CN113278841B - Preparation method for strengthening beryllium-aluminum alloy by adopting liquid silicon polymer and beryllium-aluminum alloy - Google Patents
Preparation method for strengthening beryllium-aluminum alloy by adopting liquid silicon polymer and beryllium-aluminum alloy Download PDFInfo
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- CN113278841B CN113278841B CN202110380090.1A CN202110380090A CN113278841B CN 113278841 B CN113278841 B CN 113278841B CN 202110380090 A CN202110380090 A CN 202110380090A CN 113278841 B CN113278841 B CN 113278841B
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C1/00—Making non-ferrous alloys
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
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- C22C1/1047—Alloys containing non-metals starting from a melt by mixing and casting liquid metal matrix composites
- C22C1/1052—Alloys containing non-metals starting from a melt by mixing and casting liquid metal matrix composites by mixing and casting metal matrix composites with reaction
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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Abstract
The invention provides a preparation method for strengthening beryllium-aluminum alloy by adopting liquid silicon polymer, which comprises the following steps: step one, mixing beryllium particles, aluminum particles and liquid silicon polymer, compacting the mixture, and placing the mixture in a vacuum medium-frequency induction furnace; heating to 400-1000 ℃, then filling ammonia reaction gas, preserving heat, obtaining a silicon-containing ceramic phase, and then filling protective gas; step three, continuously heating to 1250-1320 ℃, then smelting and uniformly stirring; and step four, under the protection of argon, refining the smelting liquid, standing until the temperature is reduced to 1200-1300 ℃, and then casting the smelted liquid into a ceramic mould shell for cooling. The invention also provides the beryllium-aluminum alloy. The invention can hinder the sliding of crystal boundary, inhibit the crystal grain growth of beryllium-aluminum alloy system and strengthen the mechanical property of the beryllium-aluminum alloy.
Description
Technical Field
The invention belongs to the technical field of aluminum alloy material metallurgy, and particularly relates to a preparation method for strengthening a beryllium-aluminum alloy by adopting a liquid silicon polymer and the beryllium-aluminum alloy.
Background
The beryllium-aluminum alloy (with the Be content of 55-62 wt%) has the excellent characteristics of light weight, high specific stiffness, high specific strength, good thermal stability, high toughness, corrosion resistance, easiness in processing and the like, and is applied to the aerospace industry, the computer manufacturing industry and the automobile processing industry. However, because of the large melting point difference and low intersolubility of beryllium and aluminum elements, the solidification temperature range is wide, so that the microstructure of the beryllium-aluminum composite material has the characteristics of a particle reinforced aluminum-based composite material, namely, a high-strength particle beryllium phase is a reinforced phase (generally, the grain size is about 100 microns) and is dispersedly distributed in a matrix aluminum phase, when the beryllium-aluminum composite material is subjected to external load, stress is mainly concentrated on the particle Be phase due to the elastic modulus difference of two phases in the beryllium-aluminum composite material, and strain is mainly distributed on the matrix Al phase, so that the beryllium-aluminum composite material has an inverted toughness-strength relationship, and the sizes of a matrix and a reinforcement body have important influence on the performance of the beryllium-aluminum composite material. Under the same process condition, when the size of matrix particles and the volume fraction of the reinforcing body are fixed, the mechanical strength of the alloy is firstly increased and then reduced along with the reduction of the grain size according to the Hall-Petch formula. However, the free energy of an alloy system is increased due to the fact that the grains are reduced and the number of grain boundaries in unit volume is increased, so that the microstructure of the alloy of the system is unstable, and the grain growth rate is rapidly increased along with the increase of the process temperature, so that the free energy of the system is reduced. Therefore, controlling the growth of crystal grains and enhancing the matching degree of the matrix phase and the enhanced phase in the beryllium-aluminum alloy are important ways for realizing the strengthening of the beryllium-aluminum alloy.
The existing fine-grained alloy strengthening mainly adopts the following two ways: one is that the rapid cooling process produces fine crystal to realize the strengthening of alloy structure. The other is to add solid fine-grained materials such as zirconia, silicon nitride, silicon carbide, alumina and the like into the alloy structure, so that a good strengthening effect is achieved. However, when the solid fine-grained material is added, the key point for realizing the strengthening is how to deal with the problems of agglomeration and adsorption of the fine-grained material due to large specific surface area. Typically, ultrasonic assisted casting processes, friction stir welding processes, and mechanical ball milling in combination with hot pressing/secondary machining processes are employed. The preparation cost and the preparation period of the alloy are increased.
Disclosure of Invention
The invention aims to provide a preparation method for strengthening a beryllium-aluminum alloy by adopting a liquid silicon polymer, which can inhibit grain boundary sliding, inhibit the crystal grain growth of a beryllium-aluminum alloy system and strengthen the mechanical property of the beryllium-aluminum alloy.
The second purpose of the invention is to provide a beryllium-aluminum alloy.
In order to achieve one of the purposes, the invention adopts the following technical scheme:
a preparation method for strengthening beryllium-aluminum alloy by adopting liquid silicon polymer comprises the following steps:
step one, mixing beryllium particles, aluminum particles and liquid silicon polymer, compacting the mixture and placing the mixture in a vacuum medium-frequency induction furnace;
step two, heating to 400-1000 ℃, then filling ammonia reaction gas, preserving heat, obtaining a silicon-containing ceramic phase, and then filling protective gas;
step three, continuously heating to 1250-1320 ℃, then smelting and uniformly stirring;
and step four, under the protection of argon, refining the smelting liquid, standing until the temperature is reduced to 1200-1300 ℃, and then casting the smelted liquid into a ceramic mould shell for cooling.
According to the invention, beryllium particles, aluminum particles and liquid silicon polymer react with ammonia gas reaction gas at 400-1000 ℃, the obtained silicon-containing ceramic phase is continuously heated to 1250-1320 ℃, so that after the high-melting-point beryllium particles are completely melted, the mixed liquid of beryllium, aluminum molten metal and silicon-containing ceramic is obtained, and the silicon-containing ceramic is distributed at the interface of the beryllium phase and the aluminum phase in the beryllium-aluminum alloy obtained after refining, thereby blocking grain boundary sliding, inhibiting the growth of crystal grains of a beryllium-aluminum alloy system, playing roles in strengthening fine-grain and pinning dislocation motion and strengthening alloy deformation resistance, and strengthening the mechanical property of the beryllium-aluminum alloy.
Further, in the first step, the weight of the beryllium particles is 55-62 wt% of the weight of the mixture of the beryllium particles, the aluminum particles and the liquid silicon polymer;
the weight of the liquid silicon polymer is less than or equal to 4% of the weight of the mixture of the beryllium particles, the aluminum particles and the liquid silicon polymer;
the balance being aluminum particles.
Further, in the step one, the molecular weight of the liquid silicon polymer is 1000-50000.
Further, the liquid silicon polymer is one of polydimethylsiloxane, polycarbosilane and polycarbosilazane.
Further, in the second step, the reaction gas is ammonia gas;
the protective gas is argon.
Further, in the second step, the heat preservation time is 3-8 hours.
Further, in the fourth step, the standing time is 10-30 minutes.
In order to achieve the second purpose, the invention adopts the following technical scheme:
the beryllium-aluminum alloy is prepared by the preparation method.
The invention has the beneficial effects that:
the beryllium particles, the aluminum particles and the liquid silicon polymer react with the ammonia gas reaction gas at 400-1000 ℃ to obtain a silicon-containing ceramic phase, and the obtained silicon-containing ceramic phase is continuously heated to 1250-1320 ℃, so that the beryllium particles with high melting point are completely melted to obtain a mixed liquid of beryllium, aluminum molten liquid and the silicon-containing ceramic, and the silicon-containing ceramic is distributed at the interface of the beryllium phase and the aluminum phase in the beryllium-aluminum alloy obtained after refining, thereby blocking the sliding of the crystal boundary, inhibiting the growth of crystal grains of a beryllium-aluminum alloy system, playing the roles of strengthening the movement of fine grains and pinning dislocation and strengthening the deformation resistance of the alloy, and strengthening the mechanical property of the beryllium-aluminum alloy; the strength of the beryllium-aluminum alloy prepared by the method can be improved by 3.4-5.7%.
Detailed Description
The following detailed description of specific embodiments of the invention.
Example 1:
1. high-purity beryllium particles, high-purity aluminum particles and polydimethylsiloxane (with the molecular weight of 50000) are mixed according to the weight ratio of 62: 35.8: 2.2 stirring evenly to obtain a mixture of the three.
2. Compacting the mixture in a crucible, and feeding the crucible into a vacuum intermediate frequency induction furnace for smelting. When the temperature is raised to 1000 ℃, introducing ammonia gas, preserving the heat for 8 hours, generating silicon carbide-containing ceramic after the liquid silicon polymer fully reacts, stopping introducing the ammonia gas, and introducing protective gas argon.
3. And continuously heating to 1300 ℃, fully melting the high-melting-point beryllium particles, and fully mixing the molten metal and the silicon carbide ceramic under the stirring of the magnetic force generated by the induction coil.
4. Refining in the atmosphere of protective gas argon, and standing the mixture of the molten metal and the silicon-containing ceramic for 30 minutes. Reducing the temperature of the mixture of the molten metal and the silicon-containing ceramic to 1300 ℃, casting the mixture of the molten metal and the silicon-containing ceramic into a ceramic mould shell, cooling along the way, and demoulding. Compared with beryllium-aluminum alloy without adding, the strength of beryllium-aluminum alloy obtained by adding the liquid silicon polymer is improved by 5.7%.
Example 2:
1. mixing high-purity beryllium particles, high-purity aluminum particles and polycarbosilane (molecular weight is 1000) in a weight ratio of 55: 41.4: 3.6 stirring evenly to obtain a mixture of the three.
2. Compacting the mixture in a crucible, and feeding the crucible into a vacuum intermediate frequency induction furnace for smelting. When the temperature is increased to 550 ℃, introducing ammonia gas, preserving the heat for 5 hours, generating silicon carbide-containing ceramic after the liquid silicon polymer is fully reacted, stopping introducing the ammonia gas, and introducing protective gas argon.
3. And continuously heating to 1250 ℃, and fully mixing the molten metal and the silicon carbide ceramic under the stirring of the magnetic force generated by the induction coil after the high-melting-point beryllium particles are completely melted.
4. Refining in the protective gas argon atmosphere, and standing the mixture of the molten metal and the silicon-containing ceramic for 20 minutes. Reducing the temperature of the mixture of the molten metal and the silicon-containing ceramic to 1200 ℃, casting the mixture of the molten metal and the silicon-containing ceramic into a ceramic mould shell, cooling along the way, and demoulding. Compared with beryllium aluminum alloy without adding beryllium aluminum alloy, the strength of the beryllium aluminum alloy obtained by adding the liquid silicon polymer is improved by 3.4%.
Example 3:
1. mixing high-purity beryllium particles, high-purity aluminum particles and polycarbosilazane (with the molecular weight of 1580) in a weight ratio of 60: 36: 4, stirring uniformly to obtain a mixture of the three.
2. Compacting the mixture in a crucible, and feeding the crucible into a vacuum intermediate frequency induction furnace for smelting. When the temperature is raised to 850 ℃, introducing ammonia gas, preserving the heat for 3 hours, generating silicon carbide-containing ceramic after the liquid silicon polymer fully reacts, stopping introducing the ammonia gas, and introducing protective gas argon.
3. And continuously heating to 1320 ℃, completely melting the high-melting-point beryllium particles, and then fully mixing the molten metal and the silicon carbide ceramic under the stirring of the magnetic force generated by the induction coil.
4. Refining in the atmosphere of protective gas argon, and standing the mixture of the molten metal and the silicon-containing ceramic for 20 minutes. Reducing the temperature of the mixture of the molten metal and the silicon-containing ceramic to 1250 ℃, casting the mixture of the molten metal and the silicon-containing ceramic into a ceramic mould shell, cooling along the way, and demoulding. Compared with beryllium-aluminum alloy without adding, the strength of beryllium-aluminum alloy obtained by adding the liquid silicon polymer is improved by 4.7%.
Although the embodiments of the present invention have been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that various changes may be made and equivalents may be substituted without departing from the spirit and scope of the embodiments of the present invention.
Claims (5)
1. A preparation method for strengthening beryllium-aluminum alloy by adopting liquid silicon polymer is characterized by comprising the following steps:
step one, mixing beryllium particles, aluminum particles and liquid silicon polymer, compacting the mixture and placing the mixture in a vacuum medium-frequency induction furnace;
in the first step, the weight of the beryllium particles is 55-62 wt% of the weight of the mixture of the beryllium particles, the aluminum particles and the liquid silicon polymer;
the weight of the liquid silicon polymer is less than or equal to 4% of the weight of the mixture of the beryllium particles, the aluminum particles and the liquid silicon polymer;
the balance being aluminum particles;
in the first step, the molecular weight of the liquid silicon polymer is 1000-50000;
step two, heating to 400-1000 ℃, then filling ammonia reaction gas, preserving heat, obtaining a silicon-containing ceramic phase, and then filling protective gas;
in the second step, the heat preservation time is 3-8 hours;
step three, continuously heating to 1250-1320 ℃, then smelting and uniformly stirring;
and step four, under the protection of argon, refining the smelting liquid, standing until the temperature is reduced to 1200-1300 ℃, and then casting the smelted liquid into a ceramic mould shell for cooling.
2. The method of claim 1, wherein the liquid silicon polymer is one of polydimethylsiloxane, polycarbosilane, and polycarbosilazane.
3. The method according to claim 1, wherein in the second step, the reaction gas is ammonia gas;
the protective gas is argon.
4. The preparation method according to claim 1, wherein in the fourth step, the standing time is 10 to 30 minutes.
5. A beryllium-aluminum alloy, which is prepared by the preparation method of any one of claims 1 to 4.
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| US5872070A (en) * | 1997-01-03 | 1999-02-16 | Exxon Research And Engineering Company | Pyrolysis of ceramic precursors to nanoporous ceramics |
| CN103952796B (en) * | 2014-04-28 | 2016-04-06 | 中国人民解放军国防科学技术大学 | A kind of preparation method of silicon nitrogen boron continuous ceramic fiber |
| CN108359820A (en) * | 2018-04-04 | 2018-08-03 | 中国工程物理研究院材料研究所 | A kind of preparation method and products thereof of Ultra-fine Grained beryllium alumin(i)um alloy |
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