CN115094418B - Method for sealing micropores of layered double hydroxide coating on magnesium alloy surface - Google Patents
Method for sealing micropores of layered double hydroxide coating on magnesium alloy surface Download PDFInfo
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- CN115094418B CN115094418B CN202210711489.8A CN202210711489A CN115094418B CN 115094418 B CN115094418 B CN 115094418B CN 202210711489 A CN202210711489 A CN 202210711489A CN 115094418 B CN115094418 B CN 115094418B
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- double hydroxide
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- 229910000861 Mg alloy Inorganic materials 0.000 title claims abstract description 86
- 238000000576 coating method Methods 0.000 title claims abstract description 62
- 239000011248 coating agent Substances 0.000 title claims abstract description 60
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 title claims abstract description 55
- 238000000034 method Methods 0.000 title claims abstract description 21
- 238000007789 sealing Methods 0.000 title claims abstract description 16
- 238000005260 corrosion Methods 0.000 claims abstract description 53
- 230000007797 corrosion Effects 0.000 claims abstract description 50
- 229920002873 Polyethylenimine Polymers 0.000 claims abstract description 34
- 239000003112 inhibitor Substances 0.000 claims abstract description 25
- 229920001467 poly(styrenesulfonates) Polymers 0.000 claims abstract description 25
- 229960002796 polystyrene sulfonate Drugs 0.000 claims abstract description 16
- 239000011970 polystyrene sulfonate Substances 0.000 claims abstract description 16
- 239000000243 solution Substances 0.000 claims description 98
- 239000011259 mixed solution Substances 0.000 claims description 36
- 238000006243 chemical reaction Methods 0.000 claims description 22
- 229910052751 metal Inorganic materials 0.000 claims description 18
- 239000002184 metal Substances 0.000 claims description 18
- 238000002360 preparation method Methods 0.000 claims description 18
- 150000003839 salts Chemical class 0.000 claims description 18
- YXIWHUQXZSMYRE-UHFFFAOYSA-N 1,3-benzothiazole-2-thiol Chemical compound C1=CC=C2SC(S)=NC2=C1 YXIWHUQXZSMYRE-UHFFFAOYSA-N 0.000 claims description 12
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 12
- 238000005238 degreasing Methods 0.000 claims description 12
- 239000003513 alkali Substances 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 229910019142 PO4 Inorganic materials 0.000 claims description 7
- 239000010452 phosphate Substances 0.000 claims description 7
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 7
- MCJGNVYPOGVAJF-UHFFFAOYSA-N quinolin-8-ol Chemical compound C1=CN=C2C(O)=CC=CC2=C1 MCJGNVYPOGVAJF-UHFFFAOYSA-N 0.000 claims description 7
- VZCYOOQTPOCHFL-OWOJBTEDSA-N Fumaric acid Chemical compound OC(=O)\C=C\C(O)=O VZCYOOQTPOCHFL-OWOJBTEDSA-N 0.000 claims description 6
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims description 6
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 6
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 6
- VYLVYHXQOHJDJL-UHFFFAOYSA-K cerium trichloride Chemical compound Cl[Ce](Cl)Cl VYLVYHXQOHJDJL-UHFFFAOYSA-K 0.000 claims description 6
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 claims description 6
- 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 6
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 6
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims description 6
- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical compound [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 claims description 6
- 230000035484 reaction time Effects 0.000 claims description 6
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 6
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 6
- QDZRBIRIPNZRSG-UHFFFAOYSA-N titanium nitrate Chemical compound [O-][N+](=O)O[Ti](O[N+]([O-])=O)(O[N+]([O-])=O)O[N+]([O-])=O QDZRBIRIPNZRSG-UHFFFAOYSA-N 0.000 claims description 6
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 6
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims description 6
- 239000005725 8-Hydroxyquinoline Substances 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 229960003540 oxyquinoline Drugs 0.000 claims description 5
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 claims description 3
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims description 3
- 229910021555 Chromium Chloride Inorganic materials 0.000 claims description 3
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 3
- 229910021380 Manganese Chloride Inorganic materials 0.000 claims description 3
- GLFNIEUTAYBVOC-UHFFFAOYSA-L Manganese chloride Chemical compound Cl[Mn]Cl GLFNIEUTAYBVOC-UHFFFAOYSA-L 0.000 claims description 3
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 3
- 239000002262 Schiff base Substances 0.000 claims description 3
- 150000004753 Schiff bases Chemical class 0.000 claims description 3
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 3
- QRUDEWIWKLJBPS-UHFFFAOYSA-N benzotriazole Chemical compound C1=CC=C2N[N][N]C2=C1 QRUDEWIWKLJBPS-UHFFFAOYSA-N 0.000 claims description 3
- 239000012964 benzotriazole Substances 0.000 claims description 3
- QSWDMMVNRMROPK-UHFFFAOYSA-K chromium(3+) trichloride Chemical compound [Cl-].[Cl-].[Cl-].[Cr+3] QSWDMMVNRMROPK-UHFFFAOYSA-K 0.000 claims description 3
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 claims description 3
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims description 3
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims description 3
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims description 3
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 claims description 3
- 239000001530 fumaric acid Substances 0.000 claims description 3
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 3
- 229910001629 magnesium chloride Inorganic materials 0.000 claims description 3
- 239000011565 manganese chloride Substances 0.000 claims description 3
- 235000002867 manganese chloride Nutrition 0.000 claims description 3
- 229940099607 manganese chloride Drugs 0.000 claims description 3
- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(2+);dinitrate Chemical compound [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 0.000 claims description 3
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 3
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims description 3
- 238000005498 polishing Methods 0.000 claims description 3
- 235000010413 sodium alginate Nutrition 0.000 claims description 3
- 239000000661 sodium alginate Substances 0.000 claims description 3
- 229940005550 sodium alginate Drugs 0.000 claims description 3
- 229940083575 sodium dodecyl sulfate Drugs 0.000 claims description 3
- 239000011684 sodium molybdate Substances 0.000 claims description 3
- 235000015393 sodium molybdate Nutrition 0.000 claims description 3
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims description 3
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 claims description 3
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 claims description 3
- 239000011592 zinc chloride Substances 0.000 claims description 3
- 235000005074 zinc chloride Nutrition 0.000 claims description 3
- 229920000867 polyelectrolyte Polymers 0.000 abstract description 10
- 230000000694 effects Effects 0.000 abstract description 4
- 239000001257 hydrogen Substances 0.000 abstract description 2
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 42
- 239000011777 magnesium Substances 0.000 description 20
- 230000000052 comparative effect Effects 0.000 description 19
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 18
- 229910052749 magnesium Inorganic materials 0.000 description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 17
- 238000005406 washing Methods 0.000 description 16
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 10
- 229920000172 poly(styrenesulfonic acid) Polymers 0.000 description 10
- 229940005642 polystyrene sulfonic acid Drugs 0.000 description 10
- 230000005764 inhibitory process Effects 0.000 description 5
- 229910052757 nitrogen Inorganic materials 0.000 description 5
- 239000001488 sodium phosphate Substances 0.000 description 5
- 229910000162 sodium phosphate Inorganic materials 0.000 description 5
- 239000000758 substrate Substances 0.000 description 5
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 description 5
- 244000137852 Petrea volubilis Species 0.000 description 4
- 238000005530 etching Methods 0.000 description 4
- 239000004519 grease Substances 0.000 description 4
- 238000007602 hot air drying Methods 0.000 description 4
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- 238000001027 hydrothermal synthesis Methods 0.000 description 3
- 238000005342 ion exchange Methods 0.000 description 3
- 239000002060 nanoflake Substances 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 238000009830 intercalation Methods 0.000 description 2
- 230000002687 intercalation Effects 0.000 description 2
- 239000002135 nanosheet Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 241001089723 Metaphycus omega Species 0.000 description 1
- 102100039298 Phosphatidylserine synthase 1 Human genes 0.000 description 1
- 101710116266 Phosphatidylserine synthase 1 Proteins 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000010335 hydrothermal treatment Methods 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 238000001453 impedance spectrum Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910001092 metal group alloy Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Classifications
-
- 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
- C23C26/00—Coating not provided for in groups C23C2/00 - C23C24/00
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Treatment Of Metals (AREA)
Abstract
The invention belongs to the technical field of corrosion and protection of magnesium alloy, and particularly discloses a method for sealing micropores of a layered double hydroxide coating on the surface of magnesium alloy. The magnesium alloy with the layered double hydroxide coating is reacted in the polyethyleneimine solution, the polystyrene sulfonate solution, the corrosion inhibitor solution, the polystyrene sulfonate solution and the polyethyleneimine solution in sequence for 8-12 min in each solution system, and the closure of micropores of the layered double hydroxide coating on the surface of the magnesium alloy is completed. Compared with the existing organically modified layered double hydroxide, the method disclosed by the invention has the characteristics of high binding force and excellent anti-corrosion effect, and has better self-healing capacity through the hydrogen bond combination formed by polyelectrolyte and the layered double hydroxide. The corrosion current density of the magnesium alloy can be reduced to about 8.8x10 ‑10 A/cm 2 。
Description
Technical Field
The invention relates to the technical field of corrosion and protection of magnesium alloy, in particular to a method for sealing micropores of a layered double hydroxide coating on the surface of magnesium alloy.
Background
Magnesium alloys have various applications in different industries due to their excellent physical/chemical properties. However, magnesium alloy is a metal alloy which is active in electrochemical and chemical properties and is easy to corrode, so that proper surface treatment is required before application. Layered Double Hydroxides (LDHs) have a specific layered structure and ion exchange capacity and can exhibit self-healing advantages by capturing corrosive media and releasing corrosion inhibitors. LDHs film layers can be prepared on the surface of the magnesium alloy by coprecipitation, electrochemical deposition, in-situ growth and other methods. The obtained LDHs coating can have good corrosion protection capability on the surface in 3.5wt.% NaCl corrosive electrolyte, and the corrosion protection treatment of the magnesium alloy by adopting the LDHs film has become a great research hot spot in the field of surface engineering.
However, LDHs anticorrosive coatings have certain drawbacks, and when LDHs with a nano-sheet structure grow perpendicular to a substrate to form a film, a nano-gap of several nanometers to several hundred nanometers often exists between the nano-sheets. The gap is favorable for diffusion of the corrosive medium, and is favorable for the corrosive medium to more quickly permeate to the surface of the magnesium alloy substrate so as to corrode. In addition, a large amount of hydrophilic groups OH exist on the surface of the LDHs film, so that the hydrophilicity of the coating is increased, even super hydrophilicity is achieved, the permeability of corrosive medium to the LDHs coating is certainly increased, and the corrosion resistance of the coating to magnesium alloy is weakened. Therefore, it is necessary to carry out hole sealing treatment on the LDHs film layer by combining other methods.
Research and reports focus on physical adsorption of organic coatings directly on LDHs surfaces. For example, in a recent patent application (application number: CN 202010453188.0), applicants have used fluorosilicone oil to coat LDHs film layers, imparting self-healing and long-term corrosion protection capabilities to the coating. However, the modified film by physical adsorption does not have excellent binding force. Chinese patent (CN 202110865011.6) and Chinese patent (CN 201910870394.9) utilize corrosion inhibitor intercalation to enter the LDHs coating, and the corrosion inhibition effect is achieved through ion exchange, but the direct addition of the corrosion inhibitor to the intercalation coating can cause the problem that the corrosion inhibitor is released and then simultaneously diffuses into a corrosion medium, so that the corrosion inhibition efficiency is reduced, and the problem that micropores in the LDHs film layer cause the reduction of corrosion protection capability cannot be solved.
Therefore, how to provide a method for sealing micropores of a layered double hydroxide coating on the surface of a magnesium alloy, which can enhance the combination capability of a modified film and an LDHs film layer and improve corrosion inhibition efficiency and corrosion protection capability is a problem to be solved in the field.
Disclosure of Invention
In view of the above, the invention provides a method for sealing micropores of a layered double hydroxide coating on the surface of a magnesium alloy, so as to solve the problem that the solution of physically adsorbing an organic coating on the surface of LDHs cannot effectively improve corrosion inhibition efficiency and corrosion protection capability.
In order to achieve the above purpose, the invention adopts the following technical scheme:
a method for sealing micropores of a layered double hydroxide coating on the surface of a magnesium alloy, which comprises the following steps:
and (3) sequentially reacting the magnesium alloy with the layered double hydroxide coating in a polyethyleneimine solution, a polystyrene sulfonate solution, a corrosion inhibitor solution, a polystyrene sulfonate solution and a polyethyleneimine solution to finish the closure of micropores of the layered double hydroxide coating on the surface of the magnesium alloy.
Preferably, the mass concentration of the polyethyleneimine solution is independently 1-3 mg/mL; the mass concentration of the polystyrene sulfonate solution is independently 1-3 mg/mL; the mass concentration of the corrosion inhibitor solution is 70-90 mg/mL; the corrosion inhibitor comprises one or more of 8-hydroxyquinoline, sodium dodecyl benzene sulfonate, sodium dodecyl sulfate, schiff base, sodium alginate, sodium molybdate, cerium chloride, 2-mercaptobenzothiazole, benzotriazole, triethanolamine and fumaric acid.
Preferably, the reaction time of the magnesium alloy with the layered double hydroxide coating in each solution is independently 8-12 min;
the mass volume ratio of the magnesium alloy with the layered double hydroxide coating to the reaction solution is independently 40-45 mg:1L;
the reaction solution comprises a polyethyleneimine solution, a polystyrene sulfonate solution and a corrosion inhibitor solution.
Preferably, the preparation method of the magnesium alloy with the layered double hydroxide coating comprises the following steps:
1) Sequentially polishing and degreasing the magnesium alloy to obtain the treated magnesium alloy;
2) And placing the treated magnesium alloy into a mixed solution, and reacting to obtain the magnesium alloy with the layered double hydroxide coating.
Preferably, the degreasing in the step 1) is alkaline degreasing, the degreasing alkali liquor is formed by mixing hydroxide solution and phosphate solution, the mass concentration of hydroxide in the degreasing alkali liquor is 40-55 g/L, and the mass concentration of phosphate is 8-12 g/L; the oil removing time is 8-12 min, and the oil removing temperature is 60-70 ℃.
Preferably, the preparation method of the mixed solution in the step 2) is as follows: mixing divalent metal salt, trivalent metal salt, sodium carbonate and water, and then adjusting the pH value to obtain a mixed solution;
preferably, the divalent metal salt comprises one or more of magnesium nitrate, cobalt nitrate, nickel nitrate, zinc nitrate, manganese nitrate, copper nitrate, magnesium chloride, cobalt chloride, nickel chloride, zinc chloride, manganese chloride and copper chloride, and the mass concentration of the divalent metal salt in the mixed solution is 0.05-0.08 mol/L;
the trivalent metal salt comprises one or more of aluminum nitrate, ferric nitrate, chromium nitrate, cerium nitrate, titanium nitrate, aluminum chloride, ferric chloride, chromium chloride, cerium chloride and titanium chloride, and the mass concentration of the trivalent metal salt in the mixed solution is 0.02-0.04 mol/L;
the mass concentration of sodium carbonate in the mixed solution is 0.005-0.02 mol/L;
preferably, the pH value of the mixed solution is 11-13.
Preferably, the reaction temperature in the step 2) is 110-125 ℃ and the reaction time is 12-36 h.
Preferably, the mass-volume ratio of the magnesium alloy treated in the step 2) to the mixed solution is 40-45 mg:1L.
Compared with the prior art, the invention has the following beneficial effects:
1. the treatment method disclosed by the invention is simple, and the micropores of the layered double hydroxide coating on the surface of the magnesium alloy can be sealed by soaking and reacting in the polyethyleneimine solution, the polystyrene sulfonate solution, the corrosion inhibitor solution, the polystyrene sulfonate solution and the polyethyleneimine solution with specific concentrations in sequence;
2. compared with the existing organically modified LDHs, the LDHs of the corrosion inhibitor packaged by polyelectrolyte has higher binding force through hydrogen bonding between the polyelectrolyte and the LDHs, has better anti-corrosion effect than the LDHs of the corrosion inhibitor obtained by ion exchange, and has better self-healing capacity.
3. The self-corrosion potential of the magnesium alloy treated by the method can be increased from-1410 mV to-142 mV, and the corrosion current density can be increased from about 6.0x10 -5 A/cm 2 Down to about 8.8X10 -10 A/cm 2 。
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are required to be used in the embodiments or the description of the prior art will be briefly described below, and it is obvious that the drawings in the following description are only embodiments of the present invention, and that other drawings can be obtained according to the provided drawings without inventive effort for a person skilled in the art.
Fig. 1 is an SEM morphology of untreated magnesium alloy-LDHs, comparative examples 1-2 and the product film obtained in example 1, wherein a, b correspond to untreated magnesium alloy-LDHs; c. d corresponds to comparative example 1; e. f corresponds to comparative example 2; g. h corresponds to example 1;
FIG. 2 is an electrochemical impedance spectrum of a magnesium alloy substrate, untreated magnesium alloy-LDHs, comparative examples 1-2 and example 1 to obtain a product film layer;
FIG. 3 shows Tafel curves, corrosion potential and corrosion current density graphs of the magnesium alloy substrate, untreated magnesium alloy-LDHs, comparative examples 1-2 and example 1 to obtain product film layers, wherein a is the Tafel curve, and b is the corrosion potential and corrosion current density graph.
Detailed Description
The invention provides a method for sealing micropores of a layered double hydroxide coating on the surface of a magnesium alloy, which comprises the following steps:
and (3) sequentially reacting the magnesium alloy with the layered double hydroxide coating in a polyethyleneimine solution, a polystyrene sulfonate solution, a corrosion inhibitor solution, a polystyrene sulfonate solution and a polyethyleneimine solution to finish the closure of micropores of the layered double hydroxide coating on the surface of the magnesium alloy.
In the invention, the mass concentration of the polyethyleneimine solution is independently 1-3 mg/mL, preferably 1.5-2.5 mg/mL, and more preferably 2mg/mL; the mass concentration of the polystyrene sulfonate solution is independently 1-3 mg/mL, preferably 1.5-2.5 mg/mL, and more preferably 2mg/mL; the mass concentration of the corrosion inhibitor solution is 70-90 mg/mL, preferably 75-85 mg/mL, and more preferably 80mg/mL; the corrosion inhibitor comprises one or more of 8-hydroxyquinoline, sodium dodecyl benzene sulfonate, sodium dodecyl sulfate, schiff base, sodium alginate, sodium molybdate, cerium chloride, 2-mercaptobenzothiazole, benzotriazole, triethanolamine and fumaric acid.
In the invention, the corrosion inhibitor can also be other reagents with corrosion inhibition effect on magnesium alloy.
In the present invention, the solvent in the corrosion inhibitor solution includes ethanol and water.
In the present invention, the reaction time of the magnesium alloy with the layered double hydroxide coating in each solution is independently 8 to 12 minutes, preferably 9 to 11 minutes, and more preferably 10 minutes.
In the present invention, the reaction in each solution is followed by washing with absolute ethanol and drying with a nitrogen stream.
In the invention, the mass-volume ratio of the magnesium alloy with the layered double hydroxide coating to the reaction solution is independently 40-45 mg:1L, preferably 41 to 43mg:1L, more preferably 42mg:1L;
the reaction solution comprises a polyethyleneimine solution, a polystyrene sulfonate solution and a corrosion inhibitor solution.
In the invention, the preparation method of the magnesium alloy with the layered double hydroxide coating comprises the following steps:
1) Sequentially polishing and degreasing the magnesium alloy to obtain the treated magnesium alloy;
2) And placing the treated magnesium alloy into a mixed solution, and reacting to obtain the magnesium alloy with the layered double hydroxide coating.
In the invention, the oil removal in the step 1) is alkaline oil removal, the oil removal alkali liquor is formed by mixing hydroxide solution and phosphate solution, and the mass concentration of hydroxide in the oil removal alkali liquor is 40-55 g/L, preferably 48-52 g/L, and more preferably 50g/L; the mass concentration of the phosphate is 8-12 g/L, preferably 9-11 g/L, and more preferably 10g/L; the oil removal time is 8-12 min, preferably 9-11 min, and more preferably 10min; the degreasing temperature is 60 to 70 ℃, preferably 62 to 68 ℃, and more preferably 65 ℃.
In the present invention, the hydroxide is preferably sodium hydroxide or potassium hydroxide.
In the present invention, the phosphate is preferably sodium phosphate.
In the invention, the preparation method of the mixed solution in the step 2) comprises the following steps: mixing divalent metal salt, trivalent metal salt, sodium carbonate and water, and then adjusting the pH value to obtain a mixed solution;
preferably, the divalent metal salt comprises one or more of magnesium nitrate, cobalt nitrate, nickel nitrate, zinc nitrate, manganese nitrate, copper nitrate, magnesium chloride, cobalt chloride, nickel chloride, zinc chloride, manganese chloride and copper chloride, and the mass concentration of the divalent metal salt in the mixed solution is 0.05-0.08 mol/L, preferably 0.06-0.07 mol/L, and further preferably 0.06mol/L;
the trivalent metal salt comprises one or more of aluminum nitrate, ferric nitrate, chromium nitrate, cerium nitrate, titanium nitrate, aluminum chloride, ferric chloride, chromium chloride, cerium chloride and titanium chloride, and the mass concentration of the trivalent metal salt in the mixed solution is 0.02-0.04 mol/L, preferably 0.025-0.035 mol/L, and more preferably 0.03mol/L;
the mass concentration of sodium carbonate in the mixed solution is 0.005-0.02 mol/L, preferably 0.008-0.015 mol/L, and more preferably 0.01mol/L;
the pH of the mixed solution is 11 to 13, preferably 12.
In the present invention, the pH is preferably adjusted by using a sodium hydroxide solution having a mass concentration of 4 to 10mol/L, preferably 4 to 6mol/L, and more preferably 5mol/L.
In the present invention, the reaction temperature in the step 2) is 110 to 125 ℃, preferably 112 to 120 ℃, and more preferably 116 ℃; the reaction time is 12 to 36 hours, preferably 18 to 30 hours, more preferably 24 hours.
In the invention, the mass volume ratio of the magnesium alloy treated in the step 2) to the mixed solution is 40-45 mg:1L, preferably 42 to 44mg:1L, more preferably 43mg:1L.
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
Pretreatment of magnesium alloy: AZ31 magnesium alloy is polished by using No. 1200 sand paper, the grease on the surface is removed, and after alkaline washing is performed for 10min in an alkaline washing solution (the alkaline washing solution is a mixed solution of sodium hydroxide and sodium phosphate, the mass concentration of NaOH is 50g/L, na 3 PO 4 The mass concentration of (2) is 10 g/L), and is taken out for washing and hot air drying for standby.
Preparation of LDHs film: preparation of 0.03mol/L Al (NO) 3 ) 3 ·9H 2 O，0.06mol/LMg(NO 3 ) 2 ·6H 2 O，0.01mol/L Na 2 CO 3 With 5mol/L NaOH solution to adjust the pH to 12. Pouring the mixed solution into a 50mL reaction kettle, and vertically placing the pretreated magnesium alloy into the reaction kettle and carrying out hydrothermal reaction for 24h at 125 ℃ (the mass volume of the magnesium alloy and the mixed solution is 40 mg/L). Finally, the sample was rinsed with water and dried at 65 ℃, and the obtained sample was designated as magnesium alloy-LDHs (magnesium alloy with layered double hydroxide coating).
Preparation of polyelectrolyte/LDHs coating: under normal temperature, magnesium alloy-LDHs are sequentially soaked in 2mg/mL of polyethyleneimine solution and 2mg/mL of polystyrene sulfonic acid solution for 10min respectively, then are soaked in 90mg/mL of 8-hydroxyquinoline (8 HQ) ethanol solution for 10min, then are sequentially soaked in 2mg/mL of polystyrene sulfonic acid solution and 2mg/mL of polyethyleneimine solution for 10min, and the obtained sample is marked as PEI/PSS/8HQ/PSS/PEI. After each reaction step, the sample was purged with absolute ethanol and dried with a stream of nitrogen. Closing micropores of the layered double hydroxide coating on the surface of the magnesium alloy.
Example 2
Pretreatment of magnesium alloy: the AM60 magnesium alloy is polished by using No. 1200 sand paper, the grease on the surface is removed, and after alkaline washing is carried out for 8min in an alkaline washing solution (the alkaline washing solution is a mixed solution of sodium hydroxide and sodium phosphate, the mass concentration of NaOH is 55g/L, na 3 PO 4 The mass concentration of (2) is 8 g/L), and is taken out for washing and hot air drying for standby.
Preparation of LDHs film: preparation of 0.02mol/L Al (NO) 3 ) 3 ·9H 2 O，0.05mol/LMg(NO 3 ) 2 ·6H 2 O，0.005mol/L Na 2 CO 3 With 5mol/L NaOH solution to adjust the pH to 12. Pouring the mixed solution into a 50mL reaction kettle, and vertically placing the pretreated magnesium alloy into the reaction kettle and carrying out hydrothermal reaction for 24h at 110 ℃ (the mass volume of the magnesium alloy and the mixed solution is 45 mg/L). Finally, the sample was rinsed with water and dried at 60 ℃, and the obtained sample was designated as magnesium alloy-LDHs (magnesium alloy with layered double hydroxide coating).
Preparation of polyelectrolyte/LDHs coating: under normal temperature, magnesium alloy-LDHs are sequentially soaked in 1mg/mL of polyethyleneimine solution and 1mg/mL of polystyrene sulfonic acid solution for 12min respectively, then are soaked in 80mg/mL of 2-Mercaptobenzothiazole (MBT) ethanol solution for 12min, then are sequentially soaked in 2mg/mL of polystyrene sulfonic acid solution and 2mg/mL of polyethyleneimine solution for 12min, and the obtained sample is marked as PEI/PSS/MBT/PSS/PEI. After each reaction step, the sample was purged with absolute ethanol and dried with a stream of nitrogen. Closing micropores of the layered double hydroxide coating on the surface of the magnesium alloy.
Example 3
Pretreatment of magnesium alloy: AZ91 magnesium alloy is polished by using No. 1200 sand paper, the grease on the surface is removed, and after alkaline washing is carried out for 12min in an alkaline washing solution (the alkaline washing solution is a mixed solution of sodium hydroxide and sodium phosphate, the mass concentration of NaOH is 50g/L, na 3 PO 4 The mass concentration of (2) is 12 g/L), and is taken out for washing and hot air drying for standby.
Preparation of LDHs film: preparation of 0.04mol/L Al (NO) 3 ) 3 ·9H 2 O，0.08mol/L Mg(NO 3 ) 2 ·6H 2 O，0.02mol/L Na 2 CO 3 With 5mol/L NaOH solution to adjust the pH to 11. Pouring the mixed solution into a 50mL reaction kettle, and vertically placing the pretreated magnesium alloy into the reaction kettle and carrying out hydrothermal reaction for 20h at 120 ℃ (the mass volume of the magnesium alloy and the mixed solution is 42 mg/L). Finally, the sample was rinsed with water and dried at 65 ℃, and the obtained sample was designated as magnesium alloy-LDHs (magnesium alloy with layered double hydroxide coating).
Preparation of polyelectrolyte/LDHs coating: under normal temperature, magnesium alloy-LDHs are sequentially soaked in 2mg/mL of polyethyleneimine solution and 2mg/mL of polystyrene sulfonic acid solution for 10min respectively, then are soaked in 85mg/mL of Sodium Dodecyl Benzene Sulfonate (SDBS) ethanol solution for 10min, then are sequentially soaked in 2mg/mL of polystyrene sulfonic acid solution and 2mg/mL of polyethyleneimine solution for 10min, and the obtained sample is marked as PEI/PSS/SDBS/PSS/PEI-3. After each reaction step, the sample was purged with absolute ethanol and dried with a stream of nitrogen. Closing micropores of the layered double hydroxide coating on the surface of the magnesium alloy.
Example 4
Pretreatment of magnesium alloy: AZ31 magnesium alloy is polished by using No. 1200 sand paper, the grease on the surface is removed, and after the surface is alkali washed for 11min in alkali washing solution (the alkali washing solution is mixed solution of sodium hydroxide and sodium phosphate, the mass concentration of NaOH is 40g/L, na 3 PO 4 The mass concentration of (2) is 10 g/L), and is taken out for washing and hot air drying for standby.
Preparation of LDHs film: preparation of 0.03mol/L Al (NO) 3 ) 3 ·9H 2 O，0.06mol/L Mg(NO 3 ) 2 ·6H 2 O，0.01mol/LNa 2 CO 3 With 5mol/L NaOH solution to adjust the pH to 13. Pouring the mixed solution into a 50mL reaction kettle, and vertically placing the pretreated magnesium alloy into the reaction kettle for hydrothermal treatment at 116 ℃ for 26 hours (the mass volume of the magnesium alloy and the mixed solution is 42 mg/L). Finally, the sample was rinsed with water and dried at 65 ℃, and the obtained sample was designated as magnesium alloy-LDHs (magnesium alloy with layered double hydroxide coating).
Preparation of polyelectrolyte/LDHs coating: under normal temperature, magnesium alloy-LDHs are sequentially soaked in 2mg/mL of polyethyleneimine solution and 2mg/mL of polystyrene sulfonic acid solution for 10min respectively, then soaked in 70mg/mL of Triethanolamine (TEA) ethanol solution for 10min, then sequentially soaked in 3mg/mL of polystyrene sulfonic acid solution and 3mg/mL of polyethyleneimine solution for 8min, and the obtained sample is marked as PEI/PSS/TEA/PSS/PEI-4. After each reaction step, the sample was purged with absolute ethanol and dried with a stream of nitrogen. Closing micropores of the layered double hydroxide coating on the surface of the magnesium alloy.
Comparative example 1
The comparative example differs from example 1 only in that magnesium alloy-LDHs were immersed in a polyethylene imine solution of 2mg/mL and a polystyrene sulfonic acid solution of 2mg/mL in this order for 10 minutes at normal temperature, and the obtained sample was designated PEI/PSS-1. The sample of comparative example 1 had a self-etching potential of-580 mV and an etching current density of 27X 10 -10 A/cm 2 。
Comparative example 2
The comparative example differs from example 1 only in that magnesium alloy-LDHs were sequentially immersed in a polyethylene imine solution of 2mg/mL and a polystyrene sulfonic acid solution of 2mg/mL each for 10min at normal temperature, then immersed in an 8-hydroxyquinoline (8 HQ) ethanol solution of 90mg/mL for 10min, and the obtained sample was designated PEI/PSS/8HQ-1. Comparative example 2 sample had a self-etching potential of-254 mV and an etching current density of 12.7X10 -10 A/cm 2 。
SEM examination was performed on the samples obtained in untreated magnesium alloy-LDHs, comparative example 1, comparative example 2 and example 1, respectively, and the obtained results are shown in fig. 1. From fig. 1 it can be seen that the untreated magnesium alloy-LDHs surface is composed of a number of irregular nanoflakes perpendicular to the substrate with innumerable micro-scale pores between the nanoflakes. In comparative example 1, the pores between the nanoflakes were completely closed by the newly generated tiled polyelectrolyte. In comparative example 2, some random flaky substances were generated due to the surface adsorption of the corrosion inhibitor. In example 1, the polyelectrolyte was further tiled on the sample surface and the corrosion inhibitor was blocked under it, forming a dense flat surface. The embodiment 1 realizes the complete closure of micron-sized pores on the surface of the layered double hydroxide, and the polyelectrolyte membrane is loaded with a sufficient amount of corrosion inhibitor, so that the corrosion resistance of the coating can be fully improved.
The electrochemical impedance was measured and the measurement result is shown in fig. 2. It can be seen from fig. 2 that the charge transfer resistance (R ct ) The value was only 318. OMEGA.cm 2 R of magnesium alloy-LDHs ct The value is increased to 1.15MΩ cm 2 R of comparative example 1 ct The value reaches 3.59M omega cm 2 Comparative example 2 reached R ct The value was further increased to 68.00MΩ cm 2 EXAMPLE 1R of the finally obtained coating ct Up to 86.75 M.OMEGA.cm 2 ；
Tafel curves and corresponding corrosion potential and corrosion current density graphs are shown in FIG. 3. From FIG. 3, it can be seen that the corrosion current density (j corr ) The value reaches 60.00 mu A/cm 2 J of magnesium alloy-LDHs corr Reduced to 8.37nA/cm 2 J of comparative example 1 corr The value was reduced to 2.70nA/cm 2 J of comparative example 2 corr The value was further reduced to 1.27nA/cm 2 Example 1 j finally obtaining a coating corr As low as 0.88nA/cm 2 。
In the present specification, each embodiment is described in a progressive manner, and each embodiment is mainly described in a different point from other embodiments, and identical and similar parts between the embodiments are all enough to refer to each other.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (8)
1. A method for sealing micropores of a layered double hydroxide coating on the surface of a magnesium alloy, which is characterized by comprising the following steps:
sequentially reacting the magnesium alloy with the layered double hydroxide coating in a polyethyleneimine solution, a polystyrene sulfonate solution, a corrosion inhibitor solution, a polystyrene sulfonate solution and a polyethyleneimine solution to finish the closure of micropores of the layered double hydroxide coating on the surface of the magnesium alloy;
the mass concentration of the polyethyleneimine solution is independently 1-3 mg/mL; the mass concentration of the polystyrene sulfonate solution is independently 1-3 mg/mL; the mass concentration of the corrosion inhibitor solution is 70-90 mg/mL; the corrosion inhibitor comprises one or more of 8-hydroxyquinoline, sodium dodecyl benzene sulfonate, sodium dodecyl sulfate, schiff base, sodium alginate, sodium molybdate, cerium chloride, 2-mercaptobenzothiazole, benzotriazole, triethanolamine and fumaric acid;
the reaction time of the magnesium alloy with the layered double hydroxide coating in each solution is independently 8-12 min;
the mass volume ratio of the magnesium alloy with the layered double hydroxide coating to the reaction solution is independently 40-45 mg:1L;
the reaction solution comprises a polyethyleneimine solution, a polystyrene sulfonate solution and a corrosion inhibitor solution.
2. The method for sealing micropores of a layered double hydroxide coating on a magnesium alloy surface according to claim 1, wherein the preparation method of the magnesium alloy with the layered double hydroxide coating comprises the following steps:
1) Sequentially polishing and degreasing the magnesium alloy to obtain the treated magnesium alloy;
2) And placing the treated magnesium alloy into a mixed solution, and reacting to obtain the magnesium alloy with the layered double hydroxide coating.
3. The method for sealing the micropores of the layered double hydroxide coating on the surface of the magnesium alloy according to claim 2, wherein the degreasing in the step 1) is alkaline degreasing, the degreasing alkali solution is formed by mixing a hydroxide solution and a phosphate solution, the mass concentration of the hydroxide in the degreasing alkali solution is 40-55 g/L, and the mass concentration of the phosphate is 8-12 g/L; the oil removing time is 8-12 min, and the oil removing temperature is 60-70 ℃.
4. A method for closing micropores of a layered double hydroxide coating on a magnesium alloy surface according to claim 3, wherein the preparation method of the mixed solution in step 2) is as follows: the divalent metal salt, the trivalent metal salt, sodium carbonate and water are mixed, and then the pH value is adjusted to obtain a mixed solution.
5. The method for sealing micropores of a layered double hydroxide coating on a magnesium alloy surface according to claim 4, wherein the divalent metal salt comprises one or more of magnesium nitrate, cobalt nitrate, nickel nitrate, zinc nitrate, manganese nitrate, copper nitrate, magnesium chloride, cobalt chloride, nickel chloride, zinc chloride, manganese chloride and copper chloride, and the mass concentration of the divalent metal salt in the mixed solution is 0.05-0.08 mol/L;
the trivalent metal salt comprises one or more of aluminum nitrate, ferric nitrate, chromium nitrate, cerium nitrate, titanium nitrate, aluminum chloride, ferric chloride, chromium chloride, cerium chloride and titanium chloride, and the mass concentration of the trivalent metal salt in the mixed solution is 0.02-0.04 mol/L;
the mass concentration of sodium carbonate in the mixed solution is 0.005-0.02 mol/L.
6. The method for sealing micropores of a layered double hydroxide coating on a magnesium alloy surface according to claim 5, wherein the pH value of the mixed solution is 11 to 13.
7. The method for sealing micropores of a layered double hydroxide coating on a magnesium alloy surface according to claim 6, wherein the reaction temperature in step 2) is 110-125 ℃ and the reaction time is 12-36 h.
8. The method for sealing the micropores of the layered double hydroxide coating on the surface of the magnesium alloy according to claim 7, wherein the mass-volume ratio of the magnesium alloy treated in the step 2) to the mixed solution is 40-45 mg:1L.
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