture is 6~10 μ m.
3. varnish spraying: the specimen surface after the article on plasma oxidation carries out the varnish spraying, and spray coating liquor is formed: varnish 200g/L, solvent are ether.Spraying parameter is: powder size is 400 orders, and spraying temperature is decided to be 150 ℃, and pressure is 2.0MPa, and spray distance is 40mm, the thickness 1mm of varnish.
4. etch: etch 3s under the room temperature of hydrochloric acid 1% (weight concentration).After the taking-up, clean 1min with tap water immediately, use washed with de-ionized water 1min again.
5. chemical nickel phosphorus plating:
Chemical plating fluid is formed: basic nickel carbonate 15g/L, inferior sodium phosphate 20g/L, Trisodium Citrate 5g/L, matt salt 10g/L, sodium acetate 15g/L, thiocarbamide 4mg/L, oxysuccinic acid 6mg/L, ammoniacal liquor 15mL/L.The nickel chemical plating technology parameter is: service temperature is 85 ℃, and the electroless plating time is 30min, and the chemical plating thickness of acquisition is 8 μ m.
Bonding strength>the 30MPa of the compound coating that obtains by present embodiment, surperficial Vickers' hardness maximum can reach 800HV, and anti-neutral salt spray test reaches more than the 1500h.
Embodiment 4
Be with embodiment 1 difference:
1. material is prepared: after ZM6 magnesiumalloy cutting polishing, the polishing, in acetone soln, use the ultrasonic cleaning oil removing, then at deionized water for ultrasonic cleaning and removing organic matter removal and impurity.
2. plasma oxidation: in the electrolytic solution, sodium hydroxide 3g/L, water glass 20g/L, sodium phosphate 10g/L, all the other are water, temperature is 50 ℃; Adopt pulse mode to carry out oxidation, pulse-repetition is 1000Hz, and current density is 4A/dm 2, oxidization time is 90 minutes, and oxide thickness is 20 μ m, and this sull is a porous ceramic film, and porosity is 30%, the aperture is 3~8 μ m.
3. sealing: sealing treatment liquid is chromic anhydride 400g/L, and all the other are water, temperature: 50 ℃, and the time: 40min.After the taking-up, clean 2min with tap water immediately, use washed with de-ionized water 2min again.
4.ABS resin spraying: the specimen surface after the article on plasma oxidation carries out the ABS resin spraying, and spray coating liquor is formed: ABS resin 200g/L, solvent are DMSO 99.8MIN..Spraying parameter is: powder size is 400 orders, and spray pressure is 2.0MPa, and spray distance is 30mm, and the thickness of ABS resin coating is at 2mm.
5. chemical nickel phosphorus plating:
Chemical plating fluid is formed: basic nickel carbonate 10g/L, inferior sodium phosphate 20g/L, Trisodium Citrate 4g/L, matt salt 15g/L, sodium acetate 10g/L, thiocarbamide 2mg/L, oxysuccinic acid 6mg/L, ammoniacal liquor 20mL/L.The nickel chemical plating technology parameter is: service temperature is 85 ℃, and the electroless plating time is 50min, and the chemical plating thickness of acquisition is 8 μ m.
Bonding strength>the 50MPa of the compound coating that is obtained by present embodiment, surperficial Vickers' hardness maximum can reach 700HV, no peeling and bubbling phenomenon after 3.5%NaCl solution floating coat soaks 1000h.
Embodiment 5
Be with embodiment 2 differences:
1. material is prepared: after Mg-Gd-Y magnesiumalloy cutting polishing, the polishing, in acetone soln, use the ultrasonic cleaning oil removing, then at deionized water for ultrasonic cleaning and removing organic matter removal and impurity.
2. plasma oxidation: in the electrolytic solution, sodium hydroxide 3g/L, water glass 10g/L, sodium phosphate 10g/L, all the other are water, temperature is 50 ℃; Adopt pulse mode to carry out oxidation, pulse-repetition is 800Hz, and current density is 8A/dm 2, oxidization time is 100 minutes, and oxide thickness is 15 μ m, and this sull is a porous ceramic film, and porosity is 50%, the aperture is 6~10 μ m.
3. varnish spraying: the specimen surface after the article on plasma oxidation carries out the varnish spraying, and spray coating liquor is formed: varnish 150g/L, solvent are ether.Spraying parameter is: powder size is 300 orders, and spraying temperature is decided to be 200 ℃, and pressure is 2.0MPa, and spray distance is 20mm, and the thickness of varnish is at 3mm.
4. etch: etch 3s under the room temperature of hydrochloric acid 1% (weight concentration).After the taking-up, clean 1min with tap water immediately, use washed with de-ionized water 1min again.
5. chemical nickel phosphorus plating:
Chemical plating fluid is formed: basic nickel carbonate 12g/L, inferior sodium phosphate 25g/L, Trisodium Citrate 3g/L, matt salt 12g/L, sodium acetate 15g/L, thiocarbamide 2mg/L, oxysuccinic acid 5mg/L, ammoniacal liquor 10mL/L.The nickel chemical plating technology parameter is: service temperature is 90 ℃, and the electroless plating time is 50min, and the chemical plating thickness of acquisition is 10 μ m.
Bonding strength>the 35MPa of the compound coating that obtains by present embodiment, surperficial Vickers' hardness maximum can reach 950HV, and anti-neutral salt spray test reaches more than the 1500h.
Embodiment 6
Be with embodiment 1 difference:
1. material is prepared: after MB8 magnesiumalloy cutting polishing, the polishing, in acetone soln, use the ultrasonic cleaning oil removing, then at deionized water for ultrasonic cleaning and removing organic matter removal and impurity.
2. plasma oxidation: in the electrolytic solution, sodium hydroxide 3g/L, water glass 20g/L, sodium phosphate 10g/L, all the other are water, temperature is 50 ℃; Adopt pulse mode to carry out oxidation, pulse-repetition is 2000Hz, and current density is 5A/dm 2, oxidization time is 100 minutes, and oxide thickness is 30 μ m, and this sull is a porous ceramic film, and porosity is 60%, the aperture is 5~10 μ m.
3. sealing: sealing treatment liquid is chromic anhydride 400g/L, and all the other are water, temperature: 60 ℃, and the time: 50min.After the taking-up, clean 3min with tap water immediately, use washed with de-ionized water 3min again.
4.ABS resin spraying: the specimen surface after the article on plasma oxidation carries out the ABS resin spraying, and spray coating liquor is formed: ABS resin 200g/L, solvent are DMSO 99.8MIN..Spraying parameter is: powder size is 200 orders, and spray pressure is 2.5MPa, and spray distance is 30mm, and the thickness of ABS resin coating is at 5mm.
5. chemical nickel phosphorus plating:
Chemical plating fluid is formed: basic nickel carbonate 15g/L, inferior sodium phosphate 30g/L, Trisodium Citrate 3g/L, matt salt 15g/L, sodium acetate 10g/L, thiocarbamide 2mg/L, oxysuccinic acid 6mg/L, ammoniacal liquor 20mL/L.The nickel chemical plating technology parameter is: service temperature is 90 ℃, and the electroless plating time is 50min, and the chemical plating thickness of acquisition is 8 μ m.
Bonding strength>the 25MPa of the compound coating that obtains by present embodiment, surperficial Vickers' hardness maximum can reach 800HV, and anti-neutral salt spray test reaches more than the 1000h.

Claims (1)

1. magnesiumalloy plasma oxidation ceramic membrane surface preparation method of composite coating; It is characterized in that, at first Mg alloy surface is carried out the plasma anodic oxidation, form porous ceramic film at Mg alloy surface; Carry out organic coating again and apply, carry out chemical plating nickel-phosphorus then and handle;
After the polishing of magnesium alloy sample process, polishing, oil removing pre-treatment, then magnesium alloy sample is put into electrolytic solution as anode and adopt the high voltage pulse mode that sample is carried out plasma spark discharge oxidation;
The anodised electrolytic solution of said plasma is: sodium hydroxide 1~3g/L, and water glass 5~20g/L, sodium phosphate 5~10g/L, all the other are water, temperature is 0~50 ℃; Adopt pulse mode to carry out oxidation, pulse-repetition is 100~2000Hz, and current density is 1~10A/dm 2, oxidization time is 30~120 minutes, and oxide thickness is 5~40 μ m, and this sull is a porous ceramic film, and porosity is 30%~60%, the aperture is 3~10 μ m;
Said organic coating applies and adopts ABS resin to apply or the varnish coating;
Said ABS resin applies, and spray coating liquor is formed: ABS resin 150~250g/L, solvent are DMSO 99.8MIN.; Spraying parameter is: powder size is 200~400 orders, and spray pressure is 1.5~2.5MPa, and spray distance is 20~40mm, and the thickness of ABS resin coating is at 1~5mm;
By weight percentage, consisting of of ABS resin: vinyl cyanide accounts for 15%~35%, and divinyl accounts for 5%~30%, styrene comprise 40%~60%;
Said varnish applies, and spray coating liquor is formed: varnish 100~200g/L, solvent are ether; Spraying parameter is: powder size is 200~400 orders, and spraying temperature is decided to be 150~300 ℃, and pressure is 1.5~2.5MPa, and spray distance is 10~40mm, and the thickness of varnish is at 1~3mm;
Said varnish is meant acrylic varnish, and its weight consists of: TEB 3K 30~50%; NSC 20956 10%~30%; Methylacrylic acid copolymer resins 10%~30%; Nitro-cotton 5%~10%;
Said chemical plating fluid is formed: basic nickel carbonate 10~15g/L, inferior sodium phosphate 20~30g/L, Trisodium Citrate 3~5g/L, matt salt 10~15g/L, sodium acetate 10~15g/L, thiocarbamide 2~4mg/L, oxysuccinic acid 2~6mg/L, ammoniacal liquor 10~20mL/L; The nickel chemical plating technology parameter is: service temperature is 85~90 ℃, and the electroless plating time is 30~60min, and the chemical plating thickness of acquisition is 8~10 μ m.
CN201010165323A 2010-05-07 2010-05-07 Preparation method of composite coating on magnesium alloy plasma oxide ceramic surface Expired - Fee Related CN102234803B (en)

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