CN109706337B - Preparation method of tungsten particle reinforced aluminum matrix composite material - Google Patents
Preparation method of tungsten particle reinforced aluminum matrix composite material Download PDFInfo
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- CN109706337B CN109706337B CN201811621296.3A CN201811621296A CN109706337B CN 109706337 B CN109706337 B CN 109706337B CN 201811621296 A CN201811621296 A CN 201811621296A CN 109706337 B CN109706337 B CN 109706337B
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Abstract
The invention discloses a preparation method of a tungsten particle reinforced aluminum matrix composite, belonging to the technical field of composite processing and preparation. The method comprises the following steps: (1) putting tungsten powder into a mixer by taking ethanol as a mixing medium for mixing, and drying in vacuum to obtain pretreated tungsten powder; (2) mixing aluminum powder or aluminum alloy powder with the pretreated tungsten powder obtained in the step (1) to obtain composite powder; (3) carrying out cold isostatic pressing, vacuum degassing, hot isostatic pressing sintering, upsetting, hot extrusion and heat treatment on the composite powder obtained in the step (2) to obtain a tungsten particle reinforced aluminum-based composite material; the preparation method can obviously improve the compactness of the aluminum matrix composite, refine the microstructure of the material, reduce the anisotropy of the material and expand the application range of the aluminum matrix composite.
Description
Technical Field
The invention belongs to the technical field of composite material processing and preparation, and particularly relates to a preparation method of a tungsten particle reinforced aluminum matrix composite material.
Background
The particle reinforced aluminum-based composite material generally has the advantages of high specific strength, high specific modulus, fatigue resistance, high-temperature creep resistance, heat resistance, good wear resistance, high thermal conductivity, low expansion coefficient, adjustable components, low density and the like, and is widely applied to the fields of aviation, aerospace, land transportation, electronic information and the like. For example, SiC/Al composites have found applications in the fields of helicopter rotors, electronic and optical device mounts and housings, automotive pistons and brake pads, and the like. B is4The C/Al composite material is used for nuclear fuel storage shelves, and the diamond/Al composite material is used for heat management materials and the like. The tungsten particles have high melting point and high conductivityGood thermal property and mechanical property, and is an excellent metal matrix composite reinforcing phase. The prepared tungsten particle reinforced aluminum matrix composite material has good mechanical property and heat resistance, and is a novel aluminum matrix composite structure material and a functional material.
The patent (CN105401001B) adopts a powder pretreatment-powder mixing-vacuum degassing-hot isostatic pressing process to prepare the tungsten particle reinforced aluminum matrix composite material. The patent (CN106756159A) adopts a process of high-energy ball milling-low-energy mixing-hot isostatic pressing to prepare the tungsten particle reinforced aluminum matrix composite material with a multilevel structure. The composite material prepared by the hot isostatic pressing process has low elongation, and the composite material with low volume fraction can be subjected to thermal deformation processing to improve the combination of the composite material matrix and the reinforcing phase. The hot extrusion process can effectively improve the internal metallurgical bonding state of the powder metallurgy product, but the internal metal matrix and the reinforcing phase are in a streamline distribution state due to the shearing action of three-directional compressive stress in the extrusion process, the mechanical property and the microstructure are obviously anisotropic, and the design, processing and application of the composite material are limited under certain use conditions.
Disclosure of Invention
The invention aims to provide a preparation method of a tungsten particle reinforced aluminum matrix composite material, which has the following specific technical scheme:
the preparation method of the tungsten particle reinforced aluminum matrix composite material comprises the following steps:
(1) putting tungsten powder into a mixer by taking ethanol as a mixing medium for mixing, and drying in vacuum to obtain pretreated tungsten powder;
(2) mixing aluminum powder or aluminum alloy powder with the pretreated tungsten powder obtained in the step (1) to obtain composite powder;
(3) and (3) carrying out cold isostatic pressing, vacuum degassing, hot isostatic pressing sintering, upsetting, hot extrusion and heat treatment on the composite powder obtained in the step (2) to obtain the tungsten particle reinforced aluminum-based composite material.
In the step (2), the purity of the tungsten powder is more than 99%, and the particle size is 7-8 μm; the purity of the aluminum powder or the aluminum alloy powder is more than 99.5 percent, and the particle diameter of the particles is 7-100 mu m.
In the composite powder in the step (2), the mass percent of the pretreated tungsten powder is 27-70%, and the mass percent of the aluminum powder or the aluminum alloy powder is 30-73%.
In the step (3), the hydraulic medium and the composite powder are isolated by the rubber sheath, and the composite powder is subjected to cold isostatic pressing, wherein the cold isostatic pressing pressure is 50-200 MPa, and the pressure maintaining time is 10-40 min.
In the step (3), the cold isostatic pressing billet is placed in an aluminum sheath, vacuum degassing is carried out at the temperature of 400--3And after Pa, sealing the aluminum sheath.
In the step (3), the temperature of hot isostatic pressing sintering is 450-; and after hot isostatic pressing sintering, turning off the aluminum skin on the surface.
In the step (3), the blank with the aluminum skin on the surface turned off after the hot isostatic pressing sintering is heated to 400-470 ℃, the temperature is kept for 2 hours, and then the upsetting is carried out, wherein the strain rate of the upsetting is 0.001s-1～0.01s-1The upsetting ratio is 0.65, and solid steel gaskets are added on two sides of the blank in the upsetting process.
In the step (3), the extrusion ratio of hot extrusion is 8-25, and the extrusion rate is 0.5-10 mm/s.
In the step (3), the heat treatment temperature is 380-550 ℃, the heat treatment time is 0.2-2h, and water quenching cooling is adopted after the heat treatment; thus obtaining the tungsten particle reinforced aluminum matrix composite material.
The invention has the beneficial effects that:
(1) the preparation method can obviously improve the compactness of the aluminum matrix composite, refine the microstructure of the material, reduce the anisotropy of the material and expand the application range of the aluminum matrix composite.
(2) The tungsten particle reinforced aluminum matrix composite material prepared by the invention has the characteristics of uniform distribution of reinforced phases, high density, small anisotropy, good comprehensive mechanical property and the like; is a composite material with excellent comprehensive performance and has great application potential.
Detailed Description
The invention provides a preparation method of a tungsten particle reinforced aluminum matrix composite, which is further described with reference to the following embodiments.
The tungsten particle reinforced aluminum-based composite material provided by the invention comprises 27-70% of tungsten particles by mass and the balance of aluminum or aluminum alloy, wherein the aluminum alloy can be 2A12 aluminum alloy, 6063 aluminum alloy and other alloys, and the preparation method specifically comprises the following steps:
(1) placing tungsten powder in a double-cone mixer, mixing the tungsten powder with ethanol as a mixing medium for 10 hours at a weight ratio of grinding balls to powder of 1:0.5-2, and vacuum-drying for 10 hours to obtain pretreated tungsten powder;
(2) mixing 27-70% of the pretreated tungsten powder obtained in the step (1) and 30-73% of aluminum powder or aluminum alloy powder in percentage by mass, uniformly mixing the powder by using a double-cone mixer under the protection of argon, wherein the weight ratio of grinding balls to powder is 1:0.5-2, and the mixing time is 10-24 hours, so as to obtain composite powder; wherein, the purity of the tungsten powder is more than 99 percent, and the particle size is 7-8 μm; the purity of the aluminum powder or the aluminum alloy powder is more than 99.5 percent, and the particle size is 7-100 mu m;
(3) performing cold isostatic pressing on the composite powder obtained in the step (2), and isolating a hydraulic medium (wear-resistant hydraulic oil) from the composite powder by using a rubber sheath, wherein the cold isostatic pressing pressure is 50-200 MPa, and the pressure maintaining time is 10-40 min;
(4) placing the cold isostatic pressing billet obtained in the step (3) in a pre-prepared aluminum sheath, and performing vacuum degassing at the temperature of 400-500 ℃ and the vacuum degree of lower than 1 × 10-3After Pa, sealing the aluminum sheath, wherein the degassing time is not less than 10 hours;
(5) using a hot isostatic pressing sintering method, keeping the temperature for 2 hours under the conditions that the temperature is 450-550 ℃ and the pressure is 100-200MPa, cooling along with a furnace to realize the molding of the composite material, wherein the heating rate is not higher than 10 ℃/min, using a lathe to remove aluminum skin on the surface to obtain a hot isostatic pressing state tungsten particle reinforced aluminum matrix composite material blank, and continuously machining the blank to a cylindrical sample with the specified diameter size by the lathe;
(6) heating the blank obtained in the step (5) to 400-470 ℃, and preserving heat for 2 hours; simultaneously heating the extrusion die by using a heating deviceTo the same temperature; loading the heated blank into an extrusion cylinder of a 1500MN extruder, adding solid steel gaskets on both sides of the blank ingot, starting the extruder, upsetting the composite material, wherein the upsetting strain rate is 0.001s-1～0.01s-1The upsetting ratio is 0.65; wherein the extrusion barrel temperature is 370 ℃ and 420 ℃.
(7) Taking out the solid steel gasket at the end, close to the die, of the upsetting sample, and performing hot extrusion processing on the internal billet, wherein the extrusion ratio is 8-25, and the extrusion rate is 0.5-10 mm/s;
(8) carrying out heat treatment on the extruded section by using a vertical quenching furnace, wherein the heat treatment temperature is 380-550 ℃, the heat treatment time is 0.2-2h, and water quenching cooling is adopted after the heat treatment; thus obtaining the tungsten particle reinforced aluminum matrix composite material.
According to the invention, through upsetting and hot extrusion secondary deformation treatment on the composite material, the structure is completely densified and refined, the streamline distribution state of the composite material hot extrusion pure shear metal is improved, and the anisotropy of an extruded product is obviously reduced; the density of the tungsten particle reinforced aluminum matrix composite material prepared by the steps is more than 99.5 percent, the room-temperature tensile strength is more than 280MPa, the yield strength is more than 140MPa, the elongation is 5-10 percent, and the room-temperature impact toughness is more than 6 j.cm-2。
Example 1
Preparing a tungsten particle reinforced aluminum matrix composite material consisting of 30 mass percent of tungsten and 70 mass percent of 2A12 aluminum alloy matrix (6 volume percent of pretreated tungsten powder and 94 volume percent of 2A12 aluminum alloy powder) according to the following steps:
(1) pretreatment of tungsten powder
Weighing 10kg of tungsten powder, wherein the mass ratio of the stainless steel grinding balls to the tungsten powder is 1:0.5, mixing for 10 hours by using ethanol as a mixing medium and using a double-cone mixer, and performing vacuum drying for 10 hours to obtain pretreated tungsten powder;
(2) mixing the raw materials
Mixing 6kg of the pretreated tungsten powder obtained in the step (1) with 14kg of 2A12 aluminum alloy powder, and mixing for 10 hours under the condition of argon protection by using a double-cone mixer to obtain composite powder;
(3) cold isostatic pressing
And (3) isolating the hydraulic medium (anti-wear hydraulic oil) from the composite powder obtained in the step (2) by using a rubber sheath, and performing the composite powder under the cold isostatic pressing conditions of the pressure of 100MPa and the pressure maintaining time of 25 min.
(4) Vacuum degassing
Placing the billet obtained by the cold isostatic pressing in the step (3) in a prefabricated aluminum sheath, and performing vacuum degassing at the temperature of 400 ℃ until the vacuum degree is lower than 1 × 10-3And sealing the aluminum sheath under the condition of Pa, wherein the degassing time is not less than 10 hours.
(5) Sintering by hot isostatic pressing
Heating to 495 ℃ at the heating rate of 10 ℃/min, preserving the heat for 2 hours under the hot isostatic pressing condition with the pressure of 100MPa, and cooling to room temperature along with the furnace to realize the molding of the composite material; and removing the aluminum skin from the blank to obtain the hot isostatic pressing state tungsten particle reinforced aluminum matrix composite blank, and continuously machining the blank into a cylindrical sample with the diameter of 140mm by using a lathe.
(6) Upsetting
Heating the cylindrical sample obtained in the step (5) to 450 ℃, and preserving heat for 2 hours; simultaneously heating an extrusion die to the same temperature by using a heating device, loading the heated blank into a 180mm extrusion cylinder of a 1500MN extruder, adding solid steel gaskets on both sides of a cylindrical sample, starting the extruder, upsetting the composite material, and setting the moving speed of an extrusion rod to be 0.4 mm/s; wherein the extruder barrel temperature was 420 ℃.
(7) Hot extrusion
The solid steel shim near the die end of the upset sample was removed and the internal billet was subjected to a hot extrusion process with an extrusion ratio of 15 and an extrusion rate of 2 mm/s.
(8) Thermal treatment
And (3) carrying out heat treatment on the extruded section by using a vertical quenching furnace, wherein the solid solution temperature is 470-490 ℃, the solid solution time is 2h, and the natural aging is carried out.
The density of the tungsten particle reinforced aluminum matrix composite material prepared according to the steps is 99.9%, the room-temperature tensile strength of the composite material along the extrusion direction is 380MPa, the yield strength is 230MPa, the elongation is 10%, and the impact toughness is 9.9 j.cm-2(ii) a Tensile strength at room temperature of 370MPa, yield strength of 220MPa, elongation of 10 percent and impact toughness of 9.7 j.cm in vertical extrusion direction-2。
Example 2
Different from the embodiment 1, the upsetting step is not carried out, the density of the prepared composite material is 99.8 percent, the room-temperature tensile strength of the composite material along the extrusion direction is 400MPa, the yield strength is 260MPa, the elongation is 10 percent, and the impact toughness is 10.5 j.cm-2(ii) a The room temperature tensile strength in the vertical extrusion direction is 360MPa, the yield strength is 205MPa, the elongation is 8 percent, and the impact toughness is 7.8 j.cm-2。
Example 3
Unlike example 1, the mass of the raw material tungsten powder was 11kg, and the mass of the pure aluminum powder was 9 kg. The density of the prepared tungsten particle reinforced aluminum-based composite material is 99.9 percent, the tensile strength of the composite material along the extrusion direction at room temperature is 390MPa, the yield strength is 238MPa, the elongation is 9 percent, and the impact toughness is 9.1 j.cm-2(ii) a Room temperature tensile strength 375MPa, yield strength 225MPa, elongation 8.5%, impact toughness 8.5j cm in the vertical extrusion direction-2。
Example 4
Different from the embodiment 3, the method does not carry out the upsetting step, the density of the prepared tungsten particle reinforced aluminum matrix composite material is 99.8 percent, the room-temperature tensile strength of the composite material along the extrusion direction is 415MPa, the yield strength is 270MPa, the elongation is 10 percent, and the impact toughness is 10.0 j.cm-2(ii) a Tensile strength at room temperature of 370MPa, yield strength of 225MPa, elongation of 7.5% and impact toughness of 7.2j cm in vertical extrusion direction-2。
Claims (8)
1. The preparation method of the tungsten particle reinforced aluminum matrix composite is characterized by comprising the following steps:
(1) putting tungsten powder into a mixer by taking ethanol as a mixing medium for mixing, and drying in vacuum to obtain pretreated tungsten powder;
(2) mixing aluminum powder or aluminum alloy powder with the pretreated tungsten powder obtained in the step (1) to obtain composite powder;
(3) carrying out cold isostatic pressing, vacuum degassing, hot isostatic pressing sintering, upsetting, hot extrusion and heat treatment on the composite powder obtained in the step (2) to obtain a tungsten particle reinforced aluminum-based composite material;
said step (3)) In the method, the blank with the aluminum skin on the surface turned off after the hot isostatic pressing sintering is heated to 400-470 ℃, the temperature is kept for 2 hours, and then the upsetting is carried out, wherein the strain rate of the upsetting is 0.001s-1～0.01s-1The upsetting ratio is 0.65, and solid steel gaskets are added on two sides of the blank in the upsetting process.
2. The method according to claim 1, wherein in the step (2), the purity of the tungsten powder is more than 99%, and the particle size is 7-8 μm; the purity of the aluminum powder or the aluminum alloy powder is more than 99.5 percent, and the particle diameter of the particles is 7-100 mu m.
3. The preparation method according to claim 1, wherein in the composite powder in the step (2), the mass percent of the pretreated tungsten powder is 27% -70%, and the mass percent of the aluminum powder or the aluminum alloy powder is 30% -73%.
4. The preparation method according to claim 1, wherein in the step (3), the hydraulic medium is isolated from the composite powder by a rubber sheath, and the composite powder is subjected to cold isostatic pressing, wherein the cold isostatic pressing pressure is 50MPa to 200MPa, and the pressure maintaining time is 10min to 40 min.
5. The method as claimed in claim 1, wherein in the step (3), the cold isostatic pressed ingot is placed in an aluminum sheath, and vacuum degassing is performed at 400-500 ℃ under a vacuum degree of less than 1 × 10-3And after Pa, sealing the aluminum sheath.
6. The preparation method according to claim 1, wherein in the step (3), the temperature of hot isostatic pressing sintering is 450-; and after hot isostatic pressing sintering, turning off the aluminum skin on the surface.
7. The production method according to claim 1, wherein in the step (3), the extrusion ratio of the hot extrusion is 8 to 25, and the extrusion rate is 0.5 to 10 mm/s.
8. The preparation method as claimed in claim 1, wherein in the step (3), the heat treatment temperature is 380-550 ℃, the heat treatment time is 0.2-2h, and water quenching cooling is adopted after the heat treatment.
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| CN114921690B (en) * | 2021-09-30 | 2023-06-09 | 有研工程技术研究院有限公司 | High-energy electron radiation resistant aluminum-based composite shielding material and preparation method thereof |
| CN114453586B (en) * | 2022-03-04 | 2023-07-04 | 中国核动力研究设计院 | Preparation method of tungsten-boron-aluminum composite shielding plate with high tungsten content |
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| JP3358685B2 (en) * | 1995-01-10 | 2002-12-24 | 日立粉末冶金株式会社 | Manufacturing method of low thermal expansion sintered alloy |
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| CN103773983A (en) * | 2014-01-09 | 2014-05-07 | 安泰科技股份有限公司 | Tungsten-aluminum alloy and preparation method for same |
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