CN107400915B - Have both the aluminium alloy anode oxide film and preparation method thereof of porous subsurface stratum and wearing coat - Google Patents
Have both the aluminium alloy anode oxide film and preparation method thereof of porous subsurface stratum and wearing coat Download PDFInfo
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- CN107400915B CN107400915B CN201610333907.9A CN201610333907A CN107400915B CN 107400915 B CN107400915 B CN 107400915B CN 201610333907 A CN201610333907 A CN 201610333907A CN 107400915 B CN107400915 B CN 107400915B
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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
- C25D11/08—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used containing inorganic acids
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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
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Abstract
The present invention provides a kind of aluminium alloy anode oxide films for having both porous subsurface stratum and wearing coat.The anode oxide film has three-decker, is followed successively by shielded layer, porous subsurface stratum and wearing coat outward from alloy matrix aluminum.The anode oxide film substantially increases the wear-resisting property of aluminium alloy, has widened the application field of aluminium alloy.In addition, the present invention uses anodizing, using aluminium alloy as the anode and cathode of anode oxidation process, electrolyte includes sulfuric acid, wide temperature oxidant, aluminium ion, by controlling oxidation current density, electrolyte prescription controls the speed of growth and solution rate of anode oxide film, to obtain the anode oxidation membrane that surface has both porous subsurface stratum and wearing coat.
Description
Technical field
The present invention relates to aluminum alloy surface process fields, and in particular to a kind of aluminium for having both porous subsurface stratum and wearing coat
Alloy anodized film and preparation method thereof.
Background technique
Aluminium alloy has many advantages, such as that density is small, specific strength is high, plasticity is good, easy processing molding, is to apply to be only second in industry
The metal material of steel, aluminium alloy has excellent electric conductivity, thermal conductivity and corrosion resistance, thus is widely used in Aeronautics and Astronautics, vapour
The fields such as vehicle, ocean, machine-building, nuclear industry, weapon industry.
But aluminium alloy still has shortcoming during military service at present, such as: be easy to be worn and corrode and
Failure, very big security risk and economic loss are brought to engineer application；Aluminum alloy surface through over mechanical processing can all exist
Various defects and cannot be directly thrown into practical application；Surface can generate layer oxide film to aluminium alloy under field conditions (factors), about
It is 0.01 μm -0.10 μm, this layer of oxidation film is amorphous state, and thin porous, mechanical strength is low.These problems enable aluminum alloy to not expire
The requirement of actual working condition of sufficient application field, so need to be surface-treated alloy matrix aluminum.
The surface treatment method of aluminium alloy has very much, and anodizing is most widely used and most successful at present.Anodic oxygen
Change is a kind of electrolytic acid cleaning oxydation process, and aluminium alloy matrix surface will form layer oxide film layer in this process.This layer of oxidation film
It is the film layer with shielded layer (barrier layer) and honeycomb sandwich on alloy matrix aluminum, there is high rigidity, insulation and thermal insulation
Property is good, corrosion resistance is excellent, associativity is strong and has good characterization of adsorption and good optical characteristics.However, utilizing anodic oxidation
Although the corrosion resisting property of aluminium alloy can be improved in the oxidation film that aluminum alloy surface is formed by electrochemical reaction for journey, but close to aluminium
The wear-resisting property of gold is not greatly improved.And after this layer of oxidation film is corroded during military service, surface hardness is reduced, and is led
Cause wearability decline.
Summary of the invention
There is new structural anode oxide film the present invention provides a kind of aluminium alloy matrix surface, as shown in Figure 1, should
Anode oxide film is improved in the existing aluminium alloy anode oxide film surface construction with shielded layer and porous layer wearing coat
The abrasion resistance properties of aluminium alloy anode oxide film.
That is, technical solution provided by the present invention are as follows: a kind of aluminum alloy anode for having both porous subsurface stratum and wearing coat
Oxidation film, the anode oxide film are followed successively by shielded layer, porous subsurface stratum and wearing coat from matrix outward.
Preferably, the anode oxide film with a thickness of 40 μm -50 μm.
Preferably, the wearing coat with a thickness of 2 μm -5 μm.
The wearing coat hardness with higher and preferable toughness, microhardness are greater than 250Hv, even as high as
450Hv, therefore the wear-resisting property of anode oxide film is substantially increased, wear rate, which is measured, through UMT-3 friction wear testing machine is lower than
6.41×10-4mm3/ Nm, the wear rate compared to alloy matrix aluminum under same experiment condition are 1.24 × 10-2mm3/ Nm, significantly improves
The wearability of alloy matrix aluminum, has widened the application field of aluminium alloy.
The above-mentioned aluminium alloy anode oxide film for having both porous subsurface stratum and wearing coat is prepared the present invention also provides a kind of
Method, using anodizing, using alloy matrix aluminum as anode, using aluminium alloy as cathode, electrolyte includes sulfuric acid, width
Warm oxidant and aluminium ion, by control oxidation current density, electrolyte prescription and control anode oxide film growth speed
Degree and solution rate, to obtain the anode oxide film that surface has both porous subsurface stratum and wearing coat.
Preferably, alloy matrix aluminum is carried out cleaning pretreatment to remove surface impurity before anodized.As
A kind of implementation, first mechanically polishes aluminium alloy matrix surface, then carries out ungrease treatment, to remove surface grease, connects
Washed, carry out neutralization reaction later, neutralize the alkaline solution that skimming processes remain in aluminum alloy surface, then in anhydrous second
It is cleaned by ultrasonic in alcohol, enables aluminum alloy to surface and remained without other impurities, finally by the aluminium alloy cleaned up with being dried with nitrogen,
The contact with aluminum alloy surface should be prevented to prevent contaminated surface during drying.
Preferably, oxidation current is direct current constant current, further preferably, adjustment oxidate current is 4-10A/
dm2。
Preferably, oxidization time 30-60min.
Preferably, oxidizing temperature is room temperature.
Preferably, in anode oxidation process, electrolyte prescription are as follows: 45-180g/L sulfuric acid, 10-16g/L wide temperature oxidation
Agent, 5-10g/L aluminium ion.The described warm oxidant of width is unlimited, including one of phosphoric acid, oxalic acid, tartaric acid, pyruvic acid etc. or
The two or more combination of person.The source of aluminum ion is unlimited, including one of aluminium hydroxide, aluminum sulfate, meta-aluminate etc. or
The two or more offers of person.
Preferably, should also wash using deionized water after anodic oxidation reactions, then carry out drying and processing.
In conclusion the present invention uses anodizing, on the one hand in anode oxidation process, using aluminium alloy as cathode
And aluminium ion is added in the electrolytic solution, control the course of dissolution of oxidation film in anode oxidation process；On the other hand, in electrolyte
The wide warm oxidant of middle addition, has widened the temperature range of anodic oxidation, so that temperature is to anode oxide film in anode oxidation process
The influence of growth reduces.The two combines, realize aluminium alloy matrix surface be made have both porous subsurface stratum and wearing coat
Anode oxidation membrane.This method is simple to operation, and being well combined of obtained anode oxide film, coefficient of friction is low, it is good to have
Good mechanical property, can significantly improve the wear-resisting property of aluminium alloy.
Detailed description of the invention
Fig. 1 is the structural schematic diagram for the aluminium alloy anode oxide film that the present invention has both porous subsurface stratum and wearing coat；
Fig. 2 is the schematic perspective view of structure shown in Fig. 1；
Fig. 3 is the scanning electron microscope (SEM) photograph of aluminium alloy anode oxide film obtained in the embodiment of the present invention 1；
Fig. 4 is the enlarged drawing of boxed area in Fig. 3；
Fig. 5 is the longitudinal cross-section scanning electron microscope (SEM) photograph of aluminium alloy anode oxide film obtained in the embodiment of the present invention 1；
Fig. 6 is the enlarged drawing of Blocked portion in Fig. 5.
Specific embodiment
Present invention is further described in detail for embodiment with reference to the accompanying drawing, it should be pointed out that implementation as described below
Example is intended to convenient for the understanding of the present invention, and does not play any restriction effect to it.
Appended drawing reference in Fig. 1-2 are as follows: the wearing coat 1-；The porous subsurface stratum of 2-；3- shielded layer.
Embodiment 1:
In the present embodiment, the anode oxide film of aluminium alloy matrix surface has three-decker, as shown in Figure 1, from aluminium alloy
Matrix is followed successively by shielded layer 3, porous subsurface stratum 2, wearing coat 1 to surface.Fig. 2 is the stereochemical structure signal of the anode oxide film
Figure.
The preparation method of the anode oxide film of above-mentioned aluminium alloy matrix surface the following steps are included:
(1) it mechanically polishes
Alloy matrix aluminum is subjected to three-stage polishing, aluminium alloy is subjected to rough polishing first, then carries out fine polishing, finally
Finishing polish is carried out, mirror effect is finally obtained.
(2) ungrease treatment
Aluminium alloy after polishing is subjected to ungrease treatment, degreasing agent is the lye that mass fraction is 10%, this lye is hydrogen
At least one of sodium oxide molybdena, sodium carbonate and sodium phosphate are handled 15 minutes at 20 DEG C.
(3) anodic oxidation
Alloy matrix aluminum after ungrease treatment is put into anode oxidation groove liquid and carries out anodized, cathode is aluminium conjunction
Gold, oxidate current 4A/dm2, oxidation current is direct current constant current, and oxidizing temperature is room temperature, oxidization time 60min；
The electrolyte composition is as follows:
Sulfuric acid 45g/L；
Wide temperature oxidant 15g/L；
Aluminium ion 5g/L；
Remaining is water.
(4) it washes, dry
Alloy matrix aluminum after anodized is cleaned with deionized water, carries out drying and processing after washing, at drying
Managing temperature is 80 DEG C, and the drying and processing time is 30 minutes.
The scanning electron microscope (SEM) photograph of the anode oxide film on treated aluminum alloy base material surface is as shown in figure 3, Fig. 4 is Fig. 3
The enlarged drawing of middle boxed area.Fig. 5 is sweeping for the longitudinal cross-section of the anode oxide film on treated aluminum alloy base material surface
Electron microscope is retouched, Fig. 6 is the enlarged drawing of Blocked portion in Fig. 5.From figure 3, it can be seen that using the anode oxidation method of the present embodiment
The surface layer uniform ground of the anode oxide film of preparation, and there is good gloss.From fig. 4, it can be seen that the anode oxide film
It is cellular porous subsurface stratum below wearing coat.The anode oxide film is measured with three-decker by scanning electron microscope, is divided
It is not shielded layer, porous sub-layer and wearing coat.
The surface layer of the anode oxide film prepared after above-mentioned processing in aluminum alloy surface is analyzed by XPS spectrum figure and XRD spectra
For amorphous Al2O3.Reach 250-300Hv, wear rate 3.2 by the microhardness that microhardness measures the anode oxide film
×10-4-6.41×10-4mm3/ Nm, wear resistance and corrosion resistance are good, and anode oxide film color is deeper at this time, while also having good light
Pool.
Embodiment 2:
In the present embodiment, the anode oxide film of aluminium alloy matrix surface has three-decker, that is, from alloy matrix aluminum to table
Face is followed successively by shielded layer, porous subsurface stratum, wearing coat.
The preparation method of the anode oxide film of above-mentioned aluminium alloy matrix surface the following steps are included:
(1) it mechanically polishes
Alloy matrix aluminum is subjected to three-stage polishing, aluminium alloy is subjected to rough polishing first, then carries out fine polishing, finally
Finishing polish is carried out, mirror effect is finally obtained.
(2) ungrease treatment
Aluminium alloy after polishing is subjected to ungrease treatment, degreasing agent is the lye that mass fraction is 15%, this lye is hydrogen
At least one of sodium oxide molybdena, sodium carbonate and sodium phosphate are handled 13 minutes at 30 DEG C.
(3) anodic oxidation
Alloy matrix aluminum after ungrease treatment is put into anode oxidation groove liquid and carries out anodized, cathode is aluminium conjunction
Gold, oxidate current 6A/dm2, oxidation current is direct current constant current, and oxidizing temperature is room temperature, oxidization time 50min；
The electrolyte composition is as follows:
Sulfuric acid 90g/L；
Wide temperature oxidant 12g/L；
Aluminium ion 10g/L；
Remaining is water.
(4) it washes, dry
Alloy matrix aluminum after anodized is cleaned with deionized water, carries out drying and processing after washing, at drying
Managing temperature is 60 DEG C, and the drying and processing time is 35 minutes.
It is similar to Figure 3 in the scanning electron microscope (SEM) photograph of the anode oxide film of aluminum alloy surface preparation after above-mentioned processing, section
Scanning electron microscope (SEM) photograph similar to shown in Fig. 5 and Fig. 6, showing aluminium alloy matrix surface that the anode oxidation method of the present embodiment obtains
Anode oxide film film thickness and uniformly, have good gloss.Measuring the anode oxide film by scanning electron microscope has three-decker,
It is shielded layer, porous sub-layer and wearing coat respectively.
The surface layer of the anode oxide film prepared after above-mentioned processing in aluminum alloy surface is analyzed by XPS spectrum figure and XRD spectra
For amorphous Al2O3.Reach 410-450Hv, wear rate low 6.21 by the microhardness that microhardness measures the anode oxide film
×10-5-9.1×10-5mm3/ Nm, wear resistance and corrosion resistance are good, this anode oxidation membrane color is shallower, while having good gloss.
Embodiment 3
In the present embodiment, the anode oxide film of aluminium alloy matrix surface has three-decker, that is, from alloy matrix aluminum to table
Face is followed successively by shielded layer, porous subsurface stratum, wearing coat.
The preparation method of the anode oxide film of above-mentioned aluminium alloy matrix surface the following steps are included:
(1) it mechanically polishes
Alloy matrix aluminum is subjected to three-stage polishing, aluminium alloy is subjected to rough polishing first, then carries out fine polishing, finally
Finishing polish is carried out, mirror effect is finally obtained.
(2) ungrease treatment
Aluminium alloy after polishing is subjected to ungrease treatment, degreasing agent is the lye that mass fraction is 15%, this lye is hydrogen
At least one of sodium oxide molybdena, sodium carbonate and sodium phosphate are handled 10 minutes at 40 DEG C.
(3) anodic oxidation
Alloy matrix aluminum after ungrease treatment is put into anode oxidation groove liquid and carries out anodized, cathode is aluminium conjunction
Gold, oxidate current 8A/dm2, oxidation current is direct current constant current, and oxidizing temperature is room temperature, oxidization time 40min；
The electrolyte composition is as follows:
Sulfuric acid 180g/L；
Wide temperature oxidant 14g/L；
Aluminium ion 6g/L；
Remaining is water.
(4) it washes, dry
Alloy matrix aluminum after anodized is cleaned with deionized water, carries out drying and processing after washing, at drying
Managing temperature is 80 DEG C, and the drying and processing time is 30 minutes.
It is similar to Figure 3 in the scanning electron microscope (SEM) photograph of the anode oxide film of aluminum alloy surface preparation after above-mentioned processing, section
Scanning electron microscope (SEM) photograph similar to shown in Fig. 5 and Fig. 6, showing aluminium alloy matrix surface that the anode oxidation method of the present embodiment obtains
Anode oxide film film thickness and uniformly, have good gloss.Measuring the anode oxide film by scanning electron microscope has three-decker,
It is shielded layer, porous sub-layer and wearing coat respectively.
The surface layer of the anode oxide film prepared after above-mentioned processing in aluminum alloy surface is analyzed by XPS spectrum figure and XRD spectra
For amorphous Al2O3.Reach 380-420Hv, wear rate low 9.21 by the microhardness that microhardness measures the anode oxide film
×10-5-1。1×10-4mm3/ Nm, wear resistance and corrosion resistance are good, while also having good gloss.
Embodiment 4
In the present embodiment, the anode oxide film of aluminium alloy matrix surface has three-decker, that is, from alloy matrix aluminum to table
Face is followed successively by shielded layer, porous subsurface stratum, wearing coat.
The preparation method of the anode oxide film of above-mentioned aluminium alloy matrix surface the following steps are included:
(1) it mechanically polishes
Alloy matrix aluminum is subjected to three-stage polishing, aluminium alloy is subjected to rough polishing first, then carries out fine polishing, finally
Finishing polish is carried out, mirror effect is finally obtained.
(2) ungrease treatment
Aluminium alloy after polishing is subjected to ungrease treatment, degreasing agent is the lye that mass fraction is 20%, this lye is hydrogen
At least one of sodium oxide molybdena, sodium carbonate and sodium phosphate are handled 5 minutes at 50 DEG C.
(3) anodic oxidation
Alloy matrix aluminum after ungrease treatment is put into anode oxidation groove liquid and carries out anodized, cathode is aluminium conjunction
Gold, oxidate current 10A/dm2, oxidation current is direct current constant current, and oxidizing temperature is room temperature, oxidization time 30min；
The electrolyte composition is as follows:
Sulfuric acid 180g/L；
Wide temperature oxidant 15g/L；
Aluminium ion 6g/L；
Remaining is water.
(4) it washes, dry
Alloy matrix aluminum after anodized is cleaned with deionized water, carries out drying and processing after washing, at drying
Managing temperature is 60 DEG C, and the drying and processing time is 35 minutes.
It is similar to Figure 3 in the scanning electron microscope (SEM) photograph of the anode oxide film of aluminum alloy surface preparation after above-mentioned processing, section
Scanning electron microscope (SEM) photograph similar to shown in Fig. 5 and Fig. 6, showing aluminium alloy matrix surface that the anode oxidation method of the present embodiment obtains
Anode oxide film film thickness and uniformly, have good gloss.Measuring the anode oxide film by scanning electron microscope has three-decker,
It is shielded layer, porous sub-layer and wearing coat respectively.
The surface layer of the anode oxide film prepared after above-mentioned processing in aluminum alloy surface is analyzed by XPS spectrum figure and XRD spectra
For amorphous Al2O3.Reach 290-360Hv, wear rate 1.23 by the microhardness that microhardness measures the anode oxide film
×10-4-4.3×10-4mm3/ Nm, wear resistance and corrosion resistance are good, while also having good gloss.
Above-described embodiment has carried out system detailed description to technical solution of the present invention, it should be understood that the upper example is only
For specific embodiments of the present invention, it is not intended to restrict the invention.All any modifications made in spirit of the present invention, benefit
It fills or equivalent replacement etc., should all be included in the protection scope of the present invention.
Claims (9)
1. a kind of preparation method for the aluminium alloy anode oxide film for having both porous subsurface stratum and wearing coat, it is characterized in that: described
Anode oxide film be followed successively by shielded layer, porous subsurface stratum and wearing coat outward from matrix；
Using anodizing, using alloy matrix aluminum as anode, using aluminium alloy as cathode, electrolyte includes sulfuric acid, wide temperature
Oxidant and aluminium ion, by control oxidation current density, electrolyte prescription control anode oxide film the speed of growth and
Solution rate.
2. the preparation method of the aluminium alloy anode oxide film of porous subsurface stratum and wearing coat is had both as described in claim 1,
It is characterized in that: the anode oxide film with a thickness of 40 μm -50 μm.
3. having both the preparation side of the aluminium alloy anode oxide film of porous subsurface stratum and wearing coat as claimed in claim 1 or 2
Method measures wear rate through UMT-3 friction wear testing machine it is characterized in that: the microhardness of the wearing coat is greater than 250Hv
It is 6.41 × 10-4mm3/ Nm or less.
4. the preparation method of the aluminium alloy anode oxide film of porous subsurface stratum and wearing coat is had both as described in claim 1,
It is characterized in that: alloy matrix aluminum is pre-processed before anodized.
5. the preparation method of the aluminium alloy anode oxide film of porous subsurface stratum and wearing coat is had both as described in claim 1,
It is characterized in that: oxidation current is direct current constant current, oxidate current 4-10A/dm2。
6. the preparation method of the aluminium alloy anode oxide film of porous subsurface stratum and wearing coat is had both as described in claim 1,
It is characterized in that: the electrolyte prescription are as follows: 45-180g/L sulfuric acid, 10-15g/L wide warm oxidant, 5-10g/L aluminium ion.
7. the preparation method of the aluminium alloy anode oxide film of porous subsurface stratum and wearing coat is had both as described in claim 1,
It is characterized in that: oxidization time is 30-60min, oxidizing temperature is room temperature.
8. the preparation method of the aluminium alloy anode oxide film of porous subsurface stratum and wearing coat is had both as described in claim 1,
It is characterized in that: the warm oxidant of the width is one of phosphoric acid, oxalic acid, tartaric acid, pyruvic acid or two or more mixing.
9. the preparation method of the aluminium alloy anode oxide film of porous subsurface stratum and wearing coat is had both as described in claim 1,
It is characterized in that: the aluminium ion is selected from one of aluminium hydroxide, aluminum sulfate, meta-aluminate or two or more mixing.
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| CN114540912B (en) * | 2021-12-20 | 2024-01-09 | 西北大学 | Treatment method for low-friction solid-liquid composite lubrication of aluminum-lithium alloy surface |
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| CN102286766A (en) * | 2011-09-26 | 2011-12-21 | 西华大学 | Aluminum alloy hard anode oxidation film and process method thereof |
| CN103668386A (en) * | 2013-12-17 | 2014-03-26 | 广西理工职业技术学院 | Aluminum and aluminum alloy surface treatment method |
| CN105386109A (en) * | 2015-11-28 | 2016-03-09 | 贵州凯星液力传动机械有限公司 | Special surface treatment process and system for improving aluminum alloy part abrasive resistance |
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|---|---|---|---|---|
| JPH04362195A (en) * | 1991-06-06 | 1992-12-15 | Ishikawajima Harima Heavy Ind Co Ltd | Wear resistant structure of aluminum parts |
| CN102286766A (en) * | 2011-09-26 | 2011-12-21 | 西华大学 | Aluminum alloy hard anode oxidation film and process method thereof |
| CN103668386A (en) * | 2013-12-17 | 2014-03-26 | 广西理工职业技术学院 | Aluminum and aluminum alloy surface treatment method |
| CN105386109A (en) * | 2015-11-28 | 2016-03-09 | 贵州凯星液力传动机械有限公司 | Special surface treatment process and system for improving aluminum alloy part abrasive resistance |
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