CN110016707A - The preparation method of magnesium alloy differential arc oxidation method and differential arc oxidation iron content electrolyte - Google Patents
The preparation method of magnesium alloy differential arc oxidation method and differential arc oxidation iron content electrolyte Download PDFInfo
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- CN110016707A CN110016707A CN201910372634.2A CN201910372634A CN110016707A CN 110016707 A CN110016707 A CN 110016707A CN 201910372634 A CN201910372634 A CN 201910372634A CN 110016707 A CN110016707 A CN 110016707A
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- arc oxidation
- differential arc
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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
- C25D11/026—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
- C25D11/30—Anodisation of magnesium or alloys based thereon
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Abstract
A kind of preparation method of magnesium alloy differential arc oxidation method and differential arc oxidation iron content electrolyte.Magnesium alloy differential arc oxidation includes three pre-treatment, differential arc oxidation and post-processing steps.Differential arc oxidation iron content electrolyte component includes the following: phosphate 10-60g/L, highly basic 1-6g/L, complexing agent 2-10g/L, iron content electrolyte 5-20g/L.The complexing agent is K-IAO, triethanolamine or sorbierite, and iron content electrolyte is potassium ferric oxalate, ironic citrate or ferrous sulfate.The electrolyte stability is good, and solution still keeps stabilization not generate precipitating under alkaline environment.The present invention replaces traditional toxic cyanide using organic complexing agent, and component is simple, at low cost, easily prepared, long service life, and environmental pollution is small.Micro-arc oxidation treatment is carried out to magnesium alloy using the electrolyte, iron content black coating, uniform coating thickness can be made in Mg alloy surface, surface is smooth, with good uniformity and compactness, raw material used by this method are easy to get, and are suitble to large-scale industrial production.
Description
Technical field
The invention belongs to Mg alloy surface process fields, more particularly, to a kind of magnesium alloy differential arc oxidation method and magnesium alloy
The preparation method of differential arc oxidation iron content electrolyte.
Background technique
Magnesium alloy is with density is low, specific strength is high, good thermal conductivity and electromagnetic shielding characteristic, magnesium-alloy material easily recycle
The features such as recycling and no pollution to the environment, it is referred to as by people " green engineering material " of 21 century, but magnesium alloy has
There is higher chemical activity, it can be by serious chemical attack, greatly in wet air, sulfur-bearing atmosphere and marine atmosphere
Ground limits magnesium alloy in the extensive use of engineering field.Therefore, various surface treatments and process for modifying surface, such as differential of the arc oxygen
Change, chemical conversion, organic coating such as coat of metal etc. is by development and application in Mg alloy surface to improve its corrosion resistance.
Differential arc oxidation (MAO) is that mention magnesium alloy be to improve the important surface treatment means of corrosion stability of magnesium alloy, because it has
Similar to the crystal structure of ceramics, also referred to as ceramic membrane.The differential arc oxidation film layer of magnesium alloy can greatly improve the anti-corrosion of magnesium alloy
Property, the performances such as wearability and insulating properties, and film layer is the growth in situ on matrix, is metallurgical bonding with matrix surface, in conjunction with
Power is strong, dense uniform, can fundamentally solve defect of the magnesium alloy as structural material, while the differential of the arc film coloured also has
Certain dicoration, thermal control have wide development space.
It can assign coating different colors by adding coloring salt in microarc oxidation solution, such as addition potassium permanganate can
Yellow differential arc oxidation coating is prepared, addition potassium fluotitanate can prepare grey differential arc oxidation coating etc..Black differential arc oxidation is applied
Layer reports that most is addition vanadate, however vanadate strong toxicity, environmental pollution are larger.
Summary of the invention
In consideration of it, it is an object of that present invention to provide a kind of magnesium alloy differential arc oxidation methods and magnesium alloy differential arc oxidation to contain ferroelectricity
The preparation method of liquid is solved, to prepare magnesium alloy black differential arc oxidation coating.
A kind of magnesium alloy differential arc oxidation method, it is characterised in that include the following steps:
1) pre-treatment: polishing to magnesium alloy, alkali cleaning, dry；Soda-wash solution is 30~60g/L, ten phosphate dihydrate sodium,
20~80g/L sodium hydroxide, 0.7~1.5ml/L OP-10 wetting agent, solution-operated temperature are 60~80 DEG C, the processing time 8~
15min；
2) differential arc oxidation: the good magnesium alloy of pre-treatment is immersed in differential arc oxidation iron content electrolyte, dual-pulse power supply is used
Carry out micro-arc oxidation treatment；
3) it post-processes: the magnesium alloy sample after differential arc oxidation is rinsed, it is dry.
Further, influence of the aluminum conductor starting the arc to micro-arc oxidation process in order to prevent, the present invention is using threaded connection
Mode stamps threaded hole on the magnesium alloy, magnesium alloy is made to be connected with aluminum conductor, remaining position of aluminum conductor is used in connection, especially
It is and liquid level of electrolyte is with lower portion, and aluminum conductor is isolated with electrolyte using insulated hull, avoids aluminum conductor from generating the starting the arc existing
As.Ultrapure water used for magnesium alloy or deionized water after differential arc oxidation rinse, then heated-air drying.
Further, differential arc oxidation selects constant voltage mode, positive voltage 300-450V, negative voltage 20-60V, positive and negative arteries and veins
Punching is than being 1:1, frequency 50-400Hz, positive negative duty identical 8%-30%, oxidization time 10-20min, and electrolyte temperature is protected
It holds at 30-35 DEG C.
Further, with a thickness of 30-60um, ferro element uniformly divides obtained differential arc oxidation magnesium alloy coating on coating
Cloth, differential arc oxidation coating color are black.
A kind of preparation method for the iron content electrolyte that magnesium alloy differential arc oxidation method as described above uses, electrolyte use are
Deionized water or ultrapure aqueous solvent, micro-arc oxidation electrolyte pH value are 12-13, and electrolyte includes following ingredient: phosphate 10-
60g/L, highly basic 1-6g/L, complexing agent 2-10g/L, iron content electrolyte 5-20g/L.
Further, phosphate described in electrolyte is sodium phosphate, ammonium phosphate or calgon.
Further, complexing agent described in electrolyte is K-IAO, triethanolamine or sorbierite.
Further, iron content electrolyte described in electrolyte is potassium ferric oxalate, ironic citrate or ferrous sulfate.
Further, highly basic described in electrolyte is sodium hydroxide or potassium hydroxide.
Using magnesium alloy differential arc oxidation film layer made from differential arc oxidation iron content electrolyte of the invention and micro-arc oxidation process,
Compactness extent is high, and surface is smooth, and color is uniform, has ceramic appearance, and oxidation film layer has good cause with a thickness of 30-60um
Close property and uniformity.
Detailed description of the invention:
Fig. 1 is micro-arc oxidation device schematic diagram of the present invention,
Fig. 2 is the differential arc oxidation film layer SEM schematic diagram that embodiment 1 obtains,
Fig. 3 is the differential arc oxidation film layer XRD diagram that embodiment 1 obtains,
Fig. 4 is the differential arc oxidation film layer SEM schematic diagram that embodiment 2 obtains,
Fig. 5 is the differential arc oxidation film layer XRD diagram that embodiment 2 obtains.
Specific embodiment:
Embodiment 1:
Sample is MB2 magnesium alloy, and size is the cuboid of 40 × 40 × 10mm, concrete operation step are as follows:
1. pair MB2 magnesium alloy carries out surface mechanical pretreatment: using 240#, 400#, 600#, 1200# sand paper is successively to MB2
Magnesium alloy is polished, and to remove the impurity such as its surface spikes, oxide, is made surface-brightening, is then washed.
2. alkali cleaning: using ten phosphate dihydrate sodium of 35g/L, 30g/L sodium hydroxide, 0.8ml/L OP-10 wetting agent configures alkali
Washing lotion, control temperature is maintained at 70 DEG C in alkaline cleaning procedure, and alkali cleaning handles time 10min, then washes, dry.
3. the configuration of differential arc oxidation iron content electrolyte: use 40g/L sodium phosphate, 5g/L sorbierite, 15g/L ferrous sulfate,
It is dissolved in ultrapure water, is then stirred using mechanical agitator to being completely dissolved, is configured differential arc oxidation iron content electrolyte 10L, then make
Electrolyte pH to 12-13 is adjusted with potassium hydroxide.
4. differential arc oxidation: the MB2 magnesium alloy after pre-treatment threadedly being connect with aluminum conductor, is then immersed in
It states in configured differential arc oxidation iron content electrolyte, adjusting mao power source is constant voltage mode, forward voltage 360V, negative sense
Voltage 45V, positive negative pulse stuffing ratio are 1:1, frequency 350Hz, and positive negative duty is 13%, and oxidization time 12min uses cooling
Electrolyte temperature is maintained at 30-35 DEG C by device.
5. post-processing: well-oxygenated sample being taken out, clean with ultrapure water, then hot-air seasoning, can be obtained thickness
Degree is the magnesium alloy differential arc oxidation black coating of 38um or so.
The black differential arc oxidation film layer that embodiment 1 is obtained carries out SEM and XRD test, as a result as shown in Figure 2,3.
Embodiment 2:
Sample is ZK61M magnesium alloy, and size is the cuboid of 30 × 20 × 7mm, concrete operation step are as follows:
1. pair ZK61M magnesium alloy carries out surface mechanical pretreatment: using 240#, 400#, 600#, 1200# sand paper is successively right
ZK61M magnesium alloy is polished, and to remove the impurity such as its surface spikes, oxide, is made surface-brightening, is then washed.
2. alkali cleaning: using ten phosphate dihydrate sodium of 30g/L, 40g/L sodium hydroxide, 1ml/L OP-10 wetting agent configures alkali cleaning
Liquid, control temperature is maintained at 75 DEG C in alkaline cleaning procedure, and alkali cleaning handles time 8min, then washes, dry.
3. the configuration of differential arc oxidation iron content electrolyte: using 35g/L calgon, 5g/L K-IAO, 10g/L lemon
Lemon acid iron, is dissolved in ultrapure water, is then stirred using mechanical agitator to being completely dissolved, configures differential arc oxidation 10L containing electrolytic iron, so
Electrolyte pH to 12-13 is adjusted using sodium hydroxide afterwards.
4. differential arc oxidation: the ZK61M magnesium alloy after pre-treatment threadedly being connect with aluminum conductor, is then immersed in
In above-mentioned configured differential arc oxidation iron content electrolyte, adjusting mao power source is constant voltage mode, and forward voltage 400V is born
To voltage 40V, positive negative pulse stuffing ratio is 1:1, frequency 280Hz, positive negative duty identical 10%, oxidization time 12min, and use is cold
But electrolyte temperature is maintained at 30-35 DEG C by device.
5. post-processing: well-oxygenated sample being taken out, clean with ultrapure water, then hot-air seasoning, can be obtained thickness
Degree is the magnesium alloy differential arc oxidation black coating of 45um or so.
The black differential arc oxidation film layer that embodiment 2 is obtained carries out SEM and XRD test, as a result as shown in Figure 4,5.
Claims (9)
1. a kind of magnesium alloy differential arc oxidation method, it is characterised in that include the following steps:
1) pre-treatment: polishing to magnesium alloy, alkali cleaning, dry；Soda-wash solution be 30~60g/L, ten phosphate dihydrate sodium, 20~
80g/L sodium hydroxide, 0.7~1.5ml/L OP-10 wetting agent, solution-operated temperature are 60~80 DEG C, the processing time 8~
15min；
2) differential arc oxidation: the good magnesium alloy of pre-treatment is immersed in differential arc oxidation iron content electrolyte, is carried out using dual-pulse power supply
Micro-arc oxidation treatment；
3) it post-processes: the magnesium alloy sample after differential arc oxidation is rinsed, it is dry.
2. a kind of magnesium alloy differential arc oxidation method according to claim 1, it is characterised in that: using the side being threadedly coupled
Formula stamps threaded hole on the magnesium alloy, magnesium alloy is made to be connected with aluminum conductor, remaining position of aluminum conductor is used in connection, especially
It is and liquid level of electrolyte is with lower portion, aluminum conductor is isolated with electrolyte using insulated hull, aluminum conductor is avoided to generate starting the arc phenomenon.
3. magnesium alloy differential arc oxidation method as described in claim 1, it is characterised in that: mao power source is dipulse electricity
Source, differential arc oxidation select constant voltage mode, positive voltage 300-450V, negative voltage 20-60V, and positive negative pulse stuffing ratio is 1:1, frequency
For 50-400Hz, positive negative duty identical 8%-30%, oxidization time 10-20min, electrolyte temperature are maintained at 30-35 DEG C.
4. magnesium alloy differential arc oxidation method as described in claim 1, it is characterised in that: obtained differential arc oxidation magnesium alloy applies
With a thickness of 30-60um, ferro element is uniformly distributed layer on coating, and differential arc oxidation coating color is black.
5. a kind of preparation method for the iron content electrolyte that magnesium alloy differential arc oxidation method as described in claim 1-3 uses, special
It is deionized water or ultrapure aqueous solvent that sign, which is that electrolyte uses, and micro-arc oxidation electrolyte pH value is 12-13, and electrolyte includes such as
Lower ingredient: phosphate 10-60g/L, highly basic 1-6g/L, complexing agent 2-10g/L, iron content electrolyte 5-20g/L.
6. the differential arc oxidation method as claimed in claim 5, which is characterized in that phosphate described in electrolyte is phosphoric acid
Sodium, ammonium phosphate or calgon.
7. the differential arc oxidation method as claimed in claim 5, which is characterized in that complexing agent described in electrolyte is glucose
Sour potassium, triethanolamine or sorbierite.
8. the differential arc oxidation method as claimed in claim 5, which is characterized in that iron content electrolyte described in electrolyte is grass
Sour ferripotassium, ironic citrate or ferrous sulfate.
9. the differential arc oxidation method as claimed in claim 5, which is characterized in that highly basic described in electrolyte is sodium hydroxide
Or potassium hydroxide.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112663112A (en) * | 2020-12-02 | 2021-04-16 | 斯特凯新材料(上海)有限公司 | Preparation method of electrolyte and magnesium alloy composite black oxide ceramic membrane |
| CN113088966A (en) * | 2021-03-31 | 2021-07-09 | 中国兵器科学研究院宁波分院 | Magnesium alloy composite coating and preparation method thereof |
| CN114540918A (en) * | 2022-03-25 | 2022-05-27 | 陕西工业职业技术学院 | Electrolyte, preparation method thereof and preparation method of magnesium alloy micro-arc oxidation coating |
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| CN104630861A (en) * | 2015-01-13 | 2015-05-20 | 桂林电子科技大学 | Substrate test piece-anode bar connecting device and method |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112663112A (en) * | 2020-12-02 | 2021-04-16 | 斯特凯新材料(上海)有限公司 | Preparation method of electrolyte and magnesium alloy composite black oxide ceramic membrane |
| CN113088966A (en) * | 2021-03-31 | 2021-07-09 | 中国兵器科学研究院宁波分院 | Magnesium alloy composite coating and preparation method thereof |
| CN114540918A (en) * | 2022-03-25 | 2022-05-27 | 陕西工业职业技术学院 | Electrolyte, preparation method thereof and preparation method of magnesium alloy micro-arc oxidation coating |
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Application publication date: 20190716 |