CN110512265A - A kind of magnesium alloy surface composite film and preparation method thereof - Google Patents
A kind of magnesium alloy surface composite film and preparation method thereof Download PDFInfo
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- CN110512265A CN110512265A CN201910966943.2A CN201910966943A CN110512265A CN 110512265 A CN110512265 A CN 110512265A CN 201910966943 A CN201910966943 A CN 201910966943A CN 110512265 A CN110512265 A CN 110512265A
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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
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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
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D15/00—Electrolytic or electrophoretic production of coatings containing embedded materials, e.g. particles, whiskers, wires
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Abstract
The invention discloses a kind of magnesium alloy surface composite film preparation methods, belong to technical field of surface, comprising the following steps: prepare oxidation electrolyte；Magnesium alloy is reacted with the oxidation electrolyte in the case where voltage magnitude is the nanosecond pulse of 500 ~ 800V；The oxidation electrolyte includes: meta-aluminate or phosphate, highly basic, nano yttrium oxide powder and Neon SiC powder.The preparation method of composite membrane provided by the invention, preparation process is more environmentally-friendly, and simple process is at low cost.The present invention also provides a kind of magnesium alloy surface composite films, are made using the above method, can wear-resistance and anti-corrosion.
Description
Technical field
The present invention relates to a kind of magnesium alloy surface composite films and preparation method thereof, belong to technical field of surface.
Background technique
Magnesium alloy has the features such as specific strength, specific stiffness are high, and high damping vibration attenuation is good.However magnesium alloy is because of its intrinsic change
Learning property causes to easily corrode, and anti-corrosion just becomes the important topic of its surface treatment.
The preparation method (Chinese Patent Application No.: CN201510749871.8) of existing magnesium alloy surface composite film, first
Magnesium alloy is subjected to chemical plating in containing nickel plating bath, then carries out electricity in containing cerous nitrate and stearic sewage electric depositing solution and sinks
Product reaction, although this method has obtained a kind of super-hydrophobic composite film, but due to wherein having used heavy metal solution, make
At the pollution of environment.
The preparation method (Chinese Patent Application No.: CN201610178062.0) of existing magnesium alloy surface composite film is right
Mg alloy surface carries out differential arc oxidation and organic film plating, but such method yield rate is low, at high cost, easily leads to the precision of workpiece
It reduces.
Summary of the invention
The present invention is to provide a kind of preparation method of magnesium alloy surface composite film, and preparation process is more environmentally-friendly, and technique letter
It is single at low cost.
In order to achieve the above objectives, the technical scheme adopted by the invention is that:
A kind of preparation method of magnesium alloy surface composite film, comprising the following steps: prepare oxidation electrolyte；By magnesium alloy with it is described
Oxidation electrolyte is reacted in the case where voltage magnitude is the nanosecond pulse of 500 ~ 800V；The oxidation electrolyte includes: meta-aluminic acid
Salt or phosphate, highly basic, nano yttrium oxide powder and Neon SiC powder.
Further, the meta-aluminate or phosphate are calgon or sodium aluminate, and weight is 47 ~ 57 parts.
Further, the highly basic is sodium hydroxide or potassium hydroxide, and weight is 20 ~ 30 parts.
Further, the nano yttrium oxide powder weight is 1 part, and the Neon SiC powder weight is 1 part.
Further, the oxidation electrolyte further includes glycerine or triethanolamine weight is 20 ~ 30 parts.
Further, described to prepare oxidation electrolyte the following steps are included: by nano yttrium oxide powder and nanometer silicon carbide
Powder is placed in hydrofluoric acid solution；It is activated 1-3 minutes with ultrasonic disperse；Then dispersing agent is added and continues dispersion activation 1-3 minutes
Obtain nano yttrium oxide and nanometer silicon carbide solution；Meta-aluminate or phosphate are first added in a reservoir, adds highly basic, finally
Scattered nano yttrium oxide and nanometer silicon carbide solution is taken to be added to obtain oxidation electrolyte.
Further, the dispersing agent is tetramethylammonium hydroxide, and weight is 1 part.
Further, the pulsewidth of the nanosecond pulse is 10 ~ 100ns.
Further, the discharge time of the nanosecond pulse is 1 ~ 2 min.
A kind of preparation method of magnesium alloy surface composite film provided by the invention, the processing of all material is in normal temperature condition
Lower progress, thus the speed that composite membrane is made is fast, the time is short, simplifies treatment process, reduces costs well.This method
Oxidation electrolyte is free of heavy metal, thus the influence to environment is small.
Nano yttrium oxide powder and Neon SiC powder are added in oxidation electrolyte, polarized electronegative ion is logical
Plasma electrochemical reaction is crossed, point discharge position is adsorbed in, by the hole of plasma high-temperature sintering filling and film layer
And by sintering, the porosity of film layer is reduced, the anticorrosion wear-resisting property of film layer is improved.
The present invention also provides a kind of magnesium alloy surface composite films, can wear-resistance and anti-corrosion.
In order to achieve the above objectives, the technical scheme adopted by the invention is that: a kind of magnesium alloy surface composite film, use are above-mentioned
Method is made.
The treatment fluid is more stable in oxidation processes, almost without deposition, realizes nano particle at oxidation
Being uniformly distributed during reason.The composite membrane realizes the Even Sintering of nano particle, compound process, solves magnesium alloy table
Corrosion resistance caused by surface oxidation film voidage is excessively high and wear resistance decrease problem, improve wearability and corrosion resistance.
Specific embodiment
Essence in order to better understand the present invention, the invention will be further elaborated combined with specific embodiments below.
Part below is poidometer.
Embodiment one
Nano yttrium oxide powder and Neon SiC powder weight ratio are mixed for 1:1, take wherein 1 liter of 10g merging of 2% hydrogen fluorine
It in acid solution, is activated 1-3 minute with ultrasonic disperse, adds 10 immediately plus 1 liter of deionized water with deionized water filtering cleaning
Milliliter dispersing agent continues ultrasonic disperse activation and obtains nano yttrium oxide and nanometer silicon carbide solution in 1-3 minutes.Dispersing agent is preferably
Tetramethylammonium hydroxide.2/3 distilled water is taken in a 10L slot, successively dissolves 4700g calgon and 3000g the third three
Alcohol waits in slots reagent all after dissolution, 3000g potassium hydroxide is poured under fast stirring in tank liquor and is uniformly mixed, finally
It takes scattered nano yttrium oxide and 1 liter of nanometer silicon carbide solution is poured into slot, until being mixed thoroughly, finally add water to
10L obtains oxidation electrolyte.
Magnesium alloy AZ31 part is put into prepared oxidation electrolyte, using magnesium alloy as anode, graphite is cathode, is received
Pulse per second (PPS) pulsewidth is 10 ns, pulse voltage amplitude 800V, pulsed discharge 1 minute, i.e. realization magnesium alloy AZ31 surface abrasion resistance
The preparation of anticorrosion composite film.
As shown in table 1, the more existing normal film wear-and corrosion-resistant corrosion of composite membrane improves.
Table 1
| Sample classification | Weight/g before testing | Weight/g after experiment | Weight loss/g |
| Matrix | 0.9302 | 0.9277 | 0.0025 |
| Embodiment one | 0.9284 | 0.9275 | 0.0009 |
| Common composite membrane | 0.9233 | 0.9221 | 0.0012 |
Embodiment two
Nano yttrium oxide powder and Neon SiC powder weight ratio are mixed for 1:1 first, take the 2% of wherein 1 liter of 10g merging
It in hydrofluoric acid solution, is activated 1 minute with ultrasonic disperse, is filtered and cleaned with deionized water, immediately plus 1 liter of deionized water, added
10 milliliters of dispersing agent tetramethylammonium hydroxide continue to obtain nano yttrium oxide and nanometer silicon carbide solution in ultrasonic disperse 3 minutes.In
The deionized water that 2/3 is taken in one 10L slot, the 5700g hexamethyl cyclotrisiloxane and 2000g triethanolamine successively dissolved, etc.
After reagent all dissolves in slot, 2000g sodium hydroxide is poured into tank liquor under fast stirring, finally takes scattered nanometer
Yttrium oxide and 1 liter of nanometer silicon carbide solution pour into slot until be mixed thoroughly, and finally add water to 10L and obtain oxidization electrolysis
Liquid.
Magnesium alloy ZK60 part is put into prepared oxidation electrolyte, using ZK60 part as anode, graphite is cathode, nanosecond
Pulse is 100 ns, pulse voltage amplitude 800V, aoxidizes compound 1 minute, i.e. realization ZK60 using micro arc plasma body
The preparation of part surface abrasion resistance anticorrosion composite film.
As shown in table 2, the more existing normal film wear-and corrosion-resistant corrosion of composite membrane improves.
Table 2
| Sample classification | Weight/g before testing | Weight/g after experiment | Weight loss/g |
| Matrix | 0.9315 | 0.9285 | 0.0030 |
| Embodiment one | 0.9303 | 0.9290 | 0.0013 |
| Common composite membrane | 0.9263 | 0.9244 | 0.0019 |
Embodiment three
Nano yttrium oxide powder and Neon SiC powder weight ratio are mixed for 1:1 first, take the 2% of wherein 1 liter of 10g merging
It in hydrofluoric acid solution, is activated 2 minutes with ultrasonic disperse, is filtered and cleaned with deionized water, immediately plus 1 liter of deionized water, added
10 milliliters of dispersing agent tetramethylammonium hydroxide continuation ultrasonic disperses activation obtain nano yttrium oxide in 2 minutes and nanometer silicon carbide is molten
Liquid.2/3 distilled water is taken in a 10L slot, is successively dissolved 5200g calgon and 2500g glycerine, is waited reagent in slots
All after dissolution, 2500g potassium hydroxide is poured into tank liquor under fast stirring, until be mixed thoroughly, is finally taken point
The nano yttrium oxide dissipated and 1 liter of nanometer silicon carbide solution pour into slot, add water to 10L and obtain oxidation electrolyte.
Magnesium alloy AZ31B part is put into prepared oxidation electrolyte, using AZ31B as anode, graphite is cathode, nanosecond
Pulse is 50 ns, pulse voltage amplitude 700V, aoxidizes compound 2 minutes, i.e. realization AZ31B using micro arc plasma body
The preparation of surface abrasion resistance anticorrosion composite film.
As shown in table 3, the more existing normal film wear-and corrosion-resistant corrosion of composite membrane improves.
Table 3
| Sample classification | Weight/g before testing | Weight/g after experiment | Weight loss/g |
| Matrix | 0.9258 | 0.9235 | 0.0023 |
| Embodiment one | 0.9217 | 0.9210 | 0.0007 |
| Common composite membrane | 0.9194 | 0.9184 | 0.0010 |
Although should be pointed out that invention has been described by above embodiment, the present invention can also have other a variety of
Embodiment.Without departing from the spirit and scope of the present invention, those skilled in the art obviously can be to this hair
It is bright to make various corresponding changes and modifications, but these change and modification all should belong to appended claims of the present invention and its wait
In the range of effect object is protected.
Claims (10)
1. a kind of preparation method of magnesium alloy surface composite film, which comprises the following steps: prepare oxidation electrolyte；
Magnesium alloy is reacted with the oxidation electrolyte in the case where voltage magnitude is the nanosecond pulse of 500 ~ 800V；
The oxidation electrolyte includes: meta-aluminate or phosphate, highly basic, nano yttrium oxide powder and Neon SiC powder.
2. the preparation method of magnesium alloy surface composite film according to claim 1, it is characterised in that: the meta-aluminate is six
Sodium metaphosphate, the phosphate are sodium aluminate, and the weight of calgon or sodium aluminate is 47 ~ 57 parts.
3. the preparation method of magnesium alloy surface composite film according to claim 1, it is characterised in that: the highly basic is hydroxide
Sodium or potassium hydroxide, weight are 20 ~ 30 parts.
4. the preparation method of magnesium alloy surface composite film according to claim 1, it is characterised in that: the yttria nanopowders
Last weight is 1 part, and the Neon SiC powder weight is 1 part.
5. the preparation method of magnesium alloy surface composite film according to claim 1, it is characterised in that: the oxidation electrolyte is also
It is 20 ~ 30 parts including glycerine or triethanolamine weight.
6. the preparation method of magnesium alloy surface composite film according to claim 1, it is characterised in that: described to prepare oxidization electrolysis
Liquid the following steps are included:
It will be in nano yttrium oxide powder and Neon SiC powder merging hydrofluoric acid solution；It is activated 1-3 minutes with ultrasonic disperse；So
Dispersing agent is added afterwards to continue to disperse to activate 1-3 minutes to obtain nano yttrium oxide and nanometer silicon carbide solution；It is first added in a reservoir
Meta-aluminate or phosphate, add highly basic, and scattered nano yttrium oxide and nanometer silicon carbide solution is finally taken to be added to obtain
Oxidation electrolyte.
7. the preparation method of magnesium alloy surface composite film according to claim 6, it is characterised in that: the dispersing agent is tetramethyl
Base ammonium hydroxide, weight are 1 part.
8. the preparation method of magnesium alloy surface composite film according to claim 1, it is characterised in that: the arteries and veins of the nanosecond pulse
Width is 10 ~ 100ns.
9. the preparation method of magnesium alloy surface composite film according to claim 1, it is characterised in that: the nanosecond pulse is put
The electric time is 1 ~ 2 min.
10. a kind of magnesium alloy surface composite film wants 1 to 9 any one method to be made using right.
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| CN111172577A (en) * | 2020-01-29 | 2020-05-19 | 桂林理工大学 | Preparation method of magnesium alloy surface low-porosity micro-arc oxidation film |
| CN114703529A (en) * | 2022-04-06 | 2022-07-05 | 内蒙古工业大学 | Magnesium alloy with super-hydrophobic MAO-LDH composite membrane layer and preparation method thereof |
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| CN114703529B (en) * | 2022-04-06 | 2023-12-08 | 内蒙古工业大学 | Magnesium alloy with super-hydrophobic MAO-LDH composite membrane layer and preparation method thereof |
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