CN114273645B - Method for preparing ultrafine grain material by high-frequency vibration - Google Patents
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- 238000000034 method Methods 0.000 title claims abstract description 32
- 239000000463 material Substances 0.000 title claims abstract description 30
- 239000007769 metal material Substances 0.000 claims abstract description 42
- 239000013078 crystal Substances 0.000 claims abstract description 22
- 230000001133 acceleration Effects 0.000 claims abstract description 18
- 239000007787 solid Substances 0.000 claims description 17
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 11
- 238000001816 cooling Methods 0.000 claims description 10
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 5
- 230000001681 protective effect Effects 0.000 claims description 5
- 229910052786 argon Inorganic materials 0.000 claims description 4
- 229910000881 Cu alloy Inorganic materials 0.000 claims description 2
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 238000002360 preparation method Methods 0.000 abstract description 5
- 239000000155 melt Substances 0.000 abstract description 3
- 229910052751 metal Inorganic materials 0.000 description 22
- 239000002184 metal Substances 0.000 description 22
- 229910052782 aluminium Inorganic materials 0.000 description 15
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 15
- 230000000052 comparative effect Effects 0.000 description 11
- 229910001369 Brass Inorganic materials 0.000 description 7
- 239000010951 brass Substances 0.000 description 7
- 230000006911 nucleation Effects 0.000 description 3
- 238000010899 nucleation Methods 0.000 description 3
- 238000004321 preservation Methods 0.000 description 3
- 239000007858 starting material Substances 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 239000004411 aluminium Substances 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000007711 solidification Methods 0.000 description 2
- 230000008023 solidification Effects 0.000 description 2
- 229910000601 superalloy Inorganic materials 0.000 description 2
- 238000009864 tensile test Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- 229910000851 Alloy steel Inorganic materials 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910001128 Sn alloy Inorganic materials 0.000 description 1
- 229910001069 Ti alloy Inorganic materials 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 239000012056 semi-solid material Substances 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
Abstract
The invention relates to a new method for preparing ultrafine grain materials, which is characterized in that the semisolid metal materials are vibrated at high frequency to obtain super-strong motion acceleration, and in the process of forming the nucleus of a melt, the high-intensity sound waves generated by the super-strong motion acceleration can realize repeated breaking of crystal nuclei, so that the newly formed crystal nuclei are broken to be less than 10 mu m, even reach the nanoscale level, and finally the solidified ultrafine grains are realized, thereby obtaining the ultrafine grain materials. The high-frequency vibration can be utilized to realize the efficient preparation of the superfine crystal material, and the production cost is low and the process flow is simple.
Description
Technical Field
The invention relates to the technical field of processing and preparation of superfine crystal materials, in particular to a method for preparing superfine crystal materials by utilizing high-frequency vibration.
Background
The superfine crystal material (the grain size is 0.1-10 mu m) has excellent comprehensive mechanical property, good physical property and good corrosion resistance, and has important value and wide application prospect in the fields of industrial production and aerospace military industry. As known from Hall-Patch relation, the mechanical property of metal is inversely proportional to the grain size of the material, and ultra-fine grain strengthening is one of effective methods for improving the mechanical property of the metal material; meanwhile, after grain refinement, the composition uniformity, corrosion resistance and even physical properties of the metal material are obviously improved. However, in the actual production process, the preparation efficiency of the ultra-fine grain material is low, the production cost is high, and the process flow is complex.
Accordingly, the present invention has been made.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a novel method for preparing an ultrafine grain material, which is characterized in that the semisolid metal material is subjected to high-frequency vibration so as to obtain super-strong movement acceleration, the high-intensity sound wave generated by the super-strong movement acceleration can realize repeated breaking of crystal nucleus in the melt nucleation process, the newly formed crystal nucleus is broken to be less than 10 mu m, even to reach nanoscale level, and finally the solidified ultrafine grain is realized, so that the ultrafine grain material is obtained. The high-frequency vibration can be utilized to realize the efficient preparation of the superfine crystal material, and the production cost is low and the process flow is simple.
In order to achieve the above object, the present invention provides the following technical solutions.
A method of preparing an ultra-fine grain material comprising the steps of:
the semi-solid metal material is vibrated at the motion acceleration of 20-150G, and is solidified after vibration is stopped, so that the ultra-fine grain material is obtained.
Preferably, the motion acceleration may be, for example, 20G, 30G, 40G, 50G, 60G, 70G, 80G, 90G, 100G, 105G, 110G, 115G, 120G, 125G, 130G, 135G, 140G, 145G, or 150G. Preferably, the movement acceleration is 105-150G, preferably 120-150G. In the present invention, "G" is a gravitational acceleration. The grain size of the ultra-fine grain material is required to be smaller, and the energy input in the solidification process needs to be ensured to be large enough, so that the grain boundary is crushed to a smaller scale in the nucleation process, the larger the movement acceleration is in a certain range, the larger the sound wave energy input is easy to realize, and the crystal nucleus structure with smaller grain size is realized.
Preferably, the frequency F of the vibration is 20-500Hz, preferably 100-500Hz; amplitude A is 1-20mm, preferably 1-15mm; the vibration time is 1-60min, preferably 5-20min.
Preferably, the method of the invention is carried out in a high-frequency vibration device comprising a spring array combined in multiple stages, the effect of resonance of the vibration table and the melt being achieved by means of a multiple-stage vibration system. By adjusting the vibration frequency F and the vibration amplitude A of the high-frequency vibration device, the semisolid metal material is ensured to obtain enough movement acceleration. The high-intensity sound wave energy generated by the ultra-strong motion acceleration is utilized to realize repeated breaking of crystal nucleus, and finally, the solidified superfine crystal grains are realized, and the grain size distribution is concentrated, so that the superfine crystal material is formed.
Preferably, the forming of the semi-solid metal material includes: heating the metal material to melt the metal material, thereby obtaining a metal material melt; and cooling the metal material melt to obtain the semi-solid metal material. By means of the method that the material is completely melted and then cooled to form the semi-solid material, uniformity of the material after the metal material is completely melted can be guaranteed, and therefore tissue guarantee is provided for forming non-segregation semi-solid after subsequent solidification.
Preferably, the metal material is copper, copper alloy, aluminum alloy, titanium alloy, tin alloy, iron, alloy steel, superalloy, specialty metal or alloy of specialty metal. The superalloy refers to a metallic material capable of operating at high temperatures above 600 ℃. The special metal is a metal with a melting point of more than 2000 ℃.
Preferably, the metal material is heated in a protective atmosphere, melted and stirred. The protective atmosphere may be nitrogen or argon. Heating under a protective atmosphere can prevent the metal material from being oxidized during the heating process.
Preferably, the metallic material is heated to a temperature 60-100 ℃ above its liquidus temperature. This ensures a sufficient degree of superheat to completely melt the metallic material.
Preferably, the metal material melt is cooled to a temperature 20-60 ℃, preferably 30-50 ℃, above the solidus temperature of the metal material. When the cooling temperature is lower than 20 ℃ below solidus, the metal melt can be quickly solidified, and the process window time of the follow-up vibration breaking crystal nucleus cannot be ensured; when the cooling temperature is higher than the solidus 60 ℃, the superheat degree of the metal melt is larger, the phenomenon that the ultra-fine crystal nucleus structure obtained through vibration is easy to continue growing is easy to occur, the ultra-fine crystal nucleus in the solidified material structure cannot be ensured, and effective grain refinement cannot be realized.
Preferably, the semi-solid metal material is in a heat-retaining state during the vibration. The temperature of the semi-solid metal material is 20-60 c, preferably 30-50 c, higher than the solidus temperature of the metal material.
Preferably, after stopping the vibration, the semi-solid metal material is allowed to cool (e.g., naturally cool) and solidify.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention provides a new method for preparing an ultrafine grain material, which is characterized in that the semisolid metal material is subjected to high-frequency vibration so as to obtain super-strong motion acceleration, and in the process of melt nucleation, high-intensity sound waves generated by the super-strong motion acceleration can realize repeated breaking of crystal nucleus, so that the newly formed crystal nucleus is broken to be less than 10 mu m, even to reach nanoscale level, and finally, solidified ultrafine grains are realized, so that the ultrafine grain material is obtained. The high-frequency vibration can be utilized to realize the efficient preparation of the superfine crystal material, and the production cost is low and the process flow is simple.
2. The method has the advantages of easily obtained raw materials, simple equipment, low energy consumption, low impurity content and good safety, is suitable for preparing the metal ultrafine crystal materials of most systems, and is suitable for large-scale popularization and application.
3. The superfine crystal material obtained by the method has small average grain size, concentrated grain size distribution and stable product performance.
Drawings
FIG. 1 is a schematic representation of an apparatus used in the method of the present invention.
Reference numerals illustrate:
1 is a container, 2 is a heating system, 3 is a fixing device, 4 is a vibrating device, and 5 is a monitoring sensor.
Detailed Description
In order to make the contents of the present invention more easily understood, the technical scheme of the present invention will be further described with reference to the specific embodiments, but the present invention is not limited thereto. All techniques implemented based on the above description of the invention are intended to be included within the scope of the invention. Unless otherwise indicated, the starting materials used in the examples were all commercially available. The raw materials, instruments or procedures not described herein are those conventionally identified by one of ordinary skill in the art. The present invention uses the apparatus shown in fig. 1 to produce ultra-fine grained material.
Example 1
10kg of pure aluminum ingot (brand 1060) is placed in a container of the device shown in fig. 1, nitrogen is filled after vacuumizing, and the pure aluminum ingot is heated to 870 ℃ (the superheat degree is 100 ℃) under the protection of the nitrogen, so that the pure aluminum ingot is completely melted, and a metal melt is obtained. After the metal melt is stirred uniformly, the temperature is reduced to 700-720 ℃ (30-50 ℃ above solidus temperature), so that semi-solid metal is obtained. And then starting a vibration controller, setting the vibration frequency to be 100Hz and the vibration amplitude to be 15mm so as to enable the semi-solid metal to reach 105G acceleration, continuously vibrating for 10 minutes under the condition of heat preservation, stopping vibrating, guiding into a specific water-cooling mould, and cooling and solidifying to obtain the ultra-fine grain aluminum ingot.
Example 2
2kg of brass ingots (brand C2680-H) were placed in a vessel of the apparatus shown in FIG. 1, evacuated and then filled with argon, and the brass ingots were heated to 1200 ℃ under the protection of argon (super-heated 60 ℃) to completely melt the brass ingots, thereby obtaining a metal melt. After the metal melt is stirred uniformly, the temperature is reduced to 980-1000 ℃ (30-50 ℃ above solidus temperature), so that semi-solid metal is obtained. Starting a vibration controller, setting the vibration frequency to be 500Hz and the vibration amplitude to be 1mm so as to enable the semi-solid metal melt to reach the acceleration of 150G, continuously vibrating for 10 minutes under the condition of heat preservation, stopping vibrating, guiding into a specific water-cooling mould, and cooling and solidifying to obtain the ultra-fine grain brass ingot.
Comparative example 1
Conventional pure aluminum ingots (trade name 1060), the starting materials used in example 1.
Comparative example 2
Conventional brass ingots (trade name C2680-H), the starting materials used in example 2.
Comparative example 3
10kg of pure aluminum ingot (brand 1060) is placed in a container of the device shown in fig. 1, nitrogen is filled after vacuumizing, and the pure aluminum ingot is heated to 870 ℃ (the superheat degree is 100 ℃) under the protection of the nitrogen, so that the pure aluminum ingot is completely melted, and a metal melt is obtained. After the metal melt is stirred uniformly, the temperature is reduced to 750 ℃ (80 ℃ above solidus temperature), so that semi-solid metal is obtained. And then starting a vibration controller, setting the vibration frequency to be 100Hz and the vibration amplitude to be 15mm so as to enable the semi-solid metal to reach 105G acceleration, continuously vibrating for 10 minutes under the condition of heat preservation, stopping vibrating, guiding into a specific water-cooling mould, and cooling and solidifying to obtain the ultra-fine grain aluminum ingot.
Performance testing
The average grain sizes of the ultra-fine grain materials obtained in examples 1 and 2 and comparative examples 1 to 3 were measured by an Electron Back Scattering Diffraction (EBSD) test, and the results are shown in table 1.
TABLE 1
| Metal material | Average grain size (μm) | |
| Example 1 | Ultra-fine grain aluminum ingot | 0.75 |
| Example 2 | Ultra-fine brass ingot | 0.23 |
| Comparative example 1 | Pure metal aluminium ingot (brand 1060) | 6.82 |
| Comparative example 2 | Huang Tongding (brand C2680-H) | 8.45 |
| Comparative example 3 | Ultra-fine grain aluminum ingot | 4.02 |
The ultra-fine grain materials obtained in examples 1 and 2 and comparative examples 1 to 3 were subjected to tensile test at room temperature using GB/T228-2010 (metallic material tensile test room temperature test method), and the results are shown in Table 2 below.
TABLE 2
| Metal material | Tensile strength (MPa) | Elongation (%) | |
| Example 1 | Ultra-fine grain aluminum ingot | 238 | 22％ |
| Example 2 | Ultra-fine brass ingot | 956 | 28％ |
| Comparative example 1 | Pure metal aluminium ingot (brand 1060) | 130 | 5％ |
| Comparative example 2 | Huang Tongding (brand C2680-H) | 518 | 15％ |
| Comparative example 3 | Ultra-fine grain aluminum ingot | 187 | 12％ |
The present invention is not limited to the above-mentioned embodiments, and any changes or substitutions that can be easily understood by those skilled in the art within the technical scope of the present invention are intended to be included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (7)
1. A method for preparing an ultra-fine grain material, comprising the steps of:
vibrating the semi-solid metal material at a motion acceleration of 120-150G, and solidifying the semi-solid metal material after stopping vibrating, thereby obtaining an ultrafine crystal material;
the forming of the semi-solid metal material includes:
heating the metal material to melt the metal material, thereby obtaining a metal material melt; and
cooling the metal material melt to a temperature 20-60 ℃ higher than the solidus temperature of the metal material, thereby obtaining the semi-solid metal material;
wherein G is gravitational acceleration.
2. The method according to claim 1, wherein the vibration has a frequency F of 20-500Hz, an amplitude a of 1-20mm and a vibration time of 1-60min.
3. The method according to claim 2, characterized in that the frequency F of the vibration is 100-500Hz; amplitude A is 1-15mm; the vibration time is 5-20min.
4. The method of claim 1, wherein the metal material melt is cooled to a temperature 30-50 ℃ above the solidus temperature of the metal material.
5. The method of claim 1, wherein the metallic material is a copper alloy.
6. The method according to claim 1, wherein the metal material is heated in a protective atmosphere and stirred after being melted.
7. The method of claim 6, wherein the protective atmosphere is nitrogen or argon.
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| US3669180A (en) * | 1971-01-20 | 1972-06-13 | United Aircraft Corp | Production of fine grained ingots for the advanced superalloys |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US6638381B2 (en) * | 2001-12-18 | 2003-10-28 | The Boeing Company | Method for preparing ultra-fine grain titanium and titanium-alloy articles and articles prepared thereby |
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|---|---|---|---|---|
| US3669180A (en) * | 1971-01-20 | 1972-06-13 | United Aircraft Corp | Production of fine grained ingots for the advanced superalloys |
| GB1594977A (en) * | 1976-12-29 | 1981-08-05 | Langenecker B | Method of and apparatus for solidifying molten metal or metal alloy |
| US4832112A (en) * | 1985-10-03 | 1989-05-23 | Howmet Corporation | Method of forming a fine-grained equiaxed casting |
| US5186236A (en) * | 1990-12-21 | 1993-02-16 | Alusuisse-Lonza Services Ltd. | Process for producing a liquid-solid metal alloy phase for further processing as material in the thixotropic state |
| US5901778A (en) * | 1996-05-07 | 1999-05-11 | Agency Of Industrial Science & Technology, Ministry Of International Trade & Industry | Method of manufacturing metallic materials with extremely fine crystal grains |
| US7509993B1 (en) * | 2005-08-13 | 2009-03-31 | Wisconsin Alumni Research Foundation | Semi-solid forming of metal-matrix nanocomposites |
| CN1995419A (en) * | 2006-12-21 | 2007-07-11 | 上海交通大学 | Method of making ultrafine crystal deformed aluminium alloy |
| JP2014213330A (en) * | 2013-04-23 | 2014-11-17 | 愛三工業株式会社 | Production method of semi-solidified metal slurry |
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| CN106111950A (en) * | 2016-08-19 | 2016-11-16 | 北京科技大学 | A kind of casting has nanometer and the apparatus and method of micron mix-crystal kernel structure material |
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