CN106995932A - The preparation method of aluminum alloy surface selfreparing differential arc oxidation composite ceramics film layer - Google Patents
The preparation method of aluminum alloy surface selfreparing differential arc oxidation composite ceramics film layer Download PDFInfo
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- CN106995932A CN106995932A CN201710240975.5A CN201710240975A CN106995932A CN 106995932 A CN106995932 A CN 106995932A CN 201710240975 A CN201710240975 A CN 201710240975A CN 106995932 A CN106995932 A CN 106995932A
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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
- C25D11/026—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
- C25D11/024—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
- C25D11/04—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
- C25D15/00—Electrolytic or electrophoretic production of coatings containing embedded materials, e.g. particles, whiskers, wires
Abstract
The invention discloses a kind of preparation method of aluminum alloy surface selfreparing differential arc oxidation composite ceramics film layer, comprise the following steps：Alloy matrix aluminum is pre-processed, surface oxide layer is removed, is cleaned by ultrasonic 30 60min, rinses well and dry；Calgon and serpentine nano particle are added in electrolyte and disperseed；Alloy matrix aluminum is placed in and is dispersed with the electrolyte of serpentine nano particle as anode, differential arc oxidation is carried out using the pulse power；The constituent of electrolyte includes：Sodium metasilicate 8g/L, sodium tungstate 5g/L, potassium hydroxide 2.5g/L, EDTA 2g/L, the 600mg/L of calgon 200, the 10g/L of serpentine nano particle 5, the solvent of electrolyte is deionized water.The present invention adds serpentine micro-nano granules by differential arc oxidization technique in the electrolytic solution, the self-repair type aluminum alloy differential arc oxidation composite ceramic layer containing serpentine micro-nano granules is made, so as to increase substantially its tribological property.
Description
Technical field
The present invention relates to the technical field of surface of aluminium alloy, and in particular to a kind of aluminum alloy surface selfreparing differential of the arc oxygen
Change the preparation method of composite ceramics film layer.
Background technology
Aluminium and its alloy are because light weight, specific strength are high, thermal conductivity is good and the characteristic such as easy processing is widely used in aviation, navigate
My god, military and civilian etc. field, but the defect such as aluminum alloy surface hardness is low, easy to wear, corrosion-resistant limits it and enters one
The application of step, therefore aluminum alloy surface progress intensive treatment is had very important significance with improving its tribological property.It is existing
Some aluminum alloy surface treatment technologies mainly have chemical transformation, galvanoplastic and anodizing, but above-mentioned three kinds of aluminium alloys
There is complex process in process for treating surface, severe reaction conditions, and membrane uniformity is poor, fragility is big, easily peel off, or severe contamination
The defects such as environment.
The content of the invention
The proposition of the invention for being directed to problem above, and a kind of aluminum alloy surface selfreparing differential arc oxidation composite ceramic of research and design
The preparation method of porcelain film layer.The technological means that the present invention is used is as follows：
A kind of preparation method of aluminum alloy surface selfreparing differential arc oxidation composite ceramics film layer, comprises the following steps：
A. alloy matrix aluminum is pre-processed, removes surface oxide layer, be cleaned by ultrasonic 30-60min, rinse dry after taking-up
It is net and dry；
B. calgon and serpentine nano particle are added in electrolyte and disperseed；
C. alloy matrix aluminum is placed in and be dispersed with as anode in the electrolyte of serpentine nano particle, using the pulse power
Carry out differential arc oxidation；
Being dispersed with the constituent of the electrolyte of serpentine nano particle includes：Sodium metasilicate 8g/L, sodium tungstate 5g/L, hydrogen-oxygen
Change potassium 2.5g/L, EDTA 2g/L, calgon 200-600mg/L, serpentine nano particle 5-10g/L, the electrolyte
Solvent is deionized water；
The electrical parameter of differential arc oxidation is：Forward voltage 400-450v, negative voltage 100-150v, frequency 100-500hz, just
To dutycycle 20%, negative sense dutycycle 20%, positive negative pulse stuffing compares 1:1.
Further, the temperature of differential arc oxidation is less than 30 DEG C, and the time is 30-60min.
Further, the preparation method of the serpentine nano particle is：Jaw crusher is first passed through by block serpentine
Raw material is crushed to micron order, then refines 48-72 hours to nanoscale by high speed ball mill.
Further, the anode of differential arc oxidation is alloy matrix aluminum, and negative electrode is stainless steel electrolytic groove.
Further, the concentration of the calgon in the electrolytic solution is 200-600mg/L.
Compared with the prior art, the preparation of aluminum alloy surface selfreparing differential arc oxidation composite ceramics film layer of the present invention
Method has advantages below：
1st, can be in aluminium alloy matrix surface growth in situ ceramic layer by this method, and thicknesses of layers is controllable, Ke Yigen
The film layer for preparing required thickness according to being actually needed, substantially can be with reserve sample original size from without influenceing the size of friction pair match somebody with somebody
Close.
2nd, the obtained selfreparing differential arc oxidation composite ceramics film layer very matter prepared by this method is close, and hardness is high,
Microhardness is up to more than 1,000.
3rd, the obtained selfreparing differential arc oxidation composite ceramics film layer good corrosion resistance prepared by this method.
4th, the obtained selfreparing differential arc oxidation composite ceramics film layer prepared by this method is wear-resisting, and with iron-based gold
Belonging to has anti-attrition and the self-repair function to ferrous metals in the process of friction and wear of friction pair.
Brief description of the drawings
Fig. 1 is the surface topography map of the compound micro-arc oxidation films of serpentine described in the embodiment of the present invention.
Fig. 2 is the Cross Section Morphology figure of the compound micro-arc oxidation films of serpentine described in the embodiment of the present invention.
Fig. 3 is the granularity point of the serpentine nano particle after being modified by the way that 200mg/L calgons are scattered with surface
Butut.
Fig. 4 is the element constituent figure of traditional aluminium alloy differential arc oxidation film layer.
Fig. 5 is the element constituent figure of the compound micro-arc oxidation films of serpentine described in the embodiment of the present invention.
Fig. 6 is that traditional aluminium alloy differential arc oxidation film layer is combined micro-arc oxidation films with the serpentine described in the embodiment of the present invention
Hardness balance schemes.
Fig. 7 is that traditional aluminium alloy differential arc oxidation film layer is combined micro-arc oxidation films with the serpentine described in the embodiment of the present invention
Phase constituent comparison diagram.
Fig. 8 is that traditional aluminium alloy differential arc oxidation film layer exists with the compound micro-arc oxidation films of serpentine described in the embodiment of the present invention
Carry out coefficient of friction comparison diagram during friction-wear test.
Embodiment
A kind of preparation method of aluminum alloy surface selfreparing differential arc oxidation composite ceramics film layer, comprises the following steps：
A. alloy matrix aluminum is pre-processed, removes surface oxide layer, be cleaned by ultrasonic 30-60min, rinse dry after taking-up
Net and dry, specific processing method is that alloy matrix aluminum is carried out into pre-grinding and polishing, removes specimen surface oxide layer, then will
Alloy matrix aluminum, which is put into acetone, to be cleaned by ultrasonic about 30-60 minutes, to remove the greasy dirt and dust of specimen surface, is taken out
Rinsed well, dried rear standby with absolute ethyl alcohol after sample.
B. calgon and serpentine nano particle are added in electrolyte and disperseed, ultrasonic vibration can be passed through
Mode serpentine nano particle is disperseed, the preparation method of the serpentine nano particle is：First pass through jaw crushing
Block serpentine raw material is crushed to micron order by machine, then refines 48-72 hours to nanoscale, hexa metaphosphoric acid by high speed ball mill
Sodium is squeezed as dispersant and modification, prevents serpentine nano particle from reuniting in the electrolytic solution, it is ensured that serpentine nano particle
Particle diameter in the reasonable scope.
C. alloy matrix aluminum is placed in and be dispersed with as anode in the electrolyte of serpentine nano particle, using the pulse power
Differential arc oxidation is carried out, serpentine is made and is combined micro-arc oxidation films；It is dispersed with the constituent of the electrolyte of serpentine nano particle
Including：Sodium metasilicate 8g/L, sodium tungstate 5g/L, potassium hydroxide 2.5g/L, EDTA 2g/L, calgon 200-600mg/L, snake
Line stone nano particle 5-10g/L, the solvent of the electrolyte is deionized water, and the electrolyte solution configured need to be through magnetic agitation
60min is to ensure that electrolyte is sufficiently uniformly dissolved for 30min ultrasounds, and serpentine micro-nano granules are fully dispersed.The electricity of differential arc oxidation
Parameter is：Forward voltage 400-450v, negative voltage 100-150v, frequency 100-500hz, positive dutycycle 20%, negative sense is accounted for
Sky compares 20%, and positive negative pulse stuffing compares 1:1.The temperature of differential arc oxidation is less than 30 DEG C, and the time is 30-60min.The anode of differential arc oxidation
For alloy matrix aluminum, negative electrode is stainless steel electrolytic groove.
As depicted in figs. 1 and 2, the compound micro-arc oxidation films surface light of serpentine that the present embodiment methods described is prepared is led to
Sliding, thickness is uniform, is well combined with alloy matrix aluminum and very matter is close.As shown in Fig. 3 and following table, serpentine micro-nano granules
Epigranular is distributed between 250-445nm, has reached micro-nano rank, and be stabilized in the electrolytic solution.Such as Fig. 4 and figure
Shown in 5, traditional aluminium alloy differential arc oxidation film layer essential element composition is O and Al elements, and Si and Mg constituent contents are very low.Compare
Traditional Micro-Arc Oxidized Ceramic Layer of Aluminum Alloy, the serpentine that the present embodiment methods described is prepared is combined the Si in micro-arc oxidation films
It is obviously improved with Mg constituent contents, and exclusive source of the Mg elements in the method for the invention is serpentine micro-nano granules,
Raised while contrast Si and Mg constituent contents, it is believed that the serpentine that the method for the invention is prepared is combined differential of the arc oxygen
The raising for changing Si the and Mg constituent contents in film is due to the reason for serpentine micro-nano granules enter film layer.As shown in fig. 6,
Aluminum alloy surface hardness can be increased substantially by differential arc oxidation experiment, and use serpentine made from the method for the invention
It is multiple that compound differential arc oxidation film hardness is higher than serpentine made from traditional Micro-Arc Oxidized Ceramic Layer of Aluminum Alloy, i.e. the method for the invention
Close micro-arc oxidation films wearability more preferable.As shown in fig. 7, the main component of traditional aluminium alloy differential arc oxidation film layer for alpha-aluminium oxide and
Gamma-alumina, and the present embodiment occurs in that new phase constituent magnesium silicate and silica, this is serpentine micro-nano granules micro-
In arc oxidation test, the oxide of aluminum alloy surface molten state causes serpentine micro-nano granules to there occurs decarboxylation reaction and height
The product of temperature change phase in version generation is compound to the reason in film layer.As shown in figure 8, what the method described in the present embodiment was prepared
Serpentine is combined coefficient of friction of the micro-arc oxidation films in process of friction and wear and is significantly lower than traditional aluminium alloy differential arc oxidation film layer,
Serpentine is combined micro-arc oxidation films wearability more preferably i.e. made from the present embodiment methods described, illustrates this implementation with reference to Fig. 4 to Fig. 7
The serpentine pyrometamorphism and the product after decarboxylation reaction that serpentine made from example methods described is combined in micro-arc oxidation films exist
The effect of anti-attrition is served in process of friction and wear, this property for having anti-attrition and selfreparing with serpentine micro-nano powder is kissed
Close.
Embodiment described above is only that the preferred embodiment of the present invention is described, not to the model of the present invention
Enclose and be defined, on the premise of design spirit of the present invention is not departed from, technical side of the those of ordinary skill in the art to the present invention
In various modifications and improvement that case is made, the protection domain that claims of the present invention determination all should be fallen into.
Claims (5)
1. a kind of preparation method of aluminum alloy surface selfreparing differential arc oxidation composite ceramics film layer, comprises the following steps：
A. alloy matrix aluminum is pre-processed, removes surface oxide layer, be cleaned by ultrasonic 30-60min, rinsed well simultaneously after taking-up
Dry；
B. calgon and serpentine nano particle are added in electrolyte and disperseed；
C. alloy matrix aluminum is placed in and be dispersed with the electrolyte of serpentine nano particle as anode, carried out using the pulse power
Differential arc oxidation；
Being dispersed with the constituent of the electrolyte of serpentine nano particle includes：Sodium metasilicate 8g/L, sodium tungstate 5g/L, potassium hydroxide
2.5g/L, EDTA 2g/L, calgon 200-600mg/L, serpentine nano particle 5-10g/L, the solvent of the electrolyte
For deionized water；
The electrical parameter of differential arc oxidation is：Forward voltage 400-450v, negative voltage 100-150v, frequency 100-500hz, forward direction is accounted for
Sky compares 20%, and negative sense dutycycle 20%, positive negative pulse stuffing compares 1:1.
2. the preparation method of aluminum alloy surface selfreparing differential arc oxidation composite ceramics film layer according to claim 1, it is special
Levy and be：The temperature of differential arc oxidation is less than 30 DEG C, and the time is 30-60min.
3. the preparation method of aluminum alloy surface selfreparing differential arc oxidation composite ceramics film layer according to claim 1, it is special
Levy and be：The preparation method of the serpentine nano particle is：Jaw crusher is first passed through to be crushed to block serpentine raw material
Micron order, then 48-72 hours are refined to nanoscale by high speed ball mill.
4. the preparation method of aluminum alloy surface selfreparing differential arc oxidation composite ceramics film layer according to claim 1, it is special
Levy and be：The anode of differential arc oxidation is alloy matrix aluminum, and negative electrode is stainless steel electrolytic groove.
5. the preparation method of aluminum alloy surface selfreparing differential arc oxidation composite ceramics film layer according to claim 1, it is special
Levy and be：The concentration of the calgon in the electrolytic solution is 200-600mg/L.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109868386A (en) * | 2019-03-08 | 2019-06-11 | 安徽信息工程学院 | A kind of wear-resistant material and preparation method thereof |
| CN112981486A (en) * | 2021-03-05 | 2021-06-18 | 沈阳大学 | Preparation method of low-voltage self-repairing aluminum alloy micro-arc oxidation film |
| CN113308693A (en) * | 2021-04-30 | 2021-08-27 | 江苏龙山管件有限公司 | High-strength corrosion-resistant stainless steel pipe fitting and machining process thereof |
| CN114540915A (en) * | 2022-03-18 | 2022-05-27 | 太仓力山机械设备有限公司 | Wear-resistant and corrosion-resistant surface treatment process for aluminum alloy pulley seat of industrial heat-preservation sliding door |
| CN114892238A (en) * | 2022-04-02 | 2022-08-12 | 西安交通大学 | Method for improving corrosion resistance of magnesium alloy micro-arc oxidation film layer by pretreatment process |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109868386A (en) * | 2019-03-08 | 2019-06-11 | 安徽信息工程学院 | A kind of wear-resistant material and preparation method thereof |
| CN112981486A (en) * | 2021-03-05 | 2021-06-18 | 沈阳大学 | Preparation method of low-voltage self-repairing aluminum alloy micro-arc oxidation film |
| CN113308693A (en) * | 2021-04-30 | 2021-08-27 | 江苏龙山管件有限公司 | High-strength corrosion-resistant stainless steel pipe fitting and machining process thereof |
| CN113308693B (en) * | 2021-04-30 | 2023-02-28 | 江苏龙山管件有限公司 | High-strength corrosion-resistant stainless steel pipe fitting and machining process thereof |
| CN114540915A (en) * | 2022-03-18 | 2022-05-27 | 太仓力山机械设备有限公司 | Wear-resistant and corrosion-resistant surface treatment process for aluminum alloy pulley seat of industrial heat-preservation sliding door |
| CN114892238A (en) * | 2022-04-02 | 2022-08-12 | 西安交通大学 | Method for improving corrosion resistance of magnesium alloy micro-arc oxidation film layer by pretreatment process |
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