CN107400915A - Have porous subsurface stratum and the aluminium alloy anode oxide film of wearing coat and preparation method thereof concurrently - Google Patents
Have porous subsurface stratum and the aluminium alloy anode oxide film of wearing coat and preparation method thereof concurrently Download PDFInfo
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- CN107400915A CN107400915A CN201610333907.9A CN201610333907A CN107400915A CN 107400915 A CN107400915 A CN 107400915A CN 201610333907 A CN201610333907 A CN 201610333907A CN 107400915 A CN107400915 A CN 107400915A
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- oxide film
- aluminium alloy
- anode oxide
- wearing coat
- subsurface stratum
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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
- C25D11/16—Pretreatment, e.g. desmutting
Abstract
Porous subsurface stratum and the aluminium alloy anode oxide film of wearing coat are had concurrently the invention provides a kind of.The anode oxide film has three-decker, is followed successively by screen layer, porous subsurface stratum and wearing coat outward from alloy matrix aluminum.The anode oxide film substantially increases the anti-wear performance of aluminium alloy, has widened the application field of aluminium alloy.In addition, the present invention uses anodizing, anode and negative electrode using aluminium alloy as anode oxidation process, electrolyte includes sulfuric acid, wide warm oxidant, aluminium ion, by controlling oxidation current density, electrolyte prescription controls the speed of growth and dissolution velocity of anode oxide film, and porous subsurface stratum and the anode oxidation membrane of wearing coat are had concurrently so as to obtain surface.
Description
Technical field
The present invention relates to aluminum alloy surface process field, and in particular to a kind of to have porous subsurface stratum and the aluminium alloy of wearing coat concurrently
Anode oxide film and preparation method thereof.
Background technology
Aluminium alloy has the advantages that density is small, specific strength is high, plasticity is good, easy processing shaping, is to apply to be only second to steel in industry
Metal material, aluminium alloy has excellent electric conductivity, thermal conductivity and corrosion resistance, thus be widely used in Aeronautics and Astronautics,
The fields such as automobile, ocean, machine-building, nuclear industry, weapon industry.
But at present aluminium alloy under arms during still have weak point, such as：Easily it is worn and corrodes and lose
Effect, very big potential safety hazard and economic loss are brought to engineer applied；Aluminum alloy surface through over mechanical processing can all exist each
Plant defect and can not be directly thrown into practical application；Surface can generate layer oxide film to aluminium alloy under field conditions (factors), about
0.01 μm -0.10 μm, this layer of oxide-film is amorphous state, and thin porous, mechanical strength is low.These problems enable aluminum alloy to can not
Meet the requirement of actual working condition of application field, so need to be surface-treated alloy matrix aluminum.
The surface treatment method of aluminium alloy has a lot, and anodizing is most widely used and most successful at present.Anodic oxidation is
A kind of electrolytic acid cleaning oxydation process, in this process aluminium alloy matrix surface can form layer oxide film layer.This layer of oxide-film is position
In the film layer with screen layer (barrier layer) and honeycomb sandwich on alloy matrix aluminum, there is high rigidity, insulation and thermal insulation
Well, corrosion resistance is excellent, associativity is strong and has good characterization of adsorption and good optical characteristics.However, utilize anodic oxidation
Although process can improve the corrosion resisting property of aluminium alloy in the oxide-film that aluminum alloy surface is formed by electrochemical reaction, to aluminium
The anti-wear performance of alloy is not greatly improved.And this layer of oxide-film under arms during corroded after, case hardness reduce,
Wearability is caused to decline.
The content of the invention
The invention provides a kind of anode oxide film with new structure of aluminium alloy matrix surface, as shown in figure 1, the sun
Pole oxide-film wearing coat in the existing aluminium alloy anode oxide film surface construction with screen layer and porous layer, is improved
The abrasion resistance properties of aluminium alloy anode oxide film.
That is, technical scheme provided by the present invention is：It is a kind of to have porous subsurface stratum and the aluminium alloy anode oxide of wearing coat concurrently
Film, the anode oxide film are followed successively by screen layer, porous subsurface stratum and wearing coat outward from matrix.
Preferably, the thickness of described anode oxide film is 40 μm -50 μm.
Preferably, the thickness of described wearing coat is 2 μm -5 μm.
The wearing coat has higher hardness and preferable toughness, and its microhardness is more than 250Hv, even as high as
450Hv, therefore the anti-wear performance of anode oxide film is substantially increased, measure wear rate through UMT-3 friction wear testing machines
Less than 6.41 × 10-4mm3/ Nm, the wear rate compared to alloy matrix aluminum under same experiment condition are 1.24 × 10-2mm3/ Nm,
The wearability of alloy matrix aluminum is significantly improved, has widened the application field of aluminium alloy.
The above-mentioned side for having porous subsurface stratum and the aluminium alloy anode oxide film of wearing coat concurrently is prepared present invention also offers a kind of
Method, using anodizing, using alloy matrix aluminum as anode, include sulfuric acid, width using aluminium alloy as negative electrode, electrolyte
Warm oxidant and aluminium ion, by controlling oxidation current density, electrolyte prescription and control anode oxide film growth speed
Degree and dissolution velocity, porous subsurface stratum and the anode oxide film of wearing coat are had concurrently so as to obtain surface.
Preferably, alloy matrix aluminum is subjected to cleaning pretreatment to remove surface impurity before anodized.As one kind
Implementation, aluminium alloy matrix surface is mechanically polished first, then carry out ungrease treatment, to remove surface grease, then
Washed, carry out neutralization reaction afterwards, 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 dry up the aluminium alloy cleaned up with nitrogen,
It should prevent the contact with aluminum alloy surface from preventing 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 is：The wide temperature oxidant of 45-180g/L sulfuric acid, 10-16g/L,
5-10g/L aluminium ions.Described wide temperature oxidant is unlimited, including one kind in phosphoric acid, oxalic acid, tartaric acid, pyruvic acid etc.
Or two or more combination.Described source of aluminum ion is unlimited, including one in aluminium hydroxide, aluminum sulfate, meta-aluminate etc.
Kind or two or more offers.
Preferably, should also use deionized water to wash after anodic oxidation reactionses, then carry out drying and processing.
In summary, the present invention use anodizing, on the one hand in anode oxidation process, using aluminium alloy as negative electrode with
And aluminium ion is added in the electrolytic solution, control the course of dissolution of oxide-film in anode oxidation process；On the other hand, in electrolyte
It is middle to add wide warm oxidant, widen 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 is combined, and realizes to be made in aluminium alloy matrix surface and has porous subsurface stratum and wearing coat concurrently
Anode oxidation membrane.This method is simple to operation, and being well combined of obtained anode oxide film, coefficient of friction is low, has
Good mechanical property, the anti-wear performance of aluminium alloy can be significantly improved.
Brief description of the drawings
Fig. 1 is the structural representation that the present invention has porous subsurface stratum and the aluminium alloy anode oxide film of wearing coat concurrently；
Fig. 2 is the dimensional structure diagram of structure shown in Fig. 1；
Fig. 3 is the scanning electron microscope (SEM) photograph of obtained aluminium alloy anode oxide film 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 obtained aluminium alloy anode oxide film in the embodiment of the present invention 1；
Fig. 6 is the enlarged drawing of Blocked portion in Fig. 5.
Embodiment
Embodiment is described in further detail to the present invention below in conjunction with the accompanying drawings, it should be pointed out that embodiment described below purport
It is being easy to the understanding of the present invention, and is not playing any restriction effect to it.
Reference in Fig. 1-2 is：1- wearing coats；The porous subsurface stratums of 2-；3- screen layers.
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 base
Body is followed successively by screen layer 3, porous subsurface stratum 2, wearing coat 1 to surface.Fig. 2 is the stereochemical structure of the anode oxide film
Schematic diagram.
The preparation method of the anode oxide film of above-mentioned aluminium alloy matrix surface comprises the following steps：
(1) mechanically polish
Alloy matrix aluminum is subjected to three-stage polishing, aluminium alloy is subjected to rough polishing first, then carries out fine polishing, it is most laggard
Row finishing polish, finally obtains mirror effect.
(2) ungrease treatment
Aluminium alloy after polishing is subjected to ungrease treatment, degreasing agent is the alkali lye that mass fraction is 10%, and this alkali lye is hydrogen-oxygen
Change at least one of sodium, sodium carbonate and sodium phosphate, 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, negative electrode is aluminium alloy,
Oxidate current is 4A/dm2, oxidation current is direct current constant current, and oxidizing temperature is room temperature, oxidization time 60min；
The bath composition is as follows：
Sulfuric acid 45g/L；
Wide warm oxidant 15g/L；
Aluminium ion 5g/L；
Remaining is water.
(4) wash, dry
Alloy matrix aluminum after anodized is cleaned with deionized water, drying and processing, drying and processing temperature are carried out after washing
Spend for 80 DEG C, the drying and processing time is 30 minutes.
The scanning electron microscope (SEM) photograph of the anode oxide film on the aluminum alloy base material surface after above-mentioned processing 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 the aluminum alloy base material surface after above-mentioned processing
Electron microscope is retouched, Fig. 6 is the enlarged drawing of Blocked portion in Fig. 5.From figure 3, it can be seen that the anodic oxidation using the present embodiment
The top layer uniform ground of anode oxide film prepared by method, and there is good gloss.From fig. 4, it can be seen that the anode
It is cellular porous subsurface stratum below oxide-film wearing coat.Measuring the anode oxide film by ESEM has three-layered node
Structure, it is screen layer, porous subgrade, and wearing coat respectively.
The top layer that the anode oxide film prepared after above-mentioned processing in aluminum alloy surface is analyzed by XPS spectrum figure and XRD spectra is
Amorphous Al2O3.By microhardness measure the anode oxide film microhardness reach 250-300Hv, wear rate is
3.2×10-4-6.41×10-4mm3/ Nm, wear resistance and corrosion resistance are good, and now anode oxide film color is deeper, while also have good
Gloss.
Embodiment 2：
In the present embodiment, the anode oxide film of aluminium alloy matrix surface has three-decker, i.e. from alloy matrix aluminum to surface
It is followed successively by screen layer, porous subsurface stratum, wearing coat.
The preparation method of the anode oxide film of above-mentioned aluminium alloy matrix surface comprises the following steps：
(1) mechanically polish
Alloy matrix aluminum is subjected to three-stage polishing, aluminium alloy is subjected to rough polishing first, then carries out fine polishing, it is most laggard
Row finishing polish, finally obtains mirror effect.
(2) ungrease treatment
Aluminium alloy after polishing is subjected to ungrease treatment, degreasing agent is the alkali lye that mass fraction is 15%, and this alkali lye is hydrogen-oxygen
Change at least one of sodium, sodium carbonate and sodium phosphate, 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, negative electrode is aluminium alloy,
Oxidate current is 6A/dm2, oxidation current is direct current constant current, and oxidizing temperature is room temperature, oxidization time 50min；
The bath composition is as follows：
Sulfuric acid 90g/L；
Wide warm oxidant 12g/L；
Aluminium ion 10g/L；
Remaining is water.
(4) wash, dry
Alloy matrix aluminum after anodized is cleaned with deionized water, drying and processing, drying and processing temperature are carried out after washing
Spend for 60 DEG C, the drying and processing time is 35 minutes.
The scanning electron microscope (SEM) photograph of the anode oxide film prepared after above-mentioned processing in aluminum alloy surface is similar to Figure 3, and its section is swept
Retouch the sun for the aluminium alloy matrix surface that electron microscope obtains similar to the anode oxidation method for shown in Fig. 5 and Fig. 6, showing the present embodiment
Pole oxide-film thickness and uniformly, there is good gloss.Measuring the anode oxide film by ESEM has three-decker,
It is screen layer, porous subgrade, and wearing coat respectively.
The top layer that the anode oxide film prepared after above-mentioned processing in aluminum alloy surface is analyzed by XPS spectrum figure and XRD spectra is
Amorphous Al2O3.Measuring the microhardness of the anode oxide film by microhardness, to reach 410-450Hv, wear rate low
6.21×10-5-9.1×10-5mm3/ Nm, wear resistance and corrosion resistance are good, and this anode oxidation membrane color is shallower, while has good
Gloss.
Embodiment 3
In the present embodiment, the anode oxide film of aluminium alloy matrix surface has three-decker, i.e. from alloy matrix aluminum to surface
It is followed successively by screen layer, porous subsurface stratum, wearing coat.
The preparation method of the anode oxide film of above-mentioned aluminium alloy matrix surface comprises the following steps：
(1) mechanically polish
Alloy matrix aluminum is subjected to three-stage polishing, aluminium alloy is subjected to rough polishing first, then carries out fine polishing, it is most laggard
Row finishing polish, finally obtains mirror effect.
(2) ungrease treatment
Aluminium alloy after polishing is subjected to ungrease treatment, degreasing agent is the alkali lye that mass fraction is 15%, and this alkali lye is hydrogen-oxygen
Change at least one of sodium, sodium carbonate and sodium phosphate, 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, negative electrode is aluminium alloy,
Oxidate current is 8A/dm2, oxidation current is direct current constant current, and oxidizing temperature is room temperature, oxidization time 40min；
The bath composition is as follows：
Sulfuric acid 180g/L；
Wide warm oxidant 14g/L；
Aluminium ion 6g/L；
Remaining is water.
(4) wash, dry
Alloy matrix aluminum after anodized is cleaned with deionized water, drying and processing, drying and processing temperature are carried out after washing
Spend for 80 DEG C, the drying and processing time is 30 minutes.
The scanning electron microscope (SEM) photograph of the anode oxide film prepared after above-mentioned processing in aluminum alloy surface is similar to Figure 3, and its section is swept
Retouch the sun for the aluminium alloy matrix surface that electron microscope obtains similar to the anode oxidation method for shown in Fig. 5 and Fig. 6, showing the present embodiment
Pole oxide-film thickness and uniformly, there is good gloss.Measuring the anode oxide film by ESEM has three-decker,
It is screen layer, porous subgrade, and wearing coat respectively.
The top layer that the anode oxide film prepared after above-mentioned processing in aluminum alloy surface is analyzed by XPS spectrum figure and XRD spectra is
Amorphous Al2O3.Measuring the microhardness of the anode oxide film by microhardness, to reach 380-420Hv, wear rate low
9.21×10-5-1。1×10-4mm3/ Nm, wear resistance and corrosion resistance are good, while also have good gloss.
Embodiment 4
In the present embodiment, the anode oxide film of aluminium alloy matrix surface has three-decker, i.e. from alloy matrix aluminum to surface
It is followed successively by screen layer, porous subsurface stratum, wearing coat.
The preparation method of the anode oxide film of above-mentioned aluminium alloy matrix surface comprises the following steps：
(1) mechanically polish
Alloy matrix aluminum is subjected to three-stage polishing, aluminium alloy is subjected to rough polishing first, then carries out fine polishing, it is most laggard
Row finishing polish, finally obtains mirror effect.
(2) ungrease treatment
Aluminium alloy after polishing is subjected to ungrease treatment, degreasing agent is the alkali lye that mass fraction is 20%, and this alkali lye is hydrogen-oxygen
Change at least one of sodium, sodium carbonate and sodium phosphate, 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, negative electrode is aluminium alloy,
Oxidate current is 10A/dm2, oxidation current is direct current constant current, and oxidizing temperature is room temperature, oxidization time 30min；
The bath composition is as follows：
Sulfuric acid 180g/L；
Wide warm oxidant 15g/L；
Aluminium ion 6g/L；
Remaining is water.
(4) wash, dry
Alloy matrix aluminum after anodized is cleaned with deionized water, drying and processing, drying and processing temperature are carried out after washing
Spend for 60 DEG C, the drying and processing time is 35 minutes.
The scanning electron microscope (SEM) photograph of the anode oxide film prepared after above-mentioned processing in aluminum alloy surface is similar to Figure 3, and its section is swept
Retouch the sun for the aluminium alloy matrix surface that electron microscope obtains similar to the anode oxidation method for shown in Fig. 5 and Fig. 6, showing the present embodiment
Pole oxide-film thickness and uniformly, there is good gloss.Measuring the anode oxide film by ESEM has three-decker,
It is screen layer, porous subgrade, and wearing coat respectively.
The top layer that the anode oxide film prepared after above-mentioned processing in aluminum alloy surface is analyzed by XPS spectrum figure and XRD spectra is
Amorphous Al2O3.By microhardness measure the anode oxide film microhardness reach 290-360Hv, wear rate is
1.23×10-4-4.3×10-4mm3/ Nm, wear resistance and corrosion resistance are good, while also have 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 this
The specific embodiment of invention, is not intended to limit the invention.All any modifications made in spirit of the present invention, supplement
Or equivalent substitution etc., it should be included in the scope of the protection.
Claims (10)
1. a kind of have porous subsurface stratum and the aluminium alloy anode oxide film of wearing coat concurrently, it is characterized in that：Described anode
Oxide-film is followed successively by screen layer, porous subsurface stratum and wearing coat from matrix outward.
2. have porous subsurface stratum and the aluminium alloy anode oxide film of wearing coat concurrently as claimed in claim 1, its feature
It is：The thickness of described anode oxide film is 40 μm -50 μm.
3. have porous subsurface stratum and the aluminium alloy anode oxide film of wearing coat concurrently as claimed in claim 1 or 2, its
It is characterized in：The microhardness of described wearing coat is more than 250Hv, and abrasion is measured through UMT-3 friction wear testing machines
Rate is 6.41 × 10-4mm3/ below Nm.
4. have the system of porous subsurface stratum and the aluminium alloy anode oxide film of wearing coat concurrently as claimed in claim 1 or 2
Preparation Method, it is characterized in that：Using anodizing, using alloy matrix aluminum as anode, using aluminium alloy as negative electrode, electricity
Solving liquid includes sulfuric acid, wide warm oxidant and aluminium ion, by controlling oxidation current density, electrolyte prescription control sun
The speed of growth and dissolution velocity of pole oxide-film.
5. have the preparation side of porous subsurface stratum and the aluminium alloy anode oxide film of wearing coat concurrently as claimed in claim 4
Method, it is characterized in that：Alloy matrix aluminum is pre-processed before anodized.
6. have the preparation side of porous subsurface stratum and the aluminium alloy anode oxide film of wearing coat concurrently as claimed in claim 4
Method, it is characterized in that：Oxidation current is direct current constant current, oxidate current 4-10A/dm2。
7. have the preparation side of porous subsurface stratum and the aluminium alloy anode oxide film of wearing coat concurrently as claimed in claim 4
Method, it is characterized in that：The electrolyte prescription is：The wide temperature oxidant of 45-180g/L sulfuric acid, 10-15g/L, 5-10g/L
Aluminium ion.
8. have the preparation side of porous subsurface stratum and the aluminium alloy anode oxide film of wearing coat concurrently as claimed in claim 4
Method, it is characterized in that：Oxidization time is 30-60min, and oxidizing temperature is preferably room temperature.
9. have the preparation side of porous subsurface stratum and the aluminium alloy anode oxide film of wearing coat concurrently as claimed in claim 4
Method, it is characterized in that：Described wide temperature oxidant be phosphoric acid, oxalic acid, tartaric acid, in pyruvic acid it is one or two kinds of with
On mixing.
10. have the preparation side of porous subsurface stratum and the aluminium alloy anode oxide film of wearing coat concurrently as claimed in claim 4
Method, it is characterized in that：Described source of aluminum ion include aluminium hydroxide, aluminum sulfate, in meta-aluminate it is one or two kinds of with
On mixing.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112095132A (en) * | 2020-09-08 | 2020-12-18 | 池州市安安新材科技有限公司 | Method for anodizing surface of high-corrosion-resistance aluminum profile |
| CN114540912A (en) * | 2021-12-20 | 2022-05-27 | 西北大学 | Treatment method for low-friction solid-liquid composite lubrication of aluminum-lithium alloy surface |
| CN115548589A (en) * | 2022-10-24 | 2022-12-30 | 楚能新能源股份有限公司 | Bus bar for battery module and preparation method thereof |
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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 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112095132A (en) * | 2020-09-08 | 2020-12-18 | 池州市安安新材科技有限公司 | Method for anodizing surface of high-corrosion-resistance aluminum profile |
| CN114540912A (en) * | 2021-12-20 | 2022-05-27 | 西北大学 | Treatment method for low-friction solid-liquid composite lubrication of aluminum-lithium alloy surface |
| 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 |
| CN115548589A (en) * | 2022-10-24 | 2022-12-30 | 楚能新能源股份有限公司 | Bus bar for battery module and preparation method thereof |
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