CN103498179B - Aluminum or aluminum alloy surface oxide film and method for preparing same - Google Patents
Aluminum or aluminum alloy surface oxide film and method for preparing same Download PDFInfo
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- CN103498179B CN103498179B CN201310498581.1A CN201310498581A CN103498179B CN 103498179 B CN103498179 B CN 103498179B CN 201310498581 A CN201310498581 A CN 201310498581A CN 103498179 B CN103498179 B CN 103498179B
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Abstract
The invention discloses an aluminum or aluminum alloy surface oxide film and a method for preparing the aluminum or aluminum alloy surface oxide film. The method includes the following steps that firstly, an oxide film is formed by aluminum or aluminum alloy in an electrolyte through anodic oxidation, the electrolyte comprises sulfuric acid, nanosilicon dioxide, acrylic resin and rare-earth metal of cerate or neodymium salt; then, hole pre-sealing treatment is performed, the aluminum or the aluminum alloy undergoing the anodic oxidation is placed in trivalent chromium hole sealing liquid containing nickel ions for performing hole sealing, the hole sealing degree of the oxide film is made to reach at least 90%; finally, second-step hole sealing treatment is performed, hole sealing treatment is performed in an alkaline aqueous solution of nanoscale particles containing acrylic resin and silicon dioxide, then washing and drying are performed, and at last, the anodic oxide film undergoing double hole sealing treatment is formed. The oxide film prepared by the method has the excellent functions of preventing corrosion damage of salt mist, fungi and damp and hot at the same time.
Description
Technical field
The present invention relates to a kind of preparation method and aluminum or aluminum alloy surface film oxide obtained by this method of aluminum or aluminum alloy surface film oxide.
Background technology
Aluminium alloy due to lightweight, specific tenacity is high, more and more wider in the every field application of national economy and national defense construction.Particularly the application on the carrier-borne product in modern national defense field has been only second to iron and steel, accounts for second.But aluminium alloy in actual applications, distinct issues are that " three is anti-" (preventing salt fog, damp and hot, mould) performance haves much room for improvement.Especially in harsh marine corrosion environment, owing to being subject to the acting in conjunction of the corrosion factor such as etch, pitting, hard power cracking of high humidity and sea-salt fine particle, the life-span of alloy product shortens greatly.Because applying to exist, aluminum alloy surface produces underfilm corrosion problem because bonding force is bad; alloy product under the military service Yu Haiyang climatopes such as many Shipborne Electronic Equipment, radar and ocean weaponry; all with surface electrochemistry conversion film as rot-resistant first-selection; this zone of oxidation generating with electrolysis mode; can protect metal base; prevent its corrosion and weathering, increase surperficial flintiness and wear resisting property.
In numerous aluminium surface conversion coating technique, only have the corrosion resistance nature of differential arc oxidation can be called outstanding (the resistance to neutral salt spray test time can reach 600h), but, due to reasons such as differential arc oxidation film forming overtension, difficulty of processing are large, dimensional change amount is large, its application in electronics and the each field of equipment is restricted.At present in the world, the separately Conversion Coatings on Aluminum Alloys taking surface anticorrosion as object, the effective employing anode oxidation process that is still.Aluminum anodized film is combined with matrix firmly, hard wear resistant, and thermotolerance is very outstanding, but the resistance to neutral salt spray test time seldom exceedes 336h(14 cycle), this corrosion resisting property is substantially enough at general applied environment, but under ocean environment, has become a difficult problem.Generally praise highly in the world by improving oxidation filming quality and improve anti-corrosion capability, its process means is numerous, mainly contains: improve film density, reduce its porosity; Increase oxide thickness; Change oxide film self current potential.
Anodised film forming feature is: the atomic oxygen that anode produces is combined with body aluminium, generates aluminium sesquioxide rete.The further growth of oxide film, is by the dual function of anode electric field and electrolytic solution dissolving, makes atomic oxygen arrive aluminium body, forms oxide film.So aluminum anodized film is made up of non-porous layer and porous layer (being called again blocking layer) two portions.The anode oxidation process generally adopting has: sulphuric acid anodizing, oxalic acid anodizing and nitration mixture hard anodizing.The aftertreatment hole-sealing technology matching with it has: F-Ni system low temperature pore sealing method, dichromate pore sealing method, boiling water high temperature hole sealing method etc.The barrier propterty that is to say anode oxide film is by the lifting common guarantee of quality of forming film and sealing quality, there is no such understanding, does not just have high-quality anti-seawater oxide film.
CN1272469 C, by the method for the sacrificial aluminium alloy anode of interpolation cerium (Ce), makes the obvious refinement of aluminium alloy crystal grain, and more even, has reduced the degree of oxidation of aluminium and the current potential of impurity phase, has reduced the corrosion that microbattery (claiming again galvanic couple) causes.
The people such as Lu Min adopt electrochemistry approach, in aluminium alloy electrolysis process, nano levelly be prepared into and mix silicon complex oxide film containing silicon particle mixing in electrolytic solution, this oxide film has embodied the process of silicon and metal codeposition, film density has improved 10%, porosity reduces nearly four times, has obtained good barrier propterty.
These two kinds of methods were very obvious to the improvement of oxide film protective capacities in the last few years, but the former has just solved micro-cell corrosion problem; And the latter is mainly the porosity by reducing oxide film, improve rete density, to a certain degree promote the barrier propterty of oxide film.They cannot resist the salt fog under ocean environment, the corrosion failure that damp and hot, mould is caused simultaneously.
Promoting the protective of oxide film by improving sealing of hole, is another kind of striving direction.
Have a kind of method of with silicate solutions, anodizing of aluminium film being carried out sealing of hole processing, but the aluminum oxide rete that this method makes is very thin, the standard that the sealing of hole time also need to reach far below conventional industry.Experiment shows, although aluminium and silicon have good avidity, the oxide film that makes sealing of hole processing of silicate has obviously promoted its alkaline resistance properties, and other aspects are not improved.
Summary of the invention
In order to overcome the above problems, the invention provides a kind of preparation method and oxide film obtained by this method of aluminum or aluminum alloy surface film oxide.By changing aluminium alloy anode oxide thin film-forming method and aftertreatment hole-sealing technology method, the filmogen of the different functionalities that anodic oxidation and sealing of hole produce is superimposed upon on same oxide film, this oxide film has the good function that prevents salt fog, mould and damp and hot corrosion failure simultaneously, therefore be called " three is anti-" oxide film.
Technical program of the present invention lies in: to achieve these goals, the invention provides a kind of preparation method of aluminum or aluminum alloy surface film oxide, it is characterized in that the method comprises the following steps: first, aluminum or aluminum alloy forms oxide film by anodic oxidation in electrolytic solution, and described electrolytic solution comprises sulfuric acid, nano silicon, acrylic resin and rare earth metal cerium salt or neodymium salt; Then, carry out pre-sealing of hole processing, carry out sealing of hole by putting into through anodised aluminum or aluminum alloy the trivalent chromium pore-sealing liquid that contains nickel ion, make the sealing of hole degree of oxide film reach at least 90%; Finally, carry out the processing of second step sealing of hole, in the alkaline aqueous solution of the nanometer particle that contains acrylic resin and silicon-dioxide, carry out sealing of hole processing, then wash, be dried, the final anode oxide film forming through two step sealing of hole processing.
The each concentration of component of anodic oxidation electrolyte of the present invention is: sulfuric acid 150-200g/l, and nano silicon 1-3.5g/l, acrylic resin 0.9-3g/l, rare earth metal cerium salt or neodymium salt, count 0.5-1g/l with cerium or neodymium; Technological specification is: direct current or the pulse power for power acquisition, current density is 1-2A/dm
2, under the voltage of 18-22V, electrolysis 30-50min, tank liquor temperature 10-22 DEG C.Process by this step, can obtain thickness and reach 20 microns of above aluminum anodized films, nano silicon can select acidic silicasol or neutral silicon sol, and it can promote film density more than 15%; Mixing of acrylic resin, can play the effect of mould fungus inhibition, and it makes oxide film increase hydrophobicity simultaneously; Rare earth metal salt can be selected vitriol or the carbonate of cerium or neodymium, and it makes the obvious refinement of aluminium alloy crystal grain, and more even, has reduced the current potential of impurity phase in aluminium alloy, has reduced the corrosion that microbattery causes.
Two zone of oxidation structures that this anode electrolysis generates, a kind of is the very thin non-porous layer (also crying blocking layer) forming in the top of substrate, can play the effect that prevents attack, its thickness is relevant with one-tenth membrane voltage, and this layer probably accounts for 2% of rete total thickness; Another kind is the unformed oxide skin of porous, is the main component of anode oxide film.Therefore, sealing of hole becomes another means of oxide film enhancing protective capacities, for non-corrosibility reaches the strongest, must carry out sealing of hole processing by antianode oxide film.
The present invention takes dual sealing of hole to do the method for aftertreatment, has improved oxide film density and complex protection capability.
Pre-sealing of hole of the present invention is processed the pore-sealing liquid adopting and is comprised: chromium nitrate 1-2g/l, and fluorine zirconic acid 0.4-0.8g/l, trisodium citrate 0.4-0.6g/l, single nickel salt 0.01-0.03g/l, technological specification is: 35 ± 5 DEG C of temperature; PH value 4.5 ± 0.5, time 40 ± 1min or press 1min/ μ m calculate.This trivalent chromium pore-sealing liquid that contains nickel ion, can make the sealing of hole degree of oxide film reach at least 90%.
Second step sealing of hole of the present invention is processed the pore-sealing liquid adopting and is comprised: acrylic resin 45-52g/l, acid esters 0.5-1g/l in dodecyl second, nano silicon 11-15g/l, glycol glycerin ether 5-10g/l, working specification is: under room temperature condition, soak 1-2min.By this processing, generation one deck in oxide film surface has the organic coating film of hydrophobic function.
The present invention also provides a kind of aluminum or aluminum alloy surface film oxide, and wherein, this oxide film is prepared by method of the present invention.
With prior art comparison, the present invention has following outstanding advantages: anode oxide film has good resisting sea water erosion performance; Anode oxide film, in having good resisting sea water erosion performance, also possesses identical with other oxide film ornamental; Anode oxide film has good alkaline resistance properties.
Embodiment
Embodiment 1.
Commercial-purity aluminium " three is anti-" oxide film becomes film test.
Adopt commercial-purity aluminium 1050A, it consists of (massfraction, %): Si≤0.25, and 0.000≤Fe≤0.400, Cu≤0.05, Mn≤0.05, Mg≤0.05, Zn≤0.07, Ti≤0.05, other≤0.03, Al >=99.50.
By test piece polishing, with carrying out again alkali electroless oil removing after acetone degreasing degreasing, then carry out anodic oxidation treatment.Anodic oxidation electrolyte formula: sulfuric acid 180g/l, acidic silicasol 1.5g/l, acrylic resin 0.9g/l, cerium salt 0.5g/l(is in cerium).Be 2A/dm in current density
2, temperature is electrolysis 30min under the condition of 20 DEG C, then washes with deionized water, cold wind dries up.
The pre-pore-sealing liquid of preparation trivalent chromium: chromium nitrate 1.5g/l, fluorine zirconic acid 0.8g/l, trisodium citrate 0.6g/l, single nickel salt 0.03g/l, 35 DEG C of temperature; PH value 4.5 ± 0.5; Sample is put into sealing of hole groove, carry out sealing of hole processing, after 10 minutes, sample is taken out, wash with deionized water, cold wind dries up.
Preparation organic sealing liquid: add acrylic resin 52g/l in sealing of hole groove, acid esters 1g/l in dodecyl second, nano silicon 15g/l, glycol glycerin ether 7.5g/l.Sample is soaked to 3min at ambient temperature, after taking-up, wash with deionized water, cold wind dries up.
Embodiment 2.
Duralumin " three is anti-" oxide film becomes film test.
Adopt duralumin 2A12, it consists of (massfraction, %): Si≤0.50,3.8≤Cu≤4.9,1.2≤Mg≤1.8, Zn≤0.30,0.30≤Mn≤0.90, Ti≤0.15, Ni≤0.10,0.000≤Fe≤0.500,0.000≤Fe+Ni≤0.5000, other≤0.15, surplus is aluminium content.
By test piece polishing, with carrying out again alkali electroless oil removing after acetone degreasing degreasing, then carry out anodic oxidation treatment.Anodic oxidation electrolyte formula: sulfuric acid 200g/l, acidic silicasol 1.5g/l; Acrylic resin 0.9g/l; Cerium salt 0.5g/l(is in cerium), be 2A/dm in current density
2, temperature is electrolysis 50min under the condition of 20 DEG C, then washes with deionized water, cold wind dries up.
The pre-pore-sealing liquid of trivalent chromium in preparation embodiment 1, is poured in sealing of hole groove, bathes 35 DEG C of temperature, sample is put into sealing of hole groove and carry out sealing of hole processing taking-up after 20 minutes, washes with deionized water, and cold wind dries up.
Organic sealing solution in preparation embodiment 1, is poured in sealing of hole groove, at room temperature sample is put into sealing of hole groove and is carried out after sealing of hole is processed 3min taking out, and washes with deionized water, and cold wind dries up, and completes sealing of hole processing.
Embodiment 3.
Aluminium diecast alloy " three is anti-" oxide film becomes film test.
Adopt aluminium diecast alloy YL101, it consists of (massfraction, %): 9.0≤Si≤10.0, and Cu≤0.6, Mn≤0.35,0.45≤Mg≤0.65, Fe≤1.0, Ni≤0.50, Zn≤0.40, Pb≤0.10, Sn≤0.15, all the other are aluminium content.
By test piece polishing, with carrying out again alkali electroless oil removing after acetone degreasing degreasing, then carry out anodic oxidation treatment.Anodic oxidation electrolyte formula: sulfuric acid 200g/l, neutral silicon sol 2g/l; Acrylic resin 0.9g/l; Cerium salt 0.5g/l(is in cerium), be 1.5A/dm in current density
2, temperature is electrolysis 30min under the condition at 20 DEG C, then washes with deionized water, cold wind dries up.
The pre-pore-sealing liquid of preparation embodiment 1 trivalent chromium, is poured in sealing of hole groove, bathes 35 DEG C of temperature, sample is put into sealing of hole groove and carry out sealing of hole processing taking-up after 20 minutes, washes with deionized water, and cold wind dries up.
Preparation embodiment 1 organic sealing solution, is poured in sealing of hole groove, at room temperature sample is put into sealing of hole groove and is carried out after sealing of hole is processed 3min taking out, and washes with deionized water, and cold wind dries up, and completes sealing of hole processing.
Above-mentioned three kinds of samples have represented fine aluminium, wrought aluminium alloy, aluminium diecast alloy, the result of " three the is anti-" performance test to three kinds of Process on Aluminum Alloy Oxidation Film confirms, aluminium alloy " three the is anti-" oxide film that this class is prepared through multi-step, the more conventional aluminum anodized film of its barrier propterty generally exceeds more than 50%.
The concrete weather resistance of oxide film of embodiment 1-3 shows in the following areas.
Clad aluminum or the test of Process on Aluminum Alloy Oxidation Film barrier propterty.
1. after 480h artificial atmosphere corrosion test salt-fog test (GB/T 10125-2012), surface does not change.
2. after 24h copper accelerated acetic acid salt spray test (GB/T 12967.3-2008), surface does not change.
3. after 240h cyclic damp heat test (GJB150.9-86), surface does not change.
4. after 28d mould test (GJB150.10-86), mildew is 0 grade.
5. after 100 DEG C of high temperature test of 1h (GJB150.3-86), on oxide film, there is no obvious crack.
Claims (2)
1. a preparation method for aluminum or aluminum alloy surface film oxide, is characterized in that: the method comprises the following steps: first, aluminum or aluminum alloy forms oxide film by anodic oxidation in electrolytic solution, and described electrolytic solution comprises sulfuric acid, nano level SiO
2, acrylic resin and rare earth metal cerium salt or neodymium salt; Then, carry out pre-sealing of hole processing, carry out sealing of hole by putting into through anodised aluminum or aluminum alloy the trivalent chromium pore-sealing liquid that contains nickel ion, make the sealing of hole degree of oxide film reach at least 90%; Finally, carry out the processing of second step sealing of hole, in the alkaline aqueous solution of the nanometer particle that contains acrylic resin and silicon-dioxide, carry out sealing of hole processing, then wash, be dried, the final anode oxide film forming through dual sealing of hole processing, the each concentration of component of described anodic oxidation electrolyte is: sulfuric acid 150-200g/l, nanometer SiO
21-3.5g/l, acrylic resin 0.9-3g/l, rare earth metal cerium salt or neodymium salt, count 0.5-1g/l with cerium or neodymium, and technological specification is: direct current or the pulse power for power acquisition, current density is 1-2A/dm
2electrolysis 30-50min under the voltage of 18-22V, tank liquor temperature 10-22 DEG C, described pre-sealing of hole is processed the pore-sealing liquid adopting and is comprised: chromium nitrate 1-2g/l, fluorine zirconic acid 0.4-0.8g/l, trisodium citrate 0.4-0.6g/l, single nickel salt 0.01-0.03g/l, technological specification is: 35 ± 5 DEG C of temperature; PH value 4.5 ± 0.5, time 40 ± 1min or press 1min/ μ m calculate, described second step sealing of hole is processed the pore-sealing liquid adopting and is comprised: acrylic resin 45-52g/l, acid esters 0.5-1g/l in dodecyl second, nano silicon 11-15g/l, glycol glycerin ether 5-10g/l, working specification is: under room temperature condition, soak 1-2min.
2. an aluminum or aluminum alloy surface film oxide, is characterized in that: this oxide film is prepared by method claimed in claim 1.
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| CN102817059B (en) * | 2012-08-18 | 2015-05-20 | 佛山金兰铝厂有限公司 | Novel hole sealing tank liquid for aluminum alloy oxidation section and sealing method by using the same |
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| JP2023144470A (en) * | 2022-03-28 | 2023-10-11 | アイシン軽金属株式会社 | Exterior member and manufacturing method thereof |
| WO2024124716A1 (en) * | 2022-12-13 | 2024-06-20 | 合肥汉之和新材料科技有限公司 | Metal workpiece and manufacturing method therefor |
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