CN109183126A - A kind of preparation method of Mg alloy surface hydrophobic film layer - Google Patents
A kind of preparation method of Mg alloy surface hydrophobic film layer Download PDFInfo
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- CN109183126A CN109183126A CN201810910569.XA CN201810910569A CN109183126A CN 109183126 A CN109183126 A CN 109183126A CN 201810910569 A CN201810910569 A CN 201810910569A CN 109183126 A CN109183126 A CN 109183126A
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- magnesium alloy
- arc oxidation
- film layer
- sodium
- surface hydrophobic
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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
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/08—Anti-corrosive paints
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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
- C25D11/024—Anodisation under pulsed or modulated current or potential
-
- 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
Abstract
The invention discloses a kind of preparation methods of Mg alloy surface hydrophobic film layer.Firstly, being polished magnesium alloy substrate, being polished, being washed, oil removing, the pretreatment such as ultrasonic wave water washing；Then, differential arc oxidation liquid is prepared, differential arc oxidation is carried out to pretreated magnesium alloy and forms micro-arc oxidation films；Later, self assembly liquid is prepared, self assembly film forming is carried out to the magnesium alloy after differential arc oxidation；Solidify 1 ~ 2 hour at 80 DEG C finally, taking out magnesium alloy, obtains Mg alloy surface hydrophobic coating.Method of the invention is easy to operate, and prepared Mg alloy surface hydrophobic film layer is firmly combined with matrix, surfacing, roughness is small, electrochemical impedance with higher and lower corrosion electric current density, surface hydrophobic can preferably improve the corrosion resistance of magnesium alloy close to super-hydrophobic.
Description
Technical field
The invention belongs to metal material surface corrosion and protection field, in particular to a kind of Mg alloy surface hydrophobic film layer
Preparation method.
Background technique
Magnesium alloy is structural material most with prospects in non-ferrous metal, since it has very excellent characteristic,
Industrial every field suffers from extensive purposes.But the standard electrode potential of magnesium alloy is very negative, so that magnesium alloy
Corrosion resistance is very poor, to limit its application.Therefore, its corrosion resisting property is often improved by various process for treating surface.?
Mg alloy surface prepares hydrophobic film layer, and the functions such as antifouling, waterproof, automatically cleaning on the one hand can be played to Mg alloy surface；It is another
Aspect can then inhibit the corrosion of magnesium alloy, widen its application field.
Hydrophobic coating refers generally to coating of the coating surface to the static contact angle of water at 90 ° or more, super-hydrophobic coating
Generally refer to coating of the coating surface to the static contact angle of water at 150 ° or more.The super hydrophobic surface table in nature biotechnology
Reveal brilliant self-cleaning effect, such as lotus leaf surface.Since super-hydrophobic material has many unique surface propertys, such as certainly
Cleaning, anticorrosion, super-hydrophobic etc., therefore had potential application in many fields.Differential arc oxidization technique is due to its uniqueness
The advantages of become one of most promising process for treating surface of magnesium alloy.It is to develop in recent years that self-assembling technique, which prepares self-assembled film,
A kind of rapidly environmentally protective anti-corrosion method, and it has the characteristics that operating procedure is simple and environmentally-friendly.The application is sharp first
Porous micro-roughened surface is formed on magnesium alloy with differential arc oxidization technique, self-assembling technique is recycled, in its micro-rough
Iy self-assembled layer is formed on surface, obtained hydrophobic composite membrane layer is to the corrosion resisting property for improving magnesium alloy and expands answering for magnesium alloy
It is had great significance with range.
Summary of the invention
The object of the present invention is to provide a kind of preparation methods of Mg alloy surface hydrophobic film layer, to improve dredging for magnesium alloy
Aqueous and anticorrosion ability.
Specific steps are as follows:
(1) magnesium alloy is successively used to 280#, 600#, 800# and 1200# silicon carbide paper sanding and polishing step by step, is washed, then in alkali
It in property degreasing fluid oil removing 1 ~ 5 minute at 50 ~ 70 DEG C, then is washed respectively through hot water and cold water, then ultrasonic wave is clear in dehydrated alcohol
It washes 5 ~ 15 minutes, then ultrasonic cleaning 5 ~ 15 minutes in deionized water, is dried for standby at 50 DEG C；The alkaline degreasing formula of liquid
Are as follows: 10 ~ 30 g/L of sodium phosphate, 10 ~ 30 g/L of sodium hydroxide, 10 ~ 30 g/L of sodium carbonate.
It (2) will treated that magnesium alloy is put into carries out differential arc oxidation as anode in micro-arc oxidation electrolyte through step (1)
Processing, cathode is stainless steel, and using pulse differential arc oxidation mode, processing parameter is arranged are as follows: 180 ~ 220 volts of final voltage, oxygen
The change time 30 ~ 40 minutes, 50 ~ 200 hertz of pulse frequency, 30 ~ 70 % of duty ratio；After differential arc oxidation, by steaming used for magnesium alloy
Distilled water flushing is placed in drying for standby in 50 DEG C of convection oven；The Microarc oxidation electrolyte formula are as follows: 4 ~ 6 g/ of sodium metasilicate
L, 8 ~ 10 g/L of sodium fluoride, 10 ~ 12 g/L of sodium hydroxide.
(3) 40:5:5 takes dehydrated alcohol, hexadecyl trimethoxy silane and distilled water abundant in beaker by volume
Mixing, is put into magnetic stirring apparatus for beaker, moderate-speed mixer 2 hours at 40 ~ 70 DEG C, and standing about 2 hours spare.It will be through step
(2) magnesium alloy after micro-arc oxidation treatment is put into self assembly liquid, is taken out after impregnating 10 ~ 50 minutes at 40 ~ 70 DEG C, with distillation
Water rinses out extra self assembly solution, is then placed in air dry oven, in 80 DEG C progress curing process 1 ~ 2 hour, that is, make
Obtain Mg alloy surface hydrophobic film layer.
The sodium phosphate, sodium carbonate, sodium hydroxide, dehydrated alcohol, sodium metasilicate, sodium fluoride and hexadecyl trimethoxy silicon
Alkane is the chemical pure and above purity.
Method of the invention is easy to operate, and prepared Mg alloy surface hydrophobic film layer is firmly combined with matrix, and surface is flat
Whole, roughness is small, electrochemical impedance with higher and lower corrosion electric current density, and surface hydrophobic is close to super-hydrophobic, energy
Enough preferable corrosion resistances for improving magnesium alloy.
Detailed description of the invention
Fig. 1 is the SEM figure of the Mg alloy surface hydrophobic film layer of preparation of the embodiment of the present invention.
Fig. 2 is the contact angle test figure of the Mg alloy surface hydrophobic film layer of preparation of the embodiment of the present invention.
Fig. 3 is the Tafel polarization curve of the Mg alloy surface hydrophobic film layer of preparation of the embodiment of the present invention.
Fig. 4 is the AC impedance figure of the Mg alloy surface hydrophobic film layer of preparation of the embodiment of the present invention.
Specific embodiment
Embodiment:
(1) AZ91 magnesium alloy is successively used into 280#, 600#, 800# and 1200# silicon carbide paper sanding and polishing step by step, washed, then
The oil removing 1 minute in 60 DEG C of alkaline degreasing liquid, then washed respectively through hot water and cold water, the then ultrasonic cleaning in dehydrated alcohol
It is dried for standby at 10 minutes, then ultrasonic cleaning 10 minutes in deionized water, 50 DEG C；The alkaline degreasing formula of liquid are as follows: phosphorus
Sour sodium 20g/L, sodium hydroxide 20g/L, sodium carbonate 20g/L.
It (2) will treated that AZ91 magnesium alloy is put into carries out the differential of the arc as anode in micro-arc oxidation electrolyte through step (1)
Oxidation processes, cathode are stainless steel, and using pulse differential arc oxidation mode, processing parameter is arranged are as follows: 200 volts of final voltage, oxygen
The change time 30 minutes, 50 hertz of pulse frequency, duty ratio 30%；After differential arc oxidation, by AZ91 distilled water flushing used for magnesium alloy
It is placed in drying for standby in 50 DEG C of convection oven；The Microarc oxidation electrolyte formula are as follows: 5 g/L of sodium metasilicate, sodium fluoride 8
G/L, 10 g/L of sodium hydroxide.
(3) 40:5:5 takes dehydrated alcohol, hexadecyl trimethoxy silane and distilled water abundant in beaker by volume
It mixes, moderate-speed mixer 2 hours at 60 DEG C, standing about 2 hours spare.It will be through the AZ91 magnesium after step (2) micro-arc oxidation treatment
Alloy is put into self assembly liquid, is impregnated at 60 DEG C and is taken out after ten minutes, extra self assembly solution is fallen with distilled water flushing, so
After be put into air dry oven, in 80 DEG C progress curing process 1 hour, obtain Mg alloy surface hydrophobic film layer.
The sodium phosphate, sodium carbonate, sodium hydroxide, dehydrated alcohol, sodium metasilicate, sodium fluoride and hexadecyl trimethoxy silicon
Alkane is that chemistry is pure.
Mg alloy surface hydrophobic film layer thickness made from the present embodiment is about 16 μm, shows film layer table by SEM
Face is smooth.The roughness for showing film layer by roughness test is 0.348 μm, thick less than magnesium alloy surface micro-arc oxidation film
0.453 μm of rugosity.The contact angle for showing film layer by contact angle test is 145.07 °, and hydrophobicity is preferable, close to super-hydrophobic.
The test of electrochemistry corrosion resisting property is carried out to hydrophobic film layer made from the present embodiment, (there is hydrophobic film layer using three-electrode system
Magnesium alloy sample is Electrode, and platinum electrode is auxiliary electrode, and saturated calomel electrode is reference electrode), corrosive medium is quality
The NaCl solution that percent concentration is 3.5%.The electrochemical impedance of the present embodiment Mg alloy surface hydrophobic film layer obtained reaches
2.00×106Ω·cm2More than, than the electrochemical impedance 5.75 × 10 of AZ91 magnesium alloy substrate2 Ω·cm2, increase four numbers
Magnitude, the corrosion electric current density of Mg alloy surface hydrophobic film layer are 1.314 × 10-8A/cm2, than the corrosion current of magnesium alloy substrate
Density 1.951 × 10-5A/cm2, reduce three orders of magnitude, it will be apparent that improve the corrosion resisting property of magnesium alloy.
Claims (1)
1. a kind of preparation method of Mg alloy surface hydrophobic film layer, it is characterised in that specific steps are as follows:
(1) magnesium alloy is successively used to 280#, 600#, 800# and 1200# silicon carbide paper sanding and polishing step by step, is washed, then in alkali
It in property degreasing fluid oil removing 1 ~ 5 minute at 50 ~ 70 DEG C, then is washed respectively through hot water and cold water, then ultrasonic wave is clear in dehydrated alcohol
It washes 5 ~ 15 minutes, then ultrasonic cleaning 5 ~ 15 minutes in deionized water, is dried for standby at 50 DEG C；The alkaline degreasing formula of liquid
Are as follows: 10 ~ 30 g/L of sodium phosphate, 10 ~ 30 g/L of sodium hydroxide, 10 ~ 30 g/L of sodium carbonate；
It (2) will treated that magnesium alloy is put into carries out at differential arc oxidation in micro-arc oxidation electrolyte as anode through step (1)
Reason, cathode is stainless steel, and using pulse differential arc oxidation mode, processing parameter is arranged are as follows: 180 ~ 220 volts of final voltage, oxidation
Time 30 ~ 40 minutes, 50 ~ 200 hertz of pulse frequency, 30 ~ 70 % of duty ratio；After differential arc oxidation, by distillation used for magnesium alloy
Water flushing is placed in drying for standby in 50 DEG C of convection oven；The Microarc oxidation electrolyte formula are as follows: 4 ~ 6 g/L of sodium metasilicate,
8 ~ 10 g/L of sodium fluoride, 10 ~ 12 g/L of sodium hydroxide；
(3) 40:5:5 takes dehydrated alcohol, hexadecyl trimethoxy silane and distilled water sufficiently mixed in beaker by volume
It closes, beaker is put into magnetic stirring apparatus, moderate-speed mixer 2 hours at 40 ~ 70 DEG C, standing about 2 hours spare；It will be through step
(2) magnesium alloy after micro-arc oxidation treatment is put into self assembly liquid, is taken out after impregnating 10 ~ 50 minutes at 40 ~ 70 DEG C, with distillation
Water rinses out extra self assembly solution, is then placed in air dry oven, in 80 DEG C progress curing process 1 ~ 2 hour, that is, make
Obtain Mg alloy surface hydrophobic film layer；
The sodium phosphate, sodium carbonate, sodium hydroxide, dehydrated alcohol, sodium metasilicate, sodium fluoride and hexadecyl trimethoxy silane are equal
For the chemical pure and above purity.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110541099A (en) * | 2019-07-02 | 2019-12-06 | 山东大学 | Magnesium alloy surface degradable composite film layer and preparation method and application thereof |
| CN110552043A (en) * | 2019-09-26 | 2019-12-10 | 长安大学 | high-corrosion-resistance magnesium alloy hub surface treatment method |
| CN110923781A (en) * | 2019-12-13 | 2020-03-27 | 湖南湘投金天科技集团有限责任公司 | Surface treatment method for reducing galvanic current of titanium and titanium alloy |
| CN112323116A (en) * | 2020-11-06 | 2021-02-05 | 中国石油大学(华东) | Preparation method of magnesium alloy super-hydrophobic coating based on zeolite imidazole ester framework |
| CN112342590A (en) * | 2020-10-20 | 2021-02-09 | 桂林理工大学 | Preparation method of super-hydrophobic colored film on surface of aluminum alloy |
| CN115807213A (en) * | 2023-02-08 | 2023-03-17 | 潍坊科技学院 | Magnesium alloy surface super-hydrophobic composite film layer and preparation method thereof |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110541099A (en) * | 2019-07-02 | 2019-12-06 | 山东大学 | Magnesium alloy surface degradable composite film layer and preparation method and application thereof |
| CN110541099B (en) * | 2019-07-02 | 2021-04-06 | 山东大学 | Magnesium alloy surface degradable composite film layer and preparation method and application thereof |
| CN110552043A (en) * | 2019-09-26 | 2019-12-10 | 长安大学 | high-corrosion-resistance magnesium alloy hub surface treatment method |
| CN110552043B (en) * | 2019-09-26 | 2022-02-22 | 长安大学 | High-corrosion-resistance magnesium alloy hub surface treatment method |
| CN110923781A (en) * | 2019-12-13 | 2020-03-27 | 湖南湘投金天科技集团有限责任公司 | Surface treatment method for reducing galvanic current of titanium and titanium alloy |
| CN110923781B (en) * | 2019-12-13 | 2021-09-07 | 湖南湘投金天科技集团有限责任公司 | Surface treatment method for reducing galvanic current of titanium and titanium alloy |
| CN112342590A (en) * | 2020-10-20 | 2021-02-09 | 桂林理工大学 | Preparation method of super-hydrophobic colored film on surface of aluminum alloy |
| CN112323116A (en) * | 2020-11-06 | 2021-02-05 | 中国石油大学(华东) | Preparation method of magnesium alloy super-hydrophobic coating based on zeolite imidazole ester framework |
| CN112323116B (en) * | 2020-11-06 | 2022-02-11 | 中国石油大学(华东) | Preparation method of magnesium alloy super-hydrophobic coating based on zeolite imidazole ester framework |
| CN115807213A (en) * | 2023-02-08 | 2023-03-17 | 潍坊科技学院 | Magnesium alloy surface super-hydrophobic composite film layer and preparation method thereof |
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