CN115261660B - Preparation method of high-strength high-heat-conductivity aluminum alloy material - Google Patents
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- C—CHEMISTRY; METALLURGY
- 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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- B22F9/02—Making metallic powder or suspensions thereof using physical processes
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- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/0047—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents
- C22C32/0068—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents only nitrides
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- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
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Abstract
The invention discloses a preparation method of a high-strength high-heat-conductivity aluminum alloy material, and belongs to the field of non-ferrous metal materials. The preparation method comprises the steps of preparing an alkyl aluminum intermediate by using alkyl aluminum such as trimethyl aluminum and triethyl aluminum and amides such as dimethyl formamide and dimethyl acetamide as raw materials, separating the solid intermediate, uniformly mixing the separated intermediate with aluminum alloy powder, heating at a certain temperature under a vacuum condition to obtain mixed powder of aluminum nitride and aluminum alloy, filling the mixed powder into a mold, and pressing and sintering to obtain the high-strength high-heat-conductivity aluminum alloy material. The aluminum nitride is generated at low temperature, the surface of the aluminum nitride is pollution-free, the aluminum nitride has good compatibility with an aluminum matrix, the thermal conductivity of the aluminum alloy is obviously improved while the mechanical property of the alloy is improved by adding the aluminum nitride, and the aluminum nitride has wide application prospect on aluminum alloy parts such as a 5G communication base station radiator, an air conditioner radiator and the like.
Description
Technical Field
The invention relates to a preparation method of a high-strength high-heat-conductivity aluminum alloy material, belonging to the field of non-ferrous metal materials.
Background
Aluminum and its alloys have an excellent combination of properties, such as good thermal conductivity, plasticity and processability. In addition, the aluminum alloy material also has good high-temperature performance, formability, machinability, riveting performance and surface treatment performance. Therefore, the aluminum alloy is widely applied to various fields such as aerospace, aviation, automobiles, transportation, bridges, buildings, electronics, electricity, energy and power, mechanical manufacturing, electrical appliance and furniture and the like. With the development of industry and the improvement of living standard of people, the chip integration level of electronic products, communication equipment and the like is improved, so that the power of the equipment is increased, the heat productivity is increased, the heat dissipation capacity of the unit volume of the equipment is increased, and higher requirements are provided for the heat conduction performance of materials so as to ensure the service life of the products and the working stability. Pure aluminum has good thermal conductivity, with a room temperature thermal conductivity of about 237W/(m · K), second only to copper (385W/(m · K)) in metallic materials. However, the strength of pure aluminum is too low, only 69MPa, and cannot meet the application requirements of industrial production; therefore, the strength of pure aluminum is generally improved by alloying, but the thermal conductivity of aluminum alloys gradually decreases as the alloying elements increase.
The density of aluminum nitride (AlN) was 3.26g/cm 3 The Mohs hardness is 7 to 8, the theoretical thermal conductivity is as high as 320W/(m.K), and the thermal expansion coefficient is close to that of silicon. Aluminum nitride is introduced into the aluminum alloy, so that on one hand, the mechanical property of the alloy can be improved by utilizing the aluminum nitride to enhance the blocking effect of relative dislocation; on the other hand, the thermal conductivity of the aluminum alloy as a whole can be improved by utilizing the high thermal conductivity of aluminum nitride. Therefore, research and development of new aluminum-based materials containing aluminum nitride reinforced phases are valued by researchers at home and abroad, and certain progress is made. For example, chinese patent application 201910884968.8 discloses an in-situ generation method of AlN and AlB 2 The preparation method of the two-phase particle reinforced aluminum-based composite material comprises the steps of filling aluminum powder and boron nitride nanosheets into a ball milling tank according to the mass ratio (96-99) to (1-4) of the aluminum powder to the boron nitride nanosheets, and uniformly mixing the aluminum powder and the boron nitride nanosheets through ball milling in an inert gas atmosphere; and (4) putting the ball-milled powder into a die, cold-pressing and molding, and sintering. Chinese invention patent 201811453938.3 discloses high temperature resistant AlN and Al 2 O 3 The method comprises pressing superfine aluminum powder to appropriate porosity, packaging into a sheath, sealing, and drilling around to allow air to enter; heating the sheath in an air furnace at low temperature to thicken the oxide film, heating to high temperature, and generating AlN and Al by using nitrogen and oxygen in the air 2 O 3 And sintering and hot-working the powder after high-temperature treatment to finally obtain the aluminum alloy material. However, alN in the above method is generated by reacting aluminum powder with BN or air, the reaction process and the volume fraction of the product are not easy to control, and nitrogen in the aluminum powderDuring melting, a large amount of heat is generated, which causes the powder to agglomerate and even melt, so that the quality of the product cannot be controlled.
Disclosure of Invention
In order to solve the problems that the strength and the heat conductivity of the aluminum alloy cannot be considered at the same time, the generation amount of AlN is uncontrollable, the aluminum powder is agglomerated and melted, large-scale batch preparation is difficult and the like in the preparation process of the traditional aluminum alloy containing AlN, the invention aims to provide a preparation method of a high-strength high-heat-conductivity aluminum alloy material, which specifically comprises the following steps:
(1) Dissolving alkyl aluminum in amide, dripping ammonia water to obtain a mixed solution, adjusting the pH value of the mixed solution to be 8-10, then putting the mixed solution into a constant-temperature water bath kettle, heating, and cooling to obtain a solution containing an alkyl aluminum amide intermediate.
(2) Separating the alkyl aluminum amide intermediate in the solution obtained in the step (1), uniformly mixing the alkyl aluminum amide intermediate with aluminum alloy powder by adopting vacuum ball milling, then putting the mixed powder into a vacuum high-temperature furnace, and heating to obtain the mixed powder of aluminum nitride and aluminum alloy.
(3) And filling the AlN/aluminum alloy mixed powder into a mould with a corresponding shape of the part, and pressing and sintering to obtain the high-strength high-heat-conductivity aluminum alloy material.
Preferably, the alkyl aluminum in step (1) of the present invention is any one of trimethyl aluminum, triethyl aluminum, triisobutyl aluminum and dichloroethyl aluminum.
Preferably, the amide in step (1) of the present invention is any one of dimethylformamide and dimethylacetamide.
Preferably, the molar ratio of the alkyl aluminum to the amide to the ammonia water in the mixed solution in the step (1) is 1 (0.4 to 0.7) to (0.05 to 0.23).
Preferably, the heating conditions in the constant-temperature water bath kettle in the step (1) of the invention are as follows: heating at 65-80 deg.c for 4-6 hr.
Preferably, the solid alkylaluminamide intermediate in step (1) of the present invention is separated by a commercially available high speed centrifuge or rotary evaporator, and other separation methods can be used in the present invention.
Preferably, in the step (2) of the invention, the aluminum alloy powder is Al-Si, al-Cu, al-Mg or Al-Zn alloy powder, the particle size is 50 to 200nm, and the molar ratio of the aluminum alloy powder to the separated alkyl aluminum amide intermediate is 1 (0.1 to 0.3).
Preferably, the vacuum ball milling condition in the step (2) is that the vacuum degree is 0.01 to 0.5Pa, the ball milling rotating speed is 100 to 400r/min, and the ball milling time is 4 to 8h.
Preferably, the vacuum high-temperature furnace treatment in the step (2) is performed under the vacuum degree of 0.1 to 1Pa, the high-temperature furnace temperature of 350 to 450 ℃ and the heat preservation time of 1 to 3h.
Preferably, the sintering temperature in the step (3) of the invention is 580 to 630 ℃ and the time is 0.5 to 1h.
The pressing and sintering mode of the invention can be any one of cold isostatic pressing and air furnace sintering, hot isostatic pressing sintering, rapid sintering or spark plasma sintering.
Compared with the prior art, the invention has the beneficial effects that:
the aluminum nitride (AlN) is prepared by reacting the alkyl aluminum, the amide and the ammonia water together to generate an alkyl aluminum intermediate and then generating the alkyl aluminum intermediate in vacuum at 350-450 ℃, so that the uncontrollable AlN generated by the reaction of aluminum powder and BN or air in the traditional method is avoided, the reaction temperature is low, and the risk and the cost are reduced; and because the AlN reinforcement is nucleated and grows up in the aluminum matrix, the AlN surface is pollution-free, the compatibility between the matrix and the reinforcement phase is good, compared with the traditional method, because the lattice mismatch of the AlN reinforcement and the aluminum matrix is less than 3 percent, the AlN reinforcement can be used as an effective heterogeneous nucleation core, the AlN reinforcement uniformly distributed in the invention is more favorable for refining grains, and according to the Hall Peltier formula, the grain size is inversely proportional to the mechanical properties such as yield strength, and the smaller the grain size, the better the mechanical properties.
The high-strength high-thermal-conductivity aluminum alloy material prepared by the technology has the advantages that the mechanical property of the material is improved by more than 20% compared with the material without the AlN reinforcing phase due to the refining effect of AlN on crystal grains; and the AlN enhances the contribution of relative heat conductivity, so that the heat conductivity of the material is improved by more than 12 percent, and the mechanical property and the heat conductivity of the material are considered.
Drawings
FIG. 1 shows the morphology of a mixed powder of AlN and an aluminum alloy prepared by the present invention;
FIG. 2 shows the microscopic morphology of the high-strength high-thermal conductivity aluminum alloy prepared by the invention under a transmission electron microscope;
FIG. 3 is a microstructure and grain size of an aluminum alloy not prepared by the present invention;
FIG. 4 shows the microstructure and grain size of an aluminum alloy prepared by the present invention.
Detailed Description
The technical solutions in the present invention will be described clearly and completely with reference to the embodiments in the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, rather than all embodiments, and all other embodiments obtained by those skilled in the art without any creative work based on the embodiments in the present invention belong to the protection scope of the present invention.
Example 1
The embodiment relates to a preparation method of an Al-Si series high-strength high-heat-conductivity aluminum alloy material, which comprises the following specific steps:
(1) Dissolving trimethylaluminum in dimethylformamide, and dripping ammonia water to obtain a mixed solution, wherein the molar ratio of the trimethylaluminum to the dimethylformamide to the ammonia water is 1; and (3) putting the mixed solution into a constant-temperature water bath kettle, preserving the heat for 5 hours at the temperature of 75 ℃, and cooling to obtain a solution containing the trimethylaluminum amide intermediate.
(2) Separating the trimethylaluminum amide intermediate from the solution by using a rotary evaporator, putting the solution into a ball milling tank, and meanwhile, weighing ZL101 alloy (Chinese brand, al-Si alloy) powder with the particle size of 100nm, and putting the ZL101 alloy powder into the ball milling tank, wherein the molar ratio of the aluminum alloy powder to the trimethylaluminum amide intermediate is 1; ball milling is carried out for 6 hours under the vacuum degree of 0.1Pa and the rotating speed of 300 r/min.
(3) And putting the mixed powder after ball milling into a vacuum high-temperature furnace, wherein the vacuum degree of the high-temperature furnace is 0.5Pa, the temperature is 400 ℃, and the heat preservation time is 2 hours, so as to obtain the mixed powder of the aluminum nitride and the Al-Si alloy, as shown in figure 1. As can be seen from figure 1, the method can obtain the nanometer AlN and Al-Si alloy mixed powder, and the powder has better uniformity of grain diameter and no pollution on the surface.
(4) Filling the nano AlN and Al-Si alloy mixed powder into a mould, performing cold isostatic pressing and air furnace sintering (sintering temperature is 600 ℃, time is 0.5 h) to obtain the high-strength high-heat-conductivity aluminum alloy material, and performing transmission electron microscope sampling observation on the obtained aluminum alloy material, wherein the TEM appearance is shown in figure 2, and as can be seen from figure 2, alN reinforcing phases in the material are uniformly and dispersedly distributed in an aluminum matrix, and the micro interface between AlN and the aluminum matrix has no impurities and is well combined with the interface.
In contrast, an aluminum alloy material to which no AlN reinforcing phase was added was obtained by directly filling the corresponding alloy powder (for the present example, the powder was an Al — Si-based alloy powder) into a mold, and after cold isostatic pressing and air furnace sintering (sintering temperature 600 ℃, time 0.5 h).
The grain size of the high-strength high-heat-conductivity aluminum alloy material prepared by the invention is reduced to about 60 mu m from about 500 mu m without adding AlN reinforcing phase, and the grain size photos of the high-strength high-heat-conductivity aluminum alloy material and the high-strength high-heat-conductivity aluminum alloy material are shown in figures 3 and 4. Due to the obvious fine crystal strengthening effect, the tensile strength of the material is improved from 210MPa to 260MPa; due to the addition of AlN with high thermal conductivity, the thermal conductivity of the material is also increased from 150.8W/(m.K) to 172.3W/(m.K), and the aluminum alloy material with both mechanical property and thermal conductivity is obtained.
Example 2
The embodiment relates to a preparation method of an Al-Cu series high-strength high-heat-conductivity aluminum alloy material, which comprises the following specific steps:
(1) Dissolving triethylaluminum in dimethylacetamide, and dropwise adding ammonia water to obtain a mixed solution, wherein the molar ratio of triethylaluminum to dimethylacetamide to ammonia water is 1. And (3) putting the mixed solution into a constant-temperature water bath kettle, preserving the heat for 4 hours at the temperature of 80 ℃, and cooling to obtain a solution containing the triethyl aluminum amide intermediate.
(2) Separating the triethylaluminum amide intermediate from the solution by using a high-speed centrifuge, putting the triethylaluminum amide intermediate into a ball milling tank, and meanwhile, weighing ZL203 alloy (Chinese brand, al-Cu alloy) powder with the particle size of 200nm into the ball milling tank, wherein the molar ratio of the aluminum alloy powder to the triethylaluminum amide intermediate is 1; ball milling is carried out for 4 hours under the vacuum degree of 0.5Pa and the rotating speed of 100 r/min.
(3) And putting the mixed powder after ball milling into a vacuum high-temperature furnace, wherein the vacuum degree of the high-temperature furnace is 1Pa, the temperature is 450 ℃, and the heat preservation time is 1h to obtain the mixed powder of the aluminum nitride and the Al-Cu alloy.
(4) Filling the mixed powder of the nano AlN and the Al-Cu alloy into a mould, and obtaining the high-strength high-heat-conductivity aluminum alloy material after hot isostatic pressing and air sintering (the sintering temperature is 630 ℃ and the time is 0.5 h).
In contrast, the aluminum alloy material without the AlN reinforcing phase was prepared by directly filling the corresponding alloy powder (for the present example, the powder was Al — Cu-based alloy powder) into a mold, and obtaining the alloy after hot isostatic pressing and air furnace sintering (sintering temperature 630 ℃, time 0.5 h).
The grain size of the high-strength high-heat-conductivity aluminum alloy material prepared by the method is reduced to about 80 mu m from about 560 mu m without adding the AlN reinforcing phase. Due to the obvious fine crystal strengthening effect, the tensile strength of the material is improved from 205MPa to 278MPa. Due to the addition of AlN with high thermal conductivity, the thermal conductivity of the material is also increased from 154.9W/(m.K) to 179.6W/(m.K), and the aluminum alloy material with both mechanical property and thermal conductivity is obtained.
Example 3
The embodiment relates to a preparation method of an Al-Mg series high-strength high-heat-conductivity aluminum alloy material, which comprises the following specific steps:
(1) Dissolving triisobutyl aluminum in dimethylacetamide, and dripping ammonia water to obtain a mixed solution, wherein the molar ratio of triisobutyl aluminum to dimethylacetamide to ammonia water is (1); and (3) putting the mixed solution into a constant-temperature water bath kettle, preserving the heat for 6 hours at 65 ℃, and cooling to obtain a solution containing a triisobutylaluminumamide intermediate.
(2) Separating the triisobutylaluminamide intermediate from the solution by using a high-speed centrifuge, putting the triisobutylaluminamide intermediate into a ball milling tank, and simultaneously weighing ZL303 alloy (Chinese brand, al-Mg alloy) powder with the particle size of 50nm and putting the ZL303 alloy powder into the ball milling tank, wherein the molar ratio of the aluminum alloy powder to the triisobutylaluminamide intermediate is 1; ball milling is carried out for 8 hours under the vacuum degree of 0.01Pa and the rotating speed of 400 r/min.
(3) And putting the mixed powder after ball milling into a vacuum high-temperature furnace, wherein the vacuum degree of the high-temperature furnace is 0.1Pa, the temperature is 350 ℃, and the heat preservation time is 3 hours, so as to obtain the mixed powder of the aluminum nitride and the Al-Mg alloy.
(4) Filling the nano AlN and Al-Mg alloy mixed powder into a die, and quickly sintering (sintering temperature of 580 ℃ and time of 1 hour) to obtain the high-strength high-heat-conductivity aluminum alloy material.
In contrast, in the case of an aluminum alloy material to which no AlN reinforcing phase was added, the preparation method was such that the corresponding alloy powder (for the present example, the powder was an Al — Mg alloy powder) was directly filled into a mold and subjected to rapid sintering (sintering temperature 580 ℃, time 1 hour).
The grain size of the high-strength high-heat-conductivity aluminum alloy material prepared by the method is reduced to about 36 mu m from about 450 mu m without adding the AlN reinforcing phase. Due to the obvious fine crystal strengthening effect, the tensile strength of the material is improved from 148MPa to 189MPa. Due to the addition of AlN with high thermal conductivity, the thermal conductivity of the material is also increased from 125.6W/(m.K) to 160.7W/(m.K), and the aluminum alloy material with both mechanical property and thermal conductivity is obtained.
Example 4
The embodiment relates to a preparation method of an Al-Zn series high-strength high-heat-conductivity aluminum alloy material, which comprises the following specific steps:
(1) Dissolving dichloroethylaluminum in dimethylacetamide, and dripping ammonia water to obtain a mixed solution, wherein the molar ratio of dichloroethylaluminum, dimethylacetamide and ammonia water is 1. And (3) putting the mixed solution into a constant-temperature water bath kettle, preserving the heat for 4.5 hours at 70 ℃, and cooling to obtain a solution containing the dichloroethyl aluminum amide intermediate.
(2) Separating the dichloroethylaluminamide intermediate from the solution by using a high-speed centrifuge, putting the dichloroethylaluminamide intermediate into a ball milling tank, and simultaneously weighing ZL402 alloy (Chinese brand, al-Zn alloy) powder with the particle size of 150nm into the ball milling tank, wherein the molar ratio of the aluminum alloy powder to the dichloroethylaluminamide intermediate is 1; ball milling is carried out for 6.5h under the vacuum degree of 0.4Pa and the rotating speed of 200 r/min.
(3) And putting the mixed powder after ball milling into a vacuum high-temperature furnace, wherein the vacuum degree of the high-temperature furnace is 0.8Pa, the temperature is 370 ℃, and the heat preservation time is 2.5 hours, so as to obtain the mixed powder of the aluminum nitride and the Al-Zn alloy.
(4) The nanometer AlN and Al-Zn alloy mixed powder is filled into a die and is sintered by discharge plasma (the sintering temperature is 590 ℃, and the time is 0.8 h) to obtain the high-strength high-heat-conductivity aluminum alloy material.
In contrast, an aluminum alloy material to which no AlN reinforcing phase was added was obtained by directly filling the corresponding alloy powder (for the present example, the powder was Al-Zn-based alloy powder) into a mold and after spark plasma sintering (sintering temperature 590 ℃ C., time 0.8 h).
The grain size of the high-strength high-heat-conductivity aluminum alloy material prepared by the method is reduced to about 73 mu m from about 480 mu m without adding an AlN reinforcing phase; due to the obvious fine crystal strengthening effect, the tensile strength of the material is improved from 235MPa to 287MPa; due to the addition of AlN with high thermal conductivity, the thermal conductivity of the material is also increased from 138W/(m.K) to 157W/(m.K), and the aluminum alloy material with both mechanical property and thermal conductivity is obtained.
Claims (8)
1. The preparation method of the high-strength high-heat-conductivity aluminum alloy material is characterized by comprising the following steps of:
(1) Dissolving alkyl aluminum in amide, dripping ammonia water to obtain a mixed solution, adjusting the pH value of the mixed solution to be 8-10, then putting the mixed solution into a constant-temperature water bath kettle, heating, and cooling to obtain a solution containing an alkyl aluminum amide intermediate;
(2) Separating out the alkyl aluminum amide intermediate in the solution obtained in the step (1), uniformly mixing the alkyl aluminum amide intermediate with aluminum alloy powder by adopting vacuum ball milling, then putting the mixed powder into a vacuum high-temperature furnace, and heating to obtain mixed powder of aluminum nitride and aluminum alloy; wherein the molar ratio of the aluminum alloy powder to the separated alkyl aluminum amide intermediate is 1 (0.1 to 0.3);
(3) Filling the AlN/aluminum alloy mixed powder into a mould with a corresponding shape of a part, and pressing and sintering to obtain a high-strength high-heat-conductivity aluminum alloy material;
in the step (2), the vacuum ball milling condition is that the vacuum degree is 0.01 to 0.5Pa, the ball milling rotation speed is 100 to 400r/min, and the ball milling time is 4 to 8h;
and (3) performing vacuum high-temperature furnace treatment in the step (2) at the vacuum degree of 0.1-1Pa, the high-temperature furnace temperature of 350-450 ℃ and the heat preservation time of 1-3h.
2. The preparation method of the high-strength high-thermal-conductivity aluminum alloy material according to claim 1, wherein the preparation method comprises the following steps: the alkyl aluminum in the step (1) is any one of trimethyl aluminum, triethyl aluminum, triisobutyl aluminum and dichloroethyl aluminum.
3. The preparation method of the high-strength high-thermal-conductivity aluminum alloy material according to claim 1 or 2, characterized by comprising the following steps: the amide in the step (1) is any one of dimethylformamide and dimethylacetamide.
4. The preparation method of the high-strength high-thermal-conductivity aluminum alloy material according to claim 3, characterized by comprising the following steps: the molar ratio of the alkyl aluminum, the amide and the ammonia water in the mixed solution in the step (1) is 1 (0.4 to 0.7) to (0.05 to 0.23).
5. The preparation method of the high-strength high-thermal-conductivity aluminum alloy material according to claim 1 or 4, characterized by comprising the following steps: the heating conditions in the constant-temperature water bath kettle in the step (1) are as follows: heating at 65-80 deg.c for 4-6 hr.
6. The preparation method of the high-strength high-thermal-conductivity aluminum alloy material according to claim 5, characterized by comprising the following steps: the solid-state alkyl aluminum amide intermediate in the step (1) is separated by adopting a high-speed centrifuge or a rotary evaporator sold in the market.
7. The preparation method of the high-strength high-thermal-conductivity aluminum alloy material according to claim 1 or 6, characterized by comprising the following steps: the aluminum alloy powder in the step (2) is Al-Si series, al-Cu series, al-Mg series or Al-Zn series alloy powder, and the particle size is 50 to 200nm.
8. The preparation method of the high-strength high-thermal-conductivity aluminum alloy material according to claim 1, characterized by comprising the following steps: the sintering temperature in the step (3) is 580 to 630 ℃, and the time is 0.5 to 1h.
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