CN1687487A - Anodic oxidation method for improving corrosion resisting property at parts of edges and corners of aluminium alloy - Google Patents
Anodic oxidation method for improving corrosion resisting property at parts of edges and corners of aluminium alloy Download PDFInfo
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- CN1687487A CN1687487A CNA2005102002407A CN200510200240A CN1687487A CN 1687487 A CN1687487 A CN 1687487A CN A2005102002407 A CNA2005102002407 A CN A2005102002407A CN 200510200240 A CN200510200240 A CN 200510200240A CN 1687487 A CN1687487 A CN 1687487A
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Abstract
A method of anodic oxidation which can improve the wearable performance of edge of aluminum alloy belongs to the domain of disposal on its surface. The flow includes: wash by alkali remove oil, neutralization, process anode, soaks spreads and drying. The anode processes is reasonable, easy, cheap and can form anodic oxidation film efficiently. The invention use sealing fluid which is water-solubility. It won't thicken the part of aluminum alloy, has little dosage and has good seal when compared with other organic sealing fluid. It will seal the orifice in film and fill the crack on the edge after the sealing fluid is drying. So it improves the protection of oxidation film and the longevity of the part of aluminum alloy. The technique of anodic oxidation is the same with the part of aluminum alloy which needs protection and can't be polished.
Description
Technical field
The invention belongs to the aluminum alloy surface processing technology field.Relate to a kind of new aluminium alloy anode oxide technology.At complex-shaped, property at parts of edges and corners can not be polished and chamfered aluminum alloy part, this technology can significantly improve the corrosion resisting property of its property at parts of edges and corners.
Background technology
In the modern industry, aluminium and alloy thereof are carried out anodic oxidation can obtain porous, have the di-aluminium trioxide film of provide protection.By changing the anode oxidation process condition, can increase the hardness of film, improve solidity to corrosion, the wear resistance of film, and strengthen the insulativity of aluminium and alloy material thereof.The anodic oxidation film hardness height of aluminium and alloy thereof, good insulating, wear-resisting, solidity to corrosion is good, bonding force is strong, heat impedance is better than alloy matrix aluminum, and has very strong adsorptivity and good optical characteristic.So aluminium alloy after anodic oxidation, is used widely in construction industry, aerospace, transportation, membrane sepn field and many high leading-edge fields.It is ripe and perfect that its anode oxidation process also more and more is tending towards.
It is that the center is shifted and developed that early stage alumilite process is handled with the electrolytic solution kind.Original adoption be the anodic oxidation of electrolytic solution with acids such as bromic acid, chromic acid, the especially appearance of sulphuric acid anodizing technology makes anode oxidation process obtain significant progress.Afterwards, it is found that the performance that the oxidation power supply also can the antianode oxide film produced considerable influence.Direct current and alternating-current are to adopt anodic oxidation power supply more widely in the modern industry.The form of people's antianode oxide film is studied, and finds that anode oxide film is a kind of loose porous amorphous structure, and the corrosion resisting property that sealing of hole is handled improving film plays crucial effects.Therefore, various closing process are also come out one after another, as hydration sealing of hole, metal-salt sealing of hole, organic coating sealing of hole (electrophoresis or dipping japanning) and normal-temperature hole sealing treatment processs such as (low temperature pore sealings).
Over nearly 10 years, anode oxidation technology has obtained many new achievements.Be in the patent of CN 1100761A at publication number for example, proposed wide temperature high speed anonizing, the new approaches of oxidation have at normal temperatures and for example solved and have been the huge problem of cooling energy consumption.Adopt the pulse anodic oxidation novel process in addition, perhaps take two step anonizings, the quality of oxide film is greatly improved.Recently, make the ac oxide film quality reach the level of direct current oxidation by adding additive.In addition, for overcoming some defectives of common anode oxidation technology, Ji Cunchangzang [referring to metallic surface technology (day), 1989,40 (1): 150], once insult third-class [referring to material protection, 1997,30 (3): 13] and in electrolytic solution, added Al
2O
3, SiC, TiO
2Deng powder, [referring to metallic surface technology (day), 1987,38 (1): 67] such as high bridge wisdoms adopted the composite anode oxide of secondary oxidation.The new electrolysis process and the invention of power supply have promoted the continuous development of anodizing technology.
But former anode oxidation process all is to carry out at the surperficial position of aluminum alloy part, and technology is comparative maturity.In sour environment, adopt anode oxidation process in the past, aluminium alloy is carried out anodic oxidation, though the oxidation film corrosion resistance on surface is fine, yet property at parts of edges and corners very easily corrode, cause the shortening in work-ing life of aluminum alloy part.Especially Fu Za aluminum alloy part because property at parts of edges and corners can not be polished and chamfered in actual mechanical process, causes solidity to corrosion to reduce when adopting traditional anode oxidation process.Mainly show as, satisfy the corrosion proof anodizing condition in aluminum alloy surface position, might not be applicable to its property at parts of edges and corners.The effective closure agent of aluminum alloy surface position can not play a role to its property at parts of edges and corners.Therefore, research property at parts of edges and corners oxide film pattern and corrosion resisting property thereof are improved aluminium alloy anode oxide technology, can avoid causing a large amount of wastings of resources and financial loss.
The present invention finds that in research process the anode oxide film of aluminium alloy cracks at property at parts of edges and corners, is discrete state.The crackle width is 10～100 times of oxide film aperture, surperficial position between 1～10 μ m.Because crackle appears in rete, the oxide film attenuation of property at parts of edges and corners of aluminium alloy, discontinuous causes the property at parts of edges and corners solidity to corrosion to descend.In acidic medium, the corrosion of its property at parts of edges and corners aggravation.
Because the appearance of crackle in the past can not be as effective solution route at the oxidizing process and the closing process of aluminum alloy surface.
Summary of the invention
The purpose of this invention is to provide a kind of by new anode oxidation process, solve the problem of property at parts of edges and corners of aluminium alloy solidity to corrosion difference emphatically, improve the whole corrosion resisting property of aluminum alloy part, thus the anode oxidation method of the raising corrosion resisting property at parts of edges and corners of aluminium alloy that increases the service life.
Technical solution of the present invention is, aluminum alloy part is through the alkali cleaning oil removing, in and after the bright dipping, carry out anodic oxidation treatment with oxidizing process of the present invention, obtain Al
2O
3Oxide film.Continue it, carry out sealing treatment by closing process of the present invention.
The solution of the present invention is:
Technical process: the washing of alkali cleaning oil removing → hot water wash → deionization → in and bright dipping → deionization washing → anodizing → deionization washing → drying → dip-coating → oven dry.
The pretreatment technology parameter:
The alkali cleaning oil removing: NaOH 50～80g/L, 70～75 ℃, 7～8min,
Hot water wash: more than 80 ℃, 30～40s, once,
Deionization washing: room temperature, 30～40s, once,
In and bright dipping: HNO
330%, room temperature, 30～35s;
The oxidation processing technique parameter:
Electrolytic solution is formed (g/L): H
2SO
4(98%) 180～220,
Solution temperature (℃): 15～22,
Current density (A/dm
2): 2～3,
Oxidization time (min): 30～40;
Sealing treatment:
Confining liquid:
Epocryl 20～25%,
Deionized water 60～65%,
Butanols 7～14%,
Amylalcohol 2～4%,
Dimethylbenzene 1～2%.
Enclosure method: need the oven dry sealing after every dip-coating once,
The dip-coating number of times: 3～5 times,
Closure temperature: 200～220 ℃,
Off-period: 1～4min.
The beneficial effect that the present invention reached is, and is complex-shaped when the aluminum alloy part that needs protection, and when its property at parts of edges and corners can not carry out grinding process, can adopt this anode oxidation process.The operation of anode processing technique is reasonable, simple to operate, with low cost, can form effective anode oxide film.Especially the crackle width that produces at property at parts of edges and corners of aluminium alloy suits, and thickness is moderate.Simultaneously, the closing process among the present invention adopts water-soluble environment protective type confining liquid, compares with other organism sealing, and is little to the aluminum alloy part thickness effect, can significantly not increase the thickness of aluminum alloy part, and consumption is few, and sealing effect is good.After the confining liquid drying, both seal the fenestra at aluminum alloy surface position, filled the crackle of property at parts of edges and corners again, thereby improved the Global Macros performance of oxide film, prolonged the work-ing life of aluminum alloy part.
Description of drawings
Fig. 1 is a process flow sheet of the present invention.
Fig. 2 is the aluminum alloy specimen synoptic diagram.
Fig. 3 is the microstructure of property at parts of edges and corners behind the aluminium alloy anode oxide.
Wherein: a rib position is the morphology observation point; 1 is the crackle at rib position, and the crackle width is 4.375 μ.
Embodiment
(1) embodiment and comparative example
Get the aluminium alloy plate of thick 1mm, cut into the rectangular sheet of 50mm * 30mm, the rectangular opening of middle part intercepting 24.6mm * 13.6mm, cutting mode adopts the line cutting.Specimen shape synoptic diagram such as Fig. 2 illustrate.The a point that marks among Fig. 2 is the observation analysis point.Adopt direct supply, do hanger with aluminium wire, hanger contacts close and firm with aluminium sheet, and negative electrode adopts stereotype, the parallel both sides that are placed on sample, and cathode and anode area ratio is 1.8.
Embodiment is identical with the pretreatment condition of comparative example, and the pretreatment technology parameter is as follows:
Alkali cleaning oil removing (NaOH 50g/L, 70 ℃, 8min) → hot water wash (more than 80 ℃, 30s, once) → deionization washing (room temperature, 30s, once) → in and bright dipping (HNO
330%, room temperature, 30s) → deionization washing (room temperature, 30, once)
Embodiment
Anodizing:
Electrolytic solution is formed (g/L): H
2SO
4(98%) 180
Solution temperature (℃): 20 ± 1
Current density (A/dm
2): 2.5
Oxidization time (min): 35
Sealing treatment:
Confining liquid: Epocryl (25%), deionized water (65%), all the other are butanols (7%), amylalcohol (2%) and dimethylbenzene (1%).
Enclosure method: need the oven dry sealing after every dip-coating once
Dip-coating number of times: 5 times
Closure temperature: 200～220 ℃
Off-period: 1～4min
The operator can increase or reduce the content of confining liquid solvent in right amount according to the actual environment for use of the aluminum alloy part of required sealing, corresponding minimizing or increase the sealing number of times.
Comparative example 1～7
Comparative example 1
Comparative example 1 belongs to traditional sulphuric acid anodizing technology.
Anodizing:
Electrolytic solution is formed: H
2SO
4(98%) 10～12%
Solution temperature (℃): 20 ± 1
Current density (A/dm
2): 1～3
Oxidization time (min): 30～50
Sealing treatment:
Enclosure method: boiling water sealing
Confining liquid: deionized water
PH value: 6～9
Closure temperature (℃): 95～100
Off-period (min): 20～40
Comparative example 2
Comparative example 2 belongs to mixed acid anodic oxidation technology.
Anodizing:
Electrolytic solution is formed: H
2SO
4(98%) 6%
Oxalic acid 2%
Solution temperature (℃): 19 ± 1
Current density (A/dm
2): 2
Oxidization time (min): 35
Sealing treatment:
Enclosure method: boiling water sealing
Confining liquid: deionized water
PH value: 6.8
Closure temperature (℃): 95～100
Off-period (min): 30
Comparative example 3
Anodizing:
Electrolytic solution is formed: H
2SO
4(98%) 10%
Solution temperature (℃): 18 ± 1
Current density (A/dm
2): 2
Oxidization time (min): 35
Sealing treatment:
Enclosure method: hot metal salt sealing
Confining liquid: NiSO
41.1g/L
NH
4F????????????????????2g/L
Ammonium molybdate: 1g/L
Zinc sulfate: 1g/L
PH value: 6
Closure temperature (℃): more than 80 ℃
Off-period (min): 25
Comparative example 4
Anodizing:
Electrolytic solution is formed: H
2SO
4(98%) 10%
Solution temperature (℃): 18 ± 1
Current density (A/dm
2): 2
Oxidization time (min): 35
Sealing treatment:
Enclosure method: mix sealing method (first boiling water sealing is sealed with organism again)
Boiling water confining liquid: deionized water
PH value: 6.8
The boiling water closure temperature (℃): 95～100
Boiling water off-period (min): 25
The organism encapsulant: water-insoluble, non-drying-type encapsulant acrylic resin, thinner carries out application by 4: 1 weight ratio, and the sealing back is dried 24h naturally.
Comparative example 5
The anode processing technique parameter:
Electrolytic solution is formed: H
2SO
4(98%) 10%
Solution temperature (℃): 18 ± 1
Current density (A/dm
2): 2
Oxidization time (min): 35
The seal treatment technique parameter:
Enclosure method: mix sealing method (first boiling water sealing is sealed with organism again)
Boiling water confining liquid: deionized water
PH value: 6.8
The boiling water closure temperature (℃): 95～100
Boiling water off-period (min): 25
The organism encapsulant: water-insoluble, non-drying-type encapsulant epoxy-mica iron(ic) chloride, solidifying agent, thinner is pressed 4: 1: 0.8 weight ratio application, and the sealing back is dried 24h naturally.
Comparative example 6
The anode processing technique parameter:
Electrolytic solution is formed: H
2SO
4(98%) 10%
Solution temperature (℃): 18 ± 1
Current density (A/dm
2): 2
Oxidization time (min): 35
The seal treatment technique parameter:
Enclosure method: mix sealing method (first boiling water sealing is sealed with organism again)
Boiling water confining liquid: deionized water
pH：?????????????????????????????????6.8
The boiling water closure temperature (℃): 95～100
Boiling water off-period (min): 25
The organism encapsulant: water-insoluble, non-drying-type encapsulant urethane, solidifying agent, thinner is pressed 4: 1: 0.8 weight ratio application, and the sealing back is dried 24h naturally.
Comparative example 7
The anode processing technique parameter:
Electrolytic solution is formed: H
2SO
4(98%) 10%
Solution temperature (℃): 18 ± 1
Current density (A/dm
2): 2
Oxidization time (min): 35
The seal treatment technique parameter:
Enclosure method: mix sealing method (first boiling water sealing is sealed with organism again)
Boiling water confining liquid: deionized water
PH value: 6.8
The boiling water closure temperature (℃): 95～100
Boiling water off-period (min): 25
The organism encapsulant: water-insoluble, non-drying-type encapsulant Resins, epoxy, solidifying agent, dibutylester, talcum powder, acetone was by 4: 1: 1: 1: 1 weight ratio application, the sealing back is dried 24h naturally.
(2) Performance Detection
Aluminum alloy specimen is dried after anodic oxidation, places after the 24h, at HCl (50mL)+K
2Cr
2O
7(6g)+H
2In O (75mL) solution, detected corrosion resisting property by the chemical immersion test.Because property at parts of edges and corners specific surface position easily corrodes, therefore the time length of bubble appear in the effusion bubble hydrogen according to property at parts of edges and corners, determine the corrosion resisting property grade (seeing Table 1) of anode oxidation membrane.
Adopt above-mentioned evaluation method that the aluminum alloy specimen of embodiment of the present invention and comparative example is compared, the results are summarized in table 2.
Table 1 chemical immersion experiment rete corrosion resisting property grade
| Bubble time t (min) appears | ?t≤ ?20 | ?20＜t ?≤40 | ?40＜t ?≤60 | ?60＜t ?≤80 | ?80＜t ?≤100 | 100＜t ≤120 | 120＜t ≤140 | 140＜t ≤160 | 160＜t ≤180 | ?t＞ ?180 |
| Membranous layer corrosion resistance can grade | ?A | ?B | ?C | ?D | ?E | F | G | H | I | ?J |
Table 2 chemical immersion experiment comparative result
| The bubble time (min) appears in corner angle | Min appears in the surface) | Membranous layer corrosion resistance can grade | Detect and estimate | |
| Embodiment | ＞180 | ＞180 | J | Rete is thinner, is evenly distributed, complete, is transparence.Behind the chemical immersion, surface and property at parts of edges and corners all do not have signs of corrosion. |
| Comparative example 1 | 21～120 | ＞180 | B～F | The rete shape that is translucent, the chemical immersion rear surface is no abnormal, and the property at parts of edges and corners rete is discontinuous, matrix metal is corroded. |
| Comparative example 2 | 33 | ＞180 | B | The rete gray, position, chemical immersion rear surface is no abnormal, and that the property at parts of edges and corners rete goes out is discontinuous, matrix metal is corroded. |
| Comparative example 3 | 8 | 8 | A | The rete shape that is translucent, during chemical immersion 8min, surface and property at parts of edges and corners have a large amount of bubbles effusions, and matrix metal suffers heavy corrosion. |
| Comparative example 4 | 30 | ＞180 | B | During chemical immersion 30min, a large amount of bubbles occur at property at parts of edges and corners, surperficial position is no abnormal, and the property at parts of edges and corners matrix metal is corroded. |
| Comparative example 5 | 9 | 9 | A | Rete is thicker, gray, surface and property at parts of edges and corners all have powder and small bubbles absorption, and the bonding force of paint film is poor, rete occurs and peels off phenomenon. |
| Comparative example 6 | 44 | 22 | C | Rete is thicker, is orange.During chemical immersion 22min, bubble appears in surperficial position, and bubble appears in property at parts of edges and corners during 44min, and matrix metal is corroded. |
| Comparative example 7 | 71 | ＞180 | D | Rete is thicker, be transparence, chemical immersion rear surface situation is no abnormal, and property at parts of edges and corners is when 71min, a large amount of bubbles occur, Base Metal is corroded. |
By chemical immersion experiment comparative result (table 2), can draw embodiment, technology promptly of the present invention is to protectiveness the best of aluminum alloy specimen, and simple to operate, with low cost, and clean environment firendly has obviously improved the corrosion resisting property of property at parts of edges and corners of aluminium alloy.
Claims (3)
1. anode oxidation method that improves corrosion resisting property at parts of edges and corners of aluminium alloy, it is characterized in that may further comprise the steps: on the surface of aluminium alloy, form anode oxide film, and carry out sealing treatment with encapsulant antianode oxide film, fill the crackle of property at parts of edges and corners and the oxidation fenestra on surface; Dry processing after the sealing, crackle and fenestra are thoroughly sealed
2. a kind of anode oxidation method that improves corrosion resisting property at parts of edges and corners of aluminium alloy according to claim 1, it is characterized in that, the formation technology of anode oxide film by alkali cleaning oil removing, hot water wash, deionization washing, in and the washing of bright dipping deionization, oxidation, deionization washing form
Alkali cleaning oil removing process parameter is: NaOH 50～80g/L, 70～75 ℃, 7～8min;
The hot water wash processing parameter is: 80-120 ℃, 30～40s, 1-3 time;
Ion washing processing parameter is: deionization washing, 15-40 ℃, 30～40s, 1-3 time;
In and the bright dipping processing parameter be: HNO3 30%, 15-40 ℃, 30～35s;
The oxidizing process parameter is:
Electrolytic solution is formed (g/L): H2SO4 (98%) 180～220,
Solution temperature (℃): 15～22,
Current density (A/dm2): 2～3,
Oxidization time (min): 30～40.
3. a kind of anode oxidation method that improves corrosion resisting property at parts of edges and corners of aluminium alloy according to claim 1 is characterized in that, by weight percentage, and the consisting of of organism encapsulant:
Epocryl 20～25%,
Deionized water 60～65%,
Butanols 7～14%,
Amylalcohol 2～4%,
Dimethylbenzene 1～2%;
The closing process parameter is:
Enclosure method: need the oven dry sealing after every dip-coating once,
The dip-coating number of times: 3～5 times,
Closure temperature: 200～220 ℃,
Off-period: 1～4min.
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| CN101413139B (en) * | 2007-10-18 | 2010-12-08 | 比亚迪股份有限公司 | Aluminum alloy including differential arc oxidation film and preparation thereof |
| CN102562206A (en) * | 2012-01-18 | 2012-07-11 | 芜湖杰锋汽车动力系统有限公司 | Variable valve timing distribution regulating device and method for improving mechanical property of variable valve timing distribution regulating device |
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| CN103695982A (en) * | 2013-12-25 | 2014-04-02 | 重庆铁马工业集团有限公司 | Electrolyte for aluminum or aluminum alloy wide-temperature anodic oxidation and oxidation method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101413139B (en) * | 2007-10-18 | 2010-12-08 | 比亚迪股份有限公司 | Aluminum alloy including differential arc oxidation film and preparation thereof |
| WO2012122715A1 (en) * | 2011-03-17 | 2012-09-20 | 芜湖杰锋汽车动力系统有限公司 | Variable valve timing distribution adjusting device and a method for improving mechanical properties thereof |
| CN102562206A (en) * | 2012-01-18 | 2012-07-11 | 芜湖杰锋汽车动力系统有限公司 | Variable valve timing distribution regulating device and method for improving mechanical property of variable valve timing distribution regulating device |
| CN103695982A (en) * | 2013-12-25 | 2014-04-02 | 重庆铁马工业集团有限公司 | Electrolyte for aluminum or aluminum alloy wide-temperature anodic oxidation and oxidation method |
| CN105603490A (en) * | 2016-01-22 | 2016-05-25 | 江西宝盛半导体能源科技有限公司 | Insulating coating material with ultrahigh thermal conductivity and method for preparing insulating coating material |
| CN105671616A (en) * | 2016-03-16 | 2016-06-15 | 浙江鸿昌铝业有限公司 | Anticorrosive treatment technology for surface of aluminum profile |
| CN106655014A (en) * | 2017-01-09 | 2017-05-10 | 镇江华中电器有限公司 | Heavy duty anticorrosion surface treatment method for aluminum alloy cable laying device dedicated for the ocean |
| CN114369402A (en) * | 2021-12-18 | 2022-04-19 | 孙守英 | Aluminum alloy coating material |
| CN117885455A (en) * | 2023-12-18 | 2024-04-16 | 建民五金科技(东莞)有限公司 | Metal surface full-color pattern transfer printing method |
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