CN103276430A - Higher salt spray corrosion resisting natural color anode oxidation film treatment technology - Google Patents
Higher salt spray corrosion resisting natural color anode oxidation film treatment technology Download PDFInfo
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Abstract
The invention relates to a higher salt spray corrosion resisting natural color anode oxidation film treatment technology which comprises the steps of (1) charging, (2) alkali corrosion, (3) duplex water washing, (4) water washing, (5) chemical polishing, (6) duplex water washing, (7) water washing, (8) bright dipping, (9) water washing, (10) water washing, (11) pure water washing, (12) anode oxidation, (13) water washing, (14) water washing, (15) pure water washing, (16) nickel salt hole sealing, (17) duplex water washing, (18) pure water washing, (19) passivation, (20) duplex water washing, (21) water washing, (22) pure water washing, (23) drying, and (23) blanking. The technology is simple in processing, less in investment and low in energy consumption, improves the property of a film layer greatly, and can resist neutral salt spray corrosion for above 600H, so that the field of applications of aluminum alloy anode oxidation is expanded and improved.
Description
Technical field
The present invention relates to the true qualities anodic oxidation film treatment process in aluminum alloy surface rotproofing field, particularly a kind of anti-high salt air corrosion.
Background technology
Present domestic aluminium alloy anode oxide film, on the performance requriements of anti-neutral salt spray corrosion (NSS test), its grade has different gradess such as 96H, 120H and 240H, traditional prepared anode oxide film of nickel salt sealing, the NSS test has only 96-240H usually, the upholstery products that are used for as notebook computer, phone housing and household electrical appliances etc. more.
The conventional bulk technical process is as follows: (1) material loading; (2) ultrasound degreasing; (3) washing; (4) washing; (5) alkaline etching; (6) duplex washing; (7) washing; (8) neutralization; (9) washing; (10) washing; (11) chemical rightenning; (12) duplex washing; (13) washing; (14) bright dipping; (15) washing; (16) washing; (17) pure water is washed; (18) anodic oxidation; (19) washing; (20) washing; (21) pure water is washed; (22) nickel salt sealing of hole; (23) duplex washing; (24) pure water is washed; (25) hot pure water is washed; (26) oven dry; (27) blanking.Treatment process of attaching most importance to such as (2), (5), (8), (11), (14), (18), (22) wherein.
Above-mentioned this technology shortcoming is described as follows:
1, the pretreatment procedure of above-mentioned technology is too numerous and diverse, and Production Flow Chart is elongated, and strengthen man-hour, and it is high to cause cost to occupy, and does not meet the theory of advocating of low carbon emission reduction.
2, the oxidation film layer thickness of above-mentioned prepared is generally at 12 ± 2 microns, and oxidization time is more than 35 minutes, because the long productive temp that causes of oxidization time is slack-off, and energy consumption increases, and lengthen man-hour, i.e. cost height and efficient is low.
3, the anode oxide film of above-mentioned prepared, its corrosive power of anti-neutral salt spray deficiency generally is no more than 240H, is applied to the upholstery product more, exterior decoration product for antiseptic property is had relatively high expectations then shows relatively poor as fields such as automobile exterior spare, construction work, shipbuildings.
Summary of the invention
The object of the present invention is to provide a kind of true qualities anodic oxidation film treatment process of anti-high salt air corrosion, be primarily aimed at the deficiency that prior art exists, it is that a kind of processing procedure is simple, less investment, technology that energy consumption is low, performance with rete is greatly enhanced simultaneously, can be anti-the neutral salt spray corrosion more than 600H, thereby make the aluminium alloy anode oxide Application Areas be expanded and strengthen.
For achieving the above object, the present invention realizes like this.
A kind of true qualities anodic oxidation film treatment process of anti-high salt air corrosion is characterized in that: its processing step comprises, (1) material loading; (2) alkaline etching; (3) duplex washing; (4) washing; (5) chemical rightenning; (6) duplex washing; (7) washing; (8) bright dipping; (9) washing; (10) washing; (11) pure water is washed; (12) anodic oxidation; (13) washing; (14) washing; (15) pure water is washed; (16) nickel salt sealing of hole; (17) duplex washing; (18) pure water is washed; (19) passivation; (20) duplex washing; (21) washing; (22) pure water is washed; (23) oven dry; (24) blanking.
The true qualities anodic oxidation film treatment process of described anti-high salt air corrosion is characterized in that: in described step (2) the alkaline etching operation, the tank liquor composition is that NaOH and the concentration of 40-90g/L is the NaNO of 8-15g/L
3, temperature is 60 ± 5 ℃, the treatment time is 1-3 minute; It is to go with except the greasy dirt of product surface, natural oxidizing layer, surperficial shadow scratch etc. by saponification reaction, thereby obtains comparatively clean surface effect.
The true qualities anodic oxidation film treatment process of described anti-high salt air corrosion is characterized in that: in described step (5) the chemical rightenning operation, with H
3PO
4And H
2SO
44-5:1 preparation by volume, 95 ± 5 ℃ of temperature, the treatment time is 30-180 second; It is by two acid strong chemical reaction at high temperature, removes the product surface greasy dirt, the leveling effect is played on the surface, and reach the mirror polish effect.
The true qualities anodic oxidation film treatment process of described anti-high salt air corrosion is characterized in that: in described step (8) the bright dipping operation, working concentration is the HNO of 100-300g/L
3, temperature is normal temperature, and the treatment time is 2-5 minute, and it is to utilize nitric acid strong oxidizing property and strongly-acid effect, with goods residual black dust such as silicon, iron, manganese etc. when the chemical rightenning, and changes the throwing polishing and is used to reach light action.
The true qualities anodic oxidation film treatment process of described anti-high salt air corrosion is characterized in that: in described step (12) the anodic oxidation operation, working concentration is the H of 170-190g/l
2SO
4, temperature 14-18 ℃, current density 1.3-2A/dm
2, oxidization time is at 15-25 minute, to generate the dense oxidation film of excellent property.
The true qualities anodic oxidation film treatment process of described anti-high salt air corrosion, it is characterized in that: in described step (19) passivation procedure, working concentration is Hangzhou Surtec 650 passivation treating agents of 15-25%, temperature RT-45 ℃, pH value 2.5-3.9, treatment time: 3-6 minute, to through the anode oxide film of sealing through the row Passivation Treatment, to strengthen the erosion resistance of oxide film.
The true qualities anodic oxidation film treatment process of described anti-high salt air corrosion, it is characterized in that: described passivation treating agent needs to prepare with pure water, the pH value of the last washing together before using this passivation treating agent is between 3.5-4.5, in order to avoid excessive to the pH influence of tank liquor; After the passivation, should toast 10-30 minute with the temperature of 50-60 degree for further improving effect.
The true qualities anodic oxidation film treatment process of described anti-high salt air corrosion, it is characterized in that: in described step (16) the nickel salt sealing of hole operation, working concentration is the Kunshan Ludwig nickel salt hole sealing agent of 5-9g/l, 85 ± 5 ℃ of temperature, and the treatment time is 10-30 minute; Solution need circulate and stir and filter, and avoids bubble or impurity to be attached to product surface and causes the part sealing of hole or sealing of hole are not bad.
The true qualities anodic oxidation film treatment process of described anti-high salt air corrosion, it is characterized in that: described step (2)-(8) operation is pre-treating technology, to prepare satisfactory outward appearance, if the mute light of surface requirements is the treatment time of corresponding lengthening step (2) operation then, reduce or exempt the treatment time of step (9) operation simultaneously; If the surface requirements light is the treatment time of corresponding minimizing step (2) operation then, prolong the treatment time of step (9) operation simultaneously.
Description of drawings
Fig. 1 is the thickness-timing relationship comparison diagram of technology of the present invention and traditional technology.
Fig. 2 is this passivating solution under temperature 30 degree and 40 degree situations, the curved line relation comparison diagram in passivating solution concentration and treatment time.
Embodiment
The invention discloses a kind of true qualities anodic oxidation film treatment process of anti-high salt air corrosion, it adopts the Production Flow Chart order of existing maturation process, it is characterized in that the oxidation pre-treatment omitted one ultrasound degreasing with neutralizing treatment, and after sealing treatment, increase by one passivation, the corrosive power of anti-neutral salt spray of oxide film is promoted energetically.Its processing step specifically comprises, (1) material loading; (2) alkaline etching; (3) duplex washing; (4) washing; (5) chemical rightenning; (6) duplex washing; (7) washing; (8) bright dipping; (9) washing; (10) washing; (11) pure water is washed; (12) anodic oxidation; (13) washing; (14) washing; (15) pure water is washed; (16) nickel salt sealing of hole; (17) duplex washing; (18) pure water is washed; (19) passivation; (20) duplex washing; (21) washing; (22) pure water is washed; (23) oven dry; (24) blanking.
(2)-(8) are pre-treating technology in the above-mentioned process, preparing satisfactory outward appearance, if the mute light of surface requirements treatment time of corresponding lengthening step (2) operation then, reduce or exempt the treatment time of step (9) operation simultaneously; If the surface requirements light is the treatment time of corresponding minimizing step (2) operation then, prolong the treatment time of step (9) operation simultaneously.(16)-(19) are the anodic oxidation aftertreatment in the above-mentioned process, to improve the erosion resistance of oxide film.Wherein, operation (3), (4), (6), (7), (9), (10), (13), (14), (17), (20), (21) are washing, be to go up chemical liquid residual in the procedure to clean up, avoid polluting the treatment solution of next process, about 30-60 of washing time second is standard to obtain clean surface effect.Operation (11), (15), (18), (22) are washed for pure water, time is about 30-60 second, but it is very high to water quality requirement, require pure water conductivity below 10us/cm, impurity in the strict management and control water, especially calcium, magnesium ion and chlorion, the product that is possessed of good qualities for production provides necessary guarantee.
In the above-mentioned process, the treatment process of attaching most importance to such as (2), (5), (8), (12), (16), (19) below are described in further detail these emphasis process:
In described step (2) the alkaline etching operation, the tank liquor composition is that NaOH and the concentration of 40-90g/L is the NaNO of 8-15g/L
3, temperature is 60 ± 5 ℃, the treatment time is 1-3 minute; It is to go with except the greasy dirt of product surface, natural oxidizing layer, surperficial shadow scratch etc. by saponification reaction, thereby obtains comparatively clean surface effect.
In described step (5) the chemical rightenning operation, with H
3PO
4And H
2SO
44-5:1 preparation by volume, 95 ± 5 ℃ of temperature, the treatment time is 30-180 second; It is by two acid strong chemical reaction at high temperature, removes the product surface greasy dirt, the leveling effect is played on the surface, and reach the mirror polish effect.
In described step (8) the bright dipping operation, working concentration is the HNO of 100-300g/L
3, temperature is normal temperature, and the treatment time is 2-5 minute, and it is to utilize nitric acid strong oxidizing property and strongly-acid effect, with goods residual black dust such as silicon, iron, manganese etc. when the chemical rightenning, and changes the throwing polishing and is used to reach light action.
In described step (16) the nickel salt sealing of hole operation, working concentration is the Kunshan Ludwig nickel salt hole sealing agent of 5-9g/l, 85 ± 5 ℃ of temperature, and the treatment time is 10-30 minute; Solution need circulate and stir and filter, and avoids bubble or impurity to be attached to product surface and causes the part sealing of hole or sealing of hole are not bad.
The true qualities anodic oxidation film treatment process of described anti-high salt air corrosion is characterized in that: in described step (12) the anodic oxidation operation, working concentration is the H of 170-190g/l
2SO
4, temperature 14-18 ℃, current density 1.3-2A/dm
2, oxidization time is at 15-25 minute, to generate the dense oxidation film of excellent property.
The key process of above-mentioned generation oxide film, under the material situation identical with parameters such as oxidation tank liquor compositions, oxidization time and current density have directly determined the color of thickness and the rete of rete.Within the specific limits, oxidization time is more long, and rete is more thick, and color is more dark, becomes big, corrosion-resistant reduction because dissolving strengthens the rete porosity simultaneously; Oxidization time is more short, and rete is more thin, and the rete transparency is more high, but because of rete cross thin so that correlated performance not enough.Current density is more big, becomes speed more fast, and it is more short to prepare the required time of identical thickness, but causes goods " burn " or " turning white " phenomenon easily; Current density is more little, and rate of film build is more slow, and the time of preparation same thickness oxide film is more long, but is difficult for similar " burn " phenomenon takes place, and is comparatively safe.The two-way requirement of comprehensive production efficiency and product performance, oxidization time designed at 15-25 minute, and current density is controlled at 1.3-2.0A/dm
2, the gained oxide thickness both can guarantee that film performance was up to standard under this parameter between the 7-10 micron, and productive temp is greatly enhanced.Table one has been enumerated the relation between oxidization time, rete color and the thickness three under the traditional technology.Table two has been enumerated the relation between oxidization time under the technology of the present invention, rete color and the thickness three.Fig. 1 (seeing appended sheets of drawings) is the thickness-timing relationship comparison diagram of technology of the present invention and traditional technology.
Table one:
Table two:
In described step (19) passivation procedure, working concentration is Hangzhou Surtec 650 passivation treating agents of 15-25%, temperature RT-45 ℃, pH value 2.5-3.9, treatment time: 3-6 minute, to through the anode oxide film of sealing through the row Passivation Treatment, to strengthen the erosion resistance of oxide film.: described passivation treating agent needs with the pure water preparation, and the pH value of the last washing together before using this passivation treating agent is between 3.5-4.5, in order to avoid excessive to the pH influence of tank liquor; After the passivation, should toast 10-30 minute with the temperature of 50-60 degree for further improving effect.The mode of soaking is adopted in passivation, and the more high then soak time of concentration is more short, and the more high then soak time of temperature is more short.For obtaining good passivation effect, table three has been listed the treatment time under different concns, the temperature.Fig. 2 (seeing appended sheets of drawings) for this passivating solution under temperature 30 degree and 40 degree situations, the curved line relation comparison diagram in passivating solution concentration and treatment time.
Table three:
The present invention proposes a kind of aluminium alloy true qualities anodic oxidation film treatment process, the oxide film corrosion resistance nature that this technical process is simple and easy, energy consumption is low, prepared is superior, because process simplification, especially compressed the anodised time, thereby improved productive temp greatly, at a low price production cost, and process stabilizing.The concrete superiority of technology of the present invention is as follows:
1, simplified the technical process of aluminium alloy true qualities anodic oxidation film preparation, abandoned ultrasound degreasing and the hot pure water operation of using high energy consumption in the traditional technology, comprehensive energy consumption is saved more than 4 one-tenth, and has saved washing together.
2, the oxidation film layer thickness of prepared of the present invention (about 20 minutes of oxidization time) between 8 ± 2 microns, want about 35 minutes of thin 25%(oxidization time for 12 ± 2 microns than traditional technology thickness), oxidization time has shortened nearly 43% than traditional technology, improved production efficiency greatly.
3, the anode oxide film of prepared of the present invention, its corrosive power of anti-the neutral salt spray was at least 480 hours, and can not wait up to 600-1000 hour, and the oxide film resisting salt fog corrosion ability of traditional technology nickel salt sealing is generally at 96-240 hour, thereby make aluminium alloy anode oxide Application Areas and performance be expanded and strengthen, such as being expanded to exterior decoration usefulness by indoor decoration, as automobile exterior spare, boats and ships exterior trimming parts etc.
Being preferred embodiment of the present invention only in sum, is not to limit practical range of the present invention.Be that all equivalences of doing according to the content of the present patent application claim change and modification, all should be technology category of the present invention.
Claims (9)
1. the true qualities anodic oxidation film treatment process of an anti-high salt air corrosion, it is characterized in that: its processing step comprises, (1) material loading; (2) alkaline etching; (3) duplex washing; (4) washing; (5) chemical rightenning; (6) duplex washing; (7) washing; (8) bright dipping; (9) washing; (10) washing; (11) pure water is washed; (12) anodic oxidation; (13) washing; (14) washing; (15) pure water is washed; (16) nickel salt sealing of hole; (17) duplex washing; (18) pure water is washed; (19) passivation; (20) duplex washing; (21) washing; (22) pure water is washed; (23) oven dry; (24) blanking.
2. the true qualities anodic oxidation film treatment process of anti-high salt air corrosion according to claim 1, it is characterized in that: in described step (2) the alkaline etching operation, the tank liquor composition is that NaOH and the concentration of 40-90g/L is the NaNO3 of 8-15g/L, temperature is 60 ± 5 ℃, and the treatment time is 1-3 minute; It is to go with except the greasy dirt of product surface, natural oxidizing layer, surperficial shadow scratch etc. by saponification reaction, thereby obtains comparatively clean surface effect.
3. the true qualities anodic oxidation film treatment process of anti-high salt air corrosion according to claim 1 is characterized in that: in described step (5) the chemical rightenning operation, with H
3PO
4And H
2SO
44-5:1 preparation by volume, 95 ± 5 ℃ of temperature, the treatment time is 30-180 second; It is by two acid strong chemical reaction at high temperature, removes the product surface greasy dirt, the leveling effect is played on the surface, and reach the mirror polish effect.
4. the true qualities anodic oxidation film treatment process of anti-high salt air corrosion according to claim 1, it is characterized in that: in described step (8) the bright dipping operation, working concentration is the HNO of 100-300g/L
3, temperature is normal temperature, and the treatment time is 2-5 minute, and it is to utilize nitric acid strong oxidizing property and strongly-acid effect, with goods residual black dust such as silicon, iron, manganese etc. when the chemical rightenning, and changes the throwing polishing and is used to reach light action.
5. according to the true qualities anodic oxidation film treatment process of claim 1 or 2 or 3 or 4 described anti-high salt air corrosions, it is characterized in that: in described step (12) the anodic oxidation operation, working concentration is the H of 170-190g/l
2SO
4, temperature 14-18 ℃, current density 1.3-2A/dm
2, oxidization time is at 15-25 minute, to generate the dense oxidation film of excellent property.
6. according to the true qualities anodic oxidation film treatment process of claim 1 or 2 or 3 or 4 described anti-high salt air corrosions, it is characterized in that: in described step (19) passivation procedure, working concentration is Hangzhou Surtec 650 passivation treating agents of 15-25%, temperature RT-45 ℃, pH value 2.5-3.9, treatment time: 3-6 minute, to through the anode oxide film of sealing through the row Passivation Treatment, to strengthen the erosion resistance of oxide film.
7. the true qualities anodic oxidation film treatment process of anti-high salt air corrosion according to claim 6, it is characterized in that: described passivation treating agent needs to prepare with pure water, the pH value of the last washing together before using this passivation treating agent is between 3.5-4.5, in order to avoid excessive to the pH influence of tank liquor; After the passivation, should toast 10-30 minute with the temperature of 50-60 degree for further improving effect.
8. according to the true qualities anodic oxidation film treatment process of claim 1 or 2 or 3 or 4 described anti-high salt air corrosions, it is characterized in that: in described step (16) the nickel salt sealing of hole operation, working concentration is the Kunshan Ludwig nickel salt hole sealing agent of 5-9g/l, 85 ± 5 ℃ of temperature, the treatment time is 10-30 minute; Solution need circulate and stir and filter, and avoids bubble or impurity to be attached to product surface and causes the part sealing of hole or sealing of hole are not bad.
9. according to the true qualities anodic oxidation film treatment process of claim 1 or 2 or 3 or 4 described anti-high salt air corrosions, it is characterized in that: described step (2)-(8) operation is pre-treating technology, to prepare satisfactory outward appearance, if the mute light of surface requirements is the treatment time of corresponding lengthening step (2) operation then, reduce or exempt the treatment time of step (9) operation simultaneously; If the surface requirements light is the treatment time of corresponding minimizing step (2) operation then, prolong the treatment time of step (9) operation simultaneously.
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Cited By (6)
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| CN103526254A (en) * | 2013-10-11 | 2014-01-22 | 上海英汇科技发展有限公司 | Treatment process of acidic climate corrosion resistant natural color anodic oxidation film |
| CN104988554A (en) * | 2015-07-22 | 2015-10-21 | 上海英汇科技发展有限公司 | High-low-temperature composite type anodic oxidation hole sealing method |
| CN106637338A (en) * | 2016-12-06 | 2017-05-10 | 上海英汇科技发展有限公司 | Anodic oxidation process for automobile aluminum alloy baggage holders |
| CN107130236A (en) * | 2017-05-24 | 2017-09-05 | 四川湘邻科技有限公司 | A kind of aluminum alloy surface passivation process for improving corrosion resistance |
| CN112210809A (en) * | 2020-09-29 | 2021-01-12 | 九牧厨卫股份有限公司 | Preparation method of silver oxide film |
| CN112210808A (en) * | 2020-09-29 | 2021-01-12 | 九牧厨卫股份有限公司 | Preparation method of black film |
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| CN104988554A (en) * | 2015-07-22 | 2015-10-21 | 上海英汇科技发展有限公司 | High-low-temperature composite type anodic oxidation hole sealing method |
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| CN107130236A (en) * | 2017-05-24 | 2017-09-05 | 四川湘邻科技有限公司 | A kind of aluminum alloy surface passivation process for improving corrosion resistance |
| CN112210809A (en) * | 2020-09-29 | 2021-01-12 | 九牧厨卫股份有限公司 | Preparation method of silver oxide film |
| CN112210808A (en) * | 2020-09-29 | 2021-01-12 | 九牧厨卫股份有限公司 | Preparation method of black film |
| CN112210808B (en) * | 2020-09-29 | 2021-09-17 | 九牧厨卫股份有限公司 | Preparation method of black film |
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Application publication date: 20130904 |