CN101985750A - Treating fluid for preparing zirconium-containing coloring passive film on surface of aluminum alloy and treating method thereof - Google Patents
Treating fluid for preparing zirconium-containing coloring passive film on surface of aluminum alloy and treating method thereof Download PDFInfo
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- CN101985750A CN101985750A CN 201010542884 CN201010542884A CN101985750A CN 101985750 A CN101985750 A CN 101985750A CN 201010542884 CN201010542884 CN 201010542884 CN 201010542884 A CN201010542884 A CN 201010542884A CN 101985750 A CN101985750 A CN 101985750A
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Abstract
The invention discloses a treating fluid for preparing a zirconium-containing coloring passive film on the surface of an aluminum alloy and a treating method thereof. The zirconium chemical passive treating fluid comprises the following main components of: potassium fluoride, a pH value regulator, fluorozirconate and /or potassium fluozirconate; and the pH value of the treating fluid is between 2.5 and 4.5, and the film can be formed within 3 to 10 minutes. The color of the passive layer prepared by the method is black gray; the film layer is tightly combined with a substrate; and the film layer has high strength and high corrosion resistance. The method is simple in operating process, and a coating does not contain hexavalent chromium which is harmful to the environment and human bodies.
Description
Technical field
The present invention relates to a kind of aluminum alloy surface chemical passivation treatment process, particularly relate to treatment solution and treatment process thereof that the preparation aluminum alloy surface contains the painted passive film of zirconium, can aluminum alloy surface obtain thickness evenly, charcoal grey coating, to substitute traditional chromate conversion treatments.
Background technology
Aluminium alloy has become the second largest metallic substance that usage quantity is only second to iron and steel at present.Aluminium alloy is under the atmospheric environment condition, the surface can form one deck oxide film as thin as a wafer and exempt from erosion, but aluminium material surface natural oxide film corrosion resistance is limited, and organic coating such as natural oxide film and paint bonding force is low, aluminium is in use corroded easily, therefore aluminium must pass through effective anti-corrosive treatment, and chemical treatment has important status with its high cost performance in the corrosive protection of aluminium alloy erosion is handled." chromic salt " is most widely used in traditional Passivation Treatment.But, used the domestic relevant policies of also having put into effect the use of restriction chromium because Cr (VI) has strong carcinogenic negative interaction by the U.S. and European Union's restriction.In common chromium-free deactivation technology, rare earth technology and titanium (zirconium) technology is considered to the most promising, and is expected to replace the passivating technique of chromic salt.But rare earth passivating technique cost height, the passivating solution poor stability can not use for a long time; Tradition titanium (zirconium) is that technology has been subjected to extensive attention with its relatively low cost, but the titanium on the market (zirconium) rete that passivating technique obtained is colourless, can't carry out the scene and judge in actual production, promotes the use of thereby seriously hindered it.Therefore developing painted titanium (zirconium) passive film has very important significance.
At present, the substitute technology of chromate conversion treatments research and development are subjected to extensive concern, many generations the chromium technology occur in succession, as phosphatization, zinc phosphatization, based on the complex compound treatment process (CARBDOBOND) of titanium zirconium and fluorine, Envirox series of processes technology etc.Publication number is that 101161861,101358341,1510164,101535528,1572913,1683590,101122017,101021006,1614090 patent has related to titanium (zirconium) passivating technique; Publication number is that 1011332692,101565826,101356300,101275225,101260521,1124303,1683590,1978704,1811014,101139708,101487117,101597758,101525746,101054664 patent has related to passivating techniques such as rare earth, manganese, trivalent chromium.Though some in these technology have entered operational phase, their anti-corrosion effect still has certain gap with traditional chromate conversion treatments; Wherein the anticorrosion ability of titanium-zirconium passive film is especially remarkable, but because it does not have color, limited should the series passive film application.
Summary of the invention
The objective of the invention is to overcome the problem that prior art exists, provide a kind of low cost to obtain in aluminum alloy surface that film forming speed is fast, film-forming temperature is low, the surface colour zirconium chemical passivation treatment process of treatment solution durable.
Purpose of the present invention can realize by following technical solution.
A kind ofly prepare the treatment solution that aluminum alloy surface contains the painted passive film of zirconium, main component is Potassium monofluoride, pH value conditioning agent and fluorine zirconic acid and/or potassium fluozirconate.
The content of described main component is:
Potassium monofluoride 0.4～6.5g/L;
Fluorine zirconic acid 5～50g/L and/or potassium fluozirconate 0.05～0.55g/L;
The pH value that pH value conditioning agent is regulated treatment solution is 2.5～4.5.
The pH value of treatment solution is 2.5～4.5,
Described pH value conditioning agent is one or more in fluorine zirconic acid, hydrofluotitanic acid, Weibull, hydrofluoric acid or the phosphoric acid.
Described treatment solution also comprises tensio-active agent, and its content is 0.25～0.8g/L.
Described tensio-active agent is one or more in sodium laurylsulfonate, op-10 emulsifying agent, Vltra tears or the polyvinyl alcohol.
Use the treatment process of described treatment solution, comprise the steps:
(1) with aluminum alloy surface polishing and oil removing;
(2) immerse in the described treatment solution 3～10 minutes, aluminum alloy surface promptly obtains containing the painted passive film of zirconium.
Described oil removing is alkali cleaning oil removing and pickling degreasing.
The method of described alkali cleaning oil removing is that the preparation weight percent is 3% NaOH solution, and aluminium alloy was soaked in NaOH solution 2～5 minutes, and rinsing is clean.
Described immersion is under the ultra-sonic oscillation condition or under the heating condition.
Described pickling degreasing is for being to soak 1 minute in 10% the dilute nitric acid solution the aluminium alloy after the alkali cleaning oil removing at weight percent, and rinsing is clean.
The described painted passive film of zirconium that contains is the grey black look.
Described aluminium alloy can use 6063,6061.
For novelty of the present invention is described better, its principle is described below:
(1) film formation reaction comprises:
2Al+3O
2→Al
2O
3；
Al+3F→AlF
3；
2K
++5OH
-+4H
++2ZrF
6 2-→KZrF
3(OH)
2·H
2O+KZrF
3O·2H
2O+6F
++2H
2
React when (2) rete is dry:
KZrF
3(OH)
2·H
2O→KZrF
3O·2H
2O。
(3) rete coloring mechanism:
General zirconium passive film does not have color, and the zirconium film of this paper preparation is the grey black look, may be that crystalline structure makes this passive film present the grey black look to natural reflection of light because potassium element causes the zirconium membrane crystallization.
The present invention compares with prior art, has following advantage and beneficial effect:
(1) the present invention is suitable for the surface passivation processing of multiple series alloys.Passive film is the grey black look, and passive film and substrate combinating strength height, barrier propterty excellence are simple to operate, do not contain the sexavalent chrome to environment and human body harmful in the passive film.
(2) film forming is at room temperature carried out, and need not heat; Film forming speed is very fast, near traditional chromate treating film forming speed; Film forming is grey darkly, is easy to online judgement quality of forming film.
(3) treatment solution can be preserved 3 months.The treatment solution of configuration does not need to add oxygenant, and the scale resistance height can continue to use in the medium-term and long-term preservation of open atmospheric environment, obtains the measured conversion processing film of matter.
Description of drawings
The surperficial SEM pattern that contains the painted passive film of zirconium that Fig. 1 obtains for embodiment 1;
The EDS spectrogram that contains the painted passive film of zirconium that Fig. 2 obtains for embodiment 1;
The aluminium alloy section surface that Fig. 3 obtains for embodiment 1 contains the painted passive film electrochemical tests of zirconium, and a curve is an aluminium alloy, and b is a passive film;
The aluminium alloy extrusions high density that Fig. 4 obtains for embodiment 2 contains the painted passive film electrochemical tests of zirconium;
Fig. 5 is the surperficial zirconium passive film electrochemical tests that obtains after the simple oil removing of aluminium alloy extrusions among the embodiment 3;
The aluminium alloy section surface zirconium titanium passive film electrochemical tests that Fig. 6 obtains for embodiment 4;
Fig. 7 is 6061 aluminum alloy surface zirconium passive film electrochemical tests.
Embodiment
In order to understand technical characterstic of the present invention better, the present invention is further illustrated below in conjunction with embodiment, need to prove, embodiment is not a limiting the scope of the invention.
The aluminium alloy that present embodiment uses is 6063 or 6061.
More than two kinds of aluminium alloys be widely used in war products and civilian installation, its chemical ingredients such as following table:
Table 1 aluminum alloy chemically composition (%)
| Chemical ingredients | Si | Fe | Cu | Mn | Mg | Cr | Zn | Ti | Al |
| 6063 | 0.20-0.6 | 0.35 | 0.10 | 0.10 | 0.45-0.9 | 0.10 | 0.10 | 0.10 | Surplus |
| 6061 | 0.4-0.8 | 0.7 | 0.15-0.4 | 0.15 | 0.8-1.2 | 0.04-0.35 | 0.25 | 0.15 | Surplus |
Embodiment 1:6063 aluminium alloy section surface zirconium Passivation Treatment
Aluminum alloy surface zirconium chemical passivation treatment process comprises the steps:
(1) pre-treatment: (a) intercept 3 * 3cm from 6063 large-sized aluminium alloy section bars
2Sample and punching, remove the aluminum alloy surface dirt with the SiC liquid honing, and with tap water surface contaminants is cleaned up direct use or dry stand-by, with aluminum steel at the fixing aluminium flake sample of punching place; (b) compound concentration is the NaOH solution of 3wt%, and the aluminium flake sample is immersed etching in this solution.This step can at room temperature be handled 5 minutes, also can under the ultra-sonic oscillation condition, handle 2 minutes, clean with rinsed with deionized water afterwards, (c) sample of step (b) being handled immerses in the rare nitric acid liquid of 10% (weight percent) and flooded 1 minute, clean with rinsed with deionized water then, directly use or dry stand-by;
(2) zirconium chemical passivation treatment solution configuration: configuration zirconium inactivating treatment liquid 100ml, wherein the concentration of various compositions is as follows in the treatment solution: fluorine zirconic acid 5g/l, Potassium monofluoride 0.40g/l, potassium fluozirconate 0.55g/l, adding the phosphorus acid for adjusting pH value is 2.5.
(3) chemical passivation of aluminum alloy surface zirconium is handled: will be in the pretreated aluminum alloy specimen of step (1) is inserted the plastic containers that fill the described treatment solution of step (2) of hanger, flood under the room temperature, Passivation Treatment 10 minutes, take out sample, rinse well with tap water, preserve after natural air drying or the warm air drying.
The even film layer densification that obtains, bore hole is observed into the grey black look; Utilize scanning electron microscope analysis, this zirconium film surface topography uneven (as shown in Figure 1); Contain zirconium, aluminium, oxygen, fluorine and potassium element (as shown in Figure 2) in the EDS analysis revealed rete; Electrochemical tests result in the 3.5% sodium chloride electrolysis matter solution shows: the aluminium sample corrosion current of handling without transpassivation is 4.07 μ A; Corrosion of aluminium alloy electric current through this instance processes is 0.035 μ A, and corrosion current has reduced by two orders of magnitude (as shown in Figure 3).
Embodiment 2:6063 aluminium alloy extrusions high density zirconium Passivation Treatment
Aluminum alloy surface zirconium chemical passivation treatment process comprises the steps:
(1) pre-treatment: pre-treatment: (a) intercept 3 * 3cm from 6063 large-sized aluminium alloy section bars
2Sample and punching, remove the aluminum alloy surface dirt with the SiC liquid honing, and with tap water surface contaminants is cleaned up direct use or dry stand-by, with aluminum steel at the fixing aluminium flake sample of punching place; (b) compound concentration is the NaOH solution of 3wt%, the aluminium flake sample is immersed in this solution, handled 3 minutes at 30 ℃, clean with rinsed with deionized water afterwards, (c) sample of step (b) being handled immerses in the rare nitric acid liquid of 10% (weight percent) and flooded 1 minute, clean with rinsed with deionized water then, directly use or dry stand-by;
(2) zirconium chemical passivation treatment solution configuration: configuration zirconium inactivating treatment liquid 100ml, wherein the concentration of various compositions is as follows in the treatment solution: fluorine zirconic acid 50g/l, Potassium monofluoride 6.5g/l, potassium fluozirconate 0.55g, polyvinyl alcohol 0.25g/l, regulating pH with hydrofluoric acid is 4.0.
(3) chemical passivation of aluminum alloy surface zirconium is handled: will be in the pretreated aluminum alloy specimen of step (1) is inserted the plastic containers that fill the described treatment solution of step (2) of hanger, flood under the room temperature, Passivation Treatment 3 minutes, take out sample, rinse well with tap water, preserve after natural air drying or the warm air drying.
The even film layer densification that obtains, bore hole is observed into the grey black look, electrochemical tests as shown in Figure 4, corrosion current is 0.260 μ A.
The simple oil removing of embodiment 3:6063 aluminium alloy extrusions rear surface zirconium Passivation Treatment
Aluminum alloy surface zirconium chemical passivation treatment process comprises the steps:
(1) pre-treatment: intercept 3 * 3cm from 6063 large-sized aluminium alloy section bars
2Sample and punching, remove the aluminum alloy surface dirt with the SiC liquid honing, and with tap water surface contaminants is cleaned up direct use or dry stand-by, with aluminum steel at the fixing aluminium flake sample of punching place.
(2) zirconium chemical passivation treatment solution configuration: configuration zirconium inactivating treatment liquid 100ml, wherein the concentration of various compositions is as follows in the treatment solution: fluorine zirconic acid 20g/l, Potassium monofluoride 0.5g/l, potassium fluozirconate 0.5g/l, polyvinyl alcohol 0.8g/l, phosphorus acid for adjusting pH value are 4.0.
(3) chemical passivation of aluminum alloy surface zirconium is handled: will be in the pretreated aluminum alloy specimen of step (1) is inserted the plastic containers that fill the described treatment solution of step (2) of hanger, at room temperature flood, Passivation Treatment 8 minutes, take out sample, rinse well with tap water, preserve after natural air drying or the warm air drying.
Electrochemical tests as shown in Figure 5, corrosion current is 0.095 μ A.
Embodiment 4:6063 aluminium alloy section surface zirconium titanium Passivation Treatment
Aluminum alloy surface zirconium chemical passivation treatment process comprises the steps:
(1) pre-treatment: with embodiment 1;
(2) zirconium chemical passivation treatment solution configuration: configuration zirconium inactivating treatment liquid 100ml, wherein the concentration of various compositions is as follows in the treatment solution: fluorine zirconic acid 13g/l, Potassium monofluoride 0.5g/l, polyvinyl alcohol 0.5g/l, adding hydrofluotitanic acid and tannin acid for adjusting pH value is 4.0.
(3) chemical passivation of aluminum alloy surface zirconium is handled: will be in the pretreated aluminum alloy specimen of step (1) is inserted the plastic containers that fill the described treatment solution of step (2) of hanger, under 25 ℃ temperature, flood, Passivation Treatment 6 minutes, take out sample, rinse well with tap water, preserve after natural air drying or the warm air drying.
The even film layer densification that obtains, bore hole is observed into the grey black look, electrochemical tests as shown in Figure 6, corrosion current is 0.360 μ A.
Embodiment 5:6061 aluminum alloy surface zirconium Passivation Treatment
Aluminum alloy surface zirconium chemical passivation treatment process comprises the steps:
(1) pre-treatment: with embodiment 1;
(2) zirconium chemical passivation treatment solution configuration: configuration zirconium inactivating treatment liquid 100ml, wherein the concentration of various compositions is as follows in the treatment solution: fluorine zirconic acid 50g/l, Potassium monofluoride 6.5g/l, potassium fluozirconate 0.055g/l, polyvinyl alcohol 0.5g/l, it is 4.0 that phosphoric acid is regulated pH.
(3) chemical passivation of aluminum alloy surface zirconium is handled: will be in the pretreated aluminum alloy specimen of step (1) is inserted the plastic containers that fill the described treatment solution of step (2) of hanger, at room temperature flood, Passivation Treatment 10 minutes, take out sample, rinse well with tap water, preserve after natural air drying or the warm air drying.
The even film layer densification that obtains, bore hole is observed into the grey black look, electrochemical tests as shown in Figure 7, corrosion current is 0.105 μ A.
Treatment solution of the present invention can be preserved 3 months.The treatment solution of configuration does not need to add oxygenant, and the scale resistance height can continue to use in the medium-term and long-term preservation of open atmospheric environment, obtains the measured conversion processing film of matter.
Claims (10)
1. one kind prepares the treatment solution that aluminum alloy surface contains the painted passive film of zirconium, it is characterized in that, main component is Potassium monofluoride, pH value conditioning agent and fluorine zirconic acid and/or potassium fluozirconate.
2. treatment solution according to claim 1 is characterized in that, the content of described main component is:
Potassium monofluoride 0.4～6.5g/L;
Fluorine zirconic acid 5～50g/L and/or potassium fluozirconate 0.05～0.55g/L;
The pH value that pH value conditioning agent is regulated treatment solution is 2.5～4.5.
3. treatment solution according to claim 1 is characterized in that, described pH value conditioning agent is one or more in fluorine zirconic acid, hydrofluotitanic acid, Weibull, hydrofluoric acid or the phosphoric acid.
4. treatment solution according to claim 1 is characterized in that described treatment solution also comprises tensio-active agent, and its content is 0.25～0.8g/L.
5. treatment solution according to claim 4 is characterized in that, described tensio-active agent is one or more in sodium laurylsulfonate, op-10 emulsifying agent, Vltra tears or the polyvinyl alcohol.
6. application rights requires the treatment process of one of 1-5 described treatment solution, it is characterized in that, comprises the steps:
(1) with aluminum alloy surface polishing and oil removing;
(2) immerse in one of the claim 1-5 described treatment solution 3～10 minutes, aluminum alloy surface promptly obtains containing the painted passive film of zirconium.
7. treatment process according to claim 6 is characterized in that, described oil removing is alkali cleaning oil removing and pickling degreasing.
8. treatment process according to claim 7 is characterized in that, the method for described alkali cleaning oil removing is that the preparation weight percent is 3% NaOH solution, and aluminium alloy was soaked in NaOH solution 2～5 minutes, and rinsing is clean.
9. treatment process according to claim 8 is characterized in that, described immersion is under the ultra-sonic oscillation condition or under the heating condition.
10. treatment process according to claim 7 is characterized in that, described pickling degreasing is for being to soak 1 minute in 10% the dilute nitric acid solution the aluminium alloy after the alkali cleaning oil removing at weight percent, and rinsing is clean.
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| CN102212812A (en) * | 2011-06-13 | 2011-10-12 | 北京科技大学 | Chromium-free rare-earth environment-friendly chemical conversion treatment method of die casting aluminium alloy part |
| CN102534592A (en) * | 2012-01-10 | 2012-07-04 | 北京科技大学 | Zirconium salt chemical conversion treatment method for surface of die-casting aluminum alloy |
| CN102766862A (en) * | 2012-08-21 | 2012-11-07 | 湖南大学 | Treating fluid and method for preparing vanadium-zirconium composite conversion coatings with self-repairing performance on aluminum alloy surfaces through same |
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| CN102212812A (en) * | 2011-06-13 | 2011-10-12 | 北京科技大学 | Chromium-free rare-earth environment-friendly chemical conversion treatment method of die casting aluminium alloy part |
| CN102534592A (en) * | 2012-01-10 | 2012-07-04 | 北京科技大学 | Zirconium salt chemical conversion treatment method for surface of die-casting aluminum alloy |
| CN102534592B (en) * | 2012-01-10 | 2013-06-05 | 北京科技大学 | Zirconium salt chemical conversion treatment method for surface of die-casting aluminum alloy |
| CN102817025A (en) * | 2012-07-28 | 2012-12-12 | 蚌埠市福沃特车轮制造科技有限公司 | Low-temperature phosphating solution containing chromic acid |
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| CN103498137A (en) * | 2013-09-24 | 2014-01-08 | 华南理工大学 | Treatment liquid and treatment method for preparing zirconium-based colored conversion film on magnesium alloy surface |
| CN103806008A (en) * | 2013-12-02 | 2014-05-21 | 青岛蓝图文化传播有限公司市南分公司 | Cleaning process/method for aluminum alloy material |
| CN103614716A (en) * | 2013-12-10 | 2014-03-05 | 广西大学 | Preparation method of environment-friendly aluminum alloy surface rare-earth inorganic composite conversion coating |
| CN103789759A (en) * | 2014-02-21 | 2014-05-14 | 上海溯扬工艺控制科技有限公司 | Aluminum alloy spraying pre-treatment process |
| CN103789759B (en) * | 2014-02-21 | 2016-08-24 | 上海溯扬工艺控制科技有限公司 | A kind of aluminium alloy pre-processing process for spraying |
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Application publication date: 20110316 |