CN114351125A - Zirconium oxide-based corrosion-resistant and wear-resistant coating on surface of magnesium alloy and preparation method thereof - Google Patents
Zirconium oxide-based corrosion-resistant and wear-resistant coating on surface of magnesium alloy and preparation method thereof Download PDFInfo
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- 229910000861 Mg alloy Inorganic materials 0.000 title claims abstract description 84
- 238000000576 coating method Methods 0.000 title claims abstract description 42
- 239000011248 coating agent Substances 0.000 title claims abstract description 41
- 238000005260 corrosion Methods 0.000 title claims abstract description 27
- 230000007797 corrosion Effects 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 229910001928 zirconium oxide Inorganic materials 0.000 title claims abstract description 8
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 title claims abstract description 7
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 62
- VYFYYTLLBUKUHU-UHFFFAOYSA-N dopamine Chemical compound NCCC1=CC=C(O)C(O)=C1 VYFYYTLLBUKUHU-UHFFFAOYSA-N 0.000 claims abstract description 46
- 229960003638 dopamine Drugs 0.000 claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 13
- 239000000956 alloy Substances 0.000 claims abstract description 3
- 239000007853 buffer solution Substances 0.000 claims description 20
- 239000000243 solution Substances 0.000 claims description 17
- 238000006243 chemical reaction Methods 0.000 claims description 16
- QKNYBSVHEMOAJP-UHFFFAOYSA-N 2-amino-2-(hydroxymethyl)propane-1,3-diol;hydron;chloride Chemical compound Cl.OCC(N)(CO)CO QKNYBSVHEMOAJP-UHFFFAOYSA-N 0.000 claims description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 13
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- 238000005498 polishing Methods 0.000 claims description 11
- 244000137852 Petrea volubilis Species 0.000 claims description 10
- 238000004140 cleaning Methods 0.000 claims description 7
- CTENFNNZBMHDDG-UHFFFAOYSA-N Dopamine hydrochloride Chemical compound Cl.NCCC1=CC=C(O)C(O)=C1 CTENFNNZBMHDDG-UHFFFAOYSA-N 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 229960001149 dopamine hydrochloride Drugs 0.000 claims description 6
- 239000012456 homogeneous solution Substances 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 150000002680 magnesium Chemical class 0.000 claims description 5
- 150000003754 zirconium Chemical class 0.000 claims description 5
- 238000002791 soaking Methods 0.000 claims description 4
- 238000007664 blowing Methods 0.000 claims description 3
- UJVRJBAUJYZFIX-UHFFFAOYSA-N nitric acid;oxozirconium Chemical compound [Zr]=O.O[N+]([O-])=O.O[N+]([O-])=O UJVRJBAUJYZFIX-UHFFFAOYSA-N 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims 3
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims 2
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims 2
- DUFCMRCMPHIFTR-UHFFFAOYSA-N 5-(dimethylsulfamoyl)-2-methylfuran-3-carboxylic acid Chemical compound CN(C)S(=O)(=O)C1=CC(C(O)=O)=C(C)O1 DUFCMRCMPHIFTR-UHFFFAOYSA-N 0.000 claims 1
- IPCAPQRVQMIMAN-UHFFFAOYSA-L zirconyl chloride Chemical compound Cl[Zr](Cl)=O IPCAPQRVQMIMAN-UHFFFAOYSA-L 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 2
- 238000004729 solvothermal method Methods 0.000 abstract description 2
- 239000000758 substrate Substances 0.000 abstract description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 8
- 239000011780 sodium chloride Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 229920001690 polydopamine Polymers 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- -1 zirconium oxide ions Chemical class 0.000 description 3
- 238000007605 air drying Methods 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- TVCXDNTWFYUKRE-UHFFFAOYSA-N CO.O(Cl)Cl.[Zr] Chemical compound CO.O(Cl)Cl.[Zr] TVCXDNTWFYUKRE-UHFFFAOYSA-N 0.000 description 1
- RZKSECIXORKHQS-UHFFFAOYSA-N Heptan-3-ol Chemical compound CCCCC(O)CC RZKSECIXORKHQS-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000006056 electrooxidation reaction Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 238000007745 plasma electrolytic oxidation reaction Methods 0.000 description 1
- 239000011253 protective coating Substances 0.000 description 1
- 238000009877 rendering Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
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Abstract
The invention relates to a zirconia-based corrosion-resistant and wear-resistant coating on the surface of magnesium alloy and a preparation method thereof, belonging to the technical field of magnesium alloy materials. The preparation method comprises the steps of preparing a dopamine layer on the surface of the magnesium alloy to enhance the binding force between the zirconia coating and the substrate, and then preparing the homogeneous compact zirconia coating by adopting a solvothermal method. The magnesium alloy is commercial AZ series, ZK series and WE series magnesium alloy plates and pipes. The zirconium oxide-based coating prepared by the method can simultaneously improve the corrosion resistance and the wear resistance of the surface of the magnesium alloy, and the preparation method has the advantages of simple operation, no need of special equipment, suitability for various sectional materials and the like. The method provides a new way for preparing the corrosion-resistant and wear-resistant coating on the surface of the magnesium alloy.
Description
Technical Field
The invention belongs to the technical field of magnesium alloy materials, and particularly relates to a zirconium oxide-based film layer on the surface of a magnesium alloy and a preparation method thereof.
Background
The emission reduction of vehicles such as automobiles is particularly urgent, the light weight of the automobiles can effectively reduce oil consumption and emission on the premise of ensuring the strength and the safety performance of the whole automobiles, and the method is an important technical means for the sustainable development of the automobile industry. Magnesium alloys are currently the lightest structural materials with a density of about 1.8g/cm3About 2/3 for aluminum, 1/4 for steel, 1/3 for titanium. In addition, the magnesium alloy has excellent machining performance and can be used for manufacturing parts such as engine cylinders, transmission housings, steering wheels, vehicle doors, wheel hubs and the like. However, magnesium alloys have high chemical activity, poor corrosion resistance and low hardness, and thus the application thereof is severely limited.
The surface modification technology can effectively improve the comprehensive performance of the surface of the magnesium alloy by preparing the functional coating with a specific tissue structure, so that the magnesium alloy meets the harsh requirements in practical application, and is a research hotspot for designing and preparing novel high-performance magnesium alloys based on the surface modification technology. Zirconium oxide (ZrO)2) Because of its excellent mechanical strength, chemical stability, mechanical stability and thermal stability, it has been used as a protective coating for metal materials. At present, the most effective method for preparing the zirconia-based coating on the surface of the magnesium alloy is a plasma electrolytic oxidation technology. However, the coatings produced by this method have inevitable pores and microcracks which not only affect the hardness of the coating, but also allow corrosive media to directly enter and adsorb and concentrate into these pores and undergo chemical or electrochemical corrosion, and the accumulation of corrosion products can even lead to cracking and peeling of the coating, thereby rendering the coating ineffective in preventing corrosion of the substrate in harsh corrosive environments. Therefore, the development of a simple method for preparing a dense zirconia-based coating has strong theoretical and practical significance.
Disclosure of Invention
The invention aims to solve the technical problems of poor compactness, complex equipment, high cost and the like of a zirconia coating prepared on the surface of the existing magnesium alloy, and provides a zirconia-based corrosion-resistant wear-resistant coating on the surface of the magnesium alloy and a preparation method thereof. The invention adopts the solvothermal method to directly prepare the compact zirconia-based coating on the surface of the magnesium alloy, thereby improving the corrosion resistance and the wear resistance of the magnesium alloy.
The invention discloses a zirconia-based corrosion-resistant and wear-resistant coating on the surface of a magnesium alloy, wherein the coating is of a double-layer structure, the inner layer is a dopamine film layer, the outer layer is composed of zirconia, and the total thickness of the coating is 5-22 mu m. The coating is firmly combined with the matrix, and the wear resistance and corrosion resistance of the magnesium alloy are effectively improved.
The invention discloses a preparation method of a zirconia-based corrosion-resistant and wear-resistant coating on the surface of magnesium alloy, which comprises the following preparation steps:
(1) pretreatment of magnesium alloy: polishing the magnesium alloy block with sand paper until the surface is bright, ultrasonically cleaning and drying for later use;
(2) preparation of dopamine layer: preparing a Tris-HCl buffer solution with the pH value of 8.5, and then adding a certain amount of dopamine hydrochloride to prepare a dopamine Tris-HCl buffer solution; immersing the polished and cleaned magnesium alloy block into the buffer solution for shading and soaking for a certain time to prepare a dopamine film layer;
(3) preparation of zirconia layer: preparing a zirconium salt alcohol solution with the concentration of 0.01-0.15 mol/L, adding a 0.01 mol/LNaOH solution with a certain volume, stirring for 20 minutes, transferring the obtained homogeneous solution into a reaction kettle, placing a dopamine-modified magnesium alloy block into the reaction kettle, and placing the reaction kettle into an air-blowing drying oven to keep the temperature at 80-160 ℃ for 1-6 hours; and after cooling, taking out the magnesium alloy block, washing with deionized water and drying.
The dopamine modification layer can effectively enhance the bonding strength of the zirconia coating and promote the nucleation and growth of the subsequent zirconia coating. The use of an organic alcohol solvent effectively slows the rate of hydrolysis of the zirconium salt and promotes the film formation of the zirconia due to the high binding energy with the zirconium oxide ions. The proper reaction temperature is favorable for the uniform growth of the coating.
The method of the invention fully utilizes the characteristic of high hardness of zirconia while improving the corrosion resistance of the magnesium alloy, and improves the wear resistance of the film. The preparation method has the advantages of simple operation, no need of special equipment, more environment-friendly reagent, low preparation cost and the like. The method provides a new way for preparing the corrosion-resistant and wear-resistant coating on the surface of the magnesium alloy.
Drawings
In order to make the object, technical scheme and beneficial effect of the invention more clear, the invention provides the following drawings for explanation:
FIG. 1 is an X-ray diffraction pattern of the zirconia coating of the magnesium alloy of example 2.
FIG. 2 is a scanning electron micrograph of the zirconia coating of the magnesium alloy of example 3.
Detailed Description
The present invention will be described in detail with reference to the following examples: in this embodiment, the technical solution of the present invention is used as a precondition for implementation, and a detailed implementation manner and a specific operation process are given, but the scope of the present invention is not limited to the following embodiments.
The invention provides a preparation method for preparing a zirconia-based film layer on the surface of a magnesium alloy. The invention is further described with reference to specific examples.
Example one
(1) Pretreatment of magnesium alloy: and (3) polishing the magnesium alloy block to be bright in surface by using sand paper (sequentially polishing the magnesium alloy block to be bright in surface by using 200 #, 400 #, 800# and 1000# sand paper step by step without obvious scratches), ultrasonically cleaning the magnesium alloy block for 10min by using ethanol, and drying the magnesium alloy block by using cold air for later use.
(2) Preparation of dopamine layer: Tris-HCl buffer solution with pH of 8.5 is prepared, and then a certain amount of dopamine hydrochloride is added to prepare 1mg/ml (referring to the concentration of dopamine in the dopamine Tris-HCl buffer solution, the same is carried out in the following examples) of dopamine Tris-HCl buffer solution. And (3) immersing the polished and cleaned magnesium alloy block into the buffer solution for shading and soaking for 24 hours to prepare the dopamine film layer.
(3) Preparation of zirconia layer: preparing 0.08 mol/L zirconium oxychloride isopropanol solution, adding 0.01 mol/L NaOH solution, stirring for 20 minutes, transferring the homogeneous solution into a reaction kettle, placing the reaction kettle into a blast drying oven, and preserving heat for 1 hour at 160 ℃; after cooling, the magnesium alloy block is taken out, washed by deionized water and dried for 6 hours at the temperature of 60 ℃.
The coating prepared has a thickness of 15 μm, a hardness of 86 HB and a corrosion current density of 1.367X 10 in a 3.5% sodium chloride solution at 25 DEG C-7A/cm2。
Example two
(1) Pretreatment of magnesium alloy: and (3) polishing the magnesium alloy block to be bright in surface by using sand paper (sequentially polishing the magnesium alloy block to be bright in surface by using 200 #, 400 #, 800# and 1000# sand paper step by step without obvious scratches), ultrasonically cleaning the magnesium alloy block for 10min by using ethanol, and drying the magnesium alloy block by using cold air for later use.
(2) Preparation of dopamine layer: preparing a Tris-HCl buffer solution with the pH value of 8.5, and then adding a certain amount of dopamine hydrochloride to prepare a 3mg/ml dopamine Tris-HCl buffer solution. And (3) immersing the polished and cleaned magnesium alloy block into the buffer solution for 36h in a shading manner to prepare the poly-dopamine film layer.
(3) Preparation of zirconia layer: preparing a zirconium acetate isopropanol solution with the concentration of 0.01 mol/L, adding a 0.01 mol/L NaOH solution with the volume ratio of 1:6, stirring for 20 minutes, transferring the homogeneous solution into a reaction kettle, placing a dopamine-modified magnesium alloy block, and placing the reaction kettle in a forced air drying oven to keep the temperature at 80 ℃ for 6 hours; after cooling, the magnesium alloy block is taken out, washed by deionized water and dried for 6 hours at the temperature of 60 ℃.
The coating prepared has a thickness of 5 μm, a hardness of 83 HB and a corrosion current density of 2.677X 10 at 25 ℃ in a 3.5% sodium chloride solution-7A/cm2。
EXAMPLE III
(1) Pretreatment of magnesium alloy: and (3) polishing the magnesium alloy block to be bright in surface by using sand paper (sequentially polishing the magnesium alloy block to be bright in surface by using 200 #, 400 #, 800# and 1000# sand paper step by step without obvious scratches), ultrasonically cleaning the magnesium alloy block for 10min by using ethanol, and drying the magnesium alloy block by using cold air for later use.
(2) Preparation of dopamine layer: preparing a Tris-HCl buffer solution with the pH value of 8.5, and then adding a certain amount of dopamine hydrochloride to prepare a 3mg/ml dopamine Tris-HCl buffer solution. And (3) immersing the polished and cleaned magnesium alloy block into the buffer solution for 36h in a shading manner to prepare the poly-dopamine film layer.
(3) Preparation of zirconia layer: preparing 0.15mol/L zirconium oxychloride methanol solution, adding 0.01 mol/L NaOH solution, stirring for 20 minutes, transferring the homogeneous solution into a reaction kettle, placing a dopamine-modified magnesium alloy block, and placing the reaction kettle in a forced air drying oven to keep the temperature at 140 ℃ for 4 hours; after cooling, the magnesium alloy block is taken out, washed by deionized water and dried for 6 hours at the temperature of 60 ℃.
The coating prepared has a thickness of 18 μm, a hardness of 88 HB and a corrosion current density of 1.217X 10 in a 3.5% sodium chloride solution at 25 DEG C-7A/cm2。
Example four
(1) Pretreatment of magnesium alloy: and (3) polishing the magnesium alloy block to be bright in surface by using sand paper (sequentially polishing the magnesium alloy block to be bright in surface by using 200 #, 400 #, 800# and 1000# sand paper step by step without obvious scratches), ultrasonically cleaning the magnesium alloy block for 10min by using ethanol, and drying the magnesium alloy block by using cold air for later use.
(2) Preparation of dopamine layer: preparing a Tris-HCl buffer solution with the pH value of 8.5, and then adding a certain amount of dopamine hydrochloride to prepare a 2.5mg/ml dopamine Tris-HCl buffer solution. And (3) immersing the polished and cleaned magnesium alloy block into the buffer solution for 18h in a shading manner to prepare the polydopamine film layer.
(3) Preparation of zirconia layer: preparing a zirconium oxynitrate n-butyl propanol solution with the concentration of 0.05 mol/L, adding a 0.01 mol/LNaOH solution with the volume ratio of 1:8, stirring for 20 minutes, transferring the homogeneous solution into a reaction kettle, putting a dopamine-modified magnesium alloy block into the reaction kettle, and putting the reaction kettle into an air-blowing drying oven to keep the temperature at 120 ℃ for 3 hours; after cooling, the magnesium alloy block is taken out, washed by deionized water and dried for 6 hours at the temperature of 60 ℃.
The coating prepared has a thickness of 22 μm, a hardness of 93 HB and a corrosion current density of 0.767X 10 at 25 ℃ in a 3.5% sodium chloride solution-7A/cm2。
The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the appended claims.
Claims (7)
1. A zirconia-based corrosion-resistant and wear-resistant coating on the surface of magnesium alloy is characterized in that: the coating is of a double-layer structure, the inner layer is a dopamine film layer, the outer layer is a zirconium oxide layer, and the total thickness of the coating is 5-22 mu m.
2. A preparation method of a zirconia-based corrosion and wear resistant coating on the surface of a magnesium alloy is used for preparing the zirconia-based corrosion and wear resistant coating on the surface of the magnesium alloy as claimed in claim 1, and is characterized by comprising the following preparation steps:
(1) pretreatment of magnesium alloy: polishing the magnesium alloy block with sand paper until the surface is bright, ultrasonically cleaning and drying for later use;
(2) preparing a dopamine film layer: preparing a Tris-HCl buffer solution with the pH value of 8.5, and then adding a certain amount of dopamine hydrochloride to prepare a dopamine Tris-HCl buffer solution; immersing the polished and cleaned magnesium alloy block into the buffer solution for shading and soaking for a certain time to prepare a dopamine film layer;
(3) preparation of zirconia layer: preparing a zirconium salt alcohol solution with the concentration of 0.01-0.15 mol/L, adding a 0.01 mol/LNaOH solution with a certain volume, stirring for 20 minutes, transferring the obtained homogeneous solution into a reaction kettle, placing a dopamine-modified magnesium alloy block into the reaction kettle, and placing the reaction kettle into an air-blowing drying oven to keep the temperature at 80-160 ℃ for 1-6 hours; and after cooling, taking out the magnesium alloy block, washing with deionized water and drying.
3. The preparation method of the zirconia-based corrosion-resistant and wear-resistant coating on the surface of the magnesium alloy according to claim 2, characterized in that the magnesium alloy materials used are as follows: AZ series, ZK series and WE series magnesium alloy plate and pipe.
4. The method for preparing the zirconia-based corrosion-resistant and wear-resistant coating on the surface of the magnesium alloy according to claim 2, wherein the method comprises the following steps: and (1) sequentially polishing the magnesium alloy sheet by 200 #, 400 #, 800# and 1000# sandpaper step by step until the surface is bright and has no obvious scratch, ultrasonically cleaning the magnesium alloy sheet by using ethanol for 10min, and drying the magnesium alloy sheet by cold air for later use.
5. The method for preparing the zirconia-based corrosion and wear resistant coating on the surface of the magnesium alloy as claimed in claim 2, wherein the concentration of dopamine in the dopamine Tris-HCl buffer solution in the step (2) is 1-3 mg/ml, and the soaking time is 18-36 h.
6. The method for preparing the zirconium oxide-based corrosion-resistant and wear-resistant coating on the surface of the magnesium alloy as claimed in claim 2, wherein in the step (3), the zirconium salt is one or more of zirconyl nitrate, zirconyl chloride and zirconium acetate, the organic alcohol is one of methanol, isopropanol or n-butanol, and the volume ratio of the solution of the zirconium salt and the NaOH solution is 1: 2-8.
7. The magnesium alloy with zirconia-based corrosion and wear resistant coating on the surface prepared by the preparation method of any one of claims 2 to 5.
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