CN115404473B - Passivation solution for aluminum surface treatment, aluminum surface passivation method and anti-corrosion aluminum with nano conversion film - Google Patents
Passivation solution for aluminum surface treatment, aluminum surface passivation method and anti-corrosion aluminum with nano conversion film Download PDFInfo
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- CN115404473B CN115404473B CN202211049391.7A CN202211049391A CN115404473B CN 115404473 B CN115404473 B CN 115404473B CN 202211049391 A CN202211049391 A CN 202211049391A CN 115404473 B CN115404473 B CN 115404473B
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- 238000002161 passivation Methods 0.000 title claims abstract description 224
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 147
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 145
- 238000005260 corrosion Methods 0.000 title claims abstract description 79
- 238000006243 chemical reaction Methods 0.000 title claims abstract description 48
- 238000000034 method Methods 0.000 title claims abstract description 36
- 238000004381 surface treatment Methods 0.000 title claims abstract description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 78
- 239000000463 material Substances 0.000 claims abstract description 73
- 230000007797 corrosion Effects 0.000 claims abstract description 59
- 238000001035 drying Methods 0.000 claims abstract description 29
- 238000004506 ultrasonic cleaning Methods 0.000 claims abstract description 24
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 claims abstract description 18
- 238000004140 cleaning Methods 0.000 claims description 49
- 238000001914 filtration Methods 0.000 claims description 19
- 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 16
- 239000007788 liquid Substances 0.000 claims description 16
- 229910000838 Al alloy Inorganic materials 0.000 claims description 13
- 238000004321 preservation Methods 0.000 claims description 13
- 230000007935 neutral effect Effects 0.000 claims description 12
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 11
- 229910017604 nitric acid Inorganic materials 0.000 claims description 11
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
- 238000007664 blowing Methods 0.000 claims description 8
- 238000007654 immersion Methods 0.000 claims description 8
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 6
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 6
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 claims description 6
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims description 6
- 238000009210 therapy by ultrasound Methods 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 4
- 238000007602 hot air drying Methods 0.000 claims description 4
- SFBLKWGYRDDITM-UHFFFAOYSA-J [Ti+4].[O-]S([O-])=O.[O-]S([O-])=O Chemical compound [Ti+4].[O-]S([O-])=O.[O-]S([O-])=O SFBLKWGYRDDITM-UHFFFAOYSA-J 0.000 claims description 3
- DCKVFVYPWDKYDN-UHFFFAOYSA-L oxygen(2-);titanium(4+);sulfate Chemical compound [O-2].[Ti+4].[O-]S([O-])(=O)=O DCKVFVYPWDKYDN-UHFFFAOYSA-L 0.000 claims description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 3
- 239000011775 sodium fluoride Substances 0.000 claims description 3
- 235000013024 sodium fluoride Nutrition 0.000 claims description 3
- 235000010265 sodium sulphite Nutrition 0.000 claims description 3
- 229910000348 titanium sulfate Inorganic materials 0.000 claims description 3
- ZECMZFQURSQDRQ-UHFFFAOYSA-M [Cr](=O)(=O)([O-])F.[K+] Chemical compound [Cr](=O)(=O)([O-])F.[K+] ZECMZFQURSQDRQ-UHFFFAOYSA-M 0.000 claims description 2
- 239000008096 xylene Substances 0.000 claims description 2
- 150000003839 salts Chemical class 0.000 abstract description 30
- 230000000694 effects Effects 0.000 abstract description 19
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 abstract description 4
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 abstract description 4
- 229910052719 titanium Inorganic materials 0.000 abstract description 4
- 239000010936 titanium Substances 0.000 abstract description 4
- 229910052726 zirconium Inorganic materials 0.000 abstract description 4
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052731 fluorine Inorganic materials 0.000 abstract description 3
- 239000011737 fluorine Substances 0.000 abstract description 3
- 159000000000 sodium salts Chemical class 0.000 abstract description 3
- 230000002035 prolonged effect Effects 0.000 abstract description 2
- 238000007605 air drying Methods 0.000 abstract 1
- 239000010410 layer Substances 0.000 description 20
- 239000007921 spray Substances 0.000 description 18
- 239000011159 matrix material Substances 0.000 description 12
- 238000012360 testing method Methods 0.000 description 10
- 239000004020 conductor Substances 0.000 description 9
- 239000012459 cleaning agent Substances 0.000 description 6
- 230000007423 decrease Effects 0.000 description 5
- 229910000831 Steel Inorganic materials 0.000 description 4
- 230000006378 damage Effects 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 230000010355 oscillation Effects 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- 239000010959 steel Substances 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- 238000007739 conversion coating Methods 0.000 description 3
- 238000009792 diffusion process Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000004519 grease Substances 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 230000001681 protective effect Effects 0.000 description 3
- 230000002829 reductive effect Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical class [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 230000000903 blocking effect Effects 0.000 description 2
- 238000006056 electrooxidation reaction Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 239000011591 potassium Substances 0.000 description 2
- NROKBHXJSPEDAR-UHFFFAOYSA-M potassium fluoride Chemical compound [F-].[K+] NROKBHXJSPEDAR-UHFFFAOYSA-M 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000013589 supplement Substances 0.000 description 2
- WDJHALXBUFZDSR-UHFFFAOYSA-N Acetoacetic acid Natural products CC(=O)CC(O)=O WDJHALXBUFZDSR-UHFFFAOYSA-N 0.000 description 1
- 229910001335 Galvanized steel Inorganic materials 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000000861 blow drying Methods 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000006114 decarboxylation reaction Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005238 degreasing Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 239000003599 detergent Substances 0.000 description 1
- WOWBFOBYOAGEEA-UHFFFAOYSA-N diafenthiuron Chemical compound CC(C)C1=C(NC(=S)NC(C)(C)C)C(C(C)C)=CC(OC=2C=CC=CC=2)=C1 WOWBFOBYOAGEEA-UHFFFAOYSA-N 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 239000008397 galvanized steel Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 230000000670 limiting effect Effects 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000011698 potassium fluoride Substances 0.000 description 1
- 235000003270 potassium fluoride Nutrition 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 238000010301 surface-oxidation reaction Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- FOZHTJJTSSSURD-UHFFFAOYSA-J titanium(4+);dicarbonate Chemical compound [Ti+4].[O-]C([O-])=O.[O-]C([O-])=O FOZHTJJTSSSURD-UHFFFAOYSA-J 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- DUNKXUFBGCUVQW-UHFFFAOYSA-J zirconium tetrachloride Chemical compound Cl[Zr](Cl)(Cl)Cl DUNKXUFBGCUVQW-UHFFFAOYSA-J 0.000 description 1
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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/04—Cleaning involving contact with liquid
- B08B3/10—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration
- B08B3/12—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration by sonic or ultrasonic vibrations
-
- 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
- C23C22/37—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 hexavalent chromium 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
- C23C22/73—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 characterised by the process
-
- 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
- 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
- C23C22/86—Regeneration of coating baths
-
- 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
- C23G5/00—Cleaning or de-greasing metallic material by other methods; Apparatus for cleaning or de-greasing metallic material with organic solvents
- C23G5/02—Cleaning or de-greasing metallic material by other methods; Apparatus for cleaning or de-greasing metallic material with organic solvents using organic solvents
- C23G5/032—Cleaning or de-greasing metallic material by other methods; Apparatus for cleaning or de-greasing metallic material with organic solvents using organic solvents containing oxygen-containing compounds
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
- H01B13/22—Sheathing; Armouring; Screening; Applying other protective layers
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Chemical Treatment Of Metals (AREA)
Abstract
The invention provides a passivation solution for aluminum surface treatment, an aluminum surface passivation method and an anti-corrosion aluminum with a nano conversion film. The passivation solution for aluminum surface treatment comprises the following components: zirconium-containing salts, titanium-containing salts, potassium iodide, fluorine-containing salts, sodium salts and water. The aluminum surface passivation method comprises the following steps: ultrasonic cleaning, air drying, ultrasonic passivation and drying. The anti-corrosion aluminum material with the nano conversion film is prepared by performing surface passivation treatment on the aluminum material by the aluminum material surface passivation method. The passivation solution for aluminum surface treatment and the aluminum surface passivation method provided by the invention can be widely applied to various aluminum materials, so that a compact, continuous and flat passivation film is generated on the surface of the aluminum material, the effect of isolating an atmospheric corrosion medium is achieved, the service life of the aluminum material is prolonged, and the aluminum material can be widely applied to corrosion environments.
Description
Technical Field
The invention relates to a passivation solution for aluminum surface treatment, an aluminum surface passivation method and an anti-corrosion aluminum material with a nano conversion film, and belongs to the technical field of metal surface treatment.
Background
Overhead transmission lines in coastal and island areas are very easy to corrode and damage under the conditions of corrosive salt fog gas and high-temperature damp heat for a long time. Corrosion of overhead conductors is mainly three: chemical corrosion, electrochemical corrosion and crevice corrosion, in most cases three types of corrosion exist simultaneously. The anti-corrosion measures adopted by the overhead conductor mainly comprise the following steps: firstly, the surface of the steel core is galvanized, and the galvanized layer can protect the steel core from corrosion; secondly, aluminum ingots with excellent chemical components are optimized, impurities in aluminum are reduced, silicon content in the aluminum is reduced, and corrosion resistance of the conductor material is improved through rare earth optimization treatment; thirdly, when the lead is twisted, the anti-corrosion grease is coated between the aluminum strands.
However, the above-described corrosion protection technique has various problems and drawbacks. First, when a galvanized steel wire is used as a wire reinforcing core, zinc and aluminum can generate electrochemical corrosion in the wire due to potential difference, damage a galvanized layer and further corrode a steel core. Second, while the corrosion resistance of the wire material matrix can be improved by changing the chemical composition, there is a concomitant decrease in other properties of the aluminum wire, such as strength, conductivity, and elongation. Thirdly, the inside of the lead is coated with the anti-corrosion grease, which can protect the inner steel core in a short time, but the anti-corrosion grease can lose efficacy and deteriorate along with the time, so that the anti-corrosion capability is lost.
Disclosure of Invention
In order to solve the technical problems, the invention aims to provide a passivation solution for aluminum surface treatment, an aluminum surface passivation method and an anti-corrosion aluminum material with a nano conversion film. The passivation solution and the passivation method are adopted to treat the aluminum material, so that a nano conversion film can be formed on the surface of the aluminum material, and the corrosion resistance of the aluminum material is improved.
In order to achieve the above object, the present invention firstly provides a passivation solution for aluminum surface treatment, which comprises the following components: zirconium-containing salt 0.1-0.6g/L, titanium-containing salt 0.2-0.3g/L, potassium iodide 0.05-0.1g/L, fluorine-containing salt 0.05-0.1g/L, sodium salt 0.06-0.08g/L and water.
According to a specific embodiment of the present invention, preferably, the composition of the passivation solution for aluminum surface treatment further includes nitric acid, and the pH value of the passivation solution for aluminum surface treatment is 2.2 to 4.5, more preferably 3.0 to 3.7.
In the passivation solution, the titanium-containing salt preferably includes one or a combination of several of titanium sulfate, titanium sulfite, titanium carbonate, and the like.
In the passivation solution described above, preferably, the zirconium-containing salt includes zirconium chloride and/or potassium fluorozirconate and the like.
In the passivation solution described above, the fluorine-containing salt preferably includes one or a combination of several of potassium fluochromate, sodium fluoride, potassium fluoride, and the like.
In the passivation solution described above, preferably, the sodium salt includes sodium sulfite and/or sodium carbonate, and the like.
The preparation method of the passivation solution can uniformly mix the components in water, or nitric acid is added when the passivation solution is used without mixing nitric acid with other components, so as to reach the pH value of the passivation solution defined by the invention. The water used may be deionized water or distilled water.
In addition, the invention also provides a surface passivation method of the aluminum material, which at least comprises the following steps: and carrying out surface passivation treatment on the aluminum material by adopting the passivation solution for aluminum material surface treatment.
According to a specific embodiment of the present invention, preferably, the aluminum material surface passivation method includes the steps of: sequentially performing ultrasonic cleaning, first drying, ultrasonic passivation and second drying on the aluminum material to obtain the aluminum material subjected to surface passivation treatment; wherein, the ultrasonic passivation adopts the passivation solution for aluminum surface treatment.
In the above aluminum surface passivation method, preferably, the cleaning solution used in the ultrasonic cleaning comprises a neutral cleaning solution, the ultrasonic frequency of the ultrasonic cleaning is 20000-30000 Hz, the power is 4-6 kw, and the ultrasonic cleaning time is 2-5min.
In the above aluminum material surface passivation method, preferably, the neutral cleaning agent comprises the following components in terms of 100% of total volume: 40% -60% of dimethylbenzene and 40% -60% of acetone. The neutral detergent provided by the invention belongs to water-based organic matters, and consists of acetone generated by decarboxylation of acetoacetic acid, dimethylbenzene and other components.
The traditional cleaning of the surface of the aluminum substrate adopts acid or alkali, which has certain corrosiveness and damages the aluminum oxide film on the surface of the aluminum substrate to form corrosion pits. Meanwhile, the acid-washing or alkali-treatment solution cannot be treated in the later period, and certain harm is caused to the environment. Because the aluminum wires are stranded, the greasy dirt of the inner layer is difficult to clean, so that the passivation effect of the inner layer is also greatly reduced. In this regard, the invention provides an ultrasonic cleaning mode, wherein an ultrasonic oscillation device is added into a cleaning tank, and a neutral cleaning liquid is adopted to carry out ultrasonic cleaning on an aluminum wire. The greasy dirt of the inner layer can be cleaned due to the impact of the cleaning agent oscillation particles, so that the production effect of the passivation film in the later stage is greatly enhanced.
In the above aluminum surface passivation method, preferably, the temperature of the first drying is 40-60 ℃ for 2-5min. The first drying may be hot air blow drying. More preferably, the hot air blowing and drying device comprises 4-8 air pipes uniformly distributed on the circumference, air holes are uniformly distributed in the length direction of the air pipes, the air holes of the air pipes are obliquely formed along the opposite direction of the running of the aluminum material, and compressed air is introduced to blow the surface of the aluminum material to dry. More specifically, the hot air blowing and drying device further comprises a heating device to increase the drying speed.
In the above aluminum surface passivation method, preferably, the ultrasonic passivation temperature is 25-35 ℃, the time is 2-6min, the ultrasonic frequency is 20000-30000Hz, and the power is 4-6kw.
In the above aluminum surface passivation method, preferably, the ultrasonic passivation is performed by an ultrasonic passivation device, and the ultrasonic passivation device comprises a passivation tank, an ultrasonic oscillating plate, a heat preservation device, a circulation device and a filtering device;
Wherein the ultrasonic oscillating plate is arranged in the passivation groove;
The heat preservation device is arranged outside the passivation groove;
the circulating device comprises a circulating pump, a water collecting tank and an immersed pH value detector; the circulating pump is connected with the water collecting tank, and the immersed pH value detector is arranged in the water collecting tank;
the passivation groove is provided with a plurality of water inlets and a plurality of water outlets;
The water outlet of the passivation tank is connected with the filtering device through a pipeline and then connected with the water collecting tank through a pipeline, and the water inlet of the passivation tank is connected with the water collecting tank through a pipeline and the circulating pump.
In the above aluminum material surface passivation method, preferably, the ultrasonic passivation specifically includes: carrying out ultrasonic treatment on the aluminum material in the passivation tank and the passivation solution for aluminum material surface treatment through the ultrasonic oscillating plate, wherein the ultrasonic frequency is 20000-30000Hz, and the power is 4-6kw; simultaneously, the temperature of passivation is 25-35 ℃ through the heat preservation device; after passivation treatment for 2-6min, enabling passivation solution in the passivation tank to enter the filtering device through the water outlet for filtering, and then enter the water collecting tank; the immersion type pH value detector inside the water collecting tank detects the pH value of the passivation solution, and when the pH value is not 2.2-4.5 (more preferably, when the pH value is not 3.0-3.7), the passivation solution for aluminum surface treatment and/or nitric acid are supplemented from the outside so that the pH value of the passivation solution in the water collecting tank is 2.2-4.5 (more preferably, 3.0-3.7); and the passivation solution in the water collecting tank enters a water inlet of the passivation tank through the circulating pump.
According to the device and the step of ultrasonic passivation, the ultrasonic oscillating plate is added in the passivation groove, so that the oscillating frequency of the passivation solution is enhanced, and the passivation efficiency is enhanced. And moreover, the circulating device is arranged, so that the recycling of the passivation solution is effectively realized. Meanwhile, the optimal passivation temperature is set to be 25-35 ℃, a heating and heat preserving device is wrapped outside the passivation tank, and the passivation treatment time is 2-6 minutes, so that the excellent passivation effect is achieved. The processing time is controlled by adjusting the running speed of the aluminum wire. And the pH value of the passivation solution is controlled to be 2.2-4.5, and an immersion type pH value detector is adopted to automatically detect the pH value and automatically supplement the passivation solution and/or supplement nitric acid.
In the above aluminum material surface passivation method, preferably, the ultrasonic cleaning may be performed by using the above ultrasonic passivation device, and the passivation solution is replaced by a cleaning solution, and the treatment time of the above ultrasonic cleaning is used. More preferably, the ultrasonic cleaning specifically includes: carrying out ultrasonic treatment on aluminum materials and cleaning liquid in a cleaning tank (the cleaning tank is the passivation tank and is called as different), wherein the ultrasonic frequency is 20000-30000Hz, and the power is 4-6kw; meanwhile, the heat preservation device can be not started and can maintain normal temperature; after 2-5min of cleaning treatment, enabling the cleaning liquid in the cleaning tank to enter the filtering device through the water outlet for filtering, and then enter the water collecting tank; the immersed pH value detector inside the water collecting tank can be not started; the cleaning liquid in the water collecting tank enters the water inlet of the cleaning tank through the circulating pump.
In the above aluminum surface passivation method, preferably, the second drying temperature is 40-60 ℃ for 2-5min. The second drying can be hot air drying, and the passivated aluminum conductor is subjected to hot air drying at 40-60 ℃ and the generation of a passivation film is enhanced.
The aluminum surface passivation method of the invention uses the specially developed passivation solution to passivate the aluminum material, and forms a passivation film with nano conversion on the surface of the aluminum material. The aluminum surface passivation method has the characteristics of low cost, compact and stable passivation film layer, advanced technology and the like. The zirconium and titanium in the passivation solution provided by the invention have extremely strong affinity with oxygen, can immediately form an oxide film in the atmosphere or in a humid environment, and can repair a damaged film layer by itself only by a trace amount of oxygen or water when corrosion occurs, so that the passivation solution has self-healing property. Meanwhile, the nano conversion film has strong binding force with the aluminum matrix, and can effectively isolate corrosive media. Therefore, the formed conversion film has good corrosion resistance effect and is suitable for wires used in heavy corrosion areas. In addition, by changing the immersion time and the immersion temperature of the aluminum material in the passivation solution, the passivation film thickness generated on the surface of the aluminum matrix is changed, and different conversion film thicknesses can be suitable for areas with different corrosion grades.
In addition, the invention also provides an anti-corrosion aluminum material with the nano conversion film, which is prepared by carrying out surface passivation treatment on the aluminum material by the aluminum material surface passivation method.
In the above-described corrosion-resistant aluminum material having a nano-conversion film, preferably, the nano-conversion film is formed on the surface of the aluminum material, and the thickness of the nano-conversion film is 100nm to 800nm.
In the above-described corrosion-resistant aluminum material having a nano-conversion film, preferably, the aluminum material includes an aluminum wire, an aluminum alloy wire, or the like. The specific element composition and preparation method of the aluminum wire and the aluminum alloy wire can be conventional in the art, and are not described herein.
The nano conversion film provided by the invention can protect the aluminum material and avoid the oxidation of the surface of the lead. After the passivation treatment of the invention, the surface of the aluminum conductor is formed with a relatively flat and continuous protective film with a film thickness smaller than 1 μm, and the influence of the film thickness on the wire diameter of the aluminum conductor is negligible. The passivation film plays a good role in blocking the surface of the aluminum conductor, and obviously blocks the corrosion of corrosive media in the atmosphere and industrial environment, so that the corrosion reaction of the aluminum metal matrix is effectively inhibited, and the corrosion resistance of the aluminum conductor is enhanced.
The passivation solution for aluminum surface treatment and the aluminum surface passivation method provided by the invention can be widely applied to various aluminum materials, so that a compact, continuous and flat passivation film (namely a nano conversion film) is generated on the surface of the aluminum material, the effect of isolating an atmospheric corrosion medium is achieved, the service life of the aluminum material is prolonged, and the passivation solution can be widely applied to corrosion environments. The invention also provides an anti-corrosion aluminum material with the nano conversion film, in particular to an anti-corrosion aluminum or aluminum alloy wire with the nano conversion film. After the passivation treatment of the invention, the multi-metal salt inorganic composite passivation film with the thickness of hundreds of nanometers can be formed on the surface of the overhead conductor, thereby greatly improving the corrosion resistance of aluminum and aluminum alloy in humid, salt fog and other environments. The formed passivation film also has the performances of electric conduction, magnetic conduction and heat conduction, has little influence on the electric conduction performance of aluminum and aluminum alloy, and has the effect of repairing the surface defects of the lead. By adopting the surface passivation treatment technology provided by the invention, the corrosion protection technology of the wire breaks through the 'bimetallic corrosion' of the wire, and the novel corrosion-resistant protective film formed on the surface layer of the wire can prolong the service life of the wire and reduce the operation and maintenance cost of a power transmission line.
Drawings
FIG. 1 is a schematic view of an ultrasonic passivation device in accordance with an embodiment of the present invention;
Wherein, 1-passivation groove, 2-ultrasonic oscillation board, 3-heat preservation device, 4-circulating device, 41-circulating pump, 42-water catch bowl, 43-immersion pH value detector, 5-filter equipment.
Fig. 2 is a surface scanning electron micrograph of the anti-corrosion type aluminum wire with nano conversion film provided in example 4.
Fig. 3 is a surface scanning electron micrograph of the anti-corrosion type aluminum wire with nano conversion film provided in example 5.
Fig. 4 is a photograph of aluminum wire after salt spray corrosion.
Detailed Description
The technical solution of the present invention will be described in detail below for a clearer understanding of technical features, objects and advantageous effects of the present invention, but should not be construed as limiting the scope of the present invention.
Example 1
The embodiment provides a passivation solution for aluminum surface treatment, which comprises the following components: titanium sulfate 0.3g/L, potassium fluorozirconate 0.2g/L, potassium iodide 0.1g/L, potassium fluorochromate 0.08g/L, sodium sulfite 0.08g/L, and nitric acid and water. The pH of the passivation solution was 3.7.
Example 2
The embodiment provides a passivation solution for aluminum surface treatment, which comprises the following components: titanium sulfite 0.2g/L, potassium fluorozirconate 0.2g/L, potassium iodide 0.05g/L, sodium fluoride 0.05g/L, sodium carbonate 0.08g/L, and nitric acid and water. The pH of the passivation solution was 3.7.
Example 3
The embodiment provides an ultrasonic passivation device, as shown in fig. 1, which comprises a passivation groove 1, an ultrasonic oscillating plate 2, a heat preservation device 3, a circulating device 4 and a filtering device 5;
Wherein the ultrasonic oscillation plate 2 is arranged inside the passivation tank 1;
The heat preservation device 3 is arranged outside the passivation tank 1;
The circulating device 4 comprises a circulating pump 41, a water collecting tank 42 and an immersed pH value detector 43; the circulating pump 41 is connected to the water collection tank 42, and the immersion pH detector 43 is provided inside the water collection tank 42;
The passivation tank 1 is provided with a plurality of water inlets and a plurality of water outlets, and the specific number of the water inlets and the specific number of the water outlets can be regulated conventionally by a person skilled in the art;
the water outlet of the passivation tank 1 is connected with the filtering device 5 through a pipeline and then is connected with the water collecting tank 42 through a pipeline, and the water inlet of the passivation tank 1 is connected with the water collecting tank 42 through a pipeline and the circulating pump 41.
Example 4
The embodiment provides an aluminum surface passivation method, which comprises the following steps: and sequentially carrying out ultrasonic cleaning, first drying, ultrasonic passivation and second drying on the aluminum material to obtain the aluminum material after the surface passivation treatment.
The ultrasonic cleaning device comprises a cleaning device, a cleaning device and a cleaning device, wherein the cleaning liquid used for ultrasonic cleaning is neutral cleaning liquid, the ultrasonic frequency of the ultrasonic cleaning is 20000Hz, the power of the ultrasonic cleaning is 4kw, and the ultrasonic cleaning time is 3min; the neutral cleaning liquid comprises the following components: 50% by volume of xylene and 50% by volume of acetone.
The ultrasonic cleaning is performed by adopting an ultrasonic passivation device shown in fig. 1, except that the passivation tank is changed into a cleaning tank, and the devices used are the same and are called different. Carrying out ultrasonic treatment on the aluminum material and the cleaning liquid in the cleaning tank through the ultrasonic oscillating plate, wherein the ultrasonic frequency is 20000Hz, and the power is 4kw; meanwhile, the heat preservation device can be not started and can maintain normal temperature; after the cleaning treatment is carried out for 3 minutes, enabling the cleaning liquid in the cleaning tank to enter the filtering device through the water outlet for filtering, and then enter the water collecting tank; the immersed pH value detector inside the water collecting tank can be not started; the cleaning liquid in the water collecting tank enters the water inlet of the cleaning tank through the circulating pump.
The ultrasonic passivation device has good ultrasonic cleaning effect, and the cleaning liquid flows out from the water outlet, passes through the filtering device, the water collecting tank and the circulating pump and then enters from the water inlet again, so that the circulating cleaning is realized.
The first drying is hot air blowing drying, the temperature of the first drying is 40-60 ℃, and the time is 3min. And the hot air blowing and drying device is provided with 4-8 air pipes uniformly distributed on the circumference, air holes are uniformly distributed in the length direction of the air pipes, the air holes of the air pipes are obliquely formed along the opposite direction of the running of the aluminum material, and compressed air is introduced to blow-dry the surface of the aluminum material. More specifically, the hot air blowing and drying device further comprises a heating device to increase the drying speed.
The ultrasonic passivation specifically comprises the following steps: adopting an ultrasonic passivation device shown in fig. 1, and carrying out ultrasonic treatment on the aluminum material in the passivation tank and the passivation solution provided in the embodiment 1 through the ultrasonic oscillating plate, wherein the ultrasonic frequency is 20000Hz, and the power is 4kw; simultaneously, the temperature of passivation is 25 ℃ through the heat preservation device; after passivation treatment for 5min, enabling passivation solution in the passivation tank to enter the filtering device through the water outlet for filtering, and then enter the water collecting tank; the immersion type pH value detector inside the water collecting tank detects the pH value of the passivation solution, and when the pH value is not 3.0-3.7, the passivation solution for aluminum surface treatment or nitric acid is supplemented from the outside, so that the pH value of the passivation solution in the water collecting tank is 3.0-3.7; and the passivation solution in the water collecting tank enters a water inlet of the passivation tank through the circulating pump.
The second drying is hot air drying, the temperature of the second drying is 60 ℃, and the time is 3min.
The passivation method of this example gave an anti-corrosion aluminum material with a nano-conversion film having a thickness of 100-200nm, the surface scanning electron micrograph of which is shown in FIG. 2.
Example 5
This example provides an anti-corrosion aluminum material having a nano-conversion film obtained by the passivation method of example 4 using the passivation solution for aluminum material surface treatment provided in example 2. The surface scanning electron micrograph of the anti-corrosion type aluminum material with the nano conversion film of the present example is shown in fig. 3, and the thickness of the nano conversion film is 100-200nm.
Test analysis and comparison
1. The aluminum material is cleaned by adopting an acid cleaning agent, an alkaline cleaning agent and a neutral cleaning agent respectively, and the effects of oil stain cleaning effect and the influence on the subsequent passivation process are compared. The results are shown in Table 1 below.
TABLE 1
Conclusion: the neutral cleaning agent provided by the invention has good degreasing effect, does not corrode a base material, and does not influence passivation effect.
2. Influence of ultrasonic waves and ultrasonic frequency on cleaning and passivation effects. The results are shown in Table 2 below.
TABLE 2
| Ultrasonic frequency/Hz | Cleaning effect | Passivation effect |
| 0 | In general | Slow passivation, need to increase passivation time |
| 10000 | Good quality | Better passivation |
| 20000 | Excellent and excellent properties | Better passivation and shortened time |
| 30000 | Excellent and excellent properties | Better passivation and shortened time |
Conclusion: the invention creatively adopts the addition of ultrasonic waves, can clean the greasy dirt more thoroughly, can promote the passivation effect, shortens the passivation time and improves the efficiency. Comprehensively considering that when the ultrasonic frequency is 20000Hz, the cleaning and passivating effects are optimal, and the generated noise is small.
3. The change of the corrosion resistance of the film layer of the conversion film under the conditions of different treatment temperatures, different treatment times and different potassium fluorozirconate concentrations was detected as follows. In this experiment, the observation of the conversion coating was performed by using an electron microscope.
(1) Potassium fluorozirconate content
The passivation solution provided in example 1 was used, but potassium fluorozirconate was adjusted to have different concentrations, and after the aluminum alloy substrate was passivated by the aluminum material surface passivation method of example 4, the salt spray corrosion resistance was analyzed, and the results are shown in table 3 below.
TABLE 3 influence of the potassium fluorozirconate content on the corrosion time of salt fog
As can be seen from table 1, the aluminum alloy matrix itself was resistant to 280 hours of salt spray corrosion in a salt spray test environment (NaCl salt spray concentration 5%). In the passivation solution, the concentration of 0.2g/L potassium fluorozirconate can reach 550 hours at most. Indicating that the passivation solution plays a role in corrosion inhibition. When the concentration of potassium fluorozirconate in the passivation solution is low, the formed conversion film is incomplete, so that the corrosion resistance is poor, the corrosion resistance is enhanced along with the increase of the concentration, and when the concentration of potassium fluorozirconate in the passivation solution is 0.2g/L, the corrosion resistance of the conversion film is best. However, as the concentration of potassium fluorozirconate in the passivation solution continues to increase, the salt spray corrosion resistance time of the film layer tends to decrease, and the film layer is uneven due to the excessively high content, so that the binding force with the matrix decreases.
According to the salt spray corrosion resistance time, the film layer has good corrosion resistance under the condition that the concentration of potassium fluorozirconate in the passivation solution is 0.2 g/L.
(2) Influence of temperature on corrosion resistance of conversion film
Under the condition that the concentration of potassium fluorozirconate in the passivation solution is 0.2g/L and the ultrasonic passivation time is 5min, the influence of different temperatures on the corrosion resistance of the conversion film is studied. In chemical reaction experiments, temperature directly affects the chemical reaction rate. The diffusion of ions can be accelerated when the temperature is high, and the activity of ions is small when the temperature is low. Thus, the temperature can control the growth rate of the film. The reaction process of the passivation solution and the aluminum alloy mainly comprises that the oxidation reaction product of specific components in the passivation solution is attached to the surface of the aluminum alloy. The temperature is increased, so that the diffusion speed of ions is increased, the film forming reaction speed is accelerated, and the film formation is facilitated. When the temperature is proper, the film forming is complete, and the corrosion resistance is also enhanced. However, when the temperature is too high, the solution reacts vigorously, the balance of the forward and reverse reaction rates is broken, and the integrity and corrosion resistance of the film layer can be damaged by the temperature rise. If the gas generated in the film forming process is not removed, holes may be generated in the film layer, so that compactness is affected, and corrosion resistance of the film layer is further affected. Under the condition that the concentration of potassium fluorozirconate in the passivation solution is 0.2g/L, the ultrasonic passivation time is 5min, the ultrasonic passivation temperature is 15 ℃,20 ℃,25 ℃,30 ℃,40 ℃ and 50 ℃ respectively, the rest steps and parameters of the aluminum surface passivation method are the same as those of the embodiment 4, and the obtained aluminum material subjected to surface passivation treatment is subjected to a salt spray test, and the corrosion resistance of the aluminum material is shown in the table 4.
TABLE 4 influence of temperature on conversion film Corrosion resistance
It can be seen that the salt spray resistance time of the film layer is increased from 470 hours to 550 hours along with the temperature increase, and the salt spray resistance time of the film layer is not greatly different about 550 hours when the temperature is between 20 and 30 ℃, which indicates that the temperature increase increases the reaction rate of the passivation solution and the matrix. But the temperature exceeds 30 ℃, the reaction rate continues to increase, the deposition rate and the diffusion rate of the film layer are unbalanced, the conversion film is not compact and uniform, the salt spray resistant time begins to decrease instead, and the decreasing speed of the salt spray resistant time increases as the temperature continues to increase. Therefore, when the passivation temperature is controlled to be about 25 ℃, the reaction rate of the passivation solution and the matrix is suitable for forming a film layer, the corrosion resistance of the film layer is relatively good, and the temperature is relatively suitable for the requirements of industrial production environments.
(3) Influence of pH value on corrosion resistance of conversion film
Under the condition that the temperature of ultrasonic passivation is 25 ℃ and the time of ultrasonic passivation is 5min, the passivation solution in the embodiment 1 is adjusted to have different pH values (pH values), and the aluminum alloy matrix is subjected to passivation treatment by adopting the aluminum material surface passivation method in the embodiment 4, and then the salt spray corrosion resistance of the aluminum alloy matrix is analyzed. The results of the test for the influence of pH on the corrosion resistance of the conversion film are shown in Table 5.
TABLE 5 influence of pH on the corrosion resistance of conversion coating
The passivation solution of example 1 has an original pH of 3.7, and it is seen that the salt spray corrosion resistance increases when the pH is adjusted to 3.0 to 3.2 in the acid direction, and the salt spray corrosion resistance increases when the pH is adjusted to 3.2, but the salt spray corrosion resistance decreases rapidly when the pH is adjusted to the base direction, so that it is necessary to control the pH of the passivation solution of the present invention to 3.0 to 3.7 in order to obtain a conversion coating having better performance.
According to the test result, the optimal technological parameters of the passivation process of the invention are as follows: the pH value of the passivation solution is 3.0-3.7, the ultrasonic passivation time is 5min, the ultrasonic passivation temperature is about 25 ℃, and the concentration of potassium fluozirconate in the passivation solution is 0.2g/L.
Performance testing
The execution standard: ASTM B117-03. The sample numbers are as follows, and the wires of the following numbers ①～⑥ are placed in a salt spray test box, respectively, and the surface condition of the wires is observed periodically. The NaCl salt fog concentration is 5%, and the standing time is 1000 hours. Meanwhile, in order to verify the bonding capability of the generated passivation film and the surface of the wire, the passivation film is prevented from falling off in the wire-erecting construction process, and pulley test comparison is correspondingly carried out. And the pulley passing test method is specifically referred to Q/GDW 1815 aluminum alloy core high conductivity aluminum stranded wire. The photographs of the aluminum wire subjected to the test salt spray corrosion are shown in fig. 4. The results are shown in Table 6 below.
TABLE 6
The surface condition of the wire after 1000 hours is as follows (visual observation): ① Passivating the pulley, and slightly increasing the oxidation degree of the surface of the lead; ② Passivating the non-passing pulley, and enabling the surface of the lead to be bright without oxidation; ③ The surface of the wire is completely oxidized after the unpassivated pulley is not passivated; ④ Semi-passivating the non-passing pulley, wherein one end of the wire is passivated to be bright, and the other end of the wire is not passivated to be oxidized in a large area; ⑤、⑥ The surface oxidation degree of the two wires after passivation and pulley repair tends to be consistent.
Test results show that the passivation solution can protect an aluminum matrix and prevent the surface of a wire from being oxidized and blackened. Meanwhile, the generated passivation film has good adhesiveness with the wires, and the influence on the passivation film caused by the pulley is small. After the passivation treatment of the invention, the surface of the aluminum wire is formed with a relatively flat and continuous protective film with a thickness less than 1 μm by scanning electron microscope analysis, and the influence of the thickness of the film on the wire diameter of the aluminum wire is negligible. The passivation film layer plays a good role in blocking the surface of the aluminum wire, and obviously blocks corrosion of corrosive media in the atmosphere and industrial environment, so that corrosion reaction of an aluminum metal matrix is effectively inhibited, and corrosion resistance of the aluminum wire is enhanced.
Claims (3)
1. A method for passivating the surface of an aluminum material, which comprises the following steps:
Sequentially carrying out ultrasonic cleaning, first drying, ultrasonic passivation and second drying on the aluminum material to obtain the aluminum material after surface passivation treatment;
The ultrasonic cleaning device comprises a ultrasonic cleaning device, a cleaning device and a cleaning device, wherein the cleaning solution used for ultrasonic cleaning is neutral cleaning solution, and the cleaning device consists of the following components in percentage by total volume of the neutral cleaning solution being 100 percent: 50% xylene and 50% acetone;
The ultrasonic passivation adopts passivation solution for aluminum surface treatment; the passivation solution for aluminum surface treatment consists of the following components: titanium sulfate 0.3g/L, potassium fluorozirconate 0.2g/L, potassium iodide 0.1g/L, potassium fluorochromate 0.08g/L, sodium sulfite 0.08g/L, nitric acid and water, and the pH value of the passivation solution is 3.7; or the passivation solution for aluminum surface treatment consists of the following components: titanium sulfite 0.2g/L, potassium fluorozirconate 0.2g/L, potassium iodide 0.05g/L, sodium fluoride 0.05g/L, sodium carbonate 0.08g/L, nitric acid and water, and the pH value of the passivation solution is 3.7;
The ultrasonic passivation is carried out by an ultrasonic passivation device, and the ultrasonic passivation device comprises a passivation groove, an ultrasonic oscillating plate, a heat preservation device, a circulating device and a filtering device; the ultrasonic oscillating plate is arranged in the passivation groove; the heat preservation device is arranged outside the passivation groove; the circulating device comprises a circulating pump, a water collecting tank and an immersed pH value detector; the circulating pump is connected with the water collecting tank, and the immersed pH value detector is arranged in the water collecting tank; the passivation groove is provided with a plurality of water inlets and a plurality of water outlets; the water outlet of the passivation tank is connected with the filtering device through a pipeline and then is connected with the water collecting tank through a pipeline, and the water inlet of the passivation tank is connected with the water collecting tank through a pipeline and the circulating pump;
the ultrasonic passivation specifically comprises the following steps: carrying out ultrasonic treatment on the aluminum material in the passivation tank and the passivation solution for aluminum material surface treatment through the ultrasonic oscillating plate, wherein the ultrasonic frequency is 20000Hz, and the power is 4kw; simultaneously, the temperature of passivation is 25 ℃ through the heat preservation device; after passivation treatment for 5min, enabling passivation solution in the passivation tank to enter the filtering device through the water outlet for filtering, and then enter the water collecting tank; the immersion type pH value detector inside the water collecting tank detects the pH value of the passivation solution, and when the pH value is not 3.0-3.7, the passivation solution for aluminum surface treatment and/or nitric acid are supplemented from the outside so that the pH value of the passivation solution in the water collecting tank is 3.0-3.7; the passivation solution in the water collecting tank enters a water inlet of the passivation tank through the circulating pump;
the ultrasonic cleaning is also carried out by adopting the ultrasonic passivating device, and the passivating liquid for aluminum surface treatment is replaced by the neutral cleaning liquid; the ultrasonic cleaning specifically comprises the following steps: carrying out ultrasonic treatment on the aluminum material and neutral cleaning liquid in a cleaning tank through the ultrasonic oscillating plate, wherein the cleaning tank is the passivation tank, the ultrasonic frequency is 20000Hz, and the power is 4kw; meanwhile, the heat preservation device is not started and maintains normal temperature; after 3min of cleaning treatment, enabling the cleaning liquid in the cleaning tank to enter the filtering device through the water outlet for filtering, and then enter the water collecting tank; the immersed pH value detector in the water collecting tank is not started; the cleaning liquid in the water collecting tank enters a water inlet of the cleaning tank through the circulating pump;
The temperature of the first drying is 40-60 ℃ and the time is 3min; the first drying is hot air blowing drying; the hot air blowing and drying device comprises 4-8 air pipes uniformly distributed on the circumference, wherein air holes are uniformly distributed in the length direction of the air pipes, the air holes of the air pipes are obliquely formed along the opposite direction of the running of the aluminum material, and compressed air is introduced to blow-dry the surface of the aluminum material; the hot air blowing and drying device also comprises a heating device;
the temperature of the second drying is 60 ℃ and the time is 3min; the second drying is hot air drying;
the aluminum material is an aluminum wire and/or an aluminum alloy wire.
2. An anti-corrosion type aluminum material having a nano conversion film, which is produced by subjecting an aluminum material to a surface passivation treatment by the aluminum material surface passivation method according to claim 1.
3. The corrosion-resistant aluminum material with a nano-conversion film according to claim 2, wherein the nano-conversion film is formed on the surface of the aluminum material, and the thickness of the nano-conversion film is 100nm to 200nm.
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| CN210529061U (en) * | 2019-07-24 | 2020-05-15 | 津瑞康(天津)精密机械有限公司 | Draining type ultrasonic passivation tank |
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