CN101413139B - Aluminum alloy including differential arc oxidation film and preparation thereof - Google Patents
Aluminum alloy including differential arc oxidation film and preparation thereof Download PDFInfo
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- CN101413139B CN101413139B CN2007101636936A CN200710163693A CN101413139B CN 101413139 B CN101413139 B CN 101413139B CN 2007101636936 A CN2007101636936 A CN 2007101636936A CN 200710163693 A CN200710163693 A CN 200710163693A CN 101413139 B CN101413139 B CN 101413139B
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Abstract
The invention provides an aluminum alloy comprising a micro-arc oxidation film. The aluminum alloy comprises an aluminum alloy substrate and the micro-arc oxidation film on the aluminum alloy substrate, wherein the aluminum alloy also comprises a hole-sealing coating which is covered on the micro-arc oxidation film. The aluminum alloy has very good smudginess resisting performance.
Description
Technical field
The present invention relates to a kind of aluminium alloy that comprises micro-arc oxidation films, also relate to the preparation method that this comprises the aluminium alloy of micro-arc oxidation films.
Background technology
Differential arc oxidation (MAO) is a kind of technology that material surface is handled, be as an anode with the pending metal in the immersion differential arc oxidation electrolytic solution, another metal is as negative electrode, voltage between the two poles of the earth surpasses certain limit, electrode surface produces micro-arc discharge, concurrent living physical-chemical reaction, thus ceramic membrane generated as the pending metallic surface of anodic original position.The micro-arc oxidation films that is obtained has excellent high temperature resistant, wear-resistant and corrosion resistant performance, and hardness is very high.Thereby the metal product of handling through differential arc oxidation can be widely used in Aeronautics and Astronautics, automobile, building and electron trade.
But, metal is carried out the micropore that can there be a lot of 1-10 μ m in micro-arc oxidation films surface after differential arc oxidation is handled, this discharges in the differential arc oxidation process and causes.Because exist these micropores to make the anti-pollution energy of micro-arc oxidation films relatively poor, glossiness is lower, thereby can influence the decoration and the aesthetic of micro-arc oxidation films.Therefore be necessary that micro-arc oxidation films is carried out sealing of hole to be handled.
At " the SiO of magnesium alloy differential arc oxidation film
2The colloidal sol sealing of hole is handled research " a kind of hole sealing agent and sealing of hole treatment process that is used for the magnesium alloy differential arc oxidation film sealing of hole disclosed in (" Special Processes of Metal Castings and non-ferrous alloy " 2006 the 26th the 10th phases of volume); adopt in the document tetraethoxy; dehydrated alcohol and distilled water mixed in 4: 3: 1.28 by volume; add an amount of hydrochloric acid and mix as catalyzer; thus SiO2 colloidal sol made; SiO2 colloidal sol is carried out sealing of hole as hole sealing agent to the micro-arc oxidation films of magnesium alloy, can make this colloidal sol immerse in the hole of differential arc oxidation film layer and fill up hole, form effective sealing of hole.
Yet, with this SiO
2When colloidal sol was applied to seal the micropore of micro-arc oxidation films of aluminum alloy surface as hole sealing agent, the sealing of hole effect was relatively poor, thereby made the anti-pollution of this product can be relatively poor.And, also the micro-arc oxidation films of aluminium alloy is not carried out the effective hole sealing agent of sealing of hole so far.
Summary of the invention
The objective of the invention is to overcome above-mentioned SiO of the prior art
2The colloidal sol hole sealing agent makes the relatively poor defective of micro-arc oxidation films anti-pollution energy of aluminum alloy surface, provide a kind of anti-pollution of the micro-arc oxidation films of aluminum alloy surface that makes to comprise the aluminium alloy of micro-arc oxidation films preferably, and provide this to comprise the preparation method of the aluminium alloy of micro-arc oxidation films.
The invention provides a kind of aluminium alloy that comprises micro-arc oxidation films, described aluminium alloy comprises the micro-arc oxidation films of alloy matrix aluminum and aluminium alloy matrix surface, wherein, described aluminium alloy also comprises the sealing of hole thing, and described sealing of hole thing is positioned at the micropore on the described micro-arc oxidation films and/or is positioned at the surface of described micro-arc oxidation films.
The present invention also provides a kind of preparation method who comprises the aluminium alloy of micro-arc oxidation films, this method is included on the surface of aluminium alloy and forms micro-arc oxidation films, it is characterized in that this method also is included in the micropore on the described micro-arc oxidation films and/or the surface is gone up and formed the sealing of hole thing.
Aluminium alloy that comprises micro-arc oxidation films provided by the invention and preparation method thereof, can make the anti-pollution energy on micro-arc oxidation films surface better, after for example using various makeup (for example hand lotion, lipstick, sun screen and foundation cream) to be coated on the micro-arc oxidation films of aluminium alloy respectively, this micro-arc oxidation films all is not subjected to dirty influence.
Description of drawings
Fig. 1 is the electron-microscope scanning figure in the cross section before the aluminum alloy surface microarc oxide film hole sealing among the embodiment 1;
Fig. 2 is the electron-microscope scanning figure in the cross section behind the aluminum alloy surface microarc oxide film hole sealing among the embodiment 1;
Fig. 3 is for adopting SiO of the prior art
2Colloidal sol carries out the electron-microscope scanning figure in the cross section behind the sealing of hole to the micro-arc oxidation films of aluminum alloy surface.
Embodiment
The aluminium alloy that comprises micro-arc oxidation films provided by the invention, described aluminium alloy comprises the micro-arc oxidation films of alloy matrix aluminum and aluminium alloy matrix surface, wherein, described aluminium alloy also comprises the sealing of hole thing, and described sealing of hole thing is positioned at the micropore on the described micro-arc oxidation films and/or is positioned at the surface of described micro-arc oxidation films.
According to aluminium alloy provided by the invention, in the preferred case, the weight of sealing of hole thing is 0.001-1 gram/cm on the described micro-arc oxidation films of unit surface
2
According to aluminium alloy provided by the invention, in the preferred case, at least 90% micropore quantity is covered by the sealing of hole thing on the described micro-arc oxidation films, and more preferably at least 95% micropore quantity is covered by the sealing of hole thing.
According to aluminium alloy provided by the invention, in the preferred case, described sealing of hole thing is formed by hole sealing agent, and described hole sealing agent is one or more in Green's ceramic stain control agent, acrylic resin and the organosilicon hole sealing agent.Described hole sealing agent is preferably Green's ceramic stain control agent, described Green's ceramic stain control agent contains organosilane and the mixing solutions of siloxanes in petroleum solvent, gross weight with Green's ceramic stain control agent is a benchmark, the content of described organosilane and mixture of siloxanes is 0.2-10 weight %, the content of described petroleum solvent is 80-99% weight, wherein the weight ratio of organosilane and siloxanes is 1: 0.01-100 is preferably 1: 0.1-10.Described Green's ceramic stain control agent can be selected the product that is purchased for use, and for example the trade mark of the Green of Foshan City ceramic technology company limited is Green's ceramic stain control agent of 2332.
" petroleum solvent " described herein is for distilling the narrower light oil fraction of gained boiling spread through refining getting such as soda acids by petroleum crude oil through normal pressure.Main component is alkane, naphthenic hydrocarbon and a small amount of aromatic hydrocarbons, does not contain any additives.Petroleum solvent is usually by 98% recovered temperature or do (100% recovered temperature) and be divided into the trades mark such as 70,90,120,180,190,200.No. 70 petroleum solvents also claim perfume extraction solvent, boiling range 60-70 ℃; No. 90 petroleum solvents also claim sherwood oil, boiling range 60-90 ℃; No. 120 petroleum solvents also claim rubber solvent naphtha, boiling range 80-120 ℃; No. 180 petroleum solvents also claim the aviation washing oil, boiling range 40-180 ℃; No. 190 petroleum solvents also claim non-leaded gasoline, boiling range 40-190 ℃; No. 200 petroleum solvents also claim varnish makers' and painters' naphtha.Petroleum solvent of the present invention can be the petroleum solvent of the above-mentioned various trades mark.
According to aluminium alloy provided by the invention, the thickness of micro-arc oxidation films is the 2-300 micron.
The preparation method who comprises the aluminium alloy of micro-arc oxidation films provided by the invention is included on the surface of aluminium alloy and forms micro-arc oxidation films, and wherein, this method also is included in the micropore on the described micro-arc oxidation films and/or the surface is gone up and formed the sealing of hole thing.
According to preparation method provided by the invention, in the preferred case, the formation method of described sealing of hole thing comprises, applies hole sealing agent on described micro-arc oxidation films, and is dry then, and at least 90% micropore quantity is covered by the sealing of hole thing.
Preparation in accordance with the present invention, the method that applies hole sealing agent on described micro-arc oxidation films can adopt various coating methods, the aluminium alloy that for example will comprise micro-arc oxidation films is put into hole sealing agent immersion 0-5 minute, take out then, before this aluminium alloy drying with cotton wiping repeatedly, till the micro-arc oxidation films surface evenly, perhaps directly hole sealing agent is applied on the micro-arc oxidation films of this aluminum alloy surface, this aluminium alloy is put into baking box and is toasted under 40-100 ℃ temperature this aluminium alloy drying then, also can dry without the baking nature.
According to preparation method provided by the invention, the described method of micro-arc oxidation films that forms on the surface of aluminium alloy is for well known to a person skilled in the art method, for example this method comprises, aluminium alloy is placed the electrolyzer that fills electrolyte solution, with the aluminium alloy is anode, electrolyzer is as negative electrode, and the condition of differential arc oxidation makes aluminum alloy surface form the thick micro-arc oxidation films of 2-300 micron that is; The condition of described differential arc oxidation comprises that current density is 0.5-10A/dm
2, voltage is the 400-600 volt, and the temperature of electrolyte solution is 15-60 ℃, and the time of differential arc oxidation is 2-60 minute.
The electrolytic solution that is used to carry out differential arc oxidation can adopt and well known to a person skilled in the art various electrolytic solution, for example adopt the electrolytic solution that contains Sodium hexametaphosphate 99, water glass and sodium hydroxide, the prescription of this electrolytic solution and the content of each composition are Sodium hexametaphosphate 99 30-40g/L, water glass 2-10g/L, sodium hydroxide 0.5-5g/L.
Adopt the mode of embodiment that the present invention is described in further detail below.
Embodiment 1
Selecting model for use is that 6061 aluminum alloy materials prepares the aluminium alloy gold that comprises micro-arc oxidation films of the present invention
1, the pre-treatment of aluminum alloy materials
Above-mentioned Al alloy parts is immersed the basic solution that contains sodium hydroxide 30 grams per liters, sodium phosphate 40 grams per liters, water glass 20 grams per liters aluminum alloy base material is carried out degreasing.The temperature of degreasing is 85 ℃, and the time of degreasing is 8 minutes.Washed then 5 minutes.
2, the differential arc oxidation of aluminum alloy materials
The immersion of Al alloy parts after the above-mentioned degreasing is contained Sodium hexametaphosphate 99 35g/L, and water glass 6g/L in the electrolytic solution of sodium hydroxide 1.2g/L, is an anode with the Al alloy parts, is that negative electrode carries out differential arc oxidation with the stainless steel plate.In current density is 0.5-10A/dm
2, voltage is 400-600 volt, and the temperature of electrolyte solution is to carry out differential arc oxidation under 25 ℃ the condition, and the time of differential arc oxidation is 15 minutes, and having formed thick at aluminum alloy material surface is 8 microns micro-arc oxidation films.With the surface of electronics scanning electron microscopic observation micro-arc oxidation films, resulting electronic scanning Electronic Speculum figure sees Fig. 1.
3, the sealing of hole of micro-arc oxidation films is handled
The above-mentioned aluminium alloy that has formed micro-arc oxidation films is put into Green's ceramic stain control agent (Foshan City Green's ceramic technology company limited trade mark is 2332) to be soaked 2 minutes, take out then, even with this aluminum alloy surface of non-dust cloth wiping until the surface, there is not any vestige, put into then in the baking box and under 80 ℃ temperature, toasted 8 hours, formation is positioned at differential arc oxidation membrane micropore and lip-deep sealing of hole thing, obtains the aluminium alloy that comprises micro-arc oxidation films of the present invention.The weight that records sealing of hole thing on the unit surface micro-arc oxidation films is 0.1 gram/cm
2, at least 90% micropore quantity is covered by the sealing of hole thing on the micro-arc oxidation films.With the sealing of hole thing on the surface of electronics scanning electron microscopic observation micro-arc oxidation films, resulting electronic scanning Electronic Speculum figure sees Fig. 2.
Comparative Examples 1
Adopt SiO of the prior art
2Colloidal sol carries out sealing of hole as hole sealing agent to the aluminium alloy that carries out behind the differential arc oxidation.
According to pre-treatment and the differential arc oxidation method described among the embodiment 1 aluminium alloy is carried out pre-treatment and differential arc oxidation respectively.
Then, be mixing in 4: 3: 1.28 by volume with tetraethoxy, dehydrated alcohol and distilled water, add an amount of hydrochloric acid as catalyzer, stirred 2 hours with magnetic stirrer, finally obtain water white SiO
2Colloidal sol.
The above-mentioned aluminium alloy that has carried out the differential arc oxidation processing is immersed resulting SiO
2In the colloidal sol 20 seconds, mention equably with certain speed then, allow bottom colloidal sol fall to the greatest extent, after 5-10 minute, form the clear gel film that partly solidifies on the micro-arc oxidation films surface, seasoning at room temperature 24 hours is put into chamber type electric resistance furnace again and slowly is heated to 300 ℃ and be incubated 10 minutes, makes the hole sealing coating on micro-arc oxidation films surface.
With the hole sealing coating on the surface of electronics scanning electron microscopic observation micro-arc oxidation films, resulting electronic scanning Electronic Speculum figure sees Fig. 3.
Performance test
1, uses the electronics scanning electron microscopic observation
From Fig. 1,2,3 electronic scanning Electronic Speculum as can be seen the sample before the sealing of hole to have a lot of diameters be the hole of 1-10 micron, substantially filled and led up with sample surfaces hole behind Green's ceramic stain control agent sealing of hole, and adopted the also residual more hole of sample surfaces behind the sol-gel method sealing of hole among Fig. 3.
2, anti-pollution can be tested
Get on the hole sealing coating that an amount of hand lotion, lipstick, sun screen and foundation cream be coated to the micro-arc oxidation films surface of the aluminium alloy before the sealing of hole among the embodiment 1 and the aluminum alloy differential arc oxidation film behind the sealing of hole respectively and in the Comparative Examples 1 on the hole sealing coating of the aluminum alloy differential arc oxidation film behind the sealing of hole, in air, placed 24 hours, use the clear water flush away then, place that there is no change on the observation sample surface after 2 hours.
Observing test back sample surfaces does not have and changes into qualifiedly, and observing sample surfaces, to leave vestige be defective.Table 1 is the resulting result of above-mentioned test.
Table 1
| Hand lotion | Lipstick | Sun screen | Foundation cream | ||
| Embodiment 1 | Before the sealing of hole | Defective | Defective | Defective | Defective |
| Behind the sealing of hole | Qualified | Qualified | Qualified | Qualified | |
| Embodiment 2 | Behind the sealing of hole | Qualified | Qualified | Qualified | Qualified |
| Comparative Examples 1 | Behind the sealing of hole | Qualified | Defective | Qualified | Defective |
From the test result of table 1 as can be seen, the anti-pollution of the micro-arc oxidation films of aluminum alloy surface before sealing of hole can be relatively poor, and the anti-pollution behind the sealing of hole can be fine, and quite a lot of when in the Comparative Examples 1 though the micro-arc oxidation films of aluminum alloy surface being carried out anti-pollution energy behind the sealing of hole than sealing of hole not, can be poor than the anti-pollution of the aluminium alloy that comprises micro-arc oxidation films that is obtained in the embodiments of the invention 1.
Claims (7)
1. aluminium alloy that comprises micro-arc oxidation films, described aluminium alloy comprises the micro-arc oxidation films of alloy matrix aluminum and aluminium alloy matrix surface, it is characterized in that, described aluminium alloy also comprises the sealing of hole thing, described sealing of hole thing is positioned at the micropore on the described micro-arc oxidation films and/or is positioned at the surface of described micro-arc oxidation films, described sealing of hole thing is formed by hole sealing agent, described hole sealing agent is Green's ceramic stain control agent, described Green's ceramic stain control agent contains organosilane and the mixing solutions of siloxanes in petroleum solvent, gross weight with Green's ceramic stain control agent is a benchmark, the total content of described organosilane and siloxanes is 0.2-10 weight %, the content of described petroleum solvent is 80-99 weight %, and wherein the weight ratio of organosilane and siloxanes is 1: 0.01-100.
2. aluminium alloy according to claim 1, wherein, the weight of sealing of hole thing is 0.001-1 gram/cm on the described micro-arc oxidation films of unit surface
2
3. aluminium alloy according to claim 1, wherein, at least 90% micropore quantity is covered by the sealing of hole thing on the described micro-arc oxidation films.
4. aluminium alloy according to claim 1, wherein, in described Green's ceramic stain control agent, the weight ratio of organosilane and siloxanes is 1: 0.1-10.
5. aluminium alloy according to claim 1, wherein, the thickness of micro-arc oxidation films is the 2-300 micron.
6. described preparation method who comprises the aluminium alloy of micro-arc oxidation films of claim 1, this method is included on the surface of aluminium alloy and forms micro-arc oxidation films, it is characterized in that, this method also is included in the micropore on the described micro-arc oxidation films and/or the surface is gone up and formed the sealing of hole thing, the formation method of described sealing of hole thing comprises, on described micro-arc oxidation films, apply hole sealing agent, dry then, at least 90% micropore quantity is covered by the sealing of hole thing; Described hole sealing agent is Green's ceramic stain control agent, described Green's ceramic stain control agent contains organosilane and the mixing solutions of siloxanes in petroleum solvent, gross weight with Green's ceramic stain control agent is a benchmark, the total content of described organosilane and siloxanes is 0.2-10 weight %, the content of described petroleum solvent is 80-99 weight %, and wherein the weight ratio of organosilane and siloxanes is 1: 0.01-100.
7. preparation method according to claim 6, wherein, described method of adhering to micro-arc oxidation films on the surface of aluminium alloy comprises, aluminium alloy is placed the electrolyzer that fills electrolyte solution, with the aluminium alloy is anode, electrolyzer is as negative electrode, and the condition of differential arc oxidation makes aluminum alloy surface form the thick micro-arc oxidation films of 2-300 micron that is; The condition of described differential arc oxidation comprises that current density is 0.5-10A/dm
2, voltage is the 400-600 volt, and the temperature of electrolyte solution is 15-60 ℃, and the time of differential arc oxidation is 2-60 minute.
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