CN111925705B - Laser-modified organic glass-based protective coating on surface of magnesium alloy and preparation method thereof - Google Patents
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- C09D133/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
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Abstract
The invention discloses a laser modified organic glass-based protective coating on a magnesium alloy surface and a preparation method thereof, wherein the protective coating comprises the following components of polymethyl methacrylate and silicon dioxide, the mass percent of the silicon dioxide is 10-16.8%, and the silicon dioxide is amorphous. The preparation method of the protective coating comprises the following steps: dissolving ethyl orthosilicate in water to obtain silicon dioxide sol, dissolving polymethyl methacrylate in an organic solvent, adding the silicon dioxide sol into the organic solvent, standing and aging, coating the mixture on the surface of a magnesium alloy substrate, and drying to obtain the protective coating. The protective coating can effectively improve the processing defects of surface oxidation, ablation and the like in the laser modification processing process of the magnesium alloy. Compared with the traditional inert gas protection, the method can save cost, obviously reduce the roughness of the surface of the magnesium alloy after laser processing, and has relatively simple process.
Description
Technical Field
The invention relates to an alloy surface laser modified organic glass-based protective coating and a preparation method thereof, in particular to a magnesium alloy surface laser modified organic glass-based protective coating and a preparation method thereof.
Background
The magnesium alloy has high specific strength and specific rigidity, density very close to that of human bones and good biocompatibility, so that the magnesium alloy has good application prospect in medical instruments. But the application of the magnesium alloy is limited by the low corrosion resistance and too fast degradation in human body. In order to slow down the corrosion progress of magnesium alloy, the main surface modification technologies at present are: plasma spraying, sol-gel, organic coating film coating, laser modification and the like. In laser processing, in order to prevent the material from reacting with air during high temperature processing, it is common to introduce a suitable amount of a protective gas, such as high purity N, during processing2Ar or He. In the actual processing process, the flow of the protective gas and the regulation and control of the gas flow direction should be matched with technical parameters such as laser processing power, moving speed and the like, for example: too little or too much flow may not be effective and may even result in processing failure. In addition, when gas shielding is employed, in addition to the need to protect the molten pool, it is also necessary to properly protect the just-solidified and cooled region to prevent surface oxidation from occurring due to insufficient protection.
Disclosure of Invention
The purpose of the invention is as follows: the first purpose of the invention is to provide a magnesium alloy surface laser modified organic glass-based protective coating which can effectively prevent the surface oxidation and ablation of the magnesium alloy in the laser modification process, and the second purpose of the invention is to provide a preparation method of the protective coating.
The technical scheme is as follows: the laser modified organic glass-based protective coating for the magnesium alloy surface comprises the components of polymethyl methacrylate and silicon dioxide, wherein the mass percent of the silicon dioxide is 10-16.8%, and the silicon dioxide is in an amorphous state.
The preparation method of the laser modified organic glass-based protective coating on the surface of the magnesium alloy comprises the following steps:
(1) cutting the magnesium alloy, polishing and roughening the oxide scale layer on the surface of the magnesium alloy, sequentially cleaning with acetone and water, and drying to obtain a magnesium alloy substrate;
(2) mixing ethyl orthosilicate and ethanol according to the volume ratio of 1: 0.8-1, adding the mixture into nitric acid aqueous solution with the pH value of 0.5-2, ultrasonically stirring at room temperature, and standing to obtain clear SiO2Sol;
(3) weighing 1-1.2 g of polymethyl methacrylate powder per 10ml of organic solvent, adding the polymethyl methacrylate powder into the organic solvent in an ultrasonic stirring manner, and stirring until the polymethyl methacrylate powder is completely dissolved in the organic solvent to obtain the organic solvent in which the polymethyl methacrylate is dissolved;
(4) according to the volume ratio of 1: 5-10, SiO2Mixing the sol with an organic solvent in which polymethyl methacrylate is dissolved, and ultrasonically stirring to obtain a mixed solution;
(5) and coating the mixed solution on the surface of a magnesium alloy substrate, and drying to obtain the laser modified organic glass-based protective coating on the surface of the magnesium alloy.
Further, the thickness of the magnesium alloy laser modified organic glass-based protective coating is 0.5-1.5 mm.
In the step (1), the roughening treatment is sand paper polishing or sand blasting. In the step (1), the magnesium alloy is one of Mg-Zn-Ca, Mg-Zn-Al or Mg-Mn-Al alloy.
In the step (3), the organic solvent is one or more of toluene, xylene, dichloromethane, chloroform or tetrahydrofuran.
In the step (5), the coating adopts a dip-coating method or a spin-coating method. And (5) repeating the step 2-6 times according to the requirement of the thickness of the coating.
Preferably, the thickness of the magnesium alloy laser modified organic glass-based protective coating is 1 mm.
Has the advantages that: compared with the prior art, the invention has the following remarkable advantages: the organic glass-based protective coating modified by the laser on the surface of the magnesium alloy can effectively improve the defects of surface oxidation, ablation and the like in the laser modification processing process of the magnesium alloy; compared with the traditional inert gas protection, the method can save cost and obviously reduce the roughness of the surface of the magnesium alloy after laser processing; the process is relatively simple, the organic glass-based protective coating provided by the method can uniformly and completely cover the surface of the magnesium alloy, and compared with pure organic glass, the SiO existing in the coating is used2The nano particles can not only improve the hardness of the coating by more than 2 times, but also improve the binding force between the coating and the matrix, effectively prevent the coating from being chipped off in the processing process, improve the melting point and the burning point of the coating to different degrees, and effectively prevent the coating from being addedBurning occurs during the machining process, and in addition, refocusing of the laser is not required during the laser machining process.
Drawings
Fig. 1 is a schematic representation of a laser-machined plexiglass-based protective coating of the present invention.
Detailed Description
The technical solution of the present invention is further illustrated by the following examples.
Example 1
As shown in fig. 1, 1 is a laser, 2 is a protective coating, and 3 is a magnesium alloy, the preparation method of the laser-modified organic glass-based protective coating on the surface of the magnesium alloy in this embodiment adopts the following steps:
(1) mixing magnesium alloy Mg67Zn28Ca5After cutting, sequentially polishing the oxide scale layer on the surface of the alloy by using sand paper, roughening the surface to be processed, finally sequentially cleaning the surface by using acetone and deionized water, and blow-drying for later use;
(2) mixing ethyl orthosilicate and ethanol according to the volume ratio of 1:0.8, slowly dripping into nitric acid aqueous solution with the pH value of 0.5, ultrasonically stirring for 2 hours at room temperature, standing for 8 hours to obtain clear SiO2Sol;
(3) weighing 1g of polymethyl methacrylate powder per 10ml of organic solvent, adding the polymethyl methacrylate powder into selected toluene in an ultrasonic stirring mode, and stirring until the polymethyl methacrylate powder is completely dispersed and dissolved into the toluene;
(4) according to the volume ratio of 1:10, the SiO obtained in the step (2) is mixed2Mixing the sol with the toluene dissolved with the polymethyl methacrylate obtained in the step (3), and ultrasonically stirring for 30 min;
(5) uniformly coating the solution obtained in the step (4) on Mg by adopting a dip-coating method67Zn28Ca5Magnesium alloy surface, drying in drying oven to remove toluene, coating and drying for 2 times to obtain Mg67Zn28Ca5The surface of the magnesium alloy is laser modified with an organic glass-based protective coating.
The above for Mg67Zn28Ca5The thickness of the laser modified organic glass-based protective coating on the surface of the magnesium alloy is 0.5 mm. The protective coating comprises polymethyl methacrylate (PMMA) and silicon dioxide (SiO)2) Wherein: silicon dioxide SiO2Is 10% by mass of silicon dioxide SiO2Is in an amorphous state.
The coating can effectively avoid Mg67Zn28Ca5The surface of the alloy is cracked during laser processing, and the residual tensile stress of the surface is less than 20 MPa. The content of oxygen elements (EDS energy spectrum) on the surface of the alloy after laser processing is lower than 8 percent. The surface roughness is obviously superior to the surface quality after the gas protection processing, the quality grade is improved by more than 3 grades, and the preparation cost of the coating is relatively low.
Example 2
The preparation method of the laser modified organic glass-based protective coating on the surface of the magnesium alloy provided by the embodiment comprises the following steps:
(1) cutting the AZ31 magnesium alloy, then carrying out sand blasting treatment on the oxide scale layer on the surface of the alloy in sequence, roughening the surface to be processed, finally cleaning the surface to be processed by acetone and deionized water in sequence, and blow-drying the surface for later use;
(2) mixing ethyl orthosilicate and ethanol according to the volume ratio of 1:0.9, slowly dropping into nitric acid aqueous solution with the pH value of 2, ultrasonically stirring for 2 hours at room temperature, standing for 8 hours to obtain clear SiO2Sol;
(3) weighing 1.1g of polymethyl methacrylate powder per 10ml of organic solvent, adding the polymethyl methacrylate powder into selected xylene in an ultrasonic stirring manner, and stirring until the polymethyl methacrylate powder is completely dispersed and dissolved into the xylene;
(4) according to the volume ratio of 1:5, the SiO obtained in the step (2) is mixed2Mixing the sol with the xylene dissolved with the polymethyl methacrylate obtained in the step (3), and ultrasonically stirring for 30 min;
(5) and (3) uniformly coating the solution obtained in the step (4) on the surface of the AZ31 magnesium alloy by adopting a spin coating method, placing the magnesium alloy in a drying oven for drying treatment to remove xylene, and repeating the coating and drying for 4 times to obtain the AZ31 magnesium alloy surface laser modified organic glass-based protective coating.
The thickness of the organic glass-based protective coating for the AZ31 magnesium alloy surface laser modification is 1.5 mm. The protective coating comprises polymethyl methacrylate (PMMA) and silicon dioxide (SiO)2) Wherein: silicon dioxide SiO2Is 16.8 percent, and the silicon dioxide is amorphous.
The coating can effectively prevent the surface of the AZ31 magnesium alloy from cracking during laser processing, and the residual tensile stress of the surface is less than 15 MPa. The content of oxygen elements (EDS energy spectrum) on the surface of the alloy after laser processing is lower than 8 percent. The surface roughness is obviously superior to the surface quality after the gas protection processing, the quality grade is improved by more than 3 grades, and the preparation cost of the coating is relatively low.
Example 3
The preparation method of the laser modified organic glass-based protective coating on the surface of the magnesium alloy provided by the embodiment comprises the following steps:
(1) cutting the AZ61 magnesium alloy, sequentially polishing the oxide layer on the surface of the alloy by using sand paper, roughening the surface to be processed, finally sequentially cleaning the surface by using acetone and deionized water, and blow-drying for later use;
(2) mixing ethyl orthosilicate and ethanol according to the volume ratio of 1:1, slowly dropping into nitric acid aqueous solution with the pH value of 1, ultrasonically stirring for 2 hours at room temperature, standing for 8 hours to obtain clear SiO2Sol;
(3) weighing 1.2g of polymethyl methacrylate powder per 10ml of organic solvent, adding the polymethyl methacrylate powder into selected trichloromethane in an ultrasonic stirring mode, and stirring until the polymethyl methacrylate powder is completely dispersed and dissolved in toluene;
(4) according to the volume ratio of 1:7, the SiO obtained in the step (2) is mixed2Mixing the sol with the chloroform dissolved with the polymethyl methacrylate obtained in the step (3), and ultrasonically stirring for 30 min;
(5) and (3) uniformly coating the solution obtained in the step (4) on the surface of the AZ61 magnesium alloy by adopting a dip-coating method, placing the magnesium alloy in a drying box for drying treatment to remove trichloromethane, and repeating the coating and drying for 6 times to obtain the AZ61 magnesium alloy surface laser modified organic glass-based protective coating.
The thickness of the organic glass-based protective coating for the AZ61 magnesium alloy surface laser modification is 1.5 mm. The protective coating comprises polymethyl methacrylate (PMMA) and silicon dioxide (SiO)2) Wherein: silicon dioxide SiO2Is 11.7 percent by mass, and the silicon dioxide is amorphous.
The coating can effectively prevent the surface of the AZ61 magnesium alloy from cracking during laser processing, and the residual tensile stress of the surface is less than 15 MPa. The content of oxygen elements (EDS energy spectrum) on the surface of the alloy after laser processing is lower than 8 percent. The surface roughness is obviously superior to the surface quality after the gas protection processing, the quality grade is improved by more than 3 grades, and the preparation cost of the coating is relatively low.
Example 4
The preparation method of the laser modified organic glass-based protective coating on the surface of the magnesium alloy provided by the embodiment comprises the following steps:
(1) cutting the AM60 magnesium alloy, sequentially polishing the oxide layer on the surface of the alloy by using sand paper, roughening the surface to be processed, finally, sequentially cleaning the surface by using acetone and deionized water, and blow-drying for later use;
(2) mixing ethyl orthosilicate and ethanol according to the volume ratio of 1:0.9, slowly dripping into nitric acid aqueous solution with the pH value of 1.5, ultrasonically stirring for 2 hours at room temperature, standing for 8 hours to obtain clear SiO2Sol;
(3) weighing 1.12g of polymethyl methacrylate powder per 10ml of chloroform-tetrahydrofuran mixed solution (volume ratio is 1:1), adding the polymethyl methacrylate powder into the selected dichloromethane-tetrahydrofuran mixed solution in a small amount for multiple times in an ultrasonic stirring manner, and stirring for 30min until the polymethyl methacrylate is completely dispersed and dissolved into the dichloromethane-tetrahydrofuran mixed solution;
(4) according to the volume ratio of 1:6, the SiO obtained in the step (2) is mixed2Sol and the aboveThe mixed solution of the trichloromethane and the tetrahydrofuran dissolved with the polymethyl methacrylate obtained in the step (3) is stirred for 30min by ultrasonic;
(5) and (3) uniformly coating the solution obtained in the step (4) on the surface of the AM60 magnesium alloy by adopting a spin coating method, placing the AM60 magnesium alloy in a drying oven for drying treatment to remove trichloromethane and tetrahydrofuran, and repeating the coating and drying for 3 times to obtain the AM60 magnesium alloy surface laser modified organic glass-based protective coating.
The thickness of the organic glass-based protective coating for the AM60 magnesium alloy surface laser modification is 1 mm. The protective coating comprises polymethyl methacrylate (PMMA) and silicon dioxide (SiO)2) Wherein: silicon dioxide SiO2Is 14.2 percent by mass, and the silicon dioxide is amorphous.
The coating can effectively avoid surface cracks of the AM60 magnesium alloy during laser processing, and the residual tensile stress of the surface is less than 15 MPa. The content of oxygen elements (EDS energy spectrum) on the surface of the alloy after laser processing is lower than 8 percent. The surface roughness is obviously superior to the surface quality after the gas protection processing, the quality grade is improved by more than 3 grades, and the preparation cost of the coating is relatively low.
Claims (7)
1. A preparation method of a laser modified organic glass-based protective coating on the surface of magnesium alloy is characterized by comprising the following steps: the protective coating comprises polymethyl methacrylate and silicon dioxide, the mass percent of the silicon dioxide is 10-16.8%, the silicon dioxide is amorphous, and the protective coating comprises the following steps:
(1) cutting the magnesium alloy, polishing and roughening the oxide scale layer on the surface of the magnesium alloy, sequentially cleaning with acetone and water, and drying to obtain a magnesium alloy substrate;
(2) mixing ethyl orthosilicate and ethanol according to the volume ratio of 1: 0.8-1, adding the mixture into nitric acid aqueous solution with the pH value of 0.5-2, ultrasonically stirring at room temperature, and standing to obtain clear SiO2Sol;
(3) weighing 1-1.2 g of polymethyl methacrylate powder per 10ml of organic solvent, adding the polymethyl methacrylate powder into the organic solvent in an ultrasonic stirring manner, and stirring until the polymethyl methacrylate powder is completely dissolved in the organic solvent to obtain the organic solvent in which the polymethyl methacrylate is dissolved;
(4) according to the volume ratio of 1: 5-10, the SiO is mixed2Mixing the sol with an organic solvent in which polymethyl methacrylate is dissolved, and ultrasonically stirring to obtain a mixed solution;
(5) and coating the mixed solution on the surface of a magnesium alloy substrate, and drying to obtain the laser modified organic glass-based protective coating on the surface of the magnesium alloy.
2. The preparation method of the laser modified organic glass-based protective coating on the surface of the magnesium alloy according to claim 1, which is characterized in that: the thickness of the magnesium alloy laser modified organic glass-based protective coating is 0.5-1.5 mm.
3. The preparation method of the laser modified organic glass-based protective coating on the surface of the magnesium alloy according to claim 1, which is characterized in that: in the step (1), the roughening treatment is sand paper polishing or sand blasting.
4. The preparation method of the laser modified organic glass-based protective coating on the surface of the magnesium alloy according to claim 1, which is characterized in that: in the step (1), the magnesium alloy is one of Mg-Zn-Ca, Mg-Zn-Al or Mg-Mn-Al alloy.
5. The preparation method of the laser modified organic glass-based protective coating on the surface of the magnesium alloy according to claim 1, which is characterized in that: in the step (3), the organic solvent is one or more of toluene, xylene, dichloromethane, chloroform or tetrahydrofuran.
6. The preparation method of the laser modified organic glass-based protective coating on the surface of the magnesium alloy according to claim 1, which is characterized in that: in the step (5), the coating adopts a dip-coating method or a spin-coating method.
7. The preparation method of the laser modified organic glass-based protective coating on the surface of the magnesium alloy according to claim 1, which is characterized in that: and (5) repeating the step 2-6 times according to the requirement of the thickness of the coating.
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| JPS6199679A (en) * | 1984-10-19 | 1986-05-17 | Nisshin Steel Co Ltd | Organic coating hot-dipped aluminum coated steel sheet |
| CN105418820A (en) * | 2015-12-23 | 2016-03-23 | 华南理工大学 | Hydroxyl-containing styrene-acrylate copolymer/SiO2 hybrid emulsion, preparation method and application thereof |
| CN105862014A (en) * | 2016-04-25 | 2016-08-17 | 太原理工大学 | Method for preparing modified polymethyl methacrylate anticorrosive coating on magnesium alloy surface |
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