CN115608994A - Preparation and forming process of magnesium-based composite material lath - Google Patents
Preparation and forming process of magnesium-based composite material lath Download PDFInfo
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- CN115608994A CN115608994A CN202211155562.4A CN202211155562A CN115608994A CN 115608994 A CN115608994 A CN 115608994A CN 202211155562 A CN202211155562 A CN 202211155562A CN 115608994 A CN115608994 A CN 115608994A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- 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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/02—Compacting only
- B22F3/03—Press-moulding apparatus therefor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/1003—Use of special medium during sintering, e.g. sintering aid
- B22F3/1007—Atmosphere
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/002—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working by rapid cooling or quenching; cooling agents used therefor
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/06—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of magnesium or alloys based thereon
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- 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
- B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
Abstract
The invention provides a preparation and forming process of magnesium-based composite laths, which aims at a forming method of magnesium-based composite materials difficult to disperse, combines mechanical powder mixing, vacuum hot-pressing sintering and cladding extrusion processes, selects a preparation process with proper component proportion and reasonable collocation, can effectively disperse GNPs in a magnesium matrix, and further strengthens the mechanical properties of the materials through extrusion deformation. The method mainly comprises the following components: 0.4 to 1.0wt.% of GNPs,1 to 1.5wt.% of pure Sm powder, 6 to 9wt.% of pure Al powder, 88.5 to 92.6wt.% of pure Mg powder and AZ91 magnesium alloy pipe. The coating method adopted by the invention can overcome the defect that the sintered magnesium-based composite material cannot be subjected to heat treatment strengthening, and a fine and uniform microstructure and excellent mechanical properties are obtained through heat treatment strengthening and extrusion deformation.
Description
Technical Field
The invention belongs to the field of magnesium-based composite material preparation, and particularly relates to a method for sintering, cladding, extruding and deforming magnesium-based composite material powder difficult to disperse.
Background
The magnesium and the magnesium alloy have the characteristics of low density, high specific strength and specific stiffness, excellent electromagnetic shielding performance and easiness in recovery, and have considerable application prospects in the industries of aerospace, advanced weapons, medical instruments and the like. However, the magnesium alloy has the defects of poor corrosion resistance, limited plasticity and the like, so that the further popularization of the magnesium alloy is restricted. In order to improve the formability of magnesium alloys, it is generally necessary to heat the magnesium alloys to a certain temperature to form the magnesium alloys. And the magnesium alloy is easy to form texture in the extrusion or rolling process, so that the deformability of the magnesium alloy is reduced. In recent years, related researches prove that the defects can be eliminated by adding nano ceramic particles or nano carbon materials into a magnesium matrix, the forming capability of magnesium alloy is improved, and a novel magnesium-based composite material with better mechanical properties is prepared.
Powder metallurgy is an industrial technology for manufacturing various products by adopting metal powder or metal-based composite material powder through blank making, sintering and machining, and has unique advantages in the aspect of near-net-shape forming of materials. By adopting the process, the equal-material processing can be realized, and high dimensional precision and high surface precision are achieved. On the whole, the workpiece produced by powder metallurgy has a series of advantages of energy conservation, environmental protection, excellent performance, higher precision and the like.
The magnesium-based composite material is a metal-based composite material with great application prospect in the fields of aerospace, consumer electronics and the like, and the forming method of the magnesium-based composite material mainly comprises the following two steps: (1) The liquid phase method, also called as a casting method, has low cost and mature process, and is the mainstream method for producing the metal matrix composite on a large scale at present, however, the magnesium matrix composite prepared by the method often has particle phase segregation and agglomeration in the interior, the acting force of a reinforcing phase and a matrix material is reduced, and finally the performance of the material is reduced. (2) The solid phase method, also called powder metallurgy method, which adopts the form of solid phase diffusion bonding to prepare the magnesium-based composite material can better improve some defects in the casting method and enable the interior of the material to form uniform and fine tissues. The powder metallurgy method generally has higher requirements on equipment, and the size of the product produced by the method is smaller.
The magnesium-based composite powder can be solidified by sintering, but pores and shrinkage porosity often exist in a sintered blank, which is a common defect of preparing a metal-based composite material by a vacuum hot-pressing sintering method, so that the sintered and formed material needs to be subjected to later plastic deformation to further improve the density, refine the microstructure and improve the mechanical property of the material.
In order to improve the forming performance of magnesium alloy, various plastic deformation technologies have been developed, and the forming calculation of various metals difficult to deform is increasingly perfected. In order to improve the performance of the magnesium alloy prepared by the traditional powder metallurgy, the magnesium alloy is generally required to be subjected to subsequent plastic deformation, and the plastic deformation is utilized to generate larger strain in the material, drive the defect movement in the structure and refine the crystal grains, so that the superfine crystal material with the grain size smaller than 1 μm is finally prepared. Meanwhile, the plastic deformation can effectively regulate and control the texture inside the powder metallurgy material, weaken the texture of a strong base surface and refine crystal grains, and improve the processability and mechanical properties of the magnesium and magnesium alloy material.
Currently, the preparation of high-performance metal materials based on powder metallurgy and subsequent plastic deformation techniques generally comprises two processes: (1) Powder metallurgy, namely, material powder is compacted, sintered and cooled under the vacuum protection and then taken out; the plastic deformation process comprises the following steps: and (3) heating the sintered block, performing plastic deformation, and cooling and then taking out the sintered block. The invention provides a method for preparing a magnesium-based composite material by vacuum hot-pressing sintering and strengthening the sintered magnesium-based composite material by a cladding extrusion method. The invention can obviously improve the forming performance of the magnesium-based composite material. Meanwhile, the compact coating material can effectively prevent the sintering material from being oxidized and cracked in the heat treatment and deformation processes, and effectively optimize the deformation performance of the sintered magnesium-based composite material.
Disclosure of Invention
Aiming at the situation in the background art, the invention adopts a mechanical powder mixing-vacuum hot pressing sintering-cladding extrusion method, which can solve the problems of easy oxidation, non-compact structure, poor forming performance of the sintered magnesium-based composite material and the like in the sintering forming process of the magnesium-based composite material powder under the vacuum condition. Effectively preventing the defects of oxidation and cracking in the sintering process and the plastic processing process of the magnesium-based composite material powder, thereby improving the production efficiency and the product quality.
The raw materials used in the invention are: pure Mg powder, pure Al powder, pure Sm powder, GNPs, AZ91 magnesium alloy tubes, zirconia ball milling beads, graphite lubricant and high-purity Ar gas.
Further, the pure Mg powder, the pure Al powder and the pure Sm powder are 500-mesh aerosol powder, wherein the purity of the pure Mg powder is not less than 97%, the purity of the pure Al powder is not less than 99%, and the purity of the pure Sm powder is not less than 95%. The GNPs are single-layer nano graphene, and the sheet diameter of the GNPs is 50-200 nm. The AZ91 magnesium alloy pipe has an inner diameter of 40mm, an outer diameter of 45mm and a length of 50mm-100mm.
Further, the zirconia ball milling beads are divided into three types, and the diameters of the beads are respectively 3mm,5mm and 10mm. The graphite lubricant is prepared from deionized water and graphite powder, wherein the deionized water is 70ml, and the graphite powder is 30g.
The method for preparing the magnesium-based composite material by vacuum hot-pressing sintering comprises the following steps:
taking out pure Mg powder, pure Al powder, pure Sm powder and GNPs in a vacuum glove box according to the weight, and filling the pure Mg powder, the pure Al powder, the pure Sm powder and the GNPs into a ball milling tank according to a ball-material ratio of 1:15 putting zirconia ball milling beads, 3mm,5mm and 10mm ball milling beads, and mixing the materials according to the weight ratio of 1:1:1 are respectively put into a ball milling tank, filled with high-purity Ar gas and sealed.
Ball-milling and mixing powder by using a planetary ball mill, and setting the speed of a ball-milling tank: 400r/min, and the ball milling time is 12h. And opening the ball milling tank in the vacuum glove box after the ball milling is finished, and taking out the composite material powder which is subjected to uniform ball milling.
Preparing the graphite mould required by the process, which comprises the following steps: 1-sleeve, 2-split die, 3-pressure head, 4-cushion block and 5-sintered blank. Wherein 1-the external diameter of the sleeve is 180mm, the internal diameter is 60mm, and the length is 120mm; 2-the valve is divided into two parts, the inner diameter of the valve is 40mm, the outer diameter of the valve is 60mm, and the length of the valve is 120mm; 3-the pressure head has a diameter of 40mm and a length of 100mm; 4-the diameter of the cushion block is 40mm, and the length is 40mm.
Putting the powder subjected to uniform ball milling into a graphite mold in a vacuum glove box, transferring the assembled graphite mold into a vacuum hot-pressing sintering furnace, starting a vacuum system of the vacuum hot-pressing sintering furnace, and vacuumizing to 10 DEG C -4 Pa. Setting the sintering temperature as follows: heating from room temperature to 400 deg.C at a heating rate of 10 deg.C/min, maintaining the temperature for 30min, and heating from 400 deg.C to 480 deg.C at a heating rate of 5 deg.C/minAnd keeping the temperature for 1h. The sintering pressure is set as follows: and maintaining the pressure for 40min under the condition of 30MPa, and then increasing the sintering pressure to 100MPa and maintaining the pressure until the sintering is finished. And after sintering, cooling the sintered product in a furnace to room temperature and taking out the sintered product.
The magnesium alloy cladding extrusion method comprises the following steps:
and (3) polishing the sintered magnesium-based composite material block into a cylinder with the diameter of 40mm and the length of 30-40 mm by using 2000-mesh sand paper. And (2) taking another section of AZ91 magnesium alloy pipe with the length of 50-55 mm, polishing each surface of the AZ91 magnesium alloy pipe by using 2000-mesh sand paper, fully cleaning and drying the AZ91 magnesium alloy pipe and the magnesium-based composite material sintered block by using acetone, pressing the magnesium-based composite material sintered block into the AZ91 magnesium alloy pipe by using a small hydraulic press, and sealing two ends of the magnesium-based composite material sintered block.
The assembled magnesium-based composite material blank is put into a vacuum tube furnace for homogenization treatment, and the heat treatment process comprises the following steps: heating from room temperature to 300 ℃ at a heating rate of 10 ℃/min, subsequently heating from 300 ℃ to 415 ℃ at a heating rate of 5 ℃/min, preserving the heat at 415 ℃ for 12h, cooling the blank to room temperature after the heat treatment is finished, and taking out.
Preparing a coating extrusion die required by the process, which comprises the following steps: 6-extrusion die sleeve, 7-extrusion split mold, 8-composite material blank, 9-extrusion pressure head, 10-AZ91 magnesium alloy pipe and 11-extrusion die core. Wherein the 7-extrusion valve mould is divided into two parts, the inner diameter of the 7-extrusion valve mould is 45mm, and the outer diameter of the 7-extrusion valve mould is 60mm
And (3) placing the prepared coating extrusion die on a lower worktable of a four-column hydraulic press, switching on a power supply of a heating system, and uniformly coating the water-based graphite lubricant on an inner cavity of the coating extrusion die. And (3) putting the homogenized magnesium-based composite material blank into an extrusion die with an extrusion ratio of 16, preserving the temperature for 1h when the blank and the die reach 350 ℃, and then extruding the blank into a lath at the speed of 1 mm/s. The extruded strip was immediately quenched into water.
Cutting out the strip with the length of 100-120 mm from the extruded strip, putting the extruded strip into a vacuum drying oven for aging treatment, and keeping the temperature at 175 ℃ for 24h.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the following briefly describes the contents of the present invention and the drawings required in the embodiments.
FIG. 1 is a schematic view of a vacuum hot-pressing sintering mold according to the present invention
FIG. 2 is a schematic view of the magnesium-based composite material coating extrusion die of the present invention
FIG. 3 is a schematic view of the coating method of Mg-based composite material of the present invention
FIG. 4 is the structure diagram of the vacuum hot-pressed sintered block of Mg-based composite material
FIG. 5 is an extruded structure diagram of the Mg-based composite material of the present invention
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to specific embodiments below.
Example 1
The preparation and forming process of the magnesium-based composite material lath comprises the following components: 1wt.% pure Sm powder, 6wt.% pure Al powder, 0.5wt.% GNPs, and 92.5wt.% pure Mg powder.
A preparation and forming process of a magnesium-based composite material lath is characterized by comprising the following steps:
0.35g of GNPs, 0.7g of pure Sm powder, 4.2g of pure Al powder and 64.75g of pure Mg powder were taken out in a vacuum glove box and charged into a ball mill pot, respectively. According to the ball material ratio of 1: zirconia ball milling beads were placed in the ball milling jar, and 350g of 3mm ball milling beads, 350g of 5mm ball milling beads, and 350g of 10mm ball milling beads were placed, respectively.
And (3) filling high-purity Ar gas into the ball milling tank, sealing, and performing ball milling and powder mixing by using a planetary ball mill, wherein the ball milling rotation speed is set to be 350r/min, and the ball milling time is set to be 12 hours. And opening the ball milling tank in a vacuum glove box after the ball milling is finished, and taking out the mixed powder.
The mixed powder was charged into a prepared graphite mold in a vacuum glove box, and the mold was moved into a vacuum hot-pressing sintering furnace. Starting a vacuum system of the vacuum hot-pressing sintering furnace, and vacuumizing to 10 DEG -4 Pa. Setting the sintering temperature as follows: heating from room temperature to 400 deg.C at a heating rate of 10 deg.C/min, and heating at 40 deg.CKeeping the temperature at 0 ℃ for 30min, then heating from 400 ℃ to 480 ℃ at the heating rate of 5 ℃/min and keeping the temperature for 1h. The sintering pressure is set as follows: and maintaining the pressure for 40min under the condition of 30MPa, pressurizing to 100MPa after the pressure maintaining is finished, and maintaining the pressure until sintering is finished. And after sintering, cooling the sintered product in a furnace to room temperature and taking out the sintered product.
And (3) polishing the sintered magnesium-based composite material block into a cylinder with the diameter of 40mm and the length of 30-40 mm by using 2000-mesh sand paper. And (2) taking another section of AZ91 magnesium alloy pipe with the length of 50-55 mm, polishing each surface of the AZ91 magnesium alloy pipe by using 2000-mesh sand paper, fully cleaning and drying the AZ91 magnesium alloy pipe and the magnesium-based composite material sintered block by using acetone, pressing the magnesium-based composite material sintered block into the AZ91 magnesium alloy pipe by using a small hydraulic press, and sealing two ends of the magnesium-based composite material sintered block.
Placing the assembled magnesium-based composite material blank into a vacuum tube furnace for homogenization treatment, wherein the set temperature is as follows: heating from room temperature to 300 ℃ at the heating rate of 10 ℃/min, then heating from 300 ℃ to 415 ℃ at the heating rate of 5 ℃/min, preserving heat for 12h, and taking out after finishing heat treatment until the sample is cooled to room temperature in air.
And (3) placing the prepared coating extrusion die on a lower worktable of a four-column hydraulic press, switching on a power supply of a heating system, and uniformly coating the water-based graphite lubricant on an inner cavity of the coating extrusion die. And (3) placing the assembled magnesium-based composite material blank into an extrusion die with an extrusion ratio of 16, preserving the heat for 1h when the temperature of the blank and the die reach 350 ℃, and then extruding the blank into a lath at the speed of 1 mm/s. The extruded strip was immediately quenched into water.
A strip with the length of 100mm is cut out from an extruded strip and is placed into a vacuum drying oven for aging treatment, and the temperature is set to be 175 ℃ for 24 hours.
The sintered, extruded and aged materials were tested for their properties, and the results were HV75.8 for sintered hardness, 160MPa for compressive strength, 8% for elongation, 95HV for extruded hardness, 315MPa for tensile strength, 10% for elongation, HV110 for aged hardness, 340MPa for tensile strength, 15% for elongation.
Example two
Referring to the first embodiment of the present invention, the powder composition was changed to 0.7g of gnps, 0.7g of pure Sm powder, 5.6g of pure Al powder and 63g of pure Mg powder. The sintering temperature is changed to 460 ℃, and the sintering temperature curve and the sintering pressure are not changed. The measured alloy hardness in a sintering state is 70.8HV, the compressive strength is 155MPa, and the elongation is 9.4 percent. The extrusion hardness was 90HV, the tensile strength was 288MPa, and the elongation was 10.5%. The measured hardness at the aged state is 97HV, the tensile strength is 290MPa, and the elongation is 13.7 percent.
Comparative example 1
This example relates to a process for preparing and forming a magnesium-based composite stave having the composition of 1wt.% pure Sm powder, 6wt.% pure Al powder, 0.5wt.% GNPs, and 92.5wt.% pure Mg powder.
0.35g of GNPs, 0.7g of pure Sm powder, 4.2g of pure Al powder and 64.75g of pure Mg powder were taken out in a vacuum glove box and charged into a ball mill pot, respectively. According to the ball material ratio of 1: zirconia ball milling beads were placed in the ball milling jar, and 350g of 3mm ball milling beads, 350g of 5mm ball milling beads, and 350g of 10mm ball milling beads were placed, respectively.
And (3) filling high-purity Ar gas into the ball milling tank, sealing, and performing ball milling and powder mixing by using a planetary ball mill, wherein the ball milling rotation speed is set to be 350r/min, and the ball milling time is set to be 12 hours. And opening the ball milling tank in a vacuum glove box after the ball milling is finished, and taking out the mixed powder.
The mixed powder was charged into a prepared graphite mold in a vacuum glove box, and the mold was moved into a vacuum hot-pressing sintering furnace. Starting a vacuum system of the vacuum hot-pressing sintering furnace, and vacuumizing to 10 DEG -4 Pa. Setting the sintering temperature as follows: heating from room temperature to 400 ℃ at a heating rate of 10 ℃/min, and keeping the temperature at 400 ℃ for 30min, and then heating from 400 ℃ to 540 ℃ at a heating rate of 5 ℃/min, and keeping the temperature for 2h. The sintering pressure is set as follows: and maintaining the pressure for 40min under the condition of 30MPa, pressurizing to 100MPa after the pressure maintaining is finished, and maintaining the pressure until sintering is finished. And after sintering, cooling the sintered product in a furnace to room temperature and taking out the sintered product.
Comparative example No. two
Referring to the first embodiment of the present invention, the powder composition was changed to 1.4g of gnps, 0.7g of pure Sm powder, 5.6g of pure Al powder and 62.3g of pure Mg powder. Ball-milling the mixed powder for 12 hours at the speed of 350r/min in Ar atmosphere, taking out the powder in a vacuum glove box, and filling the powder into prepared graphiteIn a mold. And (4) moving the assembled graphite mold into a vacuum hot-pressing sintering furnace. Starting a vacuum system of the vacuum hot-pressing sintering furnace, and vacuumizing to 10 DEG -4 Pa. Setting the sintering temperature as follows: heating from room temperature to 400 ℃ at a heating rate of 10 ℃/min, and keeping the temperature at 400 ℃ for 30min, and then heating from 400 ℃ to 540 ℃ at a heating rate of 5 ℃/min, and keeping the temperature for 2h. The sintering pressure is set as follows: and maintaining the pressure for 40min under the condition of 30MPa, pressurizing to 100MPa after the pressure maintaining is finished, and maintaining the pressure until the sintering is finished. And after sintering, cooling the sintered product in a furnace to room temperature and taking out the sintered product.
The experimental results are as follows: in the first embodiment, the proportions of 1wt.% pure Sm powder, 6wt.% pure Al powder, 0.5wt.% GNPs and 92.5wt.% pure Mg powder are adopted, and after vacuum hot-pressing sintering, the GNPs are uniformly distributed in the whole matrix without agglomeration. The hardness HV110 is measured after extrusion coating and ageing at 175 ℃.
Example two the composition ratio of 1wt.% pure Sm powder, 8wt.% pure Al powder, 1wt.% GNPs and 90wt.% pure Mg powder is adopted and the sintering temperature is changed to 460 ℃, and after vacuum hot pressing sintering, the GNPs are evenly distributed in the whole matrix without agglomeration. Hardness HV97 after extrusion coating and aging at 175 ℃.
In the first comparative example, the same component proportion as that in the first example is adopted, the sintering temperature is changed to 540 ℃, the heat preservation time is changed to 2 hours, and materials are melted and seeped out of the die in the sintering process.
In the second comparative example, the composition ratio of 1wt.% pure Sm powder, 8wt.% pure Al powder, 2wt.% GNPs and 89wt.% pure Mg powder was adopted, and after vacuum hot-press sintering, the GNPs were found to aggregate throughout the matrix, and the as-sintered hardness HV55 was determined.
Claims (7)
1. A magnesium-based composite material lath is prepared and shaped by the process, which is characterized in that firstly, after a GNPs magnesium-based composite material is prepared by mechanical mixed powder composite vacuum hot-pressing sintering, the composite material is filled into an AZ91 magnesium alloy pipe and sealed, then the sealed magnesium-based composite material blank is subjected to homogenization treatment, and finally the magnesium-based composite material blank subjected to homogenization treatment is subjected to hot extrusion deformation, so that the mechanical property of the composite material is enhanced while the dispersibility of the GNPs in a magnesium matrix is improved by the process, and the high-strength magnesium-based composite material with uniform tissue is obtained;
the method comprises the following steps:
(1) Taking out GNPs, pure Mg powder, pure Al powder and pure Sm powder with corresponding mass in a vacuum glove box according to a proportion, and putting the pure Sm powder and the pure Mg powder into a ball milling tank according to a ball-material ratio of 1:15 putting zirconia balls into the ball mill, filling high-purity Ar gas into the ball mill tank, and sealing.
(2) And (3) carrying out ball milling and powder mixing by using a planetary ball mill, setting the rotating speed of a ball milling tank to be 400r/min, and ball milling time to be 12h.
(3) And (3) putting the powder subjected to uniform ball milling into a prepared graphite die, assembling the die and then transferring into a vacuum hot-pressing sintering furnace. Keeping the temperature for 1h at 480 ℃ under the pressure of 100 MPa.
(4) And (3) putting the sintered magnesium-based composite material block into an AZ91 magnesium alloy pipe, sealing, and then putting the magnesium-based composite material block into a vacuum pipe furnace for homogenization treatment. The heat treatment process comprises the following steps: heating the sample from room temperature to 300 ℃ at the heating rate of 10 ℃/min, then heating from 300 ℃ to 415 ℃ at the heating rate of 5 ℃/min, preserving the temperature for 12h after the temperature reaches 415 ℃, and taking out the sample after the heat treatment is finished until the sample is cooled to room temperature by air.
(5) And (3) placing the assembled magnesium-based composite material blank into an extrusion die with an extrusion ratio of 16, preserving the heat for 1h when the temperature of the blank and the die reach 350 ℃, and then extruding the blank into a lath at the speed of 1 mm/s.
(6) Cutting the extruded plate to a proper length, putting the extruded plate into a vacuum drying oven for aging treatment, and keeping the temperature at 175 ℃ for 24 hours.
The magnesium-based composite material processed by the steps comprises the following components:
0.4 to 1.0wt.% of GNPs,1 to 1.5wt.% of pure Sm powder, 6 to 9wt.% of pure Al powder, and 88.6 to 92.6wt.% of pure Mg powder.
2. The magnesium-based composite lath as claimed in claim 1, wherein said magnesium-based composite treated by said steps comprises the following components:
0.8 to 1.0wt.% of GNPs,1 to 1.5wt.% of pure Sm powder, 8 to 9wt.% of pure Al powder, and 88.5 to 90.2wt.% of pure Mg powder.
3. The process of claim 1, wherein the sintering temperature in step (3) is set by heating from room temperature to 400 ℃ at a ramp rate of 10 ℃/min, holding the temperature at 400 ℃ for 30min, then heating from 400 ℃ to 480 ℃ at a ramp rate of 5 ℃/min, and holding the temperature at 480 ℃ for 1h.
4. The process of claim 1, wherein the sintering process in step (3) is: and maintaining the pressure for 40min under the condition that the sintering pressure is 30MPa, and then increasing the sintering pressure to 100MPa and maintaining the pressure until the sintering is finished. And after sintering, cooling to room temperature in the furnace.
5. The process for preparing and forming a magnesium-based composite slab as claimed in claim 1, wherein the magnesium-based composite blank in the step (4) is formed by pressing the sintered mg-based composite block into the AZ91 magnesium alloy tube using a small press and sealing both ends of the assembled AZ91 magnesium alloy tube.
6. The process for preparing and forming the magnesium-based composite material lath as claimed in claim 1, wherein the method for homogenizing the magnesium-based composite material in the step (4) comprises the following steps: heating from room temperature to 300 ℃ at a heating rate of 10 ℃/min, then heating from 300 ℃ to 415 ℃ at a heating rate of 5 ℃/min, preserving heat for 12 hours at 415 ℃, finishing heat treatment, cooling the blank to room temperature in air, and taking out.
7. The process for preparing and forming the magnesium-based composite material lath as claimed in claim 1, wherein the extrusion method of the magnesium-based composite material in the step (5) comprises the following steps: placing the homogenized magnesium-based composite material blank into an extrusion die with an extrusion ratio of 16, preserving heat for 1h when the temperature of the blank and the die reach 350 ℃, then extruding the blank into a lath at the speed of 1mm/s, and immediately quenching the extruded plate into water.
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| CN202211155562.4A CN115608994A (en) | 2022-09-22 | 2022-09-22 | Preparation and forming process of magnesium-based composite material lath |
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