CN117660819B - Gao Jiangke magnesium-dissolving alloy and preparation method thereof - Google Patents
Gao Jiangke magnesium-dissolving alloy and preparation method thereof Download PDFInfo
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- 229910045601 alloy Inorganic materials 0.000 title claims description 212
- 239000000956 alloy Substances 0.000 title claims description 212
- 238000002360 preparation method Methods 0.000 title abstract description 22
- 229910000861 Mg alloy Inorganic materials 0.000 claims abstract description 151
- 239000011777 magnesium Substances 0.000 claims abstract description 77
- 238000001125 extrusion Methods 0.000 claims abstract description 72
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 64
- 230000032683 aging Effects 0.000 claims abstract description 42
- 239000012535 impurity Substances 0.000 claims abstract description 21
- 238000000265 homogenisation Methods 0.000 claims abstract description 13
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 56
- 229910052749 magnesium Inorganic materials 0.000 claims description 56
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 55
- 229910052725 zinc Inorganic materials 0.000 claims description 54
- 239000011701 zinc Substances 0.000 claims description 54
- 238000005266 casting Methods 0.000 claims description 37
- 238000000034 method Methods 0.000 claims description 33
- 239000002994 raw material Substances 0.000 claims description 30
- OWXLRKWPEIAGAT-UHFFFAOYSA-N [Mg].[Cu] Chemical compound [Mg].[Cu] OWXLRKWPEIAGAT-UHFFFAOYSA-N 0.000 claims description 29
- ATTFYOXEMHAYAX-UHFFFAOYSA-N magnesium nickel Chemical compound [Mg].[Ni] ATTFYOXEMHAYAX-UHFFFAOYSA-N 0.000 claims description 29
- QRNPTSGPQSOPQK-UHFFFAOYSA-N magnesium zirconium Chemical compound [Mg].[Zr] QRNPTSGPQSOPQK-UHFFFAOYSA-N 0.000 claims description 29
- 238000004321 preservation Methods 0.000 claims description 25
- DFIYZNMDLLCTMX-UHFFFAOYSA-N gadolinium magnesium Chemical compound [Mg].[Gd] DFIYZNMDLLCTMX-UHFFFAOYSA-N 0.000 claims description 23
- MIOQWPPQVGUZFD-UHFFFAOYSA-N magnesium yttrium Chemical compound [Mg].[Y] MIOQWPPQVGUZFD-UHFFFAOYSA-N 0.000 claims description 23
- 150000002910 rare earth metals Chemical class 0.000 claims description 20
- 238000009749 continuous casting Methods 0.000 claims description 19
- 229910052688 Gadolinium Inorganic materials 0.000 claims description 17
- 238000002844 melting Methods 0.000 claims description 17
- 230000008018 melting Effects 0.000 claims description 17
- 229910052727 yttrium Inorganic materials 0.000 claims description 17
- 229910052746 lanthanum Inorganic materials 0.000 claims description 14
- KPQBNQRPQKZQNJ-UHFFFAOYSA-N [Sm].[Mg] Chemical compound [Sm].[Mg] KPQBNQRPQKZQNJ-UHFFFAOYSA-N 0.000 claims description 11
- 229910052772 Samarium Inorganic materials 0.000 claims description 7
- 230000004907 flux Effects 0.000 claims description 7
- -1 magnesium lanthanum cerium rare earth Chemical class 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 238000010309 melting process Methods 0.000 claims description 2
- 238000001816 cooling Methods 0.000 description 18
- 239000010949 copper Substances 0.000 description 17
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 17
- 229910052802 copper Inorganic materials 0.000 description 16
- 229910052759 nickel Inorganic materials 0.000 description 16
- 229910052726 zirconium Inorganic materials 0.000 description 16
- 238000003756 stirring Methods 0.000 description 14
- 238000007670 refining Methods 0.000 description 13
- 238000005303 weighing Methods 0.000 description 12
- 229910052684 Cerium Inorganic materials 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 11
- 238000004090 dissolution Methods 0.000 description 7
- 239000002245 particle Substances 0.000 description 4
- 238000009472 formulation Methods 0.000 description 3
- 239000000155 melt Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 238000001953 recrystallisation Methods 0.000 description 2
- 238000005204 segregation Methods 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal 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
- 239000003079 shale oil Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
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Abstract
The invention discloses a high Jiang Kerong magnesium alloy and a preparation method thereof, wherein the high Jiang Kerong magnesium alloy comprises the following components in percentage by mass: zn:0.5% -2.0%; cu:0.5% -1.5%; zr:0.2% -0.5%; ni:0.5% -1.5%, X:9.2% -13.0%; the balance of Mg and unavoidable impurity elements; wherein X is a combination of light rare earth elements and heavy rare earth elements, and the weight percentage of the light rare earth elements is as follows: 0.2% -2%, the weight percentage of the heavy rare earth elements is as follows: 9% -11%. The high Jiang Kerong magnesium alloy of the invention has higher tensile strength and yield strength and better mechanical property. The preparation method of Gao Jiangke magnesium alloy is simple in scheme, and mechanical properties of Gao Jiangke magnesium alloy can be ensured not to be influenced by extrusion ratio by setting steps of homogenization, pre-ageing, ageing treatment and the like.
Description
Technical Field
The invention relates to the field of metal materials, in particular to a high Jiang Kerong magnesium alloy and a preparation method thereof.
Background
The shale gas and shale oil reserves in China are in the front of the world, the future development prospect is wide, and the conventional staged fracturing technology for the horizontal well exploitation of the current mainstream can realize the reformation of multiple strata simultaneously to improve the single well productivity, so that the construction efficiency is improved. One key component of this technology is fracturing tools, including temporary plugging balls, ball seats, bridge plugs, sliding sleeves, and the like. The fracturing tool is required to have higher dissolution rate and higher mechanical property (the tensile strength is more than or equal to 400MPa, the yield strength is more than or equal to 280MPa, and the dissolution rate is 60-90mg cm -2*h-1) in the operation process of partial mines. The extrusion ratio used in the preparation process of the existing magnesium alloy is large, and when the actual production extrusion is carried out, the extrusion ratio does not meet the preset requirement, so that the strength performance of the existing magnesium alloy is reduced, and the tensile strength of the magnesium alloy is lower than 400MPa.
Disclosure of Invention
The invention aims to provide a high Jiang Kerong magnesium alloy and a preparation method thereof, wherein the high Jiang Kerong magnesium alloy has high tensile strength and yield strength and good dissolution rate.
In order to achieve the above purpose, the embodiment of the invention provides a high Jiang Kerong magnesium alloy, which comprises the following components in percentage by mass: zn:0.5% -2.0%; cu:0.5% -1.5%; zr:0.2% -0.5%; ni:0.5% -1.5%, X:9.2% -13.0%; the balance of Mg and unavoidable impurity elements; wherein X is a combination of light rare earth elements and heavy rare earth elements, and the weight percentage of the light rare earth elements is as follows: 0.2% -2%, the weight percentage of the heavy rare earth elements is as follows: 9% -11%.
In one or more embodiments of the present invention, the light rare earth element is selected from one or more of La, ce, and Sm.
In one or more embodiments of the present invention, the heavy rare earth element is selected from one or more of Y and Gd.
Another embodiment of the present invention provides a method for preparing a high Jiang Kerong magnesium alloy, comprising:
the raw materials are proportioned: selecting magnesium ingot, zinc ingot, magnesium-zirconium intermediate alloy, magnesium-nickel intermediate alloy, magnesium-copper intermediate alloy, light rare earth alloy and heavy rare earth alloy as raw materials according to a certain proportion:
and (3) melting and casting: sequentially adding the raw materials into a resistance furnace and melting at 720-750 ℃; casting the molten raw materials into magnesium alloy ingots by adopting an electromagnetic semi-continuous casting method at 750-770 ℃;
extrusion pretreatment: sequentially carrying out homogenization treatment and pre-ageing treatment on the magnesium alloy ingot;
And (3) heat preservation extrusion: the magnesium alloy cast ingot subjected to homogenization treatment and pre-ageing treatment is subjected to heat preservation for 4-6 hours at the temperature of 350-450 ℃ and then extruded to obtain a magnesium alloy bar;
And (3) extrusion post-treatment: and aging the extruded magnesium alloy bar.
In one or more embodiments of the present invention, the light rare earth alloy is selected from one or more of a magnesium lanthanum cerium rare earth master alloy and a magnesium samarium master alloy.
In one or more embodiments of the invention, the heavy rare earth alloy is selected from one or more of magnesium yttrium master alloy and magnesium gadolinium master alloy.
In one or more embodiments of the invention, the feedstock surface is covered with flux during melting; the flux is selected from one or more of RJ-2 and RJ-5.
In one or more embodiments of the invention, the electromagnetic semi-continuous casting process has a current of between 100A and 120A and a frequency of between 15Hz and 30 Hz.
In one or more embodiments of the invention, the homogenization treatment is: the magnesium alloy ingot is subjected to heat preservation for 12 to 16 hours at 470 to 520 ℃ and then is cooled; the pre-ageing treatment is as follows: the magnesium alloy ingot is subjected to heat preservation for 48 to 84 hours at the temperature of 190 to 210 ℃; the aging treatment is as follows: and (3) preserving the heat of the extruded magnesium alloy bar for 48-72 h at the temperature of 190-210 ℃.
In one or more embodiments of the invention, the extrusion speed of the magnesium alloy bar is between 0.5mm/s and 3 mm/s; the extrusion ratio of the magnesium alloy bar is between 6 and 7.
Compared with the prior art, the high Jiang Kerong magnesium alloy according to the embodiment of the invention improves the purification degree of the magnesium alloy melt by adding the light rare earth element; the strength of the magnesium alloy is improved by adding the heavy rare earth element to meet the working condition requirement of a specific shale oil-gas well, and the high Jiang Kerong magnesium alloy has excellent mechanical property and good ingot blank quality by controlling the mass percentages of the light metal element and the heavy metal element. Therefore, the high Jiang Kerong magnesium alloy has higher tensile strength and yield strength and better mechanical property. The preparation method of Gao Jiangke magnesium-dissolved alloy has simple scheme, can improve the uniformity of the alloy structure by setting homogenization treatment, reduces segregation and ensures that the deformed structure performance is more uniform. The pre-ageing treatment can introduce preset second phase particles to provide driving force for the nucleation of recrystallized grains, so that the deformed structure has finer grains, and the strength performance of the magnesium alloy is improved. The aging treatment increases the micro-or nano-scale precipitated phase in the alloy structure, and further strengthens the strength performance of the alloy. The preparation method of the Gao Jiangke magnesium-dissolving alloy can ensure that the mechanical property of the Gao Jiangke magnesium-dissolving alloy is not influenced by the extrusion ratio and has good dissolution rate.
Drawings
FIG. 1 is a schematic flow chart of a method for preparing a high Jiang Kerong magnesium alloy according to one embodiment of the present invention.
Detailed Description
The following detailed description of embodiments of the invention is, therefore, to be taken in conjunction with the accompanying drawings, and it is to be understood that the scope of the invention is not limited to the specific embodiments.
According to the preferred embodiment of the invention, the high Jiang Kerong magnesium alloy comprises the following components in percentage by mass: zn:0.5% -2.0%; cu:0.5% -1.5%; zr:0.2% -0.5%; ni:0.5% -1.5%, X:9.2% -13.0%; the rest Mg and unavoidable impurity elements; wherein X is a combination of light rare earth elements and heavy rare earth elements, and the weight percentage of the light rare earth elements is as follows: 0.2-2% of heavy rare earth elements in percentage by mass: 9% -11%.
In one embodiment, the light rare earth element is selected from one or more of La, ce, and Sm. The heavy rare earth element is selected from one or more of Y and Gd.
In the above embodiment, by controlling the mass percentages of the various components, it is possible to obtain a high Jiang Kerong magnesium alloy that still has a high tensile strength at a low extrusion ratio.
In one embodiment, the preferable mode of the mass percentages of the components of the high Jiang Kerong magnesium alloy is as follows: 0.5% Zn, 0.5% Cu, 0.2% Zr, 0.5% Ni, 0.5% La, 0.5% Ce, 8.5% Gd and 1.5% Y, the balance being Mg and unavoidable impurities.
A further preferred formulation of the Gao Jiangke magnesium-soluble alloy is: 0.9% Zn, 1.0% Cu, 0.3% Zr, 1.0% Ni, 0.5% Sm, 6.5% Gd and 2.5% Y, the balance being Mg and unavoidable impurities.
A further preferred formulation of the Gao Jiangke magnesium-soluble alloy is: 0.9% Zn, 1.5% Cu, 0.4% Zr, 1.5% Ni, 0.1% La, 0.1% Ce, 7.5% Gd and 3.0% Y, the balance being Mg and unavoidable impurities.
A further preferred formulation of the Gao Jiangke magnesium-soluble alloy is: 2.0% Zn, 1.5% Cu, 0.5% Zr, 1.5% Ni, 1.0% Sm, 0.5% La, 0.5% Ce, 7.5% Gd and 3.5% Y, the balance being Mg and unavoidable impurities.
As shown in FIG. 1, another embodiment of the present invention discloses a method for preparing the Gao Jiangke magnesium-dissolved alloy, which comprises steps S1-S5.
Step S1, proportioning raw materials: and selecting magnesium ingots, zinc ingots, magnesium-zirconium intermediate alloy, magnesium-nickel intermediate alloy, magnesium-copper intermediate alloy, light rare earth alloy and heavy rare earth alloy as raw materials according to the proportion.
Specifically, in step S1, magnesium ingots, zinc ingots, magnesium-zirconium intermediate alloys (Mg-30 Zr), magnesium-nickel intermediate alloys (Mg-20 Ni), magnesium-copper intermediate alloys (Mg-80 Cu), light rare earth intermediate alloys (Mg-40 mm, la: ce=1:1; mg-30 Sm), and heavy rare earth intermediate alloys (Mg-30 gd; mg-25Y) are proportionally selected as raw materials. Wherein, the light rare earth alloy can be selected from one or more of magnesium lanthanum cerium rare earth intermediate alloy and magnesium samarium intermediate alloy. The heavy rare earth alloy may be selected from one or more of magnesium yttrium master alloy and magnesium gadolinium master alloy.
Step S2, melt casting: sequentially adding the raw materials into a resistance furnace to be melted at the temperature of 720-750 ℃; and casting the molten raw materials into magnesium alloy ingots by adopting an electromagnetic semi-continuous casting method at 750-770 ℃.
Specifically, in step S2, the weighed magnesium ingot and zinc ingot are placed into a resistance furnace, heat preservation is carried out at 720-750 ℃ until the magnesium ingot and the zinc ingot are completely melted, then magnesium-zirconium intermediate alloy, magnesium-nickel intermediate alloy, magnesium-copper intermediate alloy, light rare earth alloy and heavy rare earth alloy are added, the addition temperature is controlled at 740-750 ℃, and the heat preservation is carried out for half an hour after stirring until the magnesium ingot and the zinc ingot are completely melted. Further, during the melting process, the surface of each raw material is covered with a flux for reducing the burning loss of each raw material. Wherein, the zinc ingot and the magnesium ingot are melted together by heat preservation, and RJ-2 flux is covered on the surface of the raw material; the other alloys were added covered with RJ-5 flux.
Refining for 5-10 min by using RJ-5 after preserving heat for half an hour to obtain a soluble magnesium alloy melt; and then, the melted raw materials are initially cast into magnesium alloy ingots by adopting an electromagnetic semi-continuous casting method at the temperature of 750-770 ℃. Wherein, the current of the electromagnetic semi-continuous casting method is between 100A and 120A, and the frequency is between 15Hz and 30 Hz.
In the smelting process, firstly adding light rare earth alloy, fully stirring the melt, standing for a period of time, and then adding heavy rare earth alloy, so that the light rare earth alloy can react with impurities in the melt first, and the melt is purified; thereby reducing the loss of the heavy rare earth alloy caused by the purification effect and improving the yield of the heavy rare earth element.
Step S3, extrusion pretreatment: and sequentially carrying out homogenization treatment and pre-ageing treatment on the magnesium alloy ingot.
Specifically, in step S3, the homogenization treatment is: and (3) preserving the heat of the magnesium alloy ingot for 12-16 hours at 470-520 ℃ and then cooling. The pre-ageing treatment is as follows: and (3) preserving the heat of the magnesium alloy ingot for 48 to 84 hours at the temperature of 190 to 210 ℃. The homogenization treatment aims to improve the segregation of the alloy and make the structure of the alloy more uniform, so as to obtain the soluble magnesium alloy in a homogeneous state. Coarse Mg 5 RE particles can be generated in the pre-ageing treatment process, the particles can control the dynamic recrystallization behavior of the alloy, and the coarse Mg 5 RE particles can promote the transition from a small-angle grain boundary to a large-angle grain boundary in the extrusion process, so that the continuous recrystallization is promoted, the regulation and control of the grain size of a deformed structure can be realized, and the pre-ageing soluble magnesium alloy is obtained.
Step S4, heat preservation extrusion: and (3) preserving heat for 4-6 hours at the temperature of 350-450 ℃ and then extruding the magnesium alloy ingot subjected to the homogenization treatment and the pre-ageing treatment to obtain the magnesium alloy bar.
Specifically, in the step S4, the magnesium alloy ingot subjected to homogenization treatment and pre-ageing treatment is subjected to heat preservation for 4-6 hours at the temperature of 350-450 ℃ and then is extruded to obtain a magnesium alloy bar. Wherein the extrusion speed of the magnesium alloy bar is between 0.5mm/s and 3 mm/s. The extrusion ratio of the magnesium alloy bar is between 6 and 7. The diameter of the magnesium alloy cast ingot before extrusion is 70mm-80mm, and the diameter of the magnesium alloy bar obtained by extrusion is 25mm-35mm.
Step S5, extrusion post-treatment: and aging the extruded magnesium alloy bar.
Specifically, in step S5, the extruded magnesium alloy bar is subjected to aging treatment. The aging treatment is as follows: and (3) preserving the heat of the extruded magnesium alloy bar for 48-72 h at the temperature of 190-210 ℃. The aging treatment can further improve the strength performance of the magnesium alloy bar.
The invention will be further illustrated with reference to specific examples and comparative examples.
Example 1
Gao Jiangke magnesium-dissolving alloy consists of the following elements in percentage by mass: 0.5% Zn, 0.5% Cu, 0.2% Zr, 0.5% Ni, 0.5% La, 0.5% Ce, 8.5% Gd and 1.5% Y, the balance being Mg and unavoidable impurities. The preparation method comprises the following steps:
the raw materials are proportioned: weighing magnesium ingot, zinc ingot, magnesium-nickel intermediate alloy, magnesium-copper intermediate alloy, magnesium-lanthanum-cerium-rare earth intermediate alloy, magnesium-zirconium intermediate alloy, magnesium-gadolinium intermediate alloy and magnesium-yttrium intermediate alloy according to the proportion.
And (3) melting and casting: placing magnesium ingots, zinc ingots and RJ-2 into a resistance furnace, preserving heat at 750 ℃ until the magnesium ingots and the zinc ingots are completely melted, then adding magnesium-nickel intermediate alloy, magnesium-copper intermediate alloy, magnesium-lanthanum-cerium-rare earth intermediate alloy, magnesium-zirconium intermediate alloy, magnesium-gadolinium intermediate alloy and magnesium-yttrium intermediate alloy, controlling the adding temperature to 770 ℃, preserving heat for half an hour after stirring until the magnesium ingots and the zinc ingots are completely melted, and refining for 5 minutes by using RJ-5 to obtain a soluble magnesium alloy melt; and casting the soluble magnesium alloy melt into a magnesium alloy cast ingot by adopting an electromagnetic semi-continuous casting method, wherein the electromagnetic frequency of 15Hz and the current of an electromagnetic system are set to be 100A in the casting process.
Extrusion pretreatment: homogenizing treatment and pre-ageing treatment are carried out on the magnesium alloy cast ingot, and homogenizing treatment is carried out: preserving heat for 16h at 470 ℃; pre-ageing: preserving heat for 64h at 200 ℃ and then air cooling.
And (3) heat preservation extrusion: and (3) preserving the heat of the magnesium alloy ingot for 4 hours at 350 ℃, and extruding at a speed of 1.0mm/s to obtain a magnesium alloy bar with an extrusion ratio of 6.
And (3) extrusion post-treatment: and (5) preserving the heat of the extruded magnesium alloy bar for 48 hours at 200 ℃ and then cooling.
Example 2
Gao Jiangke magnesium-dissolving alloy consists of the following elements in percentage by mass: 0.9% Zn, 1.0% Cu, 0.3% Zr, 1.0% Ni, 0.5% Sm, 6.5% Gd and 2.5% Y, the balance being Mg and unavoidable impurities. The preparation method comprises the following steps:
the raw materials are proportioned: weighing magnesium ingot, zinc ingot, magnesium-nickel intermediate alloy, magnesium-copper intermediate alloy, magnesium-zirconium intermediate alloy, magnesium-samarium intermediate alloy, magnesium-gadolinium intermediate alloy and magnesium-yttrium intermediate alloy according to the proportion.
And (3) melting and casting: placing magnesium ingots, zinc ingots and RJ-2 into a resistance furnace, preserving heat at 720 ℃ until the magnesium ingots and the zinc ingots are completely melted, then adding magnesium-nickel intermediate alloy, magnesium-copper intermediate alloy, magnesium-zirconium intermediate alloy, magnesium-samarium intermediate alloy, magnesium-gadolinium intermediate alloy and magnesium-yttrium intermediate alloy, controlling the adding temperature to be 750 ℃, preserving heat for half an hour after stirring until the magnesium ingots and the zinc ingots are completely melted, and refining for 10 minutes by using RJ-5 to obtain a soluble magnesium alloy melt; the magnesium alloy cast ingot is obtained by adopting an electromagnetic semi-continuous casting method, wherein the electromagnetic frequency of 20Hz is set in the casting process, and the current of an electromagnetic system is 110A.
Extrusion pretreatment: homogenizing treatment and pre-ageing treatment are carried out on the magnesium alloy cast ingot, and homogenizing treatment is carried out: preserving heat for 14h at 500 ℃; pre-ageing: preserving heat for 64h at 200 ℃ and then air cooling.
And (3) heat preservation extrusion: and (3) preserving the heat of the magnesium alloy ingot for 6 hours at 400 ℃ and extruding at a speed of 2.0mm/s to obtain a magnesium alloy bar, wherein the extrusion ratio is 7.
And (3) extrusion post-treatment: and (5) preserving the heat of the extruded magnesium alloy bar for 48 hours at 200 ℃ and then cooling.
Example 3
Gao Jiangke magnesium-dissolving alloy consists of the following elements in percentage by mass: 0.9% Zn, 1.5% Cu, 0.4% Zr, 1.5% Ni, 0.1% La, 0.1% Ce, 7.5% Gd and 3.0% Y, the balance being Mg and unavoidable impurities. The preparation method comprises the following steps:
the raw materials are proportioned: weighing magnesium ingot, zinc ingot, magnesium-nickel intermediate alloy, magnesium-copper intermediate alloy, magnesium-lanthanum-cerium-rare earth intermediate alloy, magnesium-zirconium intermediate alloy, magnesium-gadolinium intermediate alloy and magnesium-yttrium intermediate alloy according to the proportion.
And (3) melting and casting: placing magnesium ingots, zinc ingots and RJ-2 into a resistance furnace, preserving heat at 750 ℃ until the magnesium ingots and the zinc ingots are completely melted, then adding magnesium-nickel intermediate alloy, magnesium-copper intermediate alloy, magnesium-lanthanum-cerium-rare earth intermediate alloy, magnesium-zirconium intermediate alloy, magnesium-gadolinium intermediate alloy and magnesium-yttrium intermediate alloy, controlling the adding temperature to be 750 ℃, preserving heat for half an hour after stirring until the magnesium ingots and the zinc ingots are completely melted, and refining for 5 minutes by using RJ-5 to obtain a soluble magnesium alloy melt; and casting the soluble magnesium alloy melt into a magnesium alloy cast ingot by adopting an electromagnetic semi-continuous casting method, wherein an electromagnetic frequency of 25Hz is set in the casting process, and the current of an electromagnetic system is 120A.
Extrusion pretreatment: homogenizing treatment and pre-ageing treatment are carried out on the magnesium alloy cast ingot, and homogenizing treatment is carried out: preserving heat for 10h at 520 ℃; pre-ageing: preserving heat for 64h at 200 ℃ and then air cooling.
And (3) heat preservation extrusion: and (3) preserving the heat of the magnesium alloy ingot for 4 hours at 420 ℃, and extruding at a speed of 1.0mm/s to obtain a magnesium alloy bar with an extrusion ratio of 7.
And (3) extrusion post-treatment: and (5) preserving the heat of the extruded magnesium alloy bar for 64 hours at 200 ℃ and then cooling.
Example 4
Gao Jiangke magnesium-dissolving alloy consists of the following elements in percentage by mass: 2.0% Zn, 1.5% Cu, 0.5% Zr, 1.5% Ni, 1.0% Sm, 0.5% La, 0.5% Ce, 7.5% Gd and 3.5% Y, the balance being Mg and unavoidable impurities. The preparation method comprises the following steps:
The raw materials are proportioned: weighing magnesium ingot, zinc ingot, magnesium-nickel intermediate alloy, magnesium-copper intermediate alloy, magnesium-lanthanum-cerium-rare earth intermediate alloy, magnesium-samarium intermediate alloy, magnesium-zirconium intermediate alloy, magnesium-gadolinium intermediate alloy and magnesium-yttrium intermediate alloy according to the proportion.
And (3) melting and casting: placing magnesium ingots, zinc ingots and RJ-2 into a resistance furnace, preserving heat at 750 ℃ until the magnesium ingots and the zinc ingots are completely melted, then adding magnesium-nickel intermediate alloy, magnesium-copper intermediate alloy, magnesium-lanthanum-cerium-rare earth intermediate alloy, magnesium-zirconium intermediate alloy, magnesium-samarium intermediate alloy, magnesium-gadolinium intermediate alloy and magnesium-yttrium intermediate alloy, controlling the adding temperature at 750 ℃, stirring until the magnesium ingots and the zinc ingots are completely melted, preserving heat for half an hour, and refining for 10 minutes by using RJ-5 to obtain a soluble magnesium alloy melt; the method is characterized in that a soluble magnesium alloy melt is cast into a magnesium alloy cast ingot by adopting an electromagnetic semi-continuous casting method, wherein the electromagnetic frequency of 30Hz is set in the casting process, and the current of an electromagnetic system is 110A.
Extrusion pretreatment: homogenizing treatment and pre-ageing treatment are carried out on the magnesium alloy cast ingot, and homogenizing treatment is carried out: preserving heat for 12h at 510 ℃; pre-ageing: preserving heat at 200 ℃ for 48 hours, and then air-cooling.
And (3) heat preservation extrusion: and (3) preserving the heat of the magnesium alloy ingot for 4 hours at 420 ℃, and extruding at a speed of 1.0mm/s to obtain a magnesium alloy bar with an extrusion ratio of 6.
And (3) extrusion post-treatment: and (5) preserving the heat of the extruded magnesium alloy bar for 54 hours at 200 ℃ and then cooling.
Comparative example 1
The magnesium alloy consists of the following elements in percentage by mass: 0.5% Zn, 0.5% Cu, 0.2% Zr, 0.5% Ni, 0.5% La, 0.5% Ce, 8.5% Gd and 1.5% Y, the balance being Mg and unavoidable impurities. The preparation method comprises the following steps:
the raw materials are proportioned: weighing magnesium ingot, zinc ingot, magnesium-nickel intermediate alloy, magnesium-copper intermediate alloy, magnesium-lanthanum-cerium-rare earth intermediate alloy, magnesium-zirconium intermediate alloy, magnesium-gadolinium intermediate alloy and magnesium-yttrium intermediate alloy according to the proportion.
And (3) melting and casting: placing magnesium ingots and zinc ingots into a resistance furnace, preserving heat at 750 ℃ until the magnesium ingots and zinc ingots are completely melted, then adding magnesium-nickel intermediate alloy, magnesium-copper intermediate alloy, magnesium-lanthanum-cerium-rare earth intermediate alloy, magnesium-zirconium intermediate alloy, magnesium-gadolinium intermediate alloy and magnesium-yttrium intermediate alloy, controlling the adding temperature to 770 ℃, preserving heat for half an hour after stirring until the magnesium ingots and zinc ingots are completely melted, and refining for 5min by using RJ-5 to obtain a soluble magnesium alloy melt; and casting the soluble magnesium alloy melt into a magnesium alloy cast ingot by adopting an electromagnetic semi-continuous casting method, wherein the electromagnetic frequency of 15Hz and the current of an electromagnetic system are set to be 100A in the casting process.
Extrusion pretreatment: homogenizing the magnesium alloy cast ingot: and (5) preserving heat for 16h at 470 ℃.
And (3) heat preservation extrusion: and (3) preserving the heat of the magnesium alloy ingot for 4 hours at 350 ℃, and extruding at a speed of 1.0mm/s to obtain a magnesium alloy bar with an extrusion ratio of 6.
And (3) extrusion post-treatment: and no.
Comparative example 2
Gao Jiangke magnesium-dissolving alloy consists of the following elements in percentage by mass: 0.5% Zn, 0.5% Cu, 0.2% Zr, 0.5% Ni, 0.5% La, 0.5% Ce, 8.5% Gd and 1.5% Y, the balance being Mg and unavoidable impurities. The preparation method comprises the following steps:
the raw materials are proportioned: weighing magnesium ingot, zinc ingot, magnesium-nickel intermediate alloy, magnesium-copper intermediate alloy, magnesium-lanthanum-cerium-rare earth intermediate alloy, magnesium-zirconium intermediate alloy, magnesium-gadolinium intermediate alloy and magnesium-yttrium intermediate alloy according to the proportion.
And (3) melting and casting: placing magnesium ingots, zinc ingots and RJ-2 into a resistance furnace, preserving heat at 750 ℃ until the magnesium ingots and the zinc ingots are completely melted, then adding magnesium-nickel intermediate alloy, magnesium-copper intermediate alloy, magnesium-lanthanum-cerium-rare earth intermediate alloy, magnesium-zirconium intermediate alloy, magnesium-gadolinium intermediate alloy and magnesium-yttrium intermediate alloy, controlling the adding temperature to 770 ℃, preserving heat for half an hour after stirring until the magnesium ingots and the zinc ingots are completely melted, and refining for 5 minutes by using RJ-5 to obtain a soluble magnesium alloy melt; and casting the soluble magnesium alloy melt into a magnesium alloy cast ingot by adopting an electromagnetic semi-continuous casting method, wherein the electromagnetic frequency of 15Hz and the current of an electromagnetic system are set to be 100A in the casting process.
Extrusion pretreatment: homogenizing treatment and pre-ageing treatment are carried out on the magnesium alloy cast ingot, and homogenizing treatment is carried out: preserving heat for 16h at 470 ℃; pre-ageing: preserving heat at 200 ℃ for 48 hours.
And (3) heat preservation extrusion: and (3) preserving the heat of the magnesium alloy ingot for 4 hours at 350 ℃, and extruding at a speed of 1.0mm/s to obtain a magnesium alloy bar with an extrusion ratio of 6.
And (3) extrusion post-treatment: and no.
Comparative example 3
Gao Jiangke magnesium-dissolving alloy consists of the following elements in percentage by mass: 0.5% Zn, 0.5% Cu, 0.2% Zr, 0.5% Ni, 0.5% La, 0.5% Ce, 8.5% Gd and 1.5% Y, the balance being Mg and unavoidable impurities. The preparation method comprises the following steps:
the raw materials are proportioned: weighing magnesium ingot, zinc ingot, magnesium-nickel intermediate alloy, magnesium-copper intermediate alloy, magnesium-lanthanum-cerium-rare earth intermediate alloy, magnesium-zirconium intermediate alloy, magnesium-gadolinium intermediate alloy and magnesium-yttrium intermediate alloy according to the proportion.
And (3) melting and casting: placing magnesium ingots, zinc ingots and RJ-2 into a resistance furnace, preserving heat at 750 ℃ until the magnesium ingots and the zinc ingots are completely melted, then adding magnesium-nickel intermediate alloy, magnesium-copper intermediate alloy, magnesium-lanthanum-cerium-rare earth intermediate alloy, magnesium-zirconium intermediate alloy, magnesium-gadolinium intermediate alloy and magnesium-yttrium intermediate alloy, controlling the adding temperature to 770 ℃, preserving heat for half an hour after stirring until the magnesium ingots and the zinc ingots are completely melted, and refining for 5 minutes by using RJ-5 to obtain a soluble magnesium alloy melt; and casting the soluble magnesium alloy melt into a magnesium alloy cast ingot by adopting an electromagnetic semi-continuous casting method, wherein the electromagnetic frequency of 15Hz and the current of an electromagnetic system are set to be 100A in the casting process.
Extrusion pretreatment: homogenizing the magnesium alloy cast ingot: and (5) preserving heat for 16h at 470 ℃.
And (3) heat preservation extrusion: and (3) preserving the heat of the magnesium alloy ingot for 4 hours at 350 ℃, and extruding at a speed of 1.0mm/s to obtain a magnesium alloy bar with an extrusion ratio of 6.
And (3) extrusion post-treatment: and (5) preserving the heat of the extruded magnesium alloy bar for 48 hours at 200 ℃ and then cooling.
Comparative example 4
Gao Jiangke magnesium-dissolving alloy consists of the following elements in percentage by mass: 0.5% Zn, 0.5% Cu, 0.2% Zr, 0.5% Ni, 0.5% La, 0.5% Ce, 8.5% Gd and 1.5% Y, the balance being Mg and unavoidable impurities. The preparation method comprises the following steps:
the raw materials are proportioned: weighing magnesium ingot, zinc ingot, magnesium-nickel intermediate alloy, magnesium-copper intermediate alloy, magnesium-lanthanum-cerium-rare earth intermediate alloy, magnesium-zirconium intermediate alloy, magnesium-gadolinium intermediate alloy and magnesium-yttrium intermediate alloy according to the proportion.
And (3) melting and casting: placing magnesium ingots and zinc ingots into a resistance furnace, preserving heat at 750 ℃ until the magnesium ingots and zinc ingots are completely melted, then adding magnesium-nickel intermediate alloy, magnesium-copper intermediate alloy, magnesium-lanthanum-cerium-rare earth intermediate alloy, magnesium-zirconium intermediate alloy, magnesium-gadolinium intermediate alloy and magnesium-yttrium intermediate alloy, controlling the adding temperature to 770 ℃, preserving heat for half an hour after stirring until the magnesium ingots and zinc ingots are completely melted, and refining for 5min by using RJ-5 to obtain a soluble magnesium alloy melt; and casting the soluble magnesium alloy melt into a magnesium alloy cast ingot by adopting an electromagnetic semi-continuous casting method, wherein the electromagnetic frequency of 15Hz and the current of an electromagnetic system are set to be 100A in the casting process.
Extrusion pretreatment: and no.
And (3) heat preservation extrusion: and (3) after the magnesium alloy ingot is kept at 450 ℃ for 4 hours, extruding at a speed of 3.0mm/s to obtain a magnesium alloy bar, wherein the extrusion ratio is 7.
And (3) extrusion post-treatment: and no.
Comparative example 5
Gao Jiangke magnesium-dissolving alloy consists of the following elements in percentage by mass: 2.0% Zn, 1.5% Cu, 0.5% Zr, 1.5% Ni, 7.5% Gd and 3.5% Y, the balance being Mg and unavoidable impurities. The preparation method comprises the following steps:
the raw materials are proportioned: weighing magnesium ingot, zinc ingot, magnesium-nickel intermediate alloy, magnesium-copper intermediate alloy, magnesium-zirconium intermediate alloy, magnesium-gadolinium intermediate alloy and magnesium-yttrium intermediate alloy according to the proportion.
And (3) melting and casting: placing magnesium ingots, zinc ingots and RJ-2 into a resistance furnace, preserving heat at 750 ℃ until the magnesium ingots are completely melted, then adding magnesium-nickel intermediate alloy, magnesium-copper intermediate alloy, magnesium-zirconium intermediate alloy, magnesium-gadolinium intermediate alloy and magnesium-yttrium intermediate alloy, controlling the addition temperature at 750 ℃, preserving heat for half an hour after stirring until the magnesium ingots and the zinc ingots are completely melted, and refining for 10 minutes by using RJ-5 to obtain a soluble magnesium alloy melt; the method is characterized in that a soluble magnesium alloy melt is cast into a magnesium alloy cast ingot by adopting an electromagnetic semi-continuous casting method, wherein the electromagnetic frequency of 30Hz is set in the casting process, and the current of an electromagnetic system is 110A.
Extrusion pretreatment: homogenizing treatment and pre-ageing treatment are carried out on the magnesium alloy cast ingot, and homogenizing treatment is carried out: preserving heat for 12h at 510 ℃; pre-ageing: preserving heat at 200 ℃ for 48 hours, and then air-cooling.
And (3) heat preservation extrusion: and (3) preserving the heat of the magnesium alloy ingot for 4 hours at 420 ℃, and extruding at a speed of 1.0mm/s to obtain a magnesium alloy bar with an extrusion ratio of 7.
And (3) extrusion post-treatment: and (5) preserving the heat of the extruded magnesium alloy bar for 54 hours at 200 ℃ and then cooling.
Comparative example 6
Gao Jiangke magnesium-dissolving alloy consists of the following elements in percentage by mass: 2.0% Zn, 1.5% Cu, 0.5% Zr, 1.5% Ni, 1.0% Sm, 0.5% La, 0.5% Ce, and the balance Mg and unavoidable impurities. The preparation method comprises the following steps:
The raw materials are proportioned: weighing magnesium ingot, zinc ingot, magnesium-nickel intermediate alloy, magnesium-copper intermediate alloy, magnesium-lanthanum-cerium-rare earth intermediate alloy, magnesium-samarium intermediate alloy and magnesium-zirconium intermediate alloy according to the proportion.
And (3) melting and casting: placing magnesium ingots, zinc ingots and RJ-2 into a resistance furnace, preserving heat at 750 ℃ until the magnesium ingots and the zinc ingots are completely melted, then adding magnesium-nickel intermediate alloy, magnesium-copper intermediate alloy, magnesium-lanthanum-cerium-rare earth intermediate alloy, magnesium-zirconium intermediate alloy and magnesium-samarium intermediate alloy, controlling the adding temperature to be 750 ℃, stirring until the magnesium ingots and the zinc ingots are completely melted, preserving heat for half an hour, and then refining for 10 minutes by using RJ-5 to obtain a soluble magnesium alloy melt; the method is characterized in that a soluble magnesium alloy melt is cast into a magnesium alloy cast ingot by adopting an electromagnetic semi-continuous casting method, wherein the electromagnetic frequency of 30Hz is set in the casting process, and the current of an electromagnetic system is 110A.
Extrusion pretreatment: homogenizing treatment and pre-ageing treatment are carried out on the magnesium alloy cast ingot, and homogenizing treatment is carried out: preserving heat for 12h at 510 ℃; pre-ageing: preserving heat at 200 ℃ for 48 hours, and then air-cooling.
And (3) heat preservation extrusion: and (3) preserving the heat of the magnesium alloy ingot for 4 hours at 420 ℃, and extruding at a speed of 1.0mm/s to obtain a magnesium alloy bar with an extrusion ratio of 7.
And (3) extrusion post-treatment: and (5) preserving the heat of the extruded magnesium alloy bar for 54 hours at 200 ℃ and then cooling.
Comparative example 7
Gao Jiangke magnesium-dissolving alloy consists of the following elements in percentage by mass: 0.9% Zn, 1.0% Cu, 0.3% Zr, 1.0% Ni, 6.5% Gd and 2.5% Y, the balance being Mg and unavoidable impurities. The preparation method comprises the following steps:
the raw materials are proportioned: weighing magnesium ingot, zinc ingot, magnesium-nickel intermediate alloy, magnesium-copper intermediate alloy, magnesium-zirconium intermediate alloy, magnesium-gadolinium intermediate alloy and magnesium-yttrium intermediate alloy according to the proportion.
And (3) melting and casting: placing magnesium ingots, zinc ingots and RJ-2 into a resistance furnace, preserving heat at 720 ℃ until the magnesium ingots and the zinc ingots are completely melted, then adding magnesium-nickel intermediate alloy, magnesium-copper intermediate alloy, magnesium-zirconium intermediate alloy, magnesium-gadolinium intermediate alloy and magnesium-yttrium intermediate alloy, controlling the adding temperature at 750 ℃, preserving heat for half an hour after stirring until the magnesium ingots and the zinc ingots are completely melted, and refining for 10min by using RJ-5 to obtain a soluble magnesium alloy melt; and casting the soluble magnesium alloy melt into a magnesium alloy cast ingot by adopting an electromagnetic semi-continuous casting method, wherein the electromagnetic frequency of 20Hz is set in the casting process, and the current of an electromagnetic system is 110A.
Extrusion pretreatment: homogenizing treatment and pre-ageing treatment are carried out on the magnesium alloy cast ingot, and homogenizing treatment is carried out: preserving heat for 14h at 500 ℃; pre-ageing: preserving heat for 64h at 200 ℃ and then air cooling.
And (3) heat preservation extrusion: and (3) preserving the heat of the magnesium alloy ingot for 6 hours at 400 ℃ and extruding at a speed of 2.0mm/s to obtain a magnesium alloy bar, wherein the extrusion ratio is 6.
And (3) extrusion post-treatment: and (5) preserving the heat of the extruded magnesium alloy bar for 48 hours at 200 ℃ and then cooling.
Comparative example 8
Gao Jiangke magnesium-dissolving alloy consists of the following elements in percentage by mass: 0.9% Zn, 1.0% Cu, 0.3% Zr, 1.0% Ni, 0.5% Sm, and the balance Mg and unavoidable impurities. The preparation method comprises the following steps:
The raw materials are proportioned: weighing magnesium ingot, zinc ingot, magnesium-nickel intermediate alloy, magnesium-copper intermediate alloy, magnesium-zirconium intermediate alloy and magnesium-samarium intermediate alloy according to the proportion.
And (3) melting and casting: placing magnesium ingots, zinc ingots and RJ-2 into a resistance furnace, preserving heat at 720 ℃ until the magnesium ingots and the zinc ingots are completely melted, then adding magnesium-nickel intermediate alloy, magnesium-copper intermediate alloy, magnesium-zirconium intermediate alloy and magnesium-samarium intermediate alloy, controlling the adding temperature at 750 ℃, preserving heat for half an hour after stirring until the magnesium ingots and the zinc ingots are completely melted, and refining for 10min by using RJ-5 to obtain a soluble magnesium alloy melt; the magnesium alloy cast ingot is obtained by adopting an electromagnetic semi-continuous casting method, wherein the electromagnetic frequency of 20Hz is set in the casting process, and the current of an electromagnetic system is 110A.
Extrusion pretreatment: homogenizing treatment and pre-ageing treatment are carried out on the magnesium alloy cast ingot, and homogenizing treatment is carried out: preserving heat for 14h at 500 ℃; pre-ageing: preserving heat for 64h at 200 ℃ and then air cooling.
And (3) heat preservation extrusion: and (3) preserving the heat of the magnesium alloy ingot for 6 hours at 400 ℃ and extruding at a speed of 2.0mm/s to obtain a magnesium alloy bar, wherein the extrusion ratio is 6.
And (3) extrusion post-treatment: and (5) preserving the heat of the extruded magnesium alloy bar for 48 hours at 200 ℃ and then cooling.
The magnesium alloy bars prepared in examples 1 to 4 and comparative examples 1 to 8 were subjected to mechanical properties and dissolution rate test, the dissolution rate test environment was 3.0wt.% KCl solution at 93 ℃, and the relevant test results are shown in table 1 below.
TABLE 1 mechanical Properties at Room temperature and dissolution Rate test for examples 1-4 and comparative examples 1-8
In conclusion, compared with the existing magnesium alloy, the magnesium alloy prepared by the preparation method of the high Jiang Kerong magnesium alloy has higher tensile strength and yield strength, so that the magnesium alloy has better mechanical properties.
The foregoing descriptions of specific exemplary embodiments of the present invention are presented for purposes of illustration and description. It is not intended to limit the invention to the precise form disclosed, and obviously many modifications and variations are possible in light of the above teaching. The exemplary embodiments were chosen and described in order to explain the specific principles of the invention and its practical application to thereby enable one skilled in the art to make and utilize the invention in various exemplary embodiments and with various modifications as are suited to the particular use contemplated. It is intended that the scope of the invention be defined by the claims and their equivalents.
Claims (6)
1. The high Jiang Kerong magnesium alloy is characterized by comprising the following components in percentage by mass: zn:0.5% -2.0%; cu:0.5% -1.5%; zr:0.2% -0.5%; ni:0.5% -1.5%, X:9.2% -13.0%; the balance of Mg and unavoidable impurity elements; wherein X is a combination of light rare earth elements and heavy rare earth elements, and the weight percentage of the light rare earth elements is as follows: 0.2% -2%, the weight percentage of the heavy rare earth elements is as follows: 9% -11%; the light rare earth element is selected from one or more of La, ce and Sm; the heavy rare earth element is selected from one or more of Y and Gd.
2. A method of preparing Gao Jiangke soluble magnesium alloy as claimed in claim 1, comprising:
the raw materials are proportioned: selecting magnesium ingots, zinc ingots, magnesium-zirconium intermediate alloys, magnesium-nickel intermediate alloys, magnesium-copper intermediate alloys, light rare earth alloys and heavy rare earth alloys as raw materials according to a certain proportion; wherein the light rare earth alloy is selected from one or more of magnesium lanthanum cerium rare earth intermediate alloy and magnesium samarium intermediate alloy; the heavy rare earth alloy is selected from one or more of magnesium yttrium intermediate alloy and magnesium gadolinium intermediate alloy;
and (3) melting and casting: sequentially adding the raw materials into a resistance furnace and melting at 720-750 ℃; casting the molten raw materials into magnesium alloy ingots by adopting an electromagnetic semi-continuous casting method at 750-770 ℃;
extrusion pretreatment: sequentially carrying out homogenization treatment and pre-ageing treatment on the magnesium alloy ingot;
And (3) heat preservation extrusion: the magnesium alloy cast ingot subjected to homogenization treatment and pre-ageing treatment is subjected to heat preservation for 4-6 hours at the temperature of 350-450 ℃ and then extruded to obtain a magnesium alloy bar;
And (3) extrusion post-treatment: and aging the extruded magnesium alloy bar.
3. The method for producing Gao Jiangke soluble magnesium alloy as defined in claim 2, wherein the surface of the raw material is covered with flux during the melting process; the flux is selected from one or more of RJ-2 and RJ-5.
4. The method for preparing Gao Jiangke mg-soluble alloy as claimed in claim 2, wherein the electromagnetic semi-continuous casting process has a current of 100A to 120A and a frequency of 15Hz to 30 Hz.
5. The method for preparing Gao Jiangke mg-soluble alloy as claimed in claim 2, wherein the homogenization treatment is: the magnesium alloy ingot is subjected to heat preservation for 12 to 16 hours at 470 to 520 ℃ and then is cooled; the pre-ageing treatment is as follows: the magnesium alloy ingot is subjected to heat preservation for 48 to 84 hours at the temperature of 190 to 210 ℃; the aging treatment is as follows: and (3) preserving the heat of the extruded magnesium alloy bar for 48-72 h at the temperature of 190-210 ℃.
6. The method for preparing Gao Jiangke dissolved magnesium alloy as defined in claim 2, wherein the extrusion speed of the magnesium alloy bar is between 0.5mm/s and 3 mm/s; the extrusion ratio of the magnesium alloy bar is between 6 and 7.
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