CN115142055A - Hydrophobic chemical conversion film forming liquid and aluminum alloy surface treatment method - Google Patents
Hydrophobic chemical conversion film forming liquid and aluminum alloy surface treatment method Download PDFInfo
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- 238000006243 chemical reaction Methods 0.000 title claims abstract description 104
- 239000000126 substance Substances 0.000 title claims abstract description 104
- 229910000838 Al alloy Inorganic materials 0.000 title claims abstract description 55
- 230000002209 hydrophobic effect Effects 0.000 title claims abstract description 50
- 238000000034 method Methods 0.000 title claims abstract description 27
- 238000004381 surface treatment Methods 0.000 title claims abstract description 24
- 239000007788 liquid Substances 0.000 title abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 57
- 239000002253 acid Substances 0.000 claims abstract description 23
- 238000004140 cleaning Methods 0.000 claims abstract description 16
- 230000032683 aging Effects 0.000 claims abstract description 15
- 239000000654 additive Substances 0.000 claims abstract description 10
- 230000000996 additive effect Effects 0.000 claims abstract description 10
- 150000001844 chromium Chemical class 0.000 claims abstract description 9
- 239000012535 impurity Substances 0.000 claims abstract description 3
- 238000005406 washing Methods 0.000 claims description 38
- 239000008367 deionised water Substances 0.000 claims description 37
- 229910021641 deionized water Inorganic materials 0.000 claims description 37
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 30
- 239000003513 alkali Substances 0.000 claims description 18
- 238000005238 degreasing Methods 0.000 claims description 12
- 238000000576 coating method Methods 0.000 claims description 11
- 230000002378 acidificating effect Effects 0.000 claims description 10
- 239000011248 coating agent Substances 0.000 claims description 10
- 238000007739 conversion coating Methods 0.000 claims description 10
- 230000008021 deposition Effects 0.000 claims description 10
- 239000012459 cleaning agent Substances 0.000 claims description 9
- 239000011734 sodium Substances 0.000 claims description 5
- 229910021555 Chromium Chloride Inorganic materials 0.000 claims description 4
- PHFQLYPOURZARY-UHFFFAOYSA-N chromium trinitrate Chemical compound [Cr+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O PHFQLYPOURZARY-UHFFFAOYSA-N 0.000 claims description 4
- QSWDMMVNRMROPK-UHFFFAOYSA-K chromium(3+) trichloride Chemical compound [Cl-].[Cl-].[Cl-].[Cr+3] QSWDMMVNRMROPK-UHFFFAOYSA-K 0.000 claims description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- GRWVQDDAKZFPFI-UHFFFAOYSA-H chromium(III) sulfate Chemical compound [Cr+3].[Cr+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O GRWVQDDAKZFPFI-UHFFFAOYSA-H 0.000 claims description 2
- BJZIJOLEWHWTJO-UHFFFAOYSA-H dipotassium;hexafluorozirconium(2-) Chemical compound [F-].[F-].[F-].[F-].[F-].[F-].[K+].[K+].[Zr+4] BJZIJOLEWHWTJO-UHFFFAOYSA-H 0.000 claims description 2
- RXCBCUJUGULOGC-UHFFFAOYSA-H dipotassium;tetrafluorotitanium;difluoride Chemical group [F-].[F-].[F-].[F-].[F-].[F-].[K+].[K+].[Ti+4] RXCBCUJUGULOGC-UHFFFAOYSA-H 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- 229910052708 sodium Inorganic materials 0.000 claims description 2
- 238000005260 corrosion Methods 0.000 abstract description 21
- 230000007797 corrosion Effects 0.000 abstract description 15
- 239000007888 film coating Substances 0.000 abstract description 12
- 238000009501 film coating Methods 0.000 abstract description 12
- 229910052751 metal Inorganic materials 0.000 abstract description 5
- 239000002184 metal Substances 0.000 abstract description 5
- 231100000086 high toxicity Toxicity 0.000 abstract description 3
- 229910052782 aluminium Inorganic materials 0.000 description 122
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 122
- 239000011888 foil Substances 0.000 description 121
- 239000000243 solution Substances 0.000 description 39
- 239000000758 substrate Substances 0.000 description 17
- 239000007864 aqueous solution Substances 0.000 description 15
- 238000012360 testing method Methods 0.000 description 15
- KMUONIBRACKNSN-UHFFFAOYSA-N potassium dichromate Chemical compound [K+].[K+].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O KMUONIBRACKNSN-UHFFFAOYSA-N 0.000 description 12
- 238000001878 scanning electron micrograph Methods 0.000 description 10
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 8
- 239000011651 chromium Substances 0.000 description 8
- 238000007605 air drying Methods 0.000 description 7
- 238000005554 pickling Methods 0.000 description 6
- 238000004458 analytical method Methods 0.000 description 4
- 238000005530 etching Methods 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- 150000003839 salts Chemical class 0.000 description 4
- 239000011780 sodium chloride Substances 0.000 description 4
- 239000007921 spray Substances 0.000 description 4
- ZCDOYSPFYFSLEW-UHFFFAOYSA-N chromate(2-) Chemical compound [O-][Cr]([O-])(=O)=O ZCDOYSPFYFSLEW-UHFFFAOYSA-N 0.000 description 3
- JOPOVCBBYLSVDA-UHFFFAOYSA-N chromium(6+) Chemical compound [Cr+6] JOPOVCBBYLSVDA-UHFFFAOYSA-N 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 238000007747 plating Methods 0.000 description 3
- 230000010287 polarization Effects 0.000 description 3
- 238000005275 alloying Methods 0.000 description 2
- 239000002585 base Substances 0.000 description 2
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- -1 rare earth salt Chemical class 0.000 description 2
- 238000004448 titration Methods 0.000 description 2
- 238000012876 topography Methods 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
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- 231100000315 carcinogenic Toxicity 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229910001430 chromium ion Inorganic materials 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
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- 238000009776 industrial production Methods 0.000 description 1
- 238000004372 laser cladding Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
- C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
- C23C22/34—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing fluorides or complex fluorides
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/78—Pretreatment of the material to be coated
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C2222/00—Aspects relating to chemical surface treatment of metallic material by reaction of the surface with a reactive medium
- C23C2222/10—Use of solutions containing trivalent chromium but free of hexavalent chromium
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- Chemical & Material Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Treatment Of Metals (AREA)
Abstract
The invention relates to a hydrophobic chemical conversion film-forming solution and an aluminum alloy surface treatment method. Hydrophobic chemical conversion film liquid, which comprises trivalent chromium salt, fluorozirconate, additive and water; the additive is fluotitanic acid and/or fluotitanate. The invention also provides an aluminum alloy surface treatment method, which comprises the following steps: pretreatment: carrying out impurity removal treatment on the surface of the aluminum alloy; film coating: placing the aluminum alloy in the hydrophobic chemical conversion film-forming solution of the invention for chemical conversion treatment to form a hydrophobic chemical conversion film on the surface of the aluminum alloy; and (3) natural aging: and cleaning the coated aluminum alloy, and naturally aging the aluminum alloy at normal temperature. The invention solves the problems of high toxicity, poor corrosion resistance and the like of the existing metal surface chemical conversion film.
Description
Technical Field
The invention relates to the technical field of aluminum alloy surface treatment, in particular to a hydrophobic chemical conversion film-forming solution and an aluminum alloy surface treatment method.
Background
Aluminum alloys are currently the most widely used lightweight metallic structural materials in the world. In order to satisfy the requirements of mechanical properties and the like, various alloying elements such as Cu, mg, zn, si and the like are generally added to the aluminum alloy. However, the addition of a large amount of alloying elements reduces the corrosion resistance of most aluminum alloys, and thus the requirements of industrial application cannot be met. Therefore, most aluminum alloys require a certain surface treatment before they can be put into use.
The common aluminum alloy surface treatment process comprises the following steps: electroplating, chemical conversion, anodic oxidation, micro-arc oxidation, laser cladding, sol-gel and the like. Wherein, the chemical conversion film treatment does not need an external power supply, the process operation is simple, the production cost is low, the mechanical property of the base material is not obviously influenced, and the like, and the method is widely applied to industrial production. Among them, the chromate conversion film has been widely used for a long time in the past because it is a chemical conversion film having the longest use, the best corrosion resistance, and the self-healing function.
However, long-term practical studies have found that hexavalent chromium ions contained in chromates are carcinogenic and have serious harm to human bodies, animals and the natural environment. The European Union environmental protection organization completely forbids the commercial application of the hexavalent chromium conversion film in 2017, and countries such as the United states and the Japan have strict limits on the hexavalent chromium. Thus, green and environment-friendly chromium-free conversion and chemical conversion processes are produced. The chromium-free conversion film mainly comprises zirconate conversion films, phosphates, molybdates, titanates, cobaltates, rare earth salt conversion films and the like, but is loose, poor in corrosion resistance, or complicated in working procedure, and has a protection effect and an application range which are not as good as those of the chromate conversion film.
Disclosure of Invention
One of the purposes of the invention is to provide a hydrophobic chemical conversion film-forming solution, which is used for solving the problems of high toxicity, poor corrosion resistance and the like of the existing metal surface chemical conversion film; the second purpose is to provide a surface treatment method of the aluminum alloy to improve the corrosion resistance of the aluminum alloy.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a hydrophobic chemical conversion film liquid comprises trivalent chromium salt, fluorozirconate, additive and water;
the additive is fluotitanic acid (H) 2 TiF 6 ) And/or fluorotitanates.
Preferably, the trivalent chromium salt comprises chromium sulfate (Cr) 2 (SO 4 ) 3 ) Chromium nitrate (Cr (NO) 3 ) 3 ) And chromium chloride (CrCl) 3 ) One or more of (a).
Preferably, the fluorozirconate comprises potassium fluorozirconate (K) 2 ZrF 6 ) And sodium fluorozirconate (Na) 2 ZrF 6 ) One or two of them.
Preferably, the fluorotitanate is potassium fluorotitanate (K) 2 TiF 6 )。
Preferably, the concentration of the trivalent chromium salt is 0.5 to 5g/L, the concentration of the fluorozirconate is 1 to 10g/L, and the concentration of the additive is 0.5 to 5g/L.
The invention also provides an aluminum alloy surface treatment method, which comprises the following steps:
s1, pretreatment: carrying out impurity removal treatment on the surface of the aluminum alloy;
s2, coating: adjusting the pH value of the hydrophobic chemical conversion film-forming solution to acidity, and then putting the aluminum alloy into the acidic hydrophobic chemical conversion film-forming solution for chemical conversion treatment to form a hydrophobic chemical conversion film on the surface of the aluminum alloy;
s3, natural aging: and cleaning the coated aluminum alloy, and naturally aging the aluminum alloy at normal temperature.
Wherein, the chemical conversion coating formed on the surface of the aluminum alloy is colorless.
Preferably, in the step S2, the temperature of the chemical conversion treatment is 20 to 60 ℃, the film forming rate can be effectively controlled in the temperature range, so that the film layer can rapidly and uniformly grow, and the treatment time is 60 to 600 seconds.
Preferably, in the step S1, the pretreatment comprises the steps of sequentially carrying out oil removal, alkali washing, acid washing and rinsing on the aluminum alloy;
wherein, the degreasing is carried out by adopting a degreasing cleaning agent for cleaning, the cleaning temperature is 50-60 ℃, and the cleaning time is 30-120 seconds; treating alkaline washing (to fully remove the rolling deformation layer and part of the second phase particles on the surface) by using 5-10% (wt.) sodium hydroxide (NaOH) solution, wherein the alkaline washing temperature is 30-40 ℃, and the alkaline washing time is 10-60 seconds; the acid washing adopts 30 to 40 percent (vol.) nitric acid (HNO) 3 ) Treating the solution, wherein the pickling temperature is 20-30 ℃, and the pickling time is 10-60 seconds; the rinsing is carried out by using deionized water, the rinsing temperature is 70-80 ℃, and the rinsing time is 10-60 seconds.
Preferably, in S3, the natural aging time is 48 to 120 hours.
Preferably, the thickness of the chemical conversion coating formed on the surface of the aluminum alloy is 50 nm-150 nm, and the water contact angle of the chemical conversion coating is more than 100 degrees.
The invention has the beneficial effects that:
1) The hydrophobic chemical conversion film-forming solution takes chromium salt, fluorozirconate and an additive as main components of the film-forming solution, the chromium salt has the advantages of low toxicity, good corrosion resistance, high temperature resistance, certain conductivity and good adhesive force, the fluorozirconate is taken as an oxidant and a film-forming agent and is mainly used for providing fluoride ions to dissolve an aluminum substrate so as to promote the film-forming reaction, the additive is taken as a film-forming promoter, the structure of a passivation film layer is fine, the porosity is reduced, and meanwhile, a more stable oxide is introduced into the film layer, so that a nano chemical conversion film prepared on the metal surface has good hydrophobic property, the corrosion resistance of the metal surface is effectively improved, the hydrophobic chemical conversion film has the advantages of environmental protection, and the problems of high toxicity and poor corrosion resistance of the existing chemical conversion film on the metal surface are solved;
2) According to the aluminum alloy surface treatment method, the aluminum alloy is placed in the hydrophobic chemical conversion film-forming solution, so that the chemical conversion film-forming solution and the surface of the aluminum alloy are subjected to chemical reaction, and a layer of chemical conversion film is formed on the surface of the aluminum alloy.
Drawings
FIG. 1 is a scanning electron micrograph (10 μm) of a 5056 aluminum foil after treatment in example 1;
FIG. 2 is a scanning electron micrograph (1 μm) of a 5056 aluminum foil after treatment in example 1;
FIG. 3 is a scanning electron micrograph (10 μm) of a 5056 aluminum foil after treatment in example 2;
FIG. 4 is a scanning electron micrograph (1 μm) of a 5056 aluminum foil after treatment in example 2;
FIG. 5 is a scanning electron micrograph (10 μm) of a 5056 aluminum foil after treatment in example 3;
FIG. 6 is a scanning electron micrograph (1 μm) of a 5056 aluminum foil after treatment in example 3;
FIG. 7 is a scanning electron micrograph (10 μm) of a 5056 aluminum foil after processing in example 4;
FIG. 8 is a scanning electron micrograph (1 μm) of the 5056 aluminum foil after treatment in example 4;
FIG. 9 is a scanning electron micrograph (10 μm) of a 5056 aluminum foil after processing in example 5;
FIG. 10 is a scanning electron micrograph (2 μm) of a 5056 aluminum foil after processing in example 5;
FIG. 11 is a macro topography of a 5% neutral salt spray test performed on a 5056 aluminum foil after processing in example 1;
fig. 12 is a graph showing the results of water contact angle tests performed on 5056 aluminum foil after treatment in examples 1-5;
FIG. 13 is an electrochemical impedance spectrum of 5056 aluminum foil treated in examples 1-5 in 3.5% (wt%) NaCl aqueous solution;
FIG. 14 is a graph showing the electrochemical polarization of the 5056 aluminum foil after being processed in examples 1-5 in a 3.5% (wt%) aqueous NaCl solution;
FIG. 15 is a graph showing the results of a potassium dichromate spot test on 5056 aluminum foil after treatment in examples 1, 6, and 7.
Detailed Description
Other advantages and effects of the present invention will become apparent to those skilled in the art from the disclosure herein, wherein the embodiments of the present invention are described in detail with reference to the accompanying drawings and preferred embodiments. The invention is capable of other and different embodiments and of being practiced or of being carried out in various ways, and its several details are capable of modification in various respects, all without departing from the spirit and scope of the present invention. It should be understood that the preferred embodiments are illustrative of the invention only and are not limiting upon the scope of the invention.
Example 1
An aluminum alloy surface treatment method comprises the following steps:
s1, pretreatment:
1) Oil removal treatment: putting the 5056 aluminum foil into 10wt.% oil-removing cleaning agent, keeping the temperature at 60 ℃ for 30s for oil-removing and degreasing treatment, taking out, and rinsing in 80 ℃ deionized water for 30s;
2) Alkali washing treatment: placing 5056 aluminum foil after oil removal treatment into 10wt.% NaOH aqueous solution, keeping the temperature at 40 ℃ for 30s, taking out, and rinsing in 80 ℃ deionized water for 30s;
3) Acid washing treatment: 5056 aluminum foil subjected to alkali washing treatment is placed into 30vol.% of HNO 3 Carrying out deoxidation and ash removal treatment for 30s in the aqueous solution, and then taking out and rinsing in deionized water at 80 ℃ for 30s;
4) Rinsing treatment: washing the 5056 aluminum foil subjected to acid cleaning with deionized water, and finally performing natural air drying to obtain a preprocessed 5056 aluminum foil;
s2, coating: with 1wt.% of H 2 SO 4 Blending of solutionSaving the pH value of the hydrophobic chemical conversion film-forming solution to 3.5, then placing 5056 aluminum foil subjected to pretreatment in S1 in an acidic hydrophobic chemical conversion film-forming solution for chemical conversion treatment so as to form a hydrophobic chemical conversion film on the surface of 5056 aluminum foil, wherein the temperature of the chemical conversion treatment is 40 ℃, and the time of the chemical conversion treatment is 120S;
among these, the component of the hydrophobic chemical conversion coating solution in example 1 was Cr 2 (SO 4 ) 3 、K 2 ZrF 6 、H 2 TiF 6 And water, cr 2 (SO 4 ) 3 Has a concentration of 2g/L, K 2 ZrF 6 Has a concentration of 4g/L, H 2 TiF 6 The concentration of (A) is 2g/L;
s3, natural aging: and after the film coating is finished, the 5056 aluminum foil is washed by deionized water, and then is naturally air-dried and aged for 48 hours in a normal temperature environment, so that the 5056 aluminum foil with the colorless chemical conversion film formed on the surface is obtained.
Example 2
An aluminum alloy surface treatment method comprises the following steps:
s1, pretreatment:
1) Oil removal treatment: putting the 5056 aluminum foil into 10wt.% oil-removing cleaning agent, keeping the temperature at 60 ℃ for 30s for oil-removing and degreasing treatment, taking out, and rinsing in 80 ℃ deionized water for 30s;
2) Alkali washing treatment: placing 5056 aluminum foil after oil removal treatment into 10wt.% NaOH aqueous solution, keeping the temperature at 40 ℃ for 30s, taking out, and rinsing in 80 ℃ deionized water for 30s;
3) Acid washing treatment: 5056 aluminum foil after alkali washing treatment is placed into 30vol.% of HNO 3 Carrying out deoxidation and ash removal treatment for 30s in the aqueous solution, and then taking out and rinsing in deionized water at 80 ℃ for 30s;
4) Rinsing treatment: washing the 5056 aluminum foil subjected to acid cleaning with deionized water, and finally performing natural air drying to obtain a preprocessed 5056 aluminum foil;
s2, coating: with 1wt.% of H 2 SO 4 The pH value of the hydrophobic chemical conversion film-forming solution is adjusted to 2 by the solution.0, placing the 5056 aluminum foil pretreated in S1 in an acidic hydrophobic chemical conversion film-forming solution to perform chemical conversion treatment so as to form a chemical conversion film on the surface of the 5056 aluminum foil, wherein the temperature of the chemical conversion treatment is 40 ℃, and the time of the chemical conversion treatment is 120S;
among these, the component of the hydrophobic chemical conversion coating solution in example 2 was Cr 2 (SO 4 ) 3 、Na 2 ZrF 6 、K 2 TiF 6 And water, cr 2 (SO 4 ) 3 Has a concentration of 2g/L, na 2 ZrF 6 Has a concentration of 4g/L, K 2 TiF 6 The concentration of (b) is 2g/L;
s3, natural aging: and after the film coating is finished, the 5056 aluminum foil is washed by deionized water, and then is naturally air-dried and aged for 48 hours in a normal-temperature environment, so that the 5056 aluminum foil with the colorless chemical conversion film formed on the surface is obtained.
Example 3
An aluminum alloy surface treatment method comprises the following steps:
s1, pretreatment:
1) Oil removal treatment: putting the 5056 aluminum foil into 10wt.% oil-removing cleaning agent, keeping the temperature at 60 ℃ for 30s for oil-removing and degreasing treatment, taking out, and rinsing in 80 ℃ deionized water for 30s;
2) Alkali washing treatment: placing 5056 aluminum foil after oil removal treatment into 10wt.% NaOH aqueous solution, keeping the temperature at 40 ℃ for 30s, taking out, and rinsing in 80 ℃ deionized water for 30s;
3) Acid pickling treatment: 5056 aluminum foil after alkali washing treatment is placed into 30vol.% of HNO 3 Carrying out deoxidation and ash removal treatment in the aqueous solution for 30s, and then taking out and rinsing in deionized water at the temperature of 80 ℃ for 30s;
4) Rinsing treatment: washing the 5056 aluminum foil subjected to acid cleaning with deionized water, and finally performing natural air drying to obtain a preprocessed 5056 aluminum foil;
s2, coating: with 1wt.% H 2 SO 4 Adjusting the pH value of the hydrophobic chemical conversion film-forming solution to 3.0 by using the solution, and placing 5056 aluminum foil pretreated in S1 into acidic solutionCarrying out chemical conversion treatment in the hydrophobic chemical conversion film-forming solution to form a chemical conversion film on the surface of the 5056 aluminum foil, wherein the temperature of the chemical conversion treatment is 40 ℃, and the time of the chemical conversion treatment is 120S;
among them, the hydrophobic chemical conversion deposition solution of example 3 contained Cr as a component 2 (SO 4 ) 3 、Na 2 ZrF 6 、H 2 TiF 6 And water, cr 2 (SO 4 ) 3 Has a concentration of 2g/L, na 2 ZrF 6 Has a concentration of 2g/L, H 2 TiF 6 The concentration of (A) is 2g/L;
s3, natural aging: and after the film coating is finished, the 5056 aluminum foil is washed by deionized water, and then is naturally air-dried and aged for 48 hours in a normal temperature environment, so that the 5056 aluminum foil with the colorless chemical conversion film formed on the surface is obtained.
Example 4
An aluminum alloy surface treatment method comprises the following steps:
s1, pretreatment:
1) Oil removal treatment: putting the 5056 aluminum foil into 10wt.% oil-removing cleaning agent, keeping the temperature at 60 ℃ for 30s for oil-removing and degreasing treatment, taking out, and rinsing in 80 ℃ deionized water for 30s;
2) Alkali washing treatment: placing 5056 aluminum foil after oil removal treatment into 10wt.% NaOH aqueous solution, keeping the temperature at 40 ℃ for 30s, taking out, and rinsing in 80 ℃ deionized water for 30s;
3) Acid pickling treatment: 5056 aluminum foil after alkali washing treatment is placed into 30vol.% of HNO 3 Carrying out deoxidation and ash removal treatment in the aqueous solution for 30s, and then taking out and rinsing in deionized water at the temperature of 80 ℃ for 30s;
4) Rinsing treatment: washing the 5056 aluminum foil subjected to acid cleaning with deionized water, and finally performing natural air drying to obtain a preprocessed 5056 aluminum foil;
s2, coating: with 1wt.% of H 2 SO 4 Adjusting the pH value of the hydrophobic chemical conversion film-forming solution to 4.0 by the solution, placing 5056 aluminum foil pretreated in S1 in acidic hydrophobic chemical conversion film-forming solution for chemical conversion treatment,forming a chemical conversion film on the surface of the 5056 aluminum foil, wherein the temperature of chemical conversion treatment is 40 ℃, and the time of chemical conversion treatment is 120S;
the hydrophobic chemical conversion deposition solution of example 4 contained Cr (NO) 3 ) 3 、K 2 ZrF 6 、H 2 TiF 6 And water, cr (NO) 3 ) 3 Has a concentration of 2g/L, K 2 ZrF 6 Has a concentration of 2g/L, H 2 TiF 6 The concentration of (A) is 2g/L;
s3, natural aging: and after the film coating is finished, the 5056 aluminum foil is washed by deionized water, and then is naturally air-dried and aged for 48 hours in a normal-temperature environment, so that the 5056 aluminum foil with the colorless chemical conversion film formed on the surface is obtained.
Example 5
An aluminum alloy surface treatment method comprises the following steps:
s1, pretreatment:
1) Oil removal treatment: putting the 5056 aluminum foil into 10wt.% oil-removing cleaning agent, keeping the temperature at 60 ℃ for 30s for oil-removing and degreasing treatment, taking out, and rinsing in 80 ℃ deionized water for 30s;
2) Alkali washing treatment: placing 5056 aluminum foil after oil removal treatment into 10wt.% NaOH aqueous solution, keeping the temperature at 40 ℃ for 30s, taking out, and rinsing in 80 ℃ deionized water for 30s;
3) Acid washing treatment: 5056 aluminum foil after alkali washing treatment is placed into 30vol.% of HNO 3 Carrying out deoxidation and ash removal treatment in the aqueous solution for 30s, and then taking out and rinsing in deionized water at the temperature of 80 ℃ for 30s;
4) Rinsing treatment: washing the 5056 aluminum foil subjected to acid cleaning with deionized water, and finally performing natural air drying to obtain a preprocessed 5056 aluminum foil;
s2, coating: with 1wt.% H 2 SO 4 Adjusting the pH value of the hydrophobic chemical conversion film-forming solution to 5.0 by using the solution, placing 5056 aluminum foil pretreated in S1 into acidic hydrophobic chemical conversion film-forming solution for chemical conversion treatment to form a chemical conversion film on the surface of 5056 aluminum foil, wherein the temperature of the chemical conversion treatment is 40 ℃,the time of the chemical conversion treatment is 120S;
in example 5, the hydrophobic chemical conversion deposition solution contained CrCl as a component 3 、K 2 ZrF 6 、H 2 TiF 6 And water, crCl 3 Has a concentration of 2g/L, K 2 ZrF 6 Has a concentration of 2g/L, H 2 TiF 6 The concentration of (b) is 2g/L;
s3, natural aging: and after the film coating is finished, the 5056 aluminum foil is washed by deionized water, and then is naturally air-dried and aged for 48 hours in a normal temperature environment, so that the 5056 aluminum foil with the colorless chemical conversion film formed on the surface is obtained.
Example 6
An aluminum alloy surface treatment method comprises the following steps:
s1, pretreatment:
5) Oil removal treatment: putting the 5056 aluminum foil into 10wt.% oil-removing cleaning agent, keeping the temperature at 60 ℃ for 30s for oil-removing and degreasing treatment, taking out, and rinsing in 80 ℃ deionized water for 30s;
6) Alkali washing treatment: placing 5056 aluminum foil subjected to oil removal treatment into 10wt.% NaOH aqueous solution, keeping the temperature at 40 ℃ for 30s, taking out, and rinsing in 80 ℃ deionized water for 30s;
7) Acid pickling treatment: 5056 aluminum foil subjected to alkali washing treatment is placed into 30vol.% of HNO 3 Carrying out deoxidation and ash removal treatment for 30s in the aqueous solution, and then taking out and rinsing in deionized water at 80 ℃ for 30s;
8) Rinsing treatment: washing the 5056 aluminum foil subjected to acid cleaning with deionized water, and finally performing natural air drying to obtain a preprocessed 5056 aluminum foil;
s2, coating: with 1wt.% of H 2 SO 4 Adjusting the pH value of the hydrophobic chemical conversion film-forming solution to 3.5 by using the solution, and then placing 5056 aluminum foil subjected to pretreatment in S1 into acidic hydrophobic chemical conversion film-forming solution for chemical conversion treatment so as to form a hydrophobic chemical conversion film on the surface of 5056 aluminum foil, wherein the temperature of the chemical conversion treatment is 40 ℃, and the time of the chemical conversion treatment is 120S;
among them, the embodiment 6The component of the hydrophobic chemical conversion film-forming solution in (1) is Cr 2 (SO 4 ) 3 、K 2 ZrF 6 、H 2 TiF 6 And water, cr 2 (SO 4 ) 3 Has a concentration of 0.5g/L, K 2 ZrF 6 Has a concentration of 1g/L, H 2 TiF 6 The concentration of (b) is 0.5g/L;
s3, natural aging: and after the film coating is finished, the 5056 aluminum foil is washed by deionized water, and then is naturally air-dried and aged for 48 hours in a normal temperature environment, so that the 5056 aluminum foil with the colorless chemical conversion film formed on the surface is obtained.
Example 7
An aluminum alloy surface treatment method comprises the following steps:
s1, pretreatment:
9) Oil removal treatment: putting the 5056 aluminum foil into 10wt.% oil-removing cleaning agent, keeping the temperature at 60 ℃ for 30s for oil-removing and degreasing treatment, taking out, and rinsing in 80 ℃ deionized water for 30s;
10 Alkaline washing treatment: placing 5056 aluminum foil after oil removal treatment into 10wt.% NaOH aqueous solution, keeping the temperature at 40 ℃ for 30s, taking out, and rinsing in 80 ℃ deionized water for 30s;
11 Acid pickling treatment: 5056 aluminum foil after alkali washing treatment is placed into 30vol.% of HNO 3 Carrying out deoxidation and ash removal treatment in the aqueous solution for 30s, and then taking out and rinsing in deionized water at the temperature of 80 ℃ for 30s;
12 ) rinsing treatment: washing the 5056 aluminum foil subjected to acid cleaning with deionized water, and finally performing natural air drying to obtain a preprocessed 5056 aluminum foil;
s2, coating: with 1wt.% of H 2 SO 4 Adjusting the pH value of the hydrophobic chemical conversion film-forming solution to 3.5 by using the solution, and then placing 5056 aluminum foil subjected to pretreatment in S1 into acidic hydrophobic chemical conversion film-forming solution for chemical conversion treatment so as to form a hydrophobic chemical conversion film on the surface of 5056 aluminum foil, wherein the temperature of the chemical conversion treatment is 40 ℃, and the time of the chemical conversion treatment is 120S;
among them, in example 6, the hydrophobic chemical conversion deposition solutionThe component is Cr 2 (SO 4 ) 3 、K 2 ZrF 6 、H 2 TiF 6 And water, cr 2 (SO 4 ) 3 Has a concentration of 5g/L, K 2 ZrF 6 Has a concentration of 10g/L, H 2 TiF 6 The concentration of (b) is 5g/L;
s3, natural aging: and after the film coating is finished, the 5056 aluminum foil is washed by deionized water, and then is naturally air-dried and aged for 48 hours in a normal-temperature environment, so that the 5056 aluminum foil with the colorless chemical conversion film formed on the surface is obtained.
Detection assay
1. Topography observation
The appearance of the 5056 aluminum foils treated in examples 1-5 is observed by using a scanning electron microscope, and the results are shown in fig. 1-10.
It can be seen from fig. 1 to 10 that the chemical conversion coatings formed on the surfaces of 5056 aluminum foils after the treatment in examples 1 to 5 are all dense and uniform, and due to the generation of hydrogen during the coating process, the chemical conversion coating on the surface of 5056 aluminum foil has a small amount of pores, but the whole is relatively flat, and no defects such as cracking and the like are found.
2. Salt spray test
The 5056 aluminum foil which was not subjected to the plating process and the 5056 aluminum foil after the process of example 1 were subjected to the salt spray test, and the results are shown in fig. 11.
As can be seen from fig. 11, the 5056 aluminum foil substrate without being coated showed obvious corrosion spots and corrosion products on the surface after 48 hours, while the 5056 aluminum foil substrate after being coated still showed no obvious corrosion signs on the surface after 860 hours. Thereby effectively proving that the corrosion resistance of the 5056 aluminum foil can be effectively improved by the coating film.
3. Contact Angle testing
The 5056 aluminum foils after treatment in examples 1-5 were subjected to multiple water contact angle tests, and the results are shown in fig. 12.
As is clear from the analysis in fig. 12, the average value of the water contact angle of the surface of 5056 aluminum foil after treatment in example 1 is about 107 °, the average value of the water contact angle of the surface of 5056 aluminum foil after treatment in example 2 is about 87 °, the average value of the water contact angle of the surface of 5056 aluminum foil after treatment in example 3 is about 106 °, the average value of the water contact angle of the surface of 5056 aluminum foil after treatment in example 4 is about 103 °, and the average value of the water contact angle of the surface of 5056 aluminum foil after treatment in example 5 is about 106 °, and all of them exhibit good hydrophobic properties.
4. Electrochemical impedance and electrochemical polarization testing
The 5056 aluminum foil, which was not subjected to the plating, and 5056 aluminum foil, which was treated in examples 1-5, were subjected to electrochemical impedance and electrochemical polarization tests, and the results are shown in fig. 13 and 14.
As can be seen from the analysis in FIG. 13, the electrochemical impedance modulus of the 5056 aluminum foil treated in example 1 in 3.5% NaCl solution reached 10 5 Ωcm 2 Compared with a 5056 aluminum foil substrate which is not subjected to film coating, the impedance modulus value is improved by 2-3 orders of magnitude; the electrochemical impedance modulus of 5056 aluminum foil treated in examples 2-5 reached 10 4 Ωcm 2 Compared with a 5056 aluminum foil substrate which is not coated, the impedance modulus value is improved by 1-2 orders of magnitude.
As can be seen from the analysis in FIG. 14, the self-etching current density of 5056 aluminum foil treated in example 1 is less than 10 in 3.5% NaCl solution -7 Acm -2 Compared with a 5056 aluminum foil substrate which is not subjected to film coating, the number of the aluminum foil substrate is increased by 1-2 orders of magnitude; the self-etching current density of the 5056 aluminum foil after being processed in example 2 is less than 10 -6 Acm -2 Is obviously higher than a 5056 aluminum foil substrate which is not coated with a film, and the self-corrosion potential of the aluminum foil substrate is-1.08V, which is 0.18V higher than that of the 5056 aluminum foil substrate which is not coated with the film; the self-etching current density of the 5056 aluminum foil after being processed in example 3 is less than 10 -6 Acm -2 Is obviously higher than a 5056 aluminum foil substrate which is not coated with a film, and the self-corrosion potential of the aluminum foil substrate is-0.94V, which is 0.19V higher than that of the 5056 aluminum foil substrate which is not coated with the film; the self-etching current density of 5056 aluminum foil treated in example 4 is less than 10 -6 Acm -2 The self-corrosion potential is-1.07V, which is 0.32V higher than that of 5056 aluminum foil base body which is not coated; in example 4The self-corrosion current density of the processed 5056 aluminum foil is less than 10 -6 Acm -2 Is obviously higher than that of a 5056 aluminum foil substrate which is not subjected to film coating, and the self-corrosion potential of the aluminum foil substrate is-1.09V, which is 0.17V higher than that of the 5056 aluminum foil substrate which is not subjected to film coating.
5. Potassium dichromate drop test
The spot test of potassium dichromate was carried out at 25 ℃ on 5056 aluminum foil which had not been plated, and 5056 aluminum foil treated in examples 1, 6, and 7, and the results are shown in fig. 15.
As can be seen from the analysis in fig. 15, the 5056 aluminum foil after the treatment in example 1 can withstand the 300s potassium dichromate titration test, the 5056 aluminum foil after the treatment in examples 6 and 7 can withstand the 120s potassium dichromate titration test, and the uncoated 5056 aluminum foil substrate can withstand the potassium dichromate dripping test for about 30s, thereby proving that the corrosion resistance of the aluminum foil is greatly improved after the plating.
According to the aluminum alloy surface treatment method, the aluminum alloy is placed in the hydrophobic chemical conversion film-forming liquid at a lower temperature of 20-60 ℃ within a shorter time of 60-600 s and under the atmospheric environment, so that a chemical conversion film with a water contact angle of more than 100 degrees and a thickness of 50-150 nm can be generated on the surface of the aluminum alloy through conversion. Experimental research proves that the aluminum alloy with the chemical conversion film formed on the surface can resist 860-hour neutral salt spray test, and the electrochemical impedance modulus value and the self-corrosion current are obviously improved by orders of magnitude compared with those of a matrix, so that the corrosion resistance of the aluminum alloy is effectively improved.
The above embodiments are merely preferred embodiments for fully illustrating the present invention, and the scope of the present invention is not limited thereto. The equivalent substitution or change made by the technical personnel in the technical field on the basis of the invention is all within the protection scope of the invention.
Claims (10)
1. The hydrophobic chemical conversion film-forming solution is characterized by comprising trivalent chromium salt, fluorozirconate, an additive and water;
the additive is fluotitanic acid and/or fluotitanate.
2. The hydrophobic chemical conversion deposition solution of claim 1, wherein the trivalent chromium salt comprises one or more of chromium sulfate, chromium nitrate, and chromium chloride.
3. The hydrophobic chemical conversion deposition solution of claim 1, wherein the fluorozirconate comprises one or both of potassium fluorozirconate and sodium fluorozirconate.
4. The hydrophobic chemical conversion deposition solution according to claim 1, wherein the fluorotitanate is potassium fluorotitanate.
5. The hydrophobic chemical conversion deposition solution according to claim 1, wherein the concentration of the trivalent chromium salt is 0.5 to 5g/L, the concentration of the fluorozirconate is 1 to 10g/L, and the concentration of the additive is 0.5 to 5g/L.
6. The aluminum alloy surface treatment method is characterized by comprising the following steps of:
s1, pretreatment: removing impurities from the surface of the aluminum alloy;
s2, coating: adjusting the pH of the hydrophobic chemical conversion deposition solution of any one of claims 1 to 5 to acidic, and then subjecting the aluminum alloy to a chemical conversion treatment in the acidic hydrophobic chemical conversion deposition solution to form a hydrophobic chemical conversion coating on the surface of the aluminum alloy;
s3, natural aging: and cleaning the coated aluminum alloy, and naturally aging the aluminum alloy at normal temperature.
7. The method for surface treatment of an aluminum alloy as recited in claim 6, wherein the chemical conversion treatment in S2 is performed at a temperature of 20 to 60 ℃ for a period of 60 to 600 seconds.
8. The aluminum alloy surface treatment method according to claim 6, wherein in S1, the pretreatment comprises sequentially subjecting the aluminum alloy to degreasing, alkali washing, acid washing and rinsing;
wherein, the degreasing is carried out by adopting a degreasing cleaning agent for cleaning, the cleaning temperature is 50-60 ℃, and the cleaning time is 30-120 seconds; the alkali washing is carried out by using 5-10% (wt.) sodium hydroxide solution, the alkali washing temperature is 30-40 ℃, and the alkali washing time is 10-60 seconds; the acid washing is carried out by using 30-40% (vol.) nitric acid solution, the acid washing temperature is 20-30 ℃, and the acid washing time is 10-60 seconds; the rinsing is carried out by using deionized water, the rinsing temperature is 70-80 ℃, and the rinsing time is 10-60 seconds.
9. The method for surface treatment of an aluminum alloy as recited in claim 6, wherein the natural aging time in S3 is 48 to 120 hours.
10. The surface treatment method of an aluminum alloy according to claim 6, wherein a chemical conversion coating formed on the surface of the aluminum alloy has a thickness of 50nm to 150nm and a water contact angle of the chemical conversion coating is greater than 100 °.
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