CN111020672A - Micro-arc oxidation process for Mg-Gd-Y magnesium alloy - Google Patents
Micro-arc oxidation process for Mg-Gd-Y magnesium alloy Download PDFInfo
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- C22C23/06—Alloys based on magnesium with a rare earth metal as the next major constituent
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- C25D11/30—Anodisation of magnesium or alloys based thereon
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Abstract
The invention relates to a micro-arc oxidation process of Mg-Gd-Y magnesium alloy, which comprises the following steps: s1, processing and forming the Mg-Gd-Y magnesium alloy according to a design pattern to obtain a workpiece to be oxidized; s2, preparing a micro-arc oxidation pretreatment solution; s3, preparing a micro-arc oxidation electrolytic aqueous solution; s4, placing the workpiece to be oxidized obtained in the step S1 in a pretreatment liquid; s5, taking the workpiece to be oxidized out of the pretreatment liquid, placing the workpiece to be oxidized in a first deionized water tank for washing, taking the workpiece out, placing the workpiece in a second deionized water tank for continuous washing, taking the workpiece out of the second deionized water tank, and placing the workpiece in a drying oven for drying; and S6, using the treated workpiece to be oxidized as an anode and a stainless steel plate as a cathode, and carrying out micro-arc oxidation treatment in a micro-arc oxidation electrolytic aqueous solution to obtain the oxidized workpiece. By adjusting the formula of the micro-arc oxidation electrolyte, two components of yttrium nitrate and ethylene diamine tetraacetic acid are added into the additive, so that a compact micro-arc oxidation film layer is stably formed on the surface of the Mg-Gd-Y magnesium alloy, and the corrosion resistance of the Mg-Gd-Y-Zr cast magnesium alloy is improved.
Description
Technical Field
The invention relates to the field of Mg-Gd-Y magnesium alloy surface treatment processes, in particular to a micro-arc oxidation process for Mg-Gd-Y magnesium alloy.
Background
The magnesium alloy is a light alloy, has the advantages of high specific strength, high specific rigidity, good heat conduction and electric conductivity, good electromagnetic shielding performance, damping and vibration reduction performance, easy cutting processing, low processing cost and the like, and has wide application prospect in the fields of aerospace, automobiles, electronic products and the like. When various electronic equipment chassis structural materials are used, the working temperature of the magnesium alloy is increased rapidly due to radiation and absorption of a large amount of heat in the environment. The mechanical property of the magnesium alloy material is extremely sensitive to temperature, and in order to prevent the magnesium alloy material from losing efficacy due to overhigh temperature, the Mg-Gd-Y series magnesium alloy with relatively good heat resistance is required to be selected. However, the corrosion resistance of Mg-Gd-Y-Zr magnesium alloy is rather poor, and the surface treatment is necessary to further expand the application scene and range of the high-strength casting rare earth magnesium alloy. The micro-arc oxidation technology is a new surface treatment technology, a film layer obtained by the magnesium alloy through a micro-arc oxidation process method is tightly combined with a substrate, is an in-situ growth film layer, is thick, can greatly improve the corrosion resistance of the magnesium alloy, and is simple to operate and pollution-free in the micro-arc oxidation process.
The components of the common wrought magnesium alloy are greatly different from those of the Mg-Gd-Y magnesium alloy, so that the formula and the process of micro-arc oxidation of the Mg-Gd-Y magnesium alloy are also different. Particularly, the prior micro-arc oxidation process is used for Mg-Gd-Y magnesium alloy workpieces with complex shapes, and the surface of the workpieces can not stably form a compact micro-arc oxidation film layer, which is often accompanied by defects.
Disclosure of Invention
The invention provides a micro-arc oxidation process for Mg-Gd-Y magnesium alloy to overcome the defects of the prior art, and the compact micro-arc oxidation film layer is stably formed on the surface of the Mg-Gd-Y magnesium alloy by adjusting the formula of a micro-arc oxidation electrolyte.
The invention provides a micro-arc oxidation process of Mg-Gd-Y magnesium alloy, which comprises the following steps:
s1, processing and forming the Mg-Gd-Y magnesium alloy according to a design pattern to obtain a workpiece to be oxidized;
s2, preparing a micro-arc oxidation pretreatment solution: the mass concentration of the sodium hydroxide aqueous solution is 50g/L-100 g/L;
s3, preparing a micro-arc oxidation electrolytic aqueous solution: wherein the solute comprises
Film-forming agent: sodium silicate with the mass concentration of 10g/L-20 g/L;
auxiliary agents: potassium fluoride with the mass concentration of 10g/L-15 g/L; sodium hexametaphosphate with the mass concentration of 10g/L-15 g/L; potassium hydroxide with the mass concentration of 10g/L-15 g/L;
additive: glycerol with the mass concentration of 10ml/L-15 ml/L; yttrium nitrate with the mass concentration of 1g/L-6 g/L; disodium ethylene diamine tetraacetate with the mass concentration of 1g/L-5 g/L;
s4, placing the workpiece to be oxidized obtained in the step S1 in pretreatment liquid, wherein the temperature of the pretreatment liquid is 60-80 ℃, and the placing time is 20-30 min;
s5, taking the workpiece to be oxidized from the pretreatment liquid, placing the workpiece in a first deionized water tank for washing for 1-2min, taking out the workpiece, placing the workpiece in a second deionized water tank for washing for 1-2min, taking out the workpiece from the second deionized water tank, placing the workpiece in an oven for drying, wherein the drying temperature is preferably 50-60 ℃, and the drying time is preferably 10-15 min;
s6, using the workpiece to be oxidized processed in the step S5 as an anode, using a metal material as a cathode, adjusting the positive voltage to 400-V and the negative voltage to 0V in a constant voltage mode, and performing micro-arc oxidation treatment in the micro-arc oxidation electrolyte aqueous solution prepared in the step S3, preferably controlling the temperature of the micro-arc oxidation electrolyte aqueous solution not to be higher than 40 ℃ to obtain the oxidized workpiece.
Further, also includes
And S7, placing the oxidized workpiece obtained in the step S6 in a third deionized water tank for washing for 1-2min, taking out and drying to obtain the compact and stable micro-arc oxidation layer Mg-Gd-Y series magnesium alloy oxidized workpiece.
Preferably, the Mg-Gd-Y magnesium alloy in the S1 step has a composition of, by mass, Gd: 8.50-9.50%, Y: 3.0-4.0%, Zr: 0.40-0.60%, and the balance of Mg and non-removable impurity elements.
Preferably, in the step S6, the positive voltage is adjusted to 350V in a constant voltage mode.
Optionally, the adjuvants in step S6: potassium fluoride with the mass concentration of 10g/L-15 g/L; sodium hexametaphosphate with the mass concentration of 10g/L-15 g/L;
specifically, the pretreatment liquid in step S4 may be heated by conventional heating methods in the prior art, such as heat medium heating, electric heating, microwave heating, and the like, and preferably by heating methods with good heating speed and temperature controllability, such as hot water and hot oil heating.
Specifically, the time of the micro-arc oxidation treatment in the step S6 is 5-20min, preferably 10-20 min.
Specifically, the temperature of the aqueous electrolyte solution subjected to micro-arc oxidation treatment in the step S6 is not higher than 40 ℃, a heating mode with good heating speed and temperature controllability is adopted, such as hot water and hot oil heating, and a temperature controller is used for controlling the heating mode.
Optionally, the stainless steel in the step of S6 is used as a cathode.
Specifically, in the step S7, the drying temperature of the oxidized workpiece after being taken out is 50-60 ℃, and the drying time is 10-50min, preferably 15-25 min.
The invention relates to a micro-arc oxidation process of Mg-Gd-Y magnesium alloy, which is mainly characterized in that:
1. by adjusting the formula of the micro-arc oxidation electrolyte, two components of yttrium nitrate and ethylene diamine tetraacetic acid are added into the additive, so that a compact micro-arc oxidation film layer is stably formed on the surface of the Mg-Gd-Y magnesium alloy, and the corrosion resistance of the Mg-Gd-Y-Zr cast magnesium alloy is improved;
2. the production efficiency is high, and the operation is convenient;
3. the micro-crack defects generated on the surface of the oxidized workpiece after micro-arc oxidation are less, and the product quality is stable after long-term production.
Drawings
FIG. 1 is a diagram illustrating an oxidized workpiece with a micro-arc oxidation layer having a dense, stable, uniform and consistent surface obtained in example 1;
FIG. 2 shows a micro-arc oxidized work piece with a defective surface obtained by a comparative example.
Among them, 1-defect.
Detailed Description
The raw materials adopted by all the embodiments of the invention are commercially available, the brand is a domestic brand, and the analysis is pure.
Example 1:
a micro-arc oxidation process for Mg-Gd-Y magnesium alloy comprises the following steps:
s1, processing and forming the Mg-Gd-Y magnesium alloy according to a design pattern to obtain a workpiece to be oxidized; the Mg-Gd-Y magnesium alloy comprises the following components in percentage by mass: 9.00%, Y: 3.50%, Zr: 0.50% of Mg and the balance of non-removable impurity elements;
s2, preparing a micro-arc oxidation pretreatment solution: the mass concentration of the sodium hydroxide aqueous solution is 75 g/L;
s3, preparing a micro-arc oxidation electrolytic aqueous solution: wherein the solute comprises
Film-forming agent: sodium silicate with the mass concentration of 15 g/L;
auxiliary agents: potassium fluoride with the mass concentration of 12.5 g/L; sodium hexametaphosphate with the mass concentration of 12.5 g/L; potassium hydroxide with the mass concentration of 12.5 g/L;
additive: glycerol with the mass concentration of 12.5 ml/L; yttrium nitrate with the mass concentration of 3.5 g/L; disodium ethylene diamine tetraacetate with the mass concentration of 3 g/L;
s4, placing the workpiece to be oxidized obtained in the step S1 in pretreatment liquid, wherein the temperature of the pretreatment liquid is 70 ℃, and the placing time is 25 min;
s5, taking the workpiece to be oxidized out of the pretreatment liquid, placing the workpiece in a first deionized water tank for washing for 1.5min, taking out the workpiece, placing the workpiece in a second deionized water tank for further washing for 1.5min, taking out the workpiece from the second deionized water tank, placing the workpiece in an oven for drying, wherein the drying temperature is preferably 55 ℃, and the drying time is preferably 12.5 min;
s6, using the workpiece to be oxidized processed in the step S5 as an anode, using a stainless steel plate as a cathode, adjusting the positive voltage to 350V and the negative voltage to 0V in a constant voltage mode, and performing micro-arc oxidation treatment in the micro-arc oxidation electrolyte solution prepared in the step S3, preferably controlling the temperature of the micro-arc oxidation electrolyte solution to be not higher than 40 ℃ to obtain the oxidized workpiece.
S7, placing the oxidized workpiece obtained in the step S6 in a third deionized water tank for washing for 1.5min, taking out and drying to finally obtain the compact and stable micro-arc oxidation layer Mg-Gd-Y series magnesium alloy oxidized workpiece. As shown in fig. 1.
Specifically, the pretreatment liquid in step S4 may be heated by conventional heating methods in the prior art, such as heat medium heating, electric heating, microwave heating, and the like, and preferably by heating methods with good heating speed and temperature controllability, such as hot water and hot oil heating. The present embodiment employs hot water heating.
Specifically, the time of the micro-arc oxidation treatment in the step S6 is 15 min.
Specifically, the temperature of the aqueous electrolyte solution after the micro-arc oxidation treatment in the step S6 is not higher than 40 ℃, in this embodiment, 37 to 39 ℃, a heating method with a better heating speed and temperature controllability, such as hot water and hot oil heating, is adopted, and a temperature controller is used for controlling the heating. In this embodiment, hot water heating and temperature controller control are adopted.
Specifically, in the step S7, the drying temperature after the oxidized workpiece is taken out is 55 ℃, and the drying time is 25 min.
Example 2:
a micro-arc oxidation process for Mg-Gd-Y magnesium alloy comprises the following steps:
s1, processing and forming the Mg-Gd-Y magnesium alloy according to a design pattern to obtain a workpiece to be oxidized; the Mg-Gd-Y magnesium alloy comprises the following components in percentage by mass: 8.80%, Y: 3.7%, Zr: 0.480%, the balance of Mg and non-removable impurity elements;
s2, preparing a micro-arc oxidation pretreatment solution: the mass concentration of the sodium hydroxide aqueous solution is 80 g/L;
s3, preparing a micro-arc oxidation electrolytic aqueous solution: wherein the solute comprises
Film-forming agent: sodium silicate with the mass concentration of 18 g/L;
auxiliary agents: potassium fluoride with the mass concentration of 13 g/L; sodium hexametaphosphate with the mass concentration of 13 g/L; potassium hydroxide with the mass concentration of 14 g/L;
additive: glycerol with the mass concentration of 13 ml/L; yttrium nitrate with the mass concentration of 4 g/L; disodium ethylene diamine tetraacetate with the mass concentration of 4 g/L;
s4, placing the workpiece to be oxidized obtained in the step S1 in pretreatment liquid, wherein the temperature of the pretreatment liquid is 68 ℃, and the placing time is 27 min;
s5, taking the workpiece to be oxidized from the pretreatment liquid, placing the workpiece in a first deionized water tank for washing for 1-2min, taking out the workpiece, placing the workpiece in a second deionized water tank for washing for 1-2min, taking out the workpiece from the second deionized water tank, placing the workpiece in an oven for drying, wherein the drying temperature is preferably 57 ℃, and the drying time is preferably 12 min;
s6, using the workpiece to be oxidized processed in the step S5 as an anode, using a stainless steel plate as a cathode, adjusting the positive voltage to 370V and the negative voltage to 0V in a constant voltage mode, and performing micro-arc oxidation treatment in the micro-arc oxidation electrolyte solution prepared in the step S3, preferably controlling the temperature of the micro-arc oxidation electrolyte solution not to be higher than 40 ℃ to obtain the oxidized workpiece.
S7, placing the oxidized workpiece obtained in the step S6 in a third deionized water tank for washing for 1.7min, taking out and drying to finally obtain the compact and stable micro-arc oxidation layer Mg-Gd-Y series magnesium alloy oxidized workpiece.
Specifically, the pretreatment liquid in step S4 may be heated by conventional heating methods in the prior art, such as heat medium heating, electric heating, microwave heating, and the like, and preferably by heating methods with good heating speed and temperature controllability, such as hot water and hot oil heating. In this embodiment, the heating is performed by hot water.
Specifically, the time of the micro-arc oxidation treatment in the step S6 is 10 min.
Specifically, the temperature of the aqueous electrolyte solution after the micro-arc oxidation treatment in the step S6 is not higher than 40 ℃, in this embodiment, 34 to 36 ℃, a heating method with a better heating speed and temperature controllability, such as hot water and hot oil heating, is adopted, and a temperature controller is used for controlling the heating. In this embodiment, hot water heating and temperature controller control are adopted.
Specifically, in the step S7, the drying temperature is 50 ℃ after the oxidized workpiece is taken out, and the drying time is 15 min.
Example 3:
a micro-arc oxidation process for Mg-Gd-Y magnesium alloy comprises the following steps:
s1, processing and forming the Mg-Gd-Y magnesium alloy according to a design pattern to obtain a workpiece to be oxidized; the Mg-Gd-Y magnesium alloy comprises the following components in percentage by mass: 9.20%, Y: 3.3%, Zr: 0.55%, the balance being Mg and non-removable impurity elements;
s2, preparing a micro-arc oxidation pretreatment solution: the mass concentration of the sodium hydroxide aqueous solution is 65 g/L;
s3, preparing a micro-arc oxidation electrolytic aqueous solution: wherein the solute comprises
Film-forming agent: sodium silicate with the mass concentration of 14 g/L;
auxiliary agents: potassium fluoride with the mass concentration of 11 g/L; sodium hexametaphosphate with the mass concentration of 14 g/L; potassium hydroxide with the mass concentration of 12 g/L;
additive: glycerol with the mass concentration of 12 ml/L; yttrium nitrate with the mass concentration of 3 g/L; disodium ethylene diamine tetraacetate with the mass concentration of 2 g/L;
s4, placing the workpiece to be oxidized obtained in the step S1 in a pretreatment liquid, wherein the temperature of the pretreatment liquid is 75 ℃, and the placing time is 23 min;
s5, taking the workpiece to be oxidized from the pretreatment liquid, placing the workpiece in a first deionized water tank for washing for 1-2min, taking out the workpiece, placing the workpiece in a second deionized water tank for washing for 1-2min, taking out the workpiece from the second deionized water tank, placing the workpiece in an oven for drying, wherein the drying temperature is preferably 53 ℃, and the drying time is preferably 14 min;
s6, using the workpiece to be oxidized processed in the step S5 as an anode, using a stainless steel plate as a cathode, adjusting the positive voltage to 330V and the negative voltage to 0V in a constant voltage mode, and performing micro-arc oxidation treatment in the micro-arc oxidation electrolyte solution prepared in the step S3, preferably controlling the temperature of the micro-arc oxidation electrolyte solution to be not higher than 40 ℃ to obtain the oxidized workpiece.
S7, placing the oxidized workpiece obtained in the step S6 in a third deionized water tank for washing for 1.3min, taking out and drying to obtain the compact and stable micro-arc oxidation layer Mg-Gd-Y series magnesium alloy oxidized workpiece.
Specifically, the pretreatment liquid in step S4 may be heated by conventional heating methods in the prior art, such as heat medium heating, electric heating, microwave heating, and the like, and preferably by heating methods with good heating speed and temperature controllability, such as hot water and hot oil heating. . In this embodiment, the heating is performed by hot water.
Specifically, the time of the micro-arc oxidation treatment in the step S6 is 20 min;
specifically, the temperature of the aqueous electrolyte solution after the micro-arc oxidation treatment in the step S6 is not higher than 40 ℃, in this embodiment, 37 to 39 ℃, a heating method with a better heating speed and temperature controllability, such as hot water and hot oil heating, is adopted, and a temperature controller is used for controlling the heating. In this embodiment, hot water heating and temperature controller control are adopted.
Specifically, in the step S7, the drying temperature after the oxidized workpiece is taken out is 60 ℃, and the drying time is 50 min.
Example 4:
a micro-arc oxidation process for Mg-Gd-Y magnesium alloy comprises the following steps:
s1, processing and forming the Mg-Gd-Y magnesium alloy according to a design pattern to obtain a workpiece to be oxidized; the Mg-Gd-Y magnesium alloy comprises the following components in percentage by mass: 9.50%, Y: 4.0%, Zr: 0.60% and the balance of Mg and non-removable impurity elements;
s2, preparing a micro-arc oxidation pretreatment solution: the mass concentration of the sodium hydroxide aqueous solution is 100 g/L;
s3, preparing a micro-arc oxidation electrolytic aqueous solution: wherein the solute comprises
Film-forming agent: sodium silicate with the mass concentration of 20 g/L;
auxiliary agents: potassium fluoride with the mass concentration of 15 g/L; sodium hexametaphosphate with the mass concentration of 15 g/L; potassium hydroxide with the mass concentration of 15 g/L;
additive: glycerol with the mass concentration of 15 ml/L; yttrium nitrate with the mass concentration of 6 g/L; disodium ethylene diamine tetraacetate with the mass concentration of 5 g/L;
s4, placing the workpiece to be oxidized obtained in the step S1 in a pretreatment liquid, wherein the temperature of the pretreatment liquid is 80 ℃, and the placing time is 30 min;
s5, taking the workpiece to be oxidized out of the pretreatment liquid, placing the workpiece to be oxidized in a first deionized water tank for washing for 2min, taking out the workpiece, placing the workpiece in a second deionized water tank for further washing for 1min, taking out the workpiece from the second deionized water tank, placing the workpiece in an oven for drying, wherein the drying temperature is preferably 60 ℃, and the drying time is preferably 15 min;
s6, using the workpiece to be oxidized processed in the step S5 as an anode, using a stainless steel plate as a cathode, adjusting the positive voltage to 350V and the negative voltage to 0V in a constant voltage mode, and performing micro-arc oxidation treatment in the micro-arc oxidation electrolyte solution prepared in the step S3, preferably controlling the temperature of the micro-arc oxidation electrolyte solution to be not higher than 40 ℃ to obtain the oxidized workpiece.
And S7, placing the oxidized workpiece obtained in the step S6 in a third deionized water tank for washing for 1min, taking out and drying to finally obtain the compact and stable micro-arc oxidation layer Mg-Gd-Y series magnesium alloy oxidized workpiece.
Specifically, the pretreatment liquid in step S4 may be heated by conventional heating methods in the prior art, such as heat medium heating, electric heating, microwave heating, and the like, and preferably by heating methods with good heating speed and temperature controllability, such as hot water and hot oil heating. In this example, hot oil heating is used.
Specifically, the time for the micro-arc oxidation treatment in the step S6 is 17 min.
Specifically, the temperature of the aqueous electrolyte solution after the micro-arc oxidation treatment in the step S6 is not higher than 40 ℃, in this embodiment, 38 to 40 ℃, a heating method with a better heating speed and temperature controllability, such as hot water and hot oil heating, is adopted, and a temperature controller is used for controlling the heating. In this embodiment, hot oil heating is used and the temperature controller is used for control.
Specifically, in the step S7, the drying temperature after the oxidized workpiece is taken out is 57 ℃, and the drying time is 18 min.
Example 5:
a micro-arc oxidation process for Mg-Gd-Y magnesium alloy comprises the following steps:
s1, processing and forming the Mg-Gd-Y magnesium alloy according to a design pattern to obtain a workpiece to be oxidized; the Mg-Gd-Y magnesium alloy comprises the following components in percentage by mass: 8.50%, Y: 3.0%, Zr: 0.40% and the balance of Mg and non-removable impurity elements;
s2, preparing a micro-arc oxidation pretreatment solution: the mass concentration of the sodium hydroxide aqueous solution is 50 g/L;
s3, preparing a micro-arc oxidation electrolytic aqueous solution: wherein the solute comprises
Film-forming agent: sodium silicate with the mass concentration of 10 g/L;
auxiliary agents: potassium fluoride with the mass concentration of 15 g/L; sodium hexametaphosphate with the mass concentration of 15 g/L; potassium hydroxide with the mass concentration of 15 g/L;
additive: glycerol with the mass concentration of 10 ml/L; yttrium nitrate with the mass concentration of 1 g/L; disodium ethylene diamine tetraacetate with the mass concentration of 1 g/L;
s4, placing the workpiece to be oxidized obtained in the step S1 in pretreatment liquid, wherein the temperature of the pretreatment liquid is 60 ℃, and the placing time is 20 min;
s5, taking the workpiece to be oxidized out of the pretreatment liquid, placing the workpiece to be oxidized in a first deionized water tank for washing for 1min, taking out the workpiece, placing the workpiece in a second deionized water tank for further washing for 1min, taking out the workpiece from the second deionized water tank, placing the workpiece in an oven for drying, wherein the drying temperature is preferably 50 ℃, and the drying time is preferably 10 min;
s6, using the workpiece to be oxidized processed in the step S5 as an anode, using a stainless steel plate as a cathode, adjusting the positive voltage to 350V and the negative voltage to 0V in a constant voltage mode, and performing micro-arc oxidation treatment in the micro-arc oxidation electrolyte solution prepared in the step S3, preferably controlling the temperature of the micro-arc oxidation electrolyte solution to be not higher than 40 ℃ to obtain the oxidized workpiece.
And S7, placing the oxidized workpiece obtained in the step S6 in a third deionized water tank for washing for 1min, taking out and drying to finally obtain the compact and stable micro-arc oxidation layer Mg-Gd-Y series magnesium alloy oxidized workpiece.
Specifically, the pretreatment liquid in step S4 may be heated by conventional heating methods in the prior art, such as heat medium heating, electric heating, microwave heating, and the like, and preferably by heating methods with good heating speed and temperature controllability, such as hot water and hot oil heating. In this embodiment, hot water heating is adopted.
Specifically, the time of the micro-arc oxidation treatment in the step S6 is 13 min.
Specifically, the temperature of the aqueous electrolyte solution after the micro-arc oxidation treatment in the step S6 is not higher than 40 ℃, in this embodiment, 35 to 37 ℃, a heating method with a better heating speed and temperature controllability, such as hot water and hot oil heating, is adopted, and a temperature controller is used for controlling the heating. In this embodiment, hot oil heating is used and the temperature controller is used for control.
Specifically, in the step S7, the drying temperature after the oxidized workpiece is taken out is 53 ℃, and the drying time is 23 min.
Comparative example:
a micro-arc oxidation process for Mg-Gd-Y magnesium alloy comprises the following steps:
s1, processing and forming the Mg-Gd-Y magnesium alloy according to a design pattern to obtain a workpiece to be oxidized; the Mg-Gd-Y magnesium alloy comprises the following components in percentage by mass: 9.00%, Y: 3.5%, Zr: 0.50% of Mg and the balance of non-removable impurity elements;
s2, preparing a micro-arc oxidation pretreatment solution: the mass concentration of the sodium hydroxide aqueous solution is 100 g/L;
s3, preparing a micro-arc oxidation electrolytic aqueous solution: wherein the solute comprises
Film-forming agent: sodium silicate with the mass concentration of 20 g/L;
auxiliary agents: potassium fluoride with the mass concentration of 15 g/L; sodium hexametaphosphate with the mass concentration of 15 g/L; potassium hydroxide with the mass concentration of 15 g/L;
additive: glycerol with the mass concentration of 15 ml/L;
s4, placing the workpiece to be oxidized obtained in the step S1 in a pretreatment liquid, wherein the temperature of the pretreatment liquid is 80 ℃, and the placing time is 30 min;
s5, taking the workpiece to be oxidized out of the pretreatment liquid, placing the workpiece to be oxidized in a first deionized water tank for washing for 2min, taking out the workpiece, placing the workpiece in a second deionized water tank for further washing for 2min, taking out the workpiece from the second deionized water tank, placing the workpiece in an oven for drying, wherein the drying temperature is preferably 60 ℃, and the drying time is preferably 15 min;
s6, using the workpiece to be oxidized processed in the step S5 as an anode, using a stainless steel plate as a cathode, adjusting the positive voltage to 400V and the negative voltage to 0V in a constant voltage mode, and performing micro-arc oxidation treatment in the micro-arc oxidation electrolyte solution prepared in the step S3, preferably controlling the temperature of the micro-arc oxidation electrolyte solution to be not higher than 40 ℃ to obtain the oxidized workpiece.
And S7, placing the oxidized workpiece obtained in the step S6 in a third deionized water tank for washing for 2min, taking out and drying to finally obtain the compact and stable micro-arc oxidation layer Mg-Gd-Y series magnesium alloy oxidized workpiece.
Specifically, the heating manner of the pretreatment liquid in the step S4 may be a conventional heating manner in the prior art, such as heat medium heating, electric heating, microwave heating, and the like, and in this embodiment, a heating manner with a better heating speed and temperature controllability, and hot water heating, are preferably adopted.
Specifically, the time of the micro-arc oxidation treatment in the step S6 is 18min
Specifically, the temperature of the aqueous electrolyte solution subjected to micro-arc oxidation treatment in the step S6 is not higher than 40 ℃, a heating mode with good heating speed and temperature controllability is adopted, such as hot water and hot oil heating, and a temperature controller is used for controlling the heating mode.
Specifically, in the step S7, the drying temperature after the oxidized workpiece is taken out is 55 ℃, and the drying time is 30 min.
The Mg-Gd-Y series magnesium alloy oxidized work batch 5 and 3 of this example had defects as shown in fig. 2.
Claims (10)
1. A micro-arc oxidation process for Mg-Gd-Y magnesium alloy comprises the following steps:
s1, processing and forming the Mg-Gd-Y magnesium alloy according to a design pattern to obtain a workpiece to be oxidized;
s2, preparing a micro-arc oxidation pretreatment solution: the mass concentration of the sodium hydroxide aqueous solution is 50g/L-100 g/L;
s3, preparing a micro-arc oxidation electrolytic aqueous solution: wherein the solute comprises
Film-forming agent: sodium silicate with the mass concentration of 10g/L-20 g/L;
auxiliary agents: potassium fluoride with the mass concentration of 10g/L-15 g/L; sodium hexametaphosphate with the mass concentration of 10g/L-15 g/L; potassium hydroxide with the mass concentration of 10g/L-15 g/L;
additive: glycerol with the mass concentration of 10ml/L-15 ml/L; yttrium nitrate with the mass concentration of 1g/L-6 g/L; disodium ethylene diamine tetraacetate with the mass concentration of 1g/L-5 g/L;
s4, placing the workpiece to be oxidized obtained in the step S1 in pretreatment liquid, wherein the temperature of the pretreatment liquid is 60-80 ℃, and the placing time is 20-30 min;
s5, taking the workpiece to be oxidized from the pretreatment liquid, placing the workpiece in a first deionized water tank for washing for 1-2min, taking out the workpiece, placing the workpiece in a second deionized water tank for washing for 1-2min, taking out the workpiece from the second deionized water tank, placing the workpiece in an oven for drying, wherein the drying temperature is preferably 50-60 ℃, and the drying time is preferably 10-15 min;
s6, using the workpiece to be oxidized processed in the step S5 as an anode, using a metal material as a cathode, adjusting the positive voltage to 400-V and the negative voltage to 0V in a constant voltage mode, and performing micro-arc oxidation treatment in the micro-arc oxidation electrolyte aqueous solution prepared in the step S3, preferably controlling the temperature of the micro-arc oxidation electrolyte aqueous solution not to be higher than 40 ℃ to obtain the oxidized workpiece.
2. The Mg-Gd-Y series magnesium alloy micro-arc oxidation process according to claim 1, further comprising
And S7, placing the oxidized workpiece obtained in the step S6 in a third deionized water tank for washing for 1-2min, taking out and drying to obtain the compact and stable micro-arc oxidation layer Mg-Gd-Y series magnesium alloy oxidized workpiece.
3. The Mg-Gd-Y magnesium alloy micro-arc oxidation process according to claim 1 or 2, wherein the Mg-Gd-Y magnesium alloy in the step S1 comprises, in mass percent, Gd: 8.50-9.50%, Y: 3.0-4.0%, Zr: 0.40-0.60%, and the balance of Mg and non-removable impurity elements.
4. The Mg-Gd-Y series magnesium alloy micro-arc oxidation process according to claim 1, wherein in the step S6, a constant voltage mode is selected to adjust the positive voltage to 350V.
5. The Mg-Gd-Y series magnesium alloy micro-arc oxidation process according to claim 1, wherein the auxiliary agent in the S6 step: potassium fluoride with the mass concentration of 10g/L-15 g/L; the mass concentration of the sodium hexametaphosphate is 10g/L-15 g/L.
6. The Mg-Gd-Y magnesium alloy micro-arc oxidation process according to claim 1, wherein the pretreatment liquid in the step S4 can be heated by conventional heating methods in the prior art, such as heating with heat medium, electric heating, microwave heating, etc., preferably by heating methods with good heating speed and temperature controllability, such as hot water and hot oil heating.
7. The Mg-Gd-Y series magnesium alloy micro-arc oxidation process according to claim 1, wherein the micro-arc oxidation treatment time in the S6 step is 5-20min, preferably 10-20 min.
8. The Mg-Gd-Y series magnesium alloy micro-arc oxidation process according to claim 1, wherein the temperature of the aqueous electrolyte solution after micro-arc oxidation treatment in the step S6 is not higher than 40 ℃, a heating mode with better heating speed and temperature controllability is adopted, such as hot water and hot oil heating, and a temperature controller is used for controlling.
9. The Mg-Gd-Y series magnesium alloy micro-arc oxidation process according to claim 1, wherein the stainless steel in the S6 step is used as a cathode.
10. The Mg-Gd-Y magnesium alloy micro-arc oxidation process according to claim 2, wherein in the step S7, the oxidized workpiece is taken out and dried at the temperature of 50-60 ℃ for 10-50min, preferably 15-25 min.
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