CN103276385B - A kind of method preparing the coloured passive film of high anti-corrosion in aluminum alloy surface - Google Patents
A kind of method preparing the coloured passive film of high anti-corrosion in aluminum alloy surface Download PDFInfo
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- CN103276385B CN103276385B CN201310185253.6A CN201310185253A CN103276385B CN 103276385 B CN103276385 B CN 103276385B CN 201310185253 A CN201310185253 A CN 201310185253A CN 103276385 B CN103276385 B CN 103276385B
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Abstract
The invention discloses the method preparing the coloured passive film of high anti-corrosion in aluminum alloy surface, comprise the following steps: (1) carries out pre-treatment to aluminum alloy surface; (2) aluminium alloy processed through step (1) is placed in treatment solution, constant temperature floods namely for some time obtains containing zirconium, titanium, vanadium yellow passivated film in aluminum alloy surface; Described aluminium alloy treatment solution composed as follows: hydrofluotitanic acid 0.1g/L ~ 20g/L, fluorine zirconic acid 0.1g/L ~ 30g/L, sodium metavanadate 0.2g/L ~ 40g/L, Weibull 0.1g/L ~ 20g/L.The rete that the present invention generates has color, convenient observation, and can form the passive film with high anti-corrosion fast.
Description
Technical field
The present invention relates to aluminum alloy surface chemical passivation treatment process, particularly a kind of method preparing the coloured passive film of high anti-corrosion Ti/V in aluminum alloy surface.
Background technology
Aluminium alloy has become the second largest metallic substance that usage quantity is only second to iron and steel at present.But aluminium alloy activity is comparatively large, easily corrodes, needs effects on surface to carry out anti-corrosive treatment.Conventional method is the method sprayed again after aluminum alloy surface generates complete, fine and close, the uniform passive film of one deck.Current most popular passivating method is low concentrations of chromium hydrochlorate (about 0.2% dichromate or chromic anhydride) passivation, and major cause is that this passivation technology is simple, with low cost, and the rete of formation has excellent corrosion resisting property and self-healing ability.But all containing sexavalent chrome HUMAN HEALTH and environment being existed to serious harm in conventional chromating liquid and institute's film forming thereof, along with the enhancing of people's environmental consciousness, the use of chromating is just being subject to more and more severeer restriction, researchs and develops new environmentally friendly process for treating surface extremely urgent.The more inorganic salts of current research is as molybdate, silicate, rare-earth salts, titanium zirconium composite salt etc.; organic is as silane, silicon sol, phytic acid, Weibull etc.; wherein titanium zirconium composite protection film is with its feature such as good solidity to corrosion and nontoxic pollution-free; extremely focus of attention in recent years, is described as the method being hopeful substitute chromium hydrochlorate passivating technique most.Application number be 200410026047,200510125869,200710034656,200710122088,200710158469,200910085265,201010285851 Chinese invention patent application all relate to these technology.Although these patented technologies have certain practical application foreground, all there are some shortcomings, main manifestations is: 1) the titanium zirconium passive film overwhelming majority is for colourless, and naked eyes are difficult to distinguish, and are unfavorable for the online judgement of producing; 2) complex treatment process, treatment process is complicated, realizes industrialized difficulty larger; 3) film formation time is longer, reduces production efficiency.
Summary of the invention
In order to overcome above-mentioned shortcoming of the present invention with not enough, the object of the present invention is to provide a kind of method preparing the coloured passive film of high anti-corrosion Ti/V in aluminum alloy surface, the rete that the present invention generates has color, convenient observation, and can form the passive film with high anti-corrosion fast.
Object of the present invention is achieved through the following technical solutions:
Prepare a method for the coloured passive film of high anti-corrosion in aluminum alloy surface, comprise the following steps:
(1) pre-treatment is carried out to aluminum alloy surface;
(2) aluminium alloy processed through step (1) is placed in treatment solution, namely obtains the yellow passivated film containing zirconium, titanium, vanadium in aluminum alloy surface at 25 DEG C ~ 90 DEG C dipping 10s ~ 600s; Described aluminium alloy treatment solution composed as follows:
The preferred scope of composition of described aluminium alloy treatment solution is as follows:
The pH value of described aluminium alloy treatment solution is 2.0 ~ 4.0.
Step (1) is described carries out pre-treatment to aluminum alloy surface, is specially:
By aluminum alloy surface polishing to 1000#, carry out industrial acid-washed and nitration mixture process successively.
Described industrial acid-washed, be specially:
Aluminium alloy is placed in the acidic solution of 25 ~ 35 DEG C, floods 1 ~ 3 minute, described acidic solution consist of 100g/L H
2sO
4, 20mL/L H
3pO
4, 0.3g/L OP-10,6mL/L HF.
Described nitration mixture process, is specially:
Aluminium alloy is placed in 25 ~ 35 DEG C of mixed acid solutions, floods 1 ~ 3 minute, mixed acid solution consist of nitric acid 10%wt, phosphoric acid 2.5%wt and sulfuric acid 1.5 ~ 2%wt.
Compared with prior art, the present invention has the following advantages and beneficial effect:
(1) rete generated has color, is conducive to the observation in production process and operation, and traditional titanium zirconium passive film is all without color, and naked eyes are difficult to observe;
(2) improve film forming speed, traditional titanium zirconium passive film film forming needs 20 ~ 30min, and the present invention can obtain yellow rete in 60s, shortens film formation time, improves productivity effect;
(3) improve the corrosion resisting property of rete, the corrosion electric current density of traditional titanium zirconium passive film is 0.08 μ Acm
2, the rete corrosion electric current density that the present invention obtains at short notice is 0.044 μ Acm
2.
(4) traditional titanium zirconium passive film needs at high temperature to carry out, and the present invention carries out at normal temperatures, reaches energy-conservation object.
Accompanying drawing explanation
Fig. 1 schemes through the aluminum alloy surface SEM of titanium zirconium treatment solution process;
Fig. 2 is the aluminum alloy surface SEM figure through the titanium zirconium treatment solution process containing vanadic salts;
Fig. 3 is the aluminum alloy surface SEM figure of titanium zirconium treatment solution in embodiment 2;
Fig. 4 is the aluminum alloy surface EDS collection of illustrative plates through the process of titanium zirconium treatment solution;
Fig. 5 is the aluminum alloy surface EDS collection of illustrative plates through the titanium zirconium treatment solution process containing vanadic salts;
Fig. 6 is the aluminum alloy surface EDS collection of illustrative plates of the titanium zirconium treatment solution process in embodiment 2;
Fig. 7 is the EDS figure of second phase particles in Fig. 6;
Fig. 8 is the electrochemical tests of passive film under different treatment technique.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail, but embodiments of the present invention are not limited thereto.
Embodiment 1
The method preparing the coloured passive film of high anti-corrosion in aluminum alloy surface of the present embodiment, comprises the following steps:
(1) pre-treatment is carried out to aluminum alloy surface: by aluminum alloy surface polishing to 1000#, carry out industrial acid-washed and nitration mixture process successively;
Describedly industrial acid-washedly to be specially:
Aluminium alloy is placed in the acidic solution of 25 DEG C, floods 1 minute, described acidic solution consist of 100g/L H
2sO
4, 20mL/L H
3pO
4, 0.3g/L OP-10,6mL/L HF.
Described nitration mixture process, is specially:
Aluminium alloy is placed in 25 DEG C of mixed acid solutions, floods 1 minute, mixed acid solution consist of nitric acid 10%wt, phosphoric acid 2.5%wt and sulfuric acid 1.5%wt.
(2), in the aluminium alloy treatment solution that will process through step (1), namely the yellow passivated film containing zirconium, titanium, vanadium is obtained in aluminum alloy surface at 30 DEG C of dipping 10s; Described aluminium alloy treatment solution composed as follows:
Embodiment 2
The method preparing the coloured passive film of high anti-corrosion in aluminum alloy surface of the present embodiment, comprises the following steps:
(1) pre-treatment is carried out to aluminum alloy surface: by aluminum alloy surface polishing to 1000#, carry out industrial acid-washed and nitration mixture process successively;
Describedly industrial acid-washedly to be specially:
Aluminium alloy is placed in the acidic solution of 35 DEG C, floods 3 minutes, described acidic solution consist of 100g/L H
2sO
4, 20mL/L H
3pO
4, 0.3g/L OP-10,6mL/L HF.
Described nitration mixture process, is specially:
Aluminium alloy is placed in 35 DEG C of mixed acid solutions, floods 3 minutes, mixed acid solution consist of nitric acid 10%wt, phosphoric acid 2.5%wt and sulfuric acid 2%wt.
(2), in the aluminium alloy treatment solution that will process through step (1), namely the yellow passivated film containing zirconium, titanium, vanadium is obtained in aluminum alloy surface at 30 DEG C of dipping 60s; Described aluminium alloy treatment solution composed as follows:
Embodiment 3
The method preparing the coloured passive film of high anti-corrosion in aluminum alloy surface of the present embodiment, comprises the following steps:
(1) pre-treatment is carried out to aluminum alloy surface: by aluminum alloy surface polishing to 1000#, carry out industrial acid-washed and nitration mixture process successively;
(2), in the aluminium alloy treatment solution that will process through step (1), namely the yellow passivated film containing zirconium, titanium, vanadium is obtained in aluminum alloy surface at 50 DEG C of dipping 100s; Described aluminium alloy treatment solution composed as follows:
Embodiment 4
The method preparing the coloured passive film of high anti-corrosion in aluminum alloy surface of the present embodiment, comprises the following steps:
(1) pre-treatment is carried out to aluminum alloy surface;
(2), in the aluminium alloy treatment solution that will process through step (1), namely the yellow passivated film containing zirconium, titanium, vanadium is obtained in aluminum alloy surface at 50 DEG C of dipping 100s; Described aluminium alloy treatment solution composed as follows:
Embodiment 5
The method preparing the coloured passive film of high anti-corrosion in aluminum alloy surface of the present embodiment, comprises the following steps:
(1) pre-treatment is carried out to aluminum alloy surface;
(2), in the aluminium alloy treatment solution that will process through step (1), namely the yellow passivated film containing zirconium, titanium, vanadium is obtained in aluminum alloy surface at 50 DEG C of dipping 100s; Described aluminium alloy treatment solution composed as follows:
Below coloured passive film prepared by embodiments of the invention is tested.
Test 1 spot test
Experimental technique: adopt the corrosion resisting property of acid drop experimental technique rough determination passive film: use copper sulfate 41g/L, sodium-chlor 35g/L, 0.1N hydrochloric acid 13mL/L, be made into a dropping liquid, drip 2 ~ 3 at every turn and drop to specimen surface, and start timing, when becoming incarnadine Deng some dropping liquid from blueness, timing stops, be the reaction times during this period of time, the time is longer, illustrates that sample solidity to corrosion is better.
Experimental result: the untreated aluminium alloy resistance to drop time is 13s; The resistance to drop time of the titanium zirconium passive film of embodiment 1 is 110s; The titanium zirconium passive film resistance to drop time of embodiment 2 is 259s, and the titanium zirconium passive film resistance to drop time of embodiment 3 is 30s; The titanium zirconium passive film resistance to drop time of embodiment 4 is 130s; The resistance to drop time of the titanium zirconium passive film of embodiment 5 is 53s, and compared with aluminium alloy, corrosion resisting property obtains raising in various degree.
Test 2 utilizes scanning electron microscope to carry out pattern and composition analysis
For contrasting, preparation Sample A, B, C, D, the prescription for the treatment of liquid (A is undressed sample) as shown in table 1 that each sample is used, wherein the treatment temp of B, C sample is 30 DEG C, treatment time is the treatment temp of 25min, D sample is 30 DEG C, and the treatment time is 60s.
The formula of each sample of table 1 treatment solution used
Sample B, C, D surface passivated membrane respectively as shown in Figure 1, Figure 2 and Figure 3.Relatively can find from Fig. 1 and Fig. 2: both are continuous film, but there is some holes and crackle, these holes are because under acidic conditions, evolving hydrogen reaction (2Al+6H easily occurs for aluminium and hydrogen ion
+→ 2Al
3++ 3H
2↑), cause producing pore, thus have impact on the corrosion resisting property of passive film; After adding vanadic salts, hole obviously reduces, and rete becomes finer and close, even, and the crackle on surface may be that internal stress and drying and dehydrating produce.As can see from Figure 3, after adding Weibull, can promote the growth of passive film, rete is fine and close, and crackle reduces, and make the compactness of passive film better, the power spectrum of its correspondence as shown in Figure 7.Fig. 4 is sample B surface EDS collection of illustrative plates; Fig. 5 is sample C surface EDS collection of illustrative plates; Fig. 6 is sample D surface second phase particles EDS collection of illustrative plates; Table 2,3,4,5 be respectively Fig. 4,5,6, the EDS analytical results of 7.Contrast discovery by table 4 and table 5, in table 5, the content of Fe, Si, Ti, V, F improves greatly.
Table 2 sample B surface EDS pattern analysis results
Table 3 sample C surface EDS pattern analysis results
Table 4 sample D surface EDS pattern analysis results
Table 5 sample D surface second phase particles EDS pattern analysis results
Test 3: electrochemical tests is tested
Experimental technique: sample epoxy resin is coated with envelope, exposes the working area of 10mm × 10mm, evaluated the electrochemical corrosion performance of sample by Ta Feier polarization measurement.All electrochemical measurements are all carry out on CHI660D electrochemical workstation (Shanghai Chen Hua instrument company), adopt conventional three-electrode system, supporting electrode is platinum electrode, reference electrode is saturated calomel electrode (SCE), sample to be tested is as working electrode, test soln is the 3.5%NaCl aqueous solution, under the condition of room temperature, not degasification, soaks 20min and carries out after corrosion potential is stable.The scope of polarization curve scanning is-1.5V ~-0.2V, and scanning speed is 5mV/s.Test the corresponding computer software matching of rear utilization, obtain corrosion potential E
corrwith corrosion electric current density i
corr.
Electrochemical tests result in 3.5% sodium-chlor neutral electrolyte is as shown in Fig. 8 and table 6.Fig. 8 is the polarization curve test pattern of four kinds of Sample A in table 1, B, C, D, and table 6 is its match value.Wherein E
corrfor corrosion potential, i
corrfor corrosion current, R
pfor polarization resistance.As can be seen from the table, sample B, C, D are relative to aluminium alloy A, polarization resistance R
pincreasing, from 9.467k Ω cm
2be increased to 90.030k Ω cm respectively
2, 151.220k Ω cm
2, 198.643k Ω cm
2; Corrosion electric current density i
corrmore and more less, from 5.366 μ Acm
2, 0.455 μ Acm
2, 0.2509 μ Acm
2, 0.1339 μ Acm
2.Above result shows, aluminum alloy surface generates passive film can reduce corrosion electric current density, improves the corrosion resistance of aluminium alloy.Compare B and C respectively, D is known, along with vanadic salts with organicly to add, not only reach the effect of coloring passive film, but also be conducive to the raising of passive film corrosion resisting property.Relatively C and D is known, and along with adding of Weibull, the color of passive film improves, and can obtain the yellow passivated film of even compact fast, and be conducive to the raising of corrosion resisting property in 60s.
The corrosion potential of table 6 Sample A, B, C, D, corrosion current, polarization resistance match value
Above-described embodiment is the present invention's preferably embodiment; but embodiments of the present invention are not limited by the examples; change, the modification done under other any does not deviate from spirit of the present invention and principle, substitute, combine, simplify; all should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (6)
1. prepare a method for the coloured passive film of high anti-corrosion in aluminum alloy surface, it is characterized in that, comprise the following steps:
(1) pre-treatment is carried out to aluminum alloy surface;
(2) aluminium alloy processed through step (1) is placed in treatment solution, namely obtains the yellow passivated film containing zirconium, titanium, vanadium in aluminum alloy surface at 25 DEG C ~ 90 DEG C dipping 10s ~ 600s; Described aluminium alloy treatment solution composed as follows:
2. the method preparing the coloured passive film of high anti-corrosion in aluminum alloy surface according to claim 1, is characterized in that, described aluminium alloy treatment solution composed as follows:
3. the method preparing the coloured passive film of high anti-corrosion in aluminum alloy surface according to claim 1, is characterized in that, the pH value of described aluminium alloy treatment solution is 2.0 ~ 4.0.
4. the method preparing the coloured passive film of high anti-corrosion in aluminum alloy surface according to claim 1, is characterized in that, step (1) is described carries out pre-treatment to aluminum alloy surface, is specially:
By aluminum alloy surface polishing to 1000#, carry out industrial acid-washed and nitration mixture process successively.
5. the method preparing the coloured passive film of high anti-corrosion in aluminum alloy surface according to claim 4, is characterized in that, described industrial acid-washed, is specially:
Aluminium alloy is placed in the acidic solution of 25 ~ 35 DEG C, floods 1 ~ 3 minute, described acidic solution consist of 100g/L H
2sO
4, 20mL/L H
3pO
4, 0.3g/L OP-10,6mL/L HF.
6. the method preparing the coloured passive film of high anti-corrosion in aluminum alloy surface according to claim 4, is characterized in that, described nitration mixture process, is specially:
Aluminium alloy is placed in 25 ~ 35 DEG C of mixed acid solutions, floods 1 ~ 3 minute, mixed acid solution consist of nitric acid 10%wt, phosphoric acid 2.5%wt and sulfuric acid 1.5 ~ 2%wt.
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| CN103498137B (en) * | 2013-09-24 | 2016-05-04 | 华南理工大学 | A kind for the treatment of fluid and processing method of preparing the coloured conversion film of zirconium base at Mg alloy surface |
| CN104532225A (en) * | 2014-12-15 | 2015-04-22 | 镁联科技（芜湖）有限公司 | Aluminum alloy passivator, preparation method thereof and aluminum alloy passivating method |
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| CN106048580B (en) * | 2016-07-05 | 2018-08-31 | 博罗县东明化工有限公司 | Zirconium-manganese-vanadium passivating film inorganic agent and its processing method for pack alloy |
| CN106086857B (en) * | 2016-08-25 | 2019-07-02 | 广州市泓硕环保科技有限公司 | A kind of film forming solution of aluminium based material surface collaboration Optimization-type Chrome-free yellow conversion film and its method for preparing conversion film |
| WO2019006627A1 (en) * | 2017-07-03 | 2019-01-10 | 深圳市盈恒科技有限公司 | Chromium-free passivator, aluminum part and surface passivation process therefor |
| CN107460470A (en) * | 2017-08-09 | 2017-12-12 | 泾县信达工贸有限公司 | A kind of preparation method of heat-generating disc aluminium sheet |
| CN111394718B (en) * | 2020-03-04 | 2022-11-11 | 广东东明新材科技有限公司 | Passivation solution and copper surface film forming treatment method |
| CN113235077A (en) * | 2021-05-11 | 2021-08-10 | 齐齐哈尔北方集团北方化学工业有限责任公司 | Aluminum alloy vanadium-titanium-europium passivation solution and preparation and use method thereof |
| CN114635129B (en) * | 2022-04-18 | 2023-08-29 | 中国机械总院集团武汉材料保护研究所有限公司 | Synchronous chemical conversion method suitable for various aluminum alloy and galvanized steel materials |
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