CN115216759A - Hydrophilic chemical conversion film forming liquid and aluminum alloy surface treatment method - Google Patents
Hydrophilic chemical conversion film forming liquid and aluminum alloy surface treatment method Download PDFInfo
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- CN115216759A CN115216759A CN202210804004.XA CN202210804004A CN115216759A CN 115216759 A CN115216759 A CN 115216759A CN 202210804004 A CN202210804004 A CN 202210804004A CN 115216759 A CN115216759 A CN 115216759A
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- 239000000126 substance Substances 0.000 title claims abstract description 95
- 238000006243 chemical reaction Methods 0.000 title claims abstract description 90
- 229910000838 Al alloy Inorganic materials 0.000 title claims abstract description 64
- 238000000034 method Methods 0.000 title claims abstract description 30
- 238000004381 surface treatment Methods 0.000 title claims abstract description 24
- 239000007788 liquid Substances 0.000 title claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 54
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- 239000003795 chemical substances by application Substances 0.000 claims abstract description 19
- 238000004140 cleaning Methods 0.000 claims abstract description 16
- 238000007739 conversion coating Methods 0.000 claims abstract description 15
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- 150000001844 chromium Chemical class 0.000 claims abstract description 9
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- 239000012535 impurity Substances 0.000 claims abstract description 3
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- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 3
- 238000005406 washing Methods 0.000 claims description 37
- 239000008367 deionised water Substances 0.000 claims description 36
- 229910021641 deionized water Inorganic materials 0.000 claims description 36
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 30
- 238000007789 sealing Methods 0.000 claims description 26
- 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
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical group [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 10
- 239000011248 coating agent Substances 0.000 claims description 10
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- 230000002378 acidificating effect Effects 0.000 claims description 9
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- 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
- 239000008139 complexing agent Substances 0.000 claims description 4
- 230000008021 deposition Effects 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
- 239000000565 sealant Substances 0.000 claims 2
- 238000005260 corrosion Methods 0.000 abstract description 20
- 230000007797 corrosion Effects 0.000 abstract description 16
- 238000001179 sorption measurement Methods 0.000 abstract description 7
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- 229910052782 aluminium Inorganic materials 0.000 description 112
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 112
- 239000011888 foil Substances 0.000 description 111
- 239000000243 solution Substances 0.000 description 34
- 238000012360 testing method Methods 0.000 description 17
- KMUONIBRACKNSN-UHFFFAOYSA-N potassium dichromate Chemical compound [K+].[K+].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O KMUONIBRACKNSN-UHFFFAOYSA-N 0.000 description 16
- 238000007605 air drying Methods 0.000 description 14
- 239000007864 aqueous solution Substances 0.000 description 14
- 239000007888 film coating Substances 0.000 description 9
- 238000009501 film coating Methods 0.000 description 9
- 239000011651 chromium Substances 0.000 description 8
- 238000005554 pickling Methods 0.000 description 8
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- 150000003839 salts Chemical class 0.000 description 5
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- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 4
- 238000004448 titration Methods 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
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- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
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- 229910052804 chromium Inorganic materials 0.000 description 1
- 229910001430 chromium ion Inorganic materials 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
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- 238000001514 detection method Methods 0.000 description 1
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Images
Classifications
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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
- C23C22/36—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 containing also phosphates
- C23C22/361—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 containing also phosphates containing titanium, zirconium or hafnium compounds
-
- 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
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
- C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions
- C23G1/12—Light metals
- C23G1/125—Light metals aluminium
-
- 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
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
- C23G1/14—Cleaning or pickling metallic material with solutions or molten salts with alkaline solutions
- C23G1/22—Light metals
Abstract
The invention relates to a hydrophilic chemical conversion film-forming solution and an aluminum alloy surface treatment method. Hydrophilic chemical conversion film-forming liquid, which comprises trivalent chromium salt, fluorozirconate, organic coordination agent, inorganic salt additive and water; the organic coordination agent is one or more of polyvinyl alcohol, polyethylene glycol and polyacrylamide; the inorganic salt additive is fluotitanic acid and/or fluotitanate. The invention also provides an aluminum alloy surface treatment method, which comprises the following steps: removing impurities from the surface of the aluminum alloy; placing the aluminum alloy in the hydrophilic chemical conversion film-forming solution to perform chemical conversion treatment so as to form a hydrophilic chemical conversion film on the surface of the aluminum alloy; and cleaning the coated aluminum alloy, and naturally aging the aluminum alloy at normal temperature. The invention effectively improves the adsorption capacity of the metal surface and also solves the problems of high toxicity, poor corrosion resistance, complex process and poor protection effect of the existing chemical conversion coating on the surface of the aluminum alloy.
Description
Technical Field
The invention relates to the technical field of aluminum alloy surface treatment, in particular to a hydrophilic 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 aluminum alloys. 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 used.
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
The invention aims to provide a hydrophilic chemical conversion film-forming solution to improve the adsorption capacity of a metal surface; the second purpose is to provide an aluminum alloy surface treatment method to improve the adsorption performance of the aluminum alloy surface and solve the problems of high toxicity, poor corrosion resistance, complex working procedures and poor protection effect of the existing aluminum alloy surface chemical conversion film.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a hydrophilic chemical conversion film-forming liquid comprises trivalent chromium salt, fluorozirconate, an organic coordination agent, an inorganic salt additive and water;
the organic complexing agent is one or more of polyvinyl alcohol, polyethylene glycol and polyacrylamide;
the inorganic salt 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, the concentration of the organic complexing agent is 2 to 10g/L, and the concentration of the inorganic salt additive is 0.5 to 5g/L.
The invention also provides an aluminum alloy surface treatment method, which comprises the following steps:
s1, pretreatment: removing impurities from the surface of the aluminum alloy;
s2, coating: adjusting the pH value of the hydrophilic chemical conversion film-forming solution to acidity, and putting the aluminum alloy into the acidic hydrophilic chemical conversion film-forming solution for chemical conversion treatment to form a hydrophilic 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.
Preferably, after natural aging, the method further comprises organic sealing treatment, specifically: and sealing the naturally aged aluminum alloy in an organic sealing agent.
According to the technical means, after film coating and natural aging, namely, priming treatment is carried out on the surface of the aluminum alloy, then sealing treatment is carried out, so that the corrosion resistance of the aluminum alloy is greatly improved, wherein the adsorption capacity of the aluminum alloy on the organic sealing agent is effectively improved by coating the film on the surface of the aluminum alloy through hydrophilic chemical conversion film forming liquid, and the corrosion resistance of the aluminum alloy is further improved.
Preferably, in S2, the temperature of the chemical conversion treatment is 20 to 60 ℃, the film forming rate can be controlled in the temperature range, so that the film can grow rapidly and uniformly, and the time of the chemical conversion treatment 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 4 to 24 hours.
Preferably, the organic blocking agent is a silane blocking agent.
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 less than 50 degrees.
The invention has the beneficial effects that:
1) The hydrophilic chemical conversion film-forming liquid takes chromium salt, fluorozirconate, an organic coordination agent and an inorganic salt additive as main components of the film-forming liquid, the chromium salt has the advantages of small 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 organic coordination agent can prevent the hydrolysis of trivalent chromium, can also stabilize and control the deposition speed of metal ions within a certain pH range and can improve the hydrophilicity of a film layer, the inorganic salt additive is a film-forming promoter and can passivate the structure and the porosity of the film layer, 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 hydrophilic performance, the adsorption performance of the metal surface is effectively improved, and good precondition is provided for adsorbing a sealing agent on the metal surface;
2) According to the aluminum alloy surface treatment method, the aluminum alloy is placed in the hydrophilic 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 Microscope (SEM) morphology (10 μm) of the 5056 aluminum foil after treatment in examples 1-4;
FIG. 2 is a Scanning Electron Microscope (SEM) morphology (1 μm) of the 5056 aluminum foil after being processed in examples 1-4;
FIG. 3 is a macro-topography of 5% neutral salt spray test of 5056 aluminum foil after treatment in examples 1 and 4;
fig. 4 is a graph showing the results of water contact angle tests performed on 5056 aluminum foils after treatment in example 1, example 2, example 4, and comparative example 1;
FIG. 5 is a graph showing the electrochemical polarization of 5056 aluminum foil treated in examples 1-3 in a 3.5% (wt%) aqueous NaCl solution;
FIG. 6 is a graph of the results of a potassium dichromate spot test conducted on an uncoated 5056 aluminum foil and 5056 aluminum foils after being processed as in examples 1, 5, and 6;
fig. 7 is a graph showing the results of a potassium dichromate spot test on 5056 aluminum foils after treatment in example 4 and comparative example 1.
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 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;
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 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 Adjusting the pH value of the hydrophilic chemical conversion film-forming solution to 3.5 by using the solution, placing the 5056 aluminum foil subjected to pretreatment in S1 into an acidic hydrophilic chemical conversion film-forming solution for chemical conversion treatment so as to form a hydrophilic 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 90S;
in example 1, the hydrophilic chemical conversion coating solution contained Cr 2 (SO 4 ) 3 、K 2 ZrF 6 Polyvinyl alcohol, 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, a concentration of 6g/L, H 2 TiF 6 The concentration of (A) is 2g/L;
s3, natural aging: and after the film coating is finished, washing the 5056 aluminum foil by using deionized water, and then naturally drying and aging for 8 hours in a normal-temperature environment to obtain the 5056 aluminum foil with the colorless chemical conversion film formed on the surface.
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 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;
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 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 Adjusting the pH value of the hydrophilic chemical conversion film-forming solution to 4.5 by using the solution, placing 5056 aluminum foil subjected to pretreatment in S1 in the acidic hydrophilic chemical conversion film-forming solution for chemical conversion treatment so as to form a hydrophilic 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 90S;
in example 2, the component of the hydrophilic chemical conversion coating solution was Cr (NO) 3 ) 3 、Na 2 ZrF 6 Polyvinyl alcohol, H 2 TiF 6 And water, cr (NO) 3 ) 3 Has a concentration of 2g/L, na 2 ZrF 6 Has a concentration of 4g/L, a concentration of 6g/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 8 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 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 Adjusting the pH value of the hydrophilic chemical conversion film-forming solution to 5.5 by using the solution, placing the 5056 aluminum foil pretreated in the S1 into the acidic hydrophilic chemical conversion film-forming solution for chemical conversion treatment so as to form a hydrophilic 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 90S;
in example 3, the hydrophilic chemical conversion coating solution contained CrCl 3 、Na 2 ZrF 6 Polyvinyl alcohol, H 2 TiF 6 And water, crCl 3 Has a concentration of 2g/L, na 2 ZrF 6 Has a concentration of 4g/L, a concentration of 6g/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 8 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 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;
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 Adjusting the pH value of the hydrophilic chemical conversion film-forming solution to 3.5 by using the solution, placing the 5056 aluminum foil pretreated in the S1 into the acidic hydrophilic chemical conversion film-forming solution for chemical conversion treatment so as to form a hydrophilic 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 90S;
in example 4, the hydrophilic chemical conversion coating solution contained Cr 2 (SO 4 ) 3 、K 2 ZrF 6 Polyvinyl alcohol, 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 2g/L, a concentration of 6g/L, H 2 TiF 6 The concentration of (A) is 2g/L;
s3, natural aging: after the film coating is finished, the 5056 aluminum foil is washed by deionized water, and then is placed in a normal-temperature environment for natural air drying and aging for 8 hours, so that the 5056 aluminum foil with a colorless chemical conversion film formed on the surface is obtained;
s4, placing the 5056 aluminum foil after natural air drying and aging in a silane sealing agent for sealing, taking out the aluminum foil, and drying in an oven to obtain the sealed 5056 aluminum foil.
Example 5
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 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;
7) 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;
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 hydrophilic chemical conversion film-forming solution to 3.5 by using the solution, placing the 5056 aluminum foil pretreated in the S1 into the acidic hydrophilic chemical conversion film-forming solution for chemical conversion treatment so as to form a hydrophilic 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 90S;
in example 4, the hydrophilic chemical conversion coating solution contained Cr 2 (SO 4 ) 3 、K 2 ZrF 6 Polyvinyl alcohol, 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, a concentration of 2g/L, H 2 TiF 6 The concentration of (A) is 0.5g/L;
s3, natural aging: after the film coating is finished, the 5056 aluminum foil is washed by deionized water, and then is placed in a normal-temperature environment for natural air drying and aging for 8 hours, so that the 5056 aluminum foil with a colorless chemical conversion film formed on the surface is obtained;
s4, placing the 5056 aluminum foil after natural air drying and aging in a silane sealing agent for sealing, taking out the aluminum foil, and drying in an oven to obtain the sealed 5056 aluminum foil.
Example 6
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 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;
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 for 30s in the aqueous solution, and then taking out and rinsing in deionized water at 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 hydrophilic chemical conversion film-forming solution to 3.5 by using the solution, placing the 5056 aluminum foil pretreated in the S1 into the acidic hydrophilic chemical conversion film-forming solution for chemical conversion treatment so as to form a hydrophilic 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 90S;
in example 4, the hydrophilic chemical conversion coating solution contained Cr 2 (SO 4 ) 3 、K 2 ZrF 6 Polyvinyl alcohol, 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: after the film coating is finished, the 5056 aluminum foil is washed by deionized water, and then is placed in a normal-temperature environment for natural air drying and aging for 8 hours, so that the 5056 aluminum foil with a colorless chemical conversion film formed on the surface is obtained;
s4, placing the 5056 aluminum foil subjected to natural air drying and aging into a silane sealing agent for sealing, taking out the aluminum foil and drying the aluminum foil in an oven to obtain the sealed 5056 aluminum foil.
Comparative 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 pickling 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, directly placing the 5056 aluminum foil after rinsing and air drying in a silane sealing agent for sealing, taking out the aluminum foil, and drying in an oven to obtain the sealed 5056 aluminum foil.
Detection assay
1. Topography observation
The appearance of the 5056 aluminum foil after treatment in examples 1-4 was observed by scanning electron microscopy, and the results are shown in fig. 1 and 2.
As can be seen from FIGS. 1 and 2, the chemical conversion coatings formed on the surfaces of the 5056 aluminum foils treated in examples 1-4 are dense and uniform, and a small amount of pores are formed on the surface of the 5056 aluminum foil pattern due to the generation of hydrogen during the coating process, but the whole is relatively flat, and no crack or other defects are found.
2. Salt spray test
The 5056 aluminum foil which was not subjected to the plating process, 5056 aluminum foil after the processes of examples 1 and 4 were subjected to the salt spray test, and the results are shown in fig. 3.
As can be seen from fig. 3, after 48 hours, obvious corrosion spots and corrosion products appear on the surface of the 5056 aluminum foil substrate which is not subjected to film plating, while the surface of the 5056 aluminum foil surface film layer which is subjected to film plating still does not show obvious corrosion signs after 480 hours, and further 5056 aluminum foil surface which is subjected to sealing treatment by the silane sealing agent does not show any obvious corrosion signs after 1200 hours, so that the 5056 aluminum foil which is subjected to film plating and sealing treatment by the silane sealing agent has very excellent corrosion resistance.
3. Contact Angle testing
5056 aluminum foils after treatment in example 1, example 2, example 4 and comparative example 1 were subjected to multiple water contact angle tests, and the results are shown in fig. 4.
As is clear from the analysis in fig. 4, the average value of the water contact angles of the surfaces of 5056 aluminum foil treated in example 1 is about 45 °, the average value of the water contact angles of the surfaces of 5056 aluminum foil treated in example 2 is about 33 °, and the average value of the water contact angles of the surfaces of 5056 aluminum foil treated in example 4 is about 65 °, and the average value of the water contact angles of the surfaces of 5056 aluminum foil treated in comparative example 1 is about 69 °.
4. Electrochemical polarization test
The electrochemical polarization test was performed on 5056 aluminum foil that had not been subjected to plating, and 5056 aluminum foil treated in examples 1-3, and the results are shown in fig. 5.
As analyzed in FIG. 5, in 3.5% NaCl solution, the self-corrosion potential of 5056 aluminum foil treated in example 1 is-0.84V, which is 0.42V higher than that of 5056 aluminum foil substrate without plating; the self-etching current density of 5056 aluminum foil treated in example 2 was less than 10 -6 Acm -2 The self-corrosion potential is obviously higher than that of a 5056 aluminum foil substrate which is not subjected to film coating, and is-0.86V, which is improved by 0.4V compared with that of the 5056 aluminum foil substrate which is not subjected to film coating; the self-etching current density of 5056 aluminum foil after treatment in example 3 was less than 10 -6 Acm -2 Is obviously higher than that of a 5056 aluminum foil substrate which is not coated with a film, and the self-corrosion potential of the 5056 aluminum foil substrate is-0.90V, which is improved by 0.36V compared with that of the 5056 aluminum foil substrate which is not coated with the film.
5. Potassium dichromate drop test
A potassium dichromate spot test was performed on 5056 aluminum foil, which was not plated, and 5056 aluminum foils, which were treated in examples 1, 4-6, and comparative example 1, at 25 ℃, and the results are shown in fig. 6 and 7.
As can be seen from the analysis in FIGS. 6 and 7, the 5056 aluminum foil after treatment in examples 1 and 5 can withstand the 3min potassium dichromate titration test, the 5056 aluminum foil after treatment in example 6 can withstand the 60s potassium dichromate titration test, the potassium dichromate titration resistance after silane sealing treatment in example 4 is prolonged to 13 min, and the 5056 aluminum foil without being coated can only withstand the 30s potassium dichromate titration test, so that the corrosion resistance of the 5056 aluminum foil after coating and silane sealing agent sealing treatment is obviously improved.
According to the aluminum alloy surface treatment method, the aluminum alloy is placed in the hydrophilic chemical conversion film-forming liquid at the lower temperature of 20-60 ℃ within a short time of 60-600 s and under the atmospheric environment condition, so that a layer of chemical conversion film with the water contact angle of less than 50 degrees and the thickness of 50-150 nm can be generated on the surface of the aluminum alloy through conversion, good adsorption performance is shown, and good precondition is provided for the adsorption of a subsequent organic sealing agent. Experimental research proves that the aluminum alloy with the chemical conversion film formed on the surface can resist 480 hours of neutral salt spray test, further, after organic sealing treatment is carried out on the aluminum alloy with the chemical conversion film formed on the surface, the neutral salt spray test is prolonged to 1200 hours, excellent corrosion resistance is shown, and the self-corrosion current is obviously improved by orders of magnitude compared with that 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. A hydrophilic chemical conversion film-forming liquid is characterized by comprising trivalent chromium salt, fluorozirconate, an organic coordination agent, an inorganic salt additive and water;
the organic complexing agent is one or more of polyvinyl alcohol, polyethylene glycol and polyacrylamide;
the inorganic salt additive is fluotitanic acid and/or fluotitanate.
2. The hydrophilic 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 hydrophilic chemical conversion coating solution of claim 1 wherein the fluorozirconate comprises one or both of potassium fluorozirconate and sodium fluorozirconate.
4. The hydrophilic chemical conversion deposition solution according to claim 1, wherein the fluorotitanate is potassium fluorotitanate.
5. The hydrophilic 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, the concentration of the organic complexing agent is 2 to 10g/L, and the concentration of the inorganic salt additive is 0.5 to 5g/L.
6. The aluminum alloy surface treatment method is characterized by comprising the following steps of:
s1, pretreatment: carrying out impurity removal treatment on the surface of the aluminum alloy;
s2, coating: adjusting the pH of the hydrophilic chemical conversion coating solution according to any one of claims 1 to 5 to acidic, and then subjecting the aluminum alloy to a chemical conversion treatment in the acidic hydrophilic chemical conversion coating solution to form a hydrophilic 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 aluminum alloy surface treatment method according to claim 6, further comprising an organic sealing treatment after the natural aging, specifically: and sealing the naturally aged aluminum alloy in an organic sealing agent.
8. The method for surface treatment of an aluminum alloy according to claim 6, wherein the temperature of the chemical conversion treatment in S2 is 20 to 60 ℃ and the time of the chemical conversion treatment is 60 to 600 seconds.
9. The aluminum alloy surface treatment method according to claim 7, wherein in S1, the pretreatment comprises sequentially degreasing, alkali washing, acid washing and rinsing 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; 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; rinsing with deionized water at 70-80 deg.c for 10-60 sec;
in the S3, the natural aging time is 48 to 120 hours;
the organic sealant is a silane sealant.
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 less than 50 °.
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