CN113373329A - Preparation method of nano gradient magnesium alloy - Google Patents
Preparation method of nano gradient magnesium alloy Download PDFInfo
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- CN113373329A CN113373329A CN202110533733.1A CN202110533733A CN113373329A CN 113373329 A CN113373329 A CN 113373329A CN 202110533733 A CN202110533733 A CN 202110533733A CN 113373329 A CN113373329 A CN 113373329A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C23/00—Alloys based on magnesium
- C22C23/06—Alloys based on magnesium with a rare earth metal as the next major constituent
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/06—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of magnesium or alloys based thereon
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Abstract
The invention relates to a preparation method of a nano gradient magnesium alloy, belonging to the technical field of high-strength magnesium alloy preparation. Homogenizing a semi-continuous casting blank, extruding the casting blank into a bar material, wherein the extrusion temperature is 430-480 ℃, the extrusion ratio is 13: 1-16: 1, performing peak aging treatment on an extruded alloy, keeping the temperature at 225 ℃ for 16-20 h, then performing surface mechanical grinding treatment SMAT, performing SMAT at room temperature for 60-120 min, and obtaining a wafer-shaped nano gradient magnesium alloy plate with the thickness of 2.5-5 mm and the diameter of 49 mm. The invention effectively improves the alloy strength and obtains better strength and plasticity combination.
Description
Technical Field
The invention relates to a preparation method of a nano gradient magnesium alloy, belonging to the technical field of high-strength magnesium alloy preparation.
Background
The magnesium alloy has the advantages of low density, high specific strength, good electrical and thermal conductivity and the like, and has wide application prospect in the fields of aerospace, national defense, transportation and the like. However, the lower absolute strength and poor ductility of magnesium alloys limits their further development. Researches find that magnesium alloy added with rare earth elements such as Gd, Y and the like has excellent solid solution strengthening and precipitation hardening effects and can be processed in a mode of combining deformation strengthening. The deformation processes of rolling, hot extrusion and the like of Mg-Gd-Y alloy have been studied, wherein the extruded alloy generally shows a uniform and fine grain structure, and the alloy often has better mechanical properties than the alloy after hot rolling in combination with subsequent aging treatment. However, the grain size can only be refined to about 10 μm by simply adopting extrusion deformation, and the fine grain strengthening potential of the magnesium alloy cannot be fully reflected. Therefore, how to further stimulate the material potential on the basis of the above, and the improvement of the performance becomes a key.
The Surface Mechanical Attack Treatment (SMAT) carries out irregular impact through metal shot, so that the Surface of the material is violently deformed at a certain depth to obtain ultrafine grains from nano level to submicron level, and a thicker microstructure is still reserved in an area which is close to the core and is less affected by strain to form a non-homogeneous gradient structure, thereby effectively improving the toughness of the material.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a preparation method of a nano gradient magnesium alloy, which is used for solving the problem of the performance of a magnesium alloy material
The invention adopts the following technical scheme:
a preparation method of a nano gradient magnesium alloy comprises the following steps:
the method comprises the following steps: the magnesium alloy ingot is prepared by adopting a semi-continuous casting method, and the magnesium alloy ingot comprises the following components in percentage by mass:
gd: 8.0 to 9.5; y: 2.0 to 3.5; zr: 0.3 to 0.7; the balance being Mg;
step two: homogenizing magnesium alloy ingots;
step three: carrying out extrusion deformation on the homogenized blank, specifically: homogenizing a semi-continuous casting magnesium alloy ingot, extruding the homogenized casting magnesium alloy ingot into a bar to form an extruded alloy, wherein the extrusion temperature is 430-480 ℃, and the extrusion ratio is 13: 1-16: 1;
step four: performing peak aging treatment on the extruded alloy, namely keeping the temperature at 225 ℃ for 16-20 h;
step five: performing surface mechanical grinding treatment SMAT on the extruded alloy, wherein the SMAT is performed at room temperature, the SMAT vibration frequency is 50Hz, and the total grinding time of the steel ball with the diameter of 4-8 mm is 60-120 min;
step six: performing stress relief annealing on the extruded alloy subjected to the SMAT treatment by surface mechanical grinding, wherein the annealing parameter is 200 ℃ and the temperature is kept for 2 h;
step seven: the wafer-shaped nanometer gradient magnesium alloy plate with the thickness of 2.5-5 mm and the diameter of 49mm is prepared through the steps, the grain size of the wafer-shaped nanometer gradient magnesium alloy plate is gradually increased from 50-250 nm to 10-30 mu m from the surface to the core of the plate, and through a room temperature tensile test, the tensile strength of the alloy at room temperature is more than or equal to 440MPa, the yield strength is more than or equal to 380MPa, and the elongation is more than or equal to 3%.
Further, the SMAT is ground by a grinding tank body, the top of the grinding tank body is provided with the disk-shaped extruded alloy, and the grinding tank body is internally provided with stainless steel shot.
Furthermore, the wafer-shaped nanometer gradient magnesium alloy plate comprises a violent deformation layer, a medium deformation layer and a matrix layer from the processing surface to the center of the plate.
Further, the plate is 0-300 mu m thick downwards from the processing surface and is the severe deformation layer, and the grain size of the plate is gradually increased from 50nm to more than 250 nm; a medium deformation layer with the thickness of 300-600 mu m downwards from the processing surface of the plate, and sub-crystals and twin crystals are formed inside the original extruded crystal grains; the thickness of the base layer is more than 600 mu m downwards from the processing surface of the plate.
Further, in the room temperature tensile test, the strain rate is 5 × 10-4s-1。
Further, preferably, the extrusion temperature in the third step is 450 ℃, and the extrusion ratio is 15: 1; carrying out middle peak aging treatment in the fourth step and preserving heat for 18 h; in the fifth step, the total grinding time of the steel ball with the diameter of 5mm is 100 min.
The technical scheme of the invention achieves the following technical effects:
firstly, the surface mechanical grinding treatment is adopted for room temperature deformation, so that the grain size of the surface of the magnesium alloy workpiece can be thinned to a nanometer level or a submicron level, and compared with other room temperature deformation processes such as cold rolling, the large-area cracking of the workpiece is avoided, and the grain refined structure is effectively obtained.
Secondly, by adopting surface mechanical grinding treatment, a nanocrystalline structure on the surface is gradually transited to a submicron crystal and a micron crystal structure at the center of the test piece in the magnesium alloy test piece to obtain a gradient structure, so that the alloy strength is effectively improved, the yield strength can be improved by more than 70MPa and the tensile strength is improved by more than 35MPa compared with the extrusion aging state, and meanwhile, the alloy retains certain plasticity to obtain better strength and plasticity combination.
Drawings
In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings used in the examples or the prior art descriptions are briefly introduced below.
FIG. 1 is a diagram of SMAT process;
FIG. 2 is a metallographic photograph of a nano-gradient magnesium alloy structure of the present invention after SMAT;
FIG. 3 is a TEM image of a severe deformation layer on the surface of the nano gradient magnesium alloy after SMAT: bright field image, dark field image.
Detailed Description
The following detailed description of the present invention will be made with reference to the accompanying fig. 1-3 and examples, but the present invention should not be limited to the examples.
The preparation method of the nano gradient magnesium alloy of the embodiment comprises the following steps:
the method comprises the following steps: the magnesium alloy ingot is prepared by adopting a semi-continuous casting method, and the magnesium alloy ingot comprises the following components in percentage by mass:
gd: 8.0 to 9.5; y: 2.0 to 3.5; zr: 0.3 to 0.7; the balance being Mg.
Step two: and homogenizing the magnesium alloy ingot.
Step three: carrying out extrusion deformation on the homogenized blank, specifically: homogenizing a semi-continuous casting magnesium alloy ingot, extruding the ingot into a bar to form an extruded alloy, wherein the extrusion temperature is 4350 ℃, and the extrusion ratio is 15: 1.
Step four: and (4) carrying out peak aging treatment on the extruded alloy, namely keeping the temperature at 225 ℃ for 18 h.
Step five: the surface mechanical grinding SMAT is carried out on the extruded alloy, the SMAT is carried out at room temperature, the grinding can body 1 is adopted for grinding, the top of the grinding can body 1 is provided with a disk-shaped extruded alloy 2, and the grinding can body 1 is internally provided with a stainless steel shot 3. The SMAT vibration frequency is 50Hz, and the total grinding time of the steel ball with the diameter of 5mm is 100 min.
Step six: and (3) performing stress relief annealing on the extruded alloy subjected to the SMAT treatment by surface mechanical grinding, wherein the annealing parameter is 200 ℃ and the temperature is kept for 2 h.
Step seven: the wafer-shaped nanometer gradient magnesium alloy plate with the thickness of 2.5-5 mm and the diameter of 49mm is prepared through the steps, and the grain size of the wafer-shaped nanometer gradient magnesium alloy plate is gradually increased from 50-250 nm to 10-30 mu m from the surface to the center of the plate.
Cutting a tensile sample with the thickness of 700 mu m from the plate with the mechanically ground surface along the surface, mechanically grinding the rough layer with the thickness of 100 mu m of the outer surface, and adopting the strain rate of 5 multiplied by 10 in the room temperature tensile test-4s-1The tensile strength of the alloy at room temperature is more than or equal to 440MPa, the yield strength is more than or equal to 380MPa, and the elongation is more than or equal to 3%.
After testing and surface mechanical grinding treatment, the wafer-shaped nanometer gradient magnesium alloy plate is divided into a violent deformation layer 4, a medium deformation layer 5 and a matrix layer 6 from the processed surface to the center of the plate. The thickness of the plate is 0-300 mu m from the processing surface downwards to form a severe deformation layer 4, and the grain size of the plate is gradually increased from 50nm to more than 250 nm. The thickness of the medium deformation layer 5 is 300-600 mu m downwards from the processing surface of the plate, and sub-crystals and twin crystals are formed inside original extruded crystal grains. The substrate layer 6 is thicker than 600 μm from the processed surface of the plate material.
The obtained nano gradient magnesium alloy is subjected to mechanical property test comparison according to GB/T228-2002, and the results are shown in Table 1. Compared with the extrusion + aging state sample without SMAT treatment, the tensile strength is increased by 34.5MPa, the yield strength is increased by 73.7MPa, the elongation is only reduced by 1.5 percent, and the unexpected strength effect is achieved.
TABLE 1 comparison of mechanical properties of nano-gradient magnesium alloys before and after SMAT
The above-mentioned embodiments are only given for the purpose of more clearly illustrating the technical solutions of the present invention, and are not meant to be limiting, and variations of the technical solutions of the present invention by those skilled in the art based on the common general knowledge in the art are also within the scope of the present invention.
Claims (6)
1. The preparation method of the nano gradient magnesium alloy is characterized by comprising the following steps of:
the method comprises the following steps: the magnesium alloy ingot is prepared by adopting a semi-continuous casting method, and the magnesium alloy ingot comprises the following components in percentage by mass:
gd: 8.0 to 9.5; y: 2.0 to 3.5; zr: 0.3 to 0.7; the balance being Mg;
step two: homogenizing magnesium alloy ingots;
step three: carrying out extrusion deformation on the homogenized blank, specifically: homogenizing a semi-continuous casting magnesium alloy ingot, extruding the homogenized casting magnesium alloy ingot into a bar to form an extruded alloy, wherein the extrusion temperature is 430-480 ℃, and the extrusion ratio is 13: 1-16: 1;
step four: performing peak aging treatment on the extruded alloy, namely keeping the temperature at 225 ℃ for 16-20 h;
step five: performing surface mechanical grinding treatment SMAT on the extruded alloy, wherein the SMAT is performed at room temperature, the SMAT vibration frequency is 50Hz, and the total grinding time of the steel ball with the diameter of 4-8 mm is 60-120 min;
step six: performing stress relief annealing on the extruded alloy subjected to the SMAT treatment by surface mechanical grinding, wherein the annealing parameter is 200 ℃ and the temperature is kept for 2 h;
step seven: the wafer-shaped nanometer gradient magnesium alloy plate with the thickness of 2.5-5 mm and the diameter of 49mm is prepared through the steps, the grain size of the wafer-shaped nanometer gradient magnesium alloy plate is gradually increased from 50-250 nm to 10-30 mu m from the surface to the core of the plate, and through a room temperature tensile test, the tensile strength of the alloy at room temperature is more than or equal to 440MPa, the yield strength is more than or equal to 380MPa, and the elongation is more than or equal to 3%.
2. The method for preparing the nano-gradient magnesium alloy according to claim 1, wherein the method comprises the following steps: the SMAT is ground by a grinding tank body (1), the top of the grinding tank body (1) is provided with a disk-shaped extrusion alloy (2), and a stainless steel shot (3) is arranged inside the grinding tank body (1).
3. The method for preparing the nano-gradient magnesium alloy according to claim 2, wherein the method comprises the following steps: the disc-shaped nanometer gradient magnesium alloy plate comprises a violent deformation layer (4), a medium deformation layer (5) and a matrix layer (6) from the processing surface to the center of the plate.
4. The method for preparing the nano-gradient magnesium alloy according to claim 3, wherein the method comprises the following steps: the thickness of the plate is 0-300 mu m from the processing surface downwards to form the violent deformation layer (4), and the grain size of the plate is gradually increased from 50nm to more than 250 nm; a medium deformation layer (5) with the thickness of 300-600 mu m downwards from the processing surface of the plate, and sub-crystals and twin crystals are formed inside the original extruded crystal grains; the thickness of the base layer (6) is more than 600 mu m downwards from the processing surface of the plate.
5. The method for preparing the nano-gradient magnesium alloy according to claim 1, wherein the method comprises the following steps: in the room temperature tensile test, the strain rate is 5 multiplied by 10-4s-1。
6. The method for preparing the nano-gradient magnesium alloy according to claim 1, wherein the method comprises the following steps: in the third step, the extrusion temperature is 450 ℃, and the extrusion ratio is 15: 1; carrying out middle peak aging treatment in the fourth step and preserving heat for 18 h; in the fifth step, the total grinding time of the steel ball with the diameter of 5mm is 100 min.
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Cited By (5)
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| CN113174550A (en) * | 2021-03-12 | 2021-07-27 | 江苏大学 | Preparation method of ultra-high-strength high-toughness nano-gradient twin-crystal magnesium alloy |
| CN113308626A (en) * | 2020-02-27 | 2021-08-27 | 南京理工大学 | Nickel-based alloy containing gradient nano-structure and preparation method thereof |
| CN114574791A (en) * | 2022-01-24 | 2022-06-03 | 苏州卓恰医疗科技有限公司 | Magnesium alloy hollow screw and preparation method thereof |
| CN115094357A (en) * | 2022-06-28 | 2022-09-23 | 西北有色金属研究院 | Method for realizing fusion of single-phase layer on surface of dual-phase Mg-Li alloy plate at room temperature |
| CN117448713A (en) * | 2023-12-26 | 2024-01-26 | 华北理工大学 | Low-temperature superplastic forming method of rare earth magnesium alloy |
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| CN114574791A (en) * | 2022-01-24 | 2022-06-03 | 苏州卓恰医疗科技有限公司 | Magnesium alloy hollow screw and preparation method thereof |
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| CN115094357A (en) * | 2022-06-28 | 2022-09-23 | 西北有色金属研究院 | Method for realizing fusion of single-phase layer on surface of dual-phase Mg-Li alloy plate at room temperature |
| CN115094357B (en) * | 2022-06-28 | 2022-11-22 | 西北有色金属研究院 | Method for realizing fusion of single-phase layer on surface of double-phase Mg-Li alloy plate at room temperature |
| CN117448713A (en) * | 2023-12-26 | 2024-01-26 | 华北理工大学 | Low-temperature superplastic forming method of rare earth magnesium alloy |
| CN117448713B (en) * | 2023-12-26 | 2024-03-15 | 华北理工大学 | Low-temperature superplastic forming method of rare earth magnesium alloy |
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Application publication date: 20210910 |