CN114273645A - Method for preparing ultrafine crystal material by utilizing high-frequency vibration - Google Patents
Method for preparing ultrafine crystal material by utilizing high-frequency vibration Download PDFInfo
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- CN114273645A CN114273645A CN202111619906.8A CN202111619906A CN114273645A CN 114273645 A CN114273645 A CN 114273645A CN 202111619906 A CN202111619906 A CN 202111619906A CN 114273645 A CN114273645 A CN 114273645A
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- 239000000463 material Substances 0.000 title claims abstract description 32
- 238000000034 method Methods 0.000 title claims abstract description 32
- 239000013078 crystal Substances 0.000 title abstract description 30
- 239000007769 metal material Substances 0.000 claims abstract description 43
- 230000001133 acceleration Effects 0.000 claims abstract description 18
- 229910052751 metal Inorganic materials 0.000 claims description 31
- 239000002184 metal Substances 0.000 claims description 31
- 239000007787 solid Substances 0.000 claims description 27
- 238000001816 cooling Methods 0.000 claims description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 11
- 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
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 4
- 229910045601 alloy Inorganic materials 0.000 claims description 4
- 239000000956 alloy Substances 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 4
- 229910000838 Al alloy Inorganic materials 0.000 claims description 2
- 229910000851 Alloy steel Inorganic materials 0.000 claims description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 2
- 229910000881 Cu alloy Inorganic materials 0.000 claims description 2
- 229910001128 Sn alloy Inorganic materials 0.000 claims description 2
- 229910001069 Ti alloy Inorganic materials 0.000 claims description 2
- 229910052802 copper Inorganic materials 0.000 claims description 2
- 239000010949 copper Substances 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
- 150000002739 metals Chemical class 0.000 claims 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims 1
- 229910000601 superalloy Inorganic materials 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 4
- 230000006911 nucleation Effects 0.000 abstract description 3
- 238000010899 nucleation Methods 0.000 abstract description 3
- 229910052782 aluminium Inorganic materials 0.000 description 11
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 11
- 229910001369 Brass Inorganic materials 0.000 description 8
- 239000010951 brass Substances 0.000 description 8
- 239000007858 starting material Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- 238000007711 solidification Methods 0.000 description 2
- 230000008023 solidification Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 230000009286 beneficial effect Effects 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
- 238000005516 engineering process Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 239000002994 raw material Substances 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
- 238000009864 tensile test Methods 0.000 description 1
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Abstract
The invention relates to a novel method for preparing an ultrafine crystal material, which is characterized in that a semisolid metal material is subjected to high-frequency vibration to obtain super-strong motion acceleration, high-intensity sound waves generated by the super-strong motion acceleration can repeatedly crush crystal nuclei in a melt nucleation process, the newly formed crystal nuclei are crushed to be below 10 mu m and even reach a nanoscale level, and finally solidified ultrafine crystal grains are realized, so that the ultrafine crystal material is obtained. The high-frequency vibration is utilized to realize the high-efficiency 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 ultrafine grained materials, in particular to a method for preparing an ultrafine grained material by utilizing high-frequency vibration.
Background
The ultrafine crystal material (the grain size is 0.1-10 mu m) has excellent comprehensive mechanical property, good physical property and better corrosion resistance, and has important value and wide application prospect in the fields of industrial production and aerospace military industry. According to Hall-batch relation, the mechanical property of metal is in inverse proportion to the grain size of the material, and ultrafine grain strengthening is one of effective methods for improving the mechanical property of the metal material; meanwhile, after the crystal grains are refined, the composition uniformity, the corrosion resistance and even the 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 is particularly set forth.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a novel method for preparing an ultra-fine grain material, which enables a semi-solid metal material to generate high-frequency vibration so as to obtain super-strong motion acceleration, and high-strength sound waves generated by the super-strong motion acceleration can repeatedly crush crystal nuclei in the melt nucleation process so as to crush the newly formed crystal nuclei to be less than 10 mu m and even to reach the nano-scale level, and finally realize solidified ultra-fine crystal grains so as to obtain the ultra-fine grain material. The high-frequency vibration is utilized to realize the high-efficiency 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 for preparing an ultra-fine grained material, comprising the steps of:
and vibrating the semi-solid metal material at the motion acceleration of 20-150G, and solidifying the semi-solid metal material after stopping vibration to obtain the ultrafine grained material.
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 motion acceleration is 105-. In the present invention, "G" is gravitational acceleration. The grain size is smaller in the ultra-fine grain material, and the energy input in the solidification process needs to be ensured to be large enough, so that the grain boundary is broken to a smaller scale in the crystal nucleus forming process, and the larger the motion acceleration is, the larger the sound wave energy input is easily realized in a certain range, thereby realizing the crystal nucleus structure with smaller grain size.
Preferably, the frequency F of the vibration is 20-500Hz, preferably 100-500 Hz; the amplitude A is 1-20mm, preferably 1-15 mm; the vibration time is 1-60min, preferably 5-20 min.
Preferably, the method of the invention is carried out in a high frequency vibration device comprising a multi-stage combined spring array, the effect of vibration table and melt resonance being achieved by a multi-stage vibration system. By adjusting the vibration frequency F and the amplitude A of the high-frequency vibration device, the semi-solid metal material is ensured to obtain enough motion acceleration. The crystal nucleus can be repeatedly crushed by utilizing high-strength sound wave generated by the super-strong motion acceleration, and finally, the solidified superfine crystal grains with concentrated grain size distribution are realized, 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. The mode of completely melting the material and then cooling the material to form the semi-solid material can ensure the uniformity of the material after the metal material is completely melted, thereby providing a tissue guarantee for forming the non-segregation semi-solid for subsequent solidification.
Preferably, the metal material is copper, copper alloy, aluminum alloy, titanium alloy, tin alloy, iron, alloy steel, high temperature alloy, special metal or alloy of special metal. The high-temperature alloy refers to a metal material capable of working at a high temperature of more than 600 ℃. The special metal is metal with a melting point of more than 2000 ℃.
Preferably, the metal material is heated under a protective atmosphere to be melted and then stirred. The protective atmosphere may be nitrogen or argon. Heating under a protective atmosphere can prevent the metal material from being oxidized in the heating process.
Preferably, the metallic material is heated to a temperature of 60-100 ℃ above its liquidus temperature. This ensures a sufficient degree of superheat to completely melt the metal material.
Preferably, the melt of the metallic material is cooled to a temperature 20-60 ℃, preferably 30-50 ℃ higher than the solidus temperature of the metallic material. When the cooling temperature is lower than 20 ℃ of the solidus, the metal melt can be rapidly solidified, and the time of a process window for subsequently vibrating and crushing crystal nuclei cannot be ensured; when the cooling temperature is higher than 60 ℃ of the solidus, the superheat degree of the metal melt is large, the phenomenon that the ultra-fine crystal nucleus structure obtained by vibration is easy to grow continuously is caused, 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 state of being kept warm during the vibration. The temperature of the semi-solid metal material is 20-60 deg.C, preferably 30-50 deg.C, higher than the solidus temperature of the metal material.
Preferably, after stopping the vibration, the semi-solid metal material is cooled (e.g., naturally cooled) and solidified.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention provides a novel method for preparing an ultrafine crystal material, which is characterized in that a semisolid metal material is subjected to high-frequency vibration to obtain super-strong motion acceleration, high-strength sound waves generated by the super-strong motion acceleration can repeatedly crush crystal nuclei in a melt nucleation process, the newly formed crystal nuclei are crushed to be below 10 mu m and even reach a nanoscale level, and finally solidified ultrafine crystal grains are realized, so that the ultrafine crystal material is obtained. The high-frequency vibration is utilized to realize the high-efficiency 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 available raw materials, simple equipment, low energy consumption, low impurity content and good safety, is suitable for preparing most system metal ultrafine crystal materials, and is suitable for large-scale popularization and application.
3. The superfine crystal material obtained by the method has small average grain size, centralized grain size distribution and stable product performance.
Drawings
FIG. 1 is a schematic view of an apparatus used in the method of the present invention.
Description of reference numerals:
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 facilitate understanding of the present invention, the technical solutions of the present invention are further described below with reference to specific embodiments, but the present invention is not limited thereto. All the technologies realized based on the above-mentioned contents of the present invention are covered in the protection scope of the present invention. The starting materials used in the examples are all commercial products unless otherwise specified. Materials, equipment, or operating procedures not described herein are those that can be routinely determined by one of ordinary skill in the art. The present invention uses the apparatus shown in fig. 1 to prepare an ultra-fine grained material.
Example 1
10kg of pure aluminum ingot (No. 1060) was placed in a vessel of the apparatus shown in FIG. 1, vacuum-pumped, charged with nitrogen, and heated to 870 ℃ under nitrogen protection (degree of superheat 100 ℃) to be completely melted, thereby obtaining a molten metal. And (3) uniformly stirring the metal melt, and cooling to 700-720 ℃ (30-50 ℃ above the solidus temperature) to obtain the semi-solid metal. And then, starting a vibration controller, setting the vibration frequency to be 100Hz and the amplitude to be 15mm so as to enable the semi-solid metal to reach the acceleration of 105G, keeping the semi-solid metal under the temperature for 10 minutes, stopping the vibration, introducing the semi-solid metal into a specific water-cooled mold, and cooling and solidifying the semi-solid metal to obtain the ultra-fine grain aluminum ingot.
Example 2
2kg of brass ingot (brand C2680-H) was placed in a vessel of the apparatus shown in FIG. 1, and argon gas was introduced after vacuum-pumping, and the brass ingot was heated to 1200 deg.C (degree of superheat 60 deg.C) under the protection of argon gas to be completely melted, thereby obtaining a molten metal. And (3) uniformly stirring the metal melt, and cooling to 980 ℃ and 1000 ℃ (the temperature is 30-50 ℃ above the solidus temperature), thereby obtaining the semi-solid metal. Starting a vibration controller, setting the vibration frequency to be 500Hz and the amplitude to be 1mm so as to enable the semi-solid metal melt to reach the acceleration of 150G, stopping vibration after continuously vibrating for 10 minutes at the temperature, introducing the semi-solid metal melt into a specific water-cooled mold, and cooling and solidifying to obtain the ultrafine-grained brass ingot.
Comparative example 1
A conventional pure aluminum ingot (grade 1060), the starting material used in example 1.
Comparative example 2
Conventional brass ingots (designation C2680-H), the starting material used in example 2.
Comparative example 3
10kg of pure aluminum ingot (No. 1060) was placed in a vessel of the apparatus shown in FIG. 1, vacuum-pumped, charged with nitrogen, and heated to 870 ℃ under nitrogen protection (degree of superheat 100 ℃) to be completely melted, thereby obtaining a molten metal. And (3) uniformly stirring the metal melt, and cooling to 750 ℃ (80 ℃ above the solidus temperature) to obtain the semi-solid metal. And then, starting a vibration controller, setting the vibration frequency to be 100Hz and the amplitude to be 15mm so as to enable the semi-solid metal to reach the acceleration of 105G, keeping the semi-solid metal under the temperature for 10 minutes, stopping the vibration, introducing the semi-solid metal into a specific water-cooled mold, and cooling and solidifying the semi-solid metal to obtain the ultra-fine grain aluminum ingot.
Performance testing
The average grain sizes of the ultra-fine grained materials obtained in examples 1 and 2 and comparative examples 1 to 3 were determined by Electron Back Scattering Diffraction (EBSD) testing, 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 grain brass ingot | 0.23 |
| Comparative example 1 | Pure metal aluminum ingot (brand 1060) | 6.82 |
| Comparative example 2 | Brass ingot (brand C2680-H) | 8.45 |
| Comparative example 3 | Ultra-fine grain aluminum ingot | 4.02 |
The ultra-fine grained materials obtained in examples 1 and 2 and comparative examples 1 to 3 were subjected to tensile tests at room temperature using GB/T228-.
TABLE 2
| Metal material | Tensile strength (MPa) | Elongation (%) | |
| Example 1 | Ultra-fine grain aluminum ingot | 238 | 22％ |
| Example 2 | Ultra-fine grain brass ingot | 956 | 28％ |
| Comparative example 1 | Pure metal aluminum ingot (brand 1060) | 130 | 5％ |
| Comparative example 2 | Brass ingot (brand C2680-H) | 518 | 15％ |
| Comparative example 3 | Ultra-fine grain aluminum ingot | 187 | 12％ |
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are 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 appended claims.
Claims (10)
1. A method for preparing an ultra-fine grained material, comprising the steps of:
and vibrating the semi-solid metal material at the motion acceleration of 20-150G, and solidifying the semi-solid metal material after stopping vibration to obtain the ultrafine grained material.
2. The method according to claim 1, wherein the motion acceleration is 105-150G, preferably 120-150G.
3. The method according to claim 1 or 2, wherein the vibration has a frequency F of 20-500Hz, an amplitude a of 1-20mm and a vibration time of 1-60 min.
4. The method as claimed in claim 3, wherein the frequency F of the vibration is 100-500 Hz; the amplitude A is 1-15 mm; the vibration time is 5-20 min.
5. The method of claim 1 or 2, wherein the forming of the semi-solid metal material comprises:
heating the metal material to melt the metal material, thereby obtaining a metal material melt; and
and cooling the metal material melt to obtain the semi-solid metal material.
6. The method of claim 5, wherein the metal material melt is cooled to a temperature 20-60 ℃ above the solidus temperature of the metal material.
7. The method of claim 6, wherein the metal material melt is cooled to a temperature 30-50 ℃ above the solidus temperature of the metal material.
8. The method of claim 5, wherein the metallic material is copper, copper alloy, aluminum alloy, titanium alloy, tin alloy, iron, alloy steel, superalloy, specialty metal, or alloy of specialty metals.
9. The method according to claim 5, wherein the metal material is heated to be melted and stirred under a protective atmosphere.
10. The method of claim 9, wherein the protective atmosphere is nitrogen or argon.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
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2021
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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 |
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