CN111004952B - High-performance magnesium alloy material coated with high-molecular polymer layer and preparation method thereof - Google Patents
High-performance magnesium alloy material coated with high-molecular polymer layer and preparation method thereof Download PDFInfo
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- CN111004952B CN111004952B CN201911401185.6A CN201911401185A CN111004952B CN 111004952 B CN111004952 B CN 111004952B CN 201911401185 A CN201911401185 A CN 201911401185A CN 111004952 B CN111004952 B CN 111004952B
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C23/00—Alloys based on magnesium
- C22C23/06—Alloys based on magnesium with a rare earth metal as the next major constituent
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
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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
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Abstract
The invention discloses a high-performance magnesium alloy material coated with a high polymer layer, which is characterized in that: the magnesium alloy material comprises a magnesium alloy substrate and a high polymer layer covering the surface of the substrate; the magnesium alloy substrate material comprises the following components in percentage by weight: RE: 1.5-3.0%, Zn: 0.5-1.5%, Ni: 1.0-2.5%, Zr: 0.5-0.8%, Be: 0.1 to 0.3 percent, and the balance of Mg and inevitable impurities; wherein RE is more than one of La, Ce, Tb, Ho and Lu; the high molecular polymer layer is a polymer immobilized high molecular material layer. The magnesium alloy material has excellent mechanical property, the surface film layer has strong adhesive force, the magnesium alloy material is not easy to fall off, and the corrosion resistance is obviously improved.
Description
Technical Field
The invention relates to the field of materials, in particular to a high-performance magnesium alloy material coated with a high-molecular polymer film and a preparation method thereof.
Background
The magnesium alloy is the lightest metal structure material, has small density, high specific strength and specific stiffness, good castability and machinability, and wide application prospect in the fields of automobiles, aerospace, national defense, military and the like, but has the defects of low mechanical property and poor corrosion resistance, so that the application of the magnesium alloy is greatly limited.
The Chinese patent document CN110564996A discloses a high-strength magnesium alloy material and a preparation method thereof, wherein the magnesium alloy comprises the following components: lu: 2.0-3.5 wt%, Ni: 0.8-1.5 wt%, Ca: 0.1-0.5 wt% and the balance of Mg, adding Lu, Ni and Ca alloying elements with specific proportion into the magnesium alloy, and preparing a high-strength magnesium alloy material by a casting and extrusion process, wherein the tensile strength of the magnesium alloy is up to 320-290 MPa, the yield strength is up to 260-290MPa, and the elongation is more than 8%, but the material is poor in corrosion resistance.
Chinese patent document CN109487214A discloses a method for coating a magnesium alloy surface and a corrosion-resistant magnesium alloy prepared by the method, wherein the coating method comprises the following steps: pretreating a magnesium alloy base material; sputtering and depositing metal on the surface of the pretreated magnesium alloy substrateA film; sputtering deposition of Si on the surface of a magnesium alloy substrate on which a metal film is deposited3N4Film formed by plating metal and Si on the surface of magnesium alloy3N4The film improves the corrosion resistance of the magnesium alloy, and the coating layer of the material has the problems of easy falling, easy loss of action materials and low film adhesion, thereby causing the reduction of the corrosion resistance.
Disclosure of Invention
The invention aims to provide a high-performance magnesium alloy material coated with a high-molecular polymer film and a preparation method thereof, aiming at the defects of the prior art.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a high-performance magnesium alloy material coated with a high polymer layer comprises a magnesium alloy substrate and the high polymer layer covering the surface of the substrate;
the magnesium alloy substrate material comprises the following components in percentage by weight: RE: 1.5-3.0%, Zn: 0.5-1.5%, Ni: 1.0-2.5%, Zr: 0.5-0.8%, Be: 0.1 to 0.3 percent, and the balance of Mg and inevitable impurities; wherein RE is more than one of La, Ce, Tb, Ho and Lu;
the high molecular polymer layer is a polymer immobilized high molecular material layer.
Further, the thickness of the high polymer layer is 1-15 mm.
Further, the polymer-immobilized polymer material layer is used for immobilizing a polymer material by utilizing a molecular imprinting technology and coating the polymer material on the surface of the magnesium alloy substrate.
Further, the polymer material is any one of phenolic resin, acrylate, epoxy resin and polyurethane resin.
A preparation method of a high-performance magnesium alloy material coated with a high polymer layer comprises the following preparation steps:
1) preparation of magnesium alloy substrate: under the action of protective gas, adding the components weighed according to the weight percentage into a melting furnace, heating to 700-plus-800 ℃, after the components are melted, slagging off, standing, cooling to 650-plus-700 ℃, and casting and forming to obtain the cast magnesium alloy substrate.
2) Preparation of molecular imprinting immobilized high molecular polymer: the molecular imprinting technology is utilized to immobilize the high molecular material,
a. adding the high polymer material, the functional monomer, the cross-linking agent and the initiator into the solution, adjusting the pH value by using an acid solution, uniformly stirring after adjustment, and standing for 24-36h in a dark state.
b. The functional monomer and the cross-linking agent are polymerized around the high molecular material to form the high cross-linked polymer by photo-initiation polymerization.
c. And (3) washing the mixture to be neutral by using an alkaline solution and deionized water, leaching the mixture by using absolute ethyl alcohol, and drying the mixture at a low temperature to obtain the molecularly imprinted immobilized high molecular polymer.
3) Coating the molecular imprinting immobilized high molecular polymer prepared in the step 2 on the magnesium alloy substrate prepared in the step 1, wherein the steps comprise:
a. pretreating the magnesium alloy substrate prepared in the step 1: polishing the magnesium alloy substrate to increase the surface roughness of the magnesium alloy substrate, cleaning the polished magnesium alloy substrate, and removing gas adsorption on the surface of the magnesium alloy substrate by using an ion source;
b. placing the pretreated magnesium alloy substrate in a vacuum environment, and spraying the functional monomer in the step 2a on the surface of the magnesium alloy substrate;
c. and (3) spraying the molecular imprinting immobilized high molecular polymer prepared in the step (2) on the surface of the magnesium alloy substrate sprayed with the functional monomer to realize secondary polymerization and form a high molecular polymer layer.
Further, the functional monomer is at least one of aniline, phenol, benzaldehyde, MMA, AM, TRIM, DVB and PETRA, and is used for generating a polymer through polymerization reaction and generating a compound with the high polymer material.
Further, the cross-linking agent is at least one of EDMA and divinylbenzene, so that the high polymer material and the functional monomer are cross-linked into a whole.
Further, the initiator is at least one of AIBN and ADVN for facilitating the reaction to occur.
Further, the thickness of the functional monomer sprayed on the surface of the magnesium alloy substrate is 1-10 mm.
Further, the coating method is one of a spray coating method, a dip coating method, an electrochemical deposition method, and a plasma surface technique.
Compared with the prior art, the invention has the beneficial effects that:
1. the macromolecular polymer layer provided by the invention is used for immobilizing the macromolecular material on the polymer through a molecular imprinting technology without elution, so that the immobilization capacity of the macromolecular material is increased, the action material is not easy to run off, and the corrosion resistance of the magnesium alloy is improved.
2. According to the invention, through pretreatment of the magnesium alloy substrate material, the functional monomer is sprayed on the surface of the magnesium alloy substrate material, and the prepared molecular imprinting immobilized high molecular polymer is sprayed on the treated magnesium alloy substrate by using a plasma surface technology, so that the molecular imprinting immobilized high molecular polymer and the functional monomer on the substrate are subjected to secondary polymerization, the adhesive force of the molecular imprinting immobilized high molecular polymer on the magnesium alloy substrate is increased, the molecular imprinting immobilized high molecular polymer is not easy to fall off on the surface of the magnesium alloy, and the corrosion resistance of the magnesium alloy is further improved.
3. The magnesium alloy material with sufficient strength is obtained by optimizing the component proportion of each component, the tensile strength of the magnesium alloy material is as high as 330-350MPa, the yield strength is greater than 290MPa, the elongation is greater than 15%, and the magnesium alloy material has excellent mechanical properties and can be used in various fields of automobiles, aviation and the like.
Drawings
Fig. 1 is a comparative line graph of tensile strength of the magnesium alloy materials of examples.
Fig. 2 is a comparative line graph of yield strengths of the magnesium alloy materials of the examples.
Fig. 3 is a comparative line graph of elongation of the magnesium alloy material of the example.
Fig. 4 is a comparative line graph of corrosion areas of the magnesium alloy materials of the examples.
Fig. 5 is a comparative line graph of the area of exfoliation of the magnesium alloy materials of the examples.
Detailed Description
The present invention will be further described with reference to the following examples.
The preparation methods of the following examples were all prepared using the same method, namely:
1) preparation of magnesium alloy substrate: under the action of protective gas, adding the components weighed according to the weight percentage into a melting furnace, heating to 780 ℃, slagging off after the components are melted, standing, cooling to 650 ℃, and casting to obtain the as-cast magnesium alloy substrate.
2) Preparation of molecular imprinting immobilized high molecular polymer: the molecular imprinting technology is utilized to immobilize the high molecular material,
a. adding the high polymer material, MMA, EDMA and AIBN into the solution, adjusting the pH value by using an acid solution, uniformly stirring after adjustment, and standing for 24 hours in a dark state.
b. MMA and EDMA are polymerized around the polymer material by photo-initiation to form a highly crosslinked polymer.
c. And (3) washing the mixture to be neutral by using an alkaline solution and deionized water, leaching the mixture by using absolute ethyl alcohol, and drying the mixture at a low temperature to obtain the molecularly imprinted immobilized high molecular polymer.
3) Coating the molecular imprinting immobilized high molecular polymer prepared in the step 2 on the magnesium alloy substrate prepared in the step 1, wherein the steps comprise:
a. pretreating the magnesium alloy substrate prepared in the step 1: polishing the magnesium alloy substrate to increase the surface roughness of the magnesium alloy substrate, cleaning the polished magnesium alloy substrate, and removing gas adsorption on the surface of the magnesium alloy substrate by using an ion source;
b. placing the pretreated magnesium alloy substrate in a vacuum environment, and spraying MMA on the surface of the magnesium alloy substrate, wherein the thickness of the MMA is 1 mm;
c. and (3) spraying the molecular imprinting immobilized high molecular polymer prepared in the step (2) on the surface of the magnesium alloy substrate sprayed with the functional monomer by using a plasma surface technology to realize secondary polymerization and form a high molecular polymer layer.
It should be understood that the polymer material, the functional monomer, the cross-linking agent, and the initiator in this embodiment can be purchased directly from the market, and the plasma surface technology is also the prior art and will not be described herein.
Example 1
The high-performance magnesium alloy material coated with the high polymer layer comprises the following components in percentage by weight: lu: 1.5%, Zn: 0.5%, Ni: 1.0%, Zr: 0.5%, Be: 0.1%, the balance being Mg and unavoidable impurities;
the polymer immobilized polymer material layer is a molecular imprinting immobilized epoxy resin layer and has a thickness of 4 um.
Example 2
The high-performance magnesium alloy material coated with the high polymer layer comprises the following components in percentage by weight: lu: 2.2%, Zn: 0.8%, Ni: 1.7%, Zr: 0.6%, Be: 0.15%, the balance being Mg and unavoidable impurities;
the polymer immobilized polymer material layer is a molecular imprinting immobilized epoxy resin layer and has a thickness of 4 um.
Example 3
The high-performance magnesium alloy material coated with the high polymer layer comprises the following components in percentage by weight: lu: 3.0%, Zn: 1.5%, Ni: 2.5%, Zr: 0.8%, Be: 0.3%, the balance being Mg and unavoidable impurities;
the polymer immobilized polymer material layer is a molecular imprinting immobilized epoxy resin layer and has a thickness of 4 um.
Example 4
The high-performance magnesium alloy material coated with the high polymer layer comprises the following components in percentage by weight: lu: 2.2%, Zn: 0.8%, Ni: 1.7%, Zr: 0.6%, Be: 0.15%, the balance being Mg and unavoidable impurities;
the polymer immobilized polymer material layer is a molecular imprinting immobilized polyurethane resin layer and has a thickness of 4 um.
Example 5
The high-performance magnesium alloy material coated with the high polymer layer comprises the following components in percentage by weight: lu: 2.2%, Zn: 0.8%, Ni: 1.7%, Zr: 0.6%, Be: 0.15%, the balance being Mg and unavoidable impurities;
the polymer immobilized polymer material layer is a molecular imprinting immobilized phenolic resin layer and has a thickness of 4 um.
Comparative example 1
The magnesium alloy substrate material is prepared according to the embodiment 5 in the high-strength magnesium alloy material and the preparation method thereof disclosed in Chinese patent document CN 110564996A;
the polymer immobilized polymer material layer is a molecular imprinting immobilized epoxy resin layer and has a thickness of 4 um.
Comparative example 2
The high-performance magnesium alloy material coated with the high polymer layer comprises the following components in percentage by weight: lu: 2.2%, Zn: 0.8%, Ni: 1.7%, Zr: 0.6%, Be: 0.15%, the balance being Mg and unavoidable impurities;
the coating layer is prepared and sprayed according to the magnesium alloy surface coating method disclosed in Chinese patent document CN109487214A and the example 1 in the corrosion-resistant magnesium alloy prepared by the method.
And (3) performance testing:
the mechanical property test and the neutral salt spray test are carried out on the magnesium alloy materials of the examples 1 to 5 and the comparative examples 1 to 2, wherein the neutral salt spray test is to place the prepared magnesium alloy material in a salt spray test box for one month and observe the corrosion area and the shedding area, and the area value is about; the test results were as follows:
| tensile strength/MPa | Yield strength/MPa | Elongation/percent | Area of corrosion/%) | Area of abscission/%) | |
| Example 1 | 337 | 295 | 16.2 | 4 | 2 |
| Example 2 | 348 | 296 | 17.0 | 6 | 3 |
| Example 3 | 330 | 291 | 15.4 | 5 | 3 |
| Example 4 | 345 | 297 | 17.2 | 5 | 2 |
| Example 5 | 350 | 300 | 16.8 | 8 | 5 |
| Comparative example 1 | 325 | 254 | 13.0 | 10 | 8 |
| Comparative example 2 | 348 | 297 | 17.0 | 20 | 15 |
The results show that the polymer immobilized polymer material layer increases the attaching capacity of the polymer material, so that the polymer material layer is not easy to fall off on the surface of the magnesium alloy, the acting material is not easy to lose, and the corrosion resistance of the magnesium alloy is greatly improved; the magnesium alloy material has better mechanical property.
Although the present invention has been described with reference to the preferred embodiments, it is not intended to be limited thereto. Those skilled in the art can make various changes and modifications without departing from the spirit and scope of the invention. Therefore, the protection scope of the present invention should be determined by the appended claims.
Claims (8)
1. A high-performance magnesium alloy material coated with a high polymer layer is characterized in that: the magnesium alloy material comprises a magnesium alloy substrate and a high polymer layer covering the surface of the substrate;
the magnesium alloy substrate material comprises the following components in percentage by weight: RE: 1.5-3.0%, Zn: 0.5-1.5%, Ni: 1.0-2.5%, Zr: 0.5-0.8%, Be: 0.1 to 0.3 percent, and the balance of Mg and inevitable impurities; wherein RE is more than one of La, Ce, Tb, Ho and Lu;
the polymer layer is a polymer-immobilized polymer material layer, the polymer-immobilized polymer material layer is prepared by immobilizing a polymer material on a polymer without elution by using a molecular imprinting technology and coating the polymer material on the surface of the magnesium alloy substrate, and the polymer material is any one of phenolic resin, acrylate, epoxy resin and polyurethane resin.
2. The high-performance magnesium alloy material coated with a high molecular polymer layer according to claim 1, characterized in that: the thickness of the high polymer layer is 1-15 mm.
3. A method for preparing a high-performance magnesium alloy material coated with a high molecular polymer layer according to any one of claims 1 to 2, characterized by comprising the steps of:
1) preparation of magnesium alloy substrate: under the action of protective gas, adding the components weighed according to the weight percentage into a melting furnace, heating to 700-plus-800 ℃, after the components are melted, slagging off, standing, cooling to 650-plus-700 ℃, and casting and forming to obtain an as-cast magnesium alloy substrate;
2) preparation of molecular imprinting immobilized high molecular polymer: immobilizing the high molecular material by utilizing a molecular imprinting technology;
a. adding the high polymer material, the functional monomer, the cross-linking agent and the initiator into the solution, adjusting the pH value by using an acid solution, uniformly stirring after adjustment, and standing for 24-36h in a dark state;
b. carrying out polymerization reaction by photo-initiation to enable the functional monomer and the cross-linking agent to be polymerized around the high molecular material to form a high cross-linked polymer;
c. washing the mixture to be neutral by using an alkaline solution and deionized water, leaching the mixture by using absolute ethyl alcohol, and drying the mixture at a low temperature to obtain the molecularly imprinted immobilized high molecular polymer;
3) coating the molecular imprinting immobilized high molecular polymer prepared in the step 2 on the magnesium alloy substrate prepared in the step 1, wherein the steps comprise:
a. pretreating the magnesium alloy substrate prepared in the step 1: polishing the magnesium alloy substrate to increase the surface roughness of the magnesium alloy substrate, cleaning the polished magnesium alloy substrate, and removing gas adsorption on the surface of the magnesium alloy substrate by using an ion source;
b. placing the pretreated magnesium alloy substrate in a vacuum environment, and spraying the functional monomer in the step 2a on the surface of the magnesium alloy substrate;
c. and (3) spraying the molecular imprinting immobilized high molecular polymer prepared in the step (2) on the surface of the magnesium alloy substrate sprayed with the functional monomer to realize secondary polymerization and form a high molecular polymer layer.
4. The method for producing a high-performance magnesium alloy material coated with a high-molecular polymer layer according to claim 3, characterized in that: the functional monomer is at least one of aniline, phenol, benzaldehyde, MMA, AM, TRIM, DVB and PETRA.
5. The method for producing a high-performance magnesium alloy material coated with a high-molecular polymer layer according to claim 3, characterized in that: the crosslinking agent is at least one of EDMA and divinylbenzene.
6. The method for producing a high-performance magnesium alloy material coated with a high-molecular polymer layer according to claim 3, characterized in that: the initiator is at least one of AIBN and ADVN.
7. The method for producing a high-performance magnesium alloy material coated with a high-molecular polymer layer according to claim 3, characterized in that: the thickness of the functional monomer sprayed on the surface of the magnesium alloy substrate is 1-10 mm.
8. The method for producing a high-performance magnesium alloy material coated with a high-molecular polymer layer according to claim 3, characterized in that: the coating method is one of a spray coating method, a dip coating method, an electrochemical deposition method and a plasma surface technology.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104487496A (en) * | 2012-04-13 | 2015-04-01 | 布鲁塞尔私立大学 | Materials coated with calixarenes |
| CN107532249A (en) * | 2015-04-08 | 2018-01-02 | 宝山钢铁股份有限公司 | Formable magnesium-based wrought alloy |
| CN108441658A (en) * | 2018-03-05 | 2018-08-24 | 北京易联结科技发展有限公司 | A kind of high-strength magnesium alloy and preparation method thereof with medium fast reaction |
| JP3220760U (en) * | 2018-11-30 | 2019-04-04 | 株式会社ショウエイ | Anti-friction sheet |
| CN110064072A (en) * | 2019-04-18 | 2019-07-30 | 上海交通大学医学院附属第九人民医院 | A kind of magnesium alloy bracket and preparation method thereof for eye socket bone defect healing |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104487496A (en) * | 2012-04-13 | 2015-04-01 | 布鲁塞尔私立大学 | Materials coated with calixarenes |
| CN107532249A (en) * | 2015-04-08 | 2018-01-02 | 宝山钢铁股份有限公司 | Formable magnesium-based wrought alloy |
| CN108441658A (en) * | 2018-03-05 | 2018-08-24 | 北京易联结科技发展有限公司 | A kind of high-strength magnesium alloy and preparation method thereof with medium fast reaction |
| JP3220760U (en) * | 2018-11-30 | 2019-04-04 | 株式会社ショウエイ | Anti-friction sheet |
| CN110064072A (en) * | 2019-04-18 | 2019-07-30 | 上海交通大学医学院附属第九人民医院 | A kind of magnesium alloy bracket and preparation method thereof for eye socket bone defect healing |
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