High-flux preparation device and method for metal matrix composite
Technical Field
The invention relates to a high-flux preparation device and method of a metal matrix composite material.
Background
A 'material genetic engineering' plan is proposed abroad, a high-throughput preparation technology is utilized to complete preparation of a large number of samples in a short time, and the aim of reducing cost and research and development period by half is fulfilled. The structure and structure of the metal matrix composite material are unique, the metal matrix composite material comprises reinforcing phases with different types, granularities and morphologies, matrix alloys with different components and interfaces with adjustable components, structure and micro-area performance, and the composite mechanism and the micro-structure evolution mechanism of the metal matrix composite material are more complex than those of the traditional alloy and have more obvious structure performance design advantages. Wherein the matrix alloy composition directly affects the wetting properties, the interfacial reaction behavior, and the final properties of the composite. Therefore, the method for preparing the metal matrix composite material with different matrixes at high flux is an important support for realizing half cost and half period reduction in the process of researching and developing the metal matrix composite material.
In summary, there is no apparatus and method for high throughput preparation of bulk samples of different liquid metal matrices and reinforcements. Nor has an apparatus and method capable of high throughput preparation of bulk samples of different reinforcements.
For example, in "a diamond/aluminum composite material and a high-efficiency preparation method thereof" (CN201711045332.1), it is proposed to arrange a plurality of molds in the same crucible in an air pressure infiltration furnace, then fill the same type of diamond powder into the plurality of molds, then place the forming mold into the crucible in the air pressure infiltration furnace, place the aluminum metal block on the upper surface of the forming mold in the crucible, heat the two together to the melting point of aluminum metal of 10-300 ℃ under vacuum, and then introduce a gas to infiltrate the molten aluminum metal into the diamond preform; and then cooling the furnace body to room temperature, taking out the forming die, removing the aluminum metal on the outer surface of the die, and finally demoulding. The method utilizes the design of multiple dies, improves the use efficiency of the furnace and the productivity of each furnace, achieves the aim of improving the production efficiency, has small usage amount of aluminum metal, and reduces the cost of raw materials. However, the patent also only obtains a plurality of samples of one type of diamond/aluminum composite material in one preparation process, and can not realize the high-throughput preparation of metal matrix composite material samples of more than 2 base alloy types.
Disclosure of Invention
The invention provides a high-throughput preparation device and method for a metal matrix composite material, and aims to solve the problems that the existing preparation method for the composite material cannot realize high-throughput preparation of block samples of different liquid metal matrixes and reinforcements and cannot realize high-throughput preparation of block samples of different reinforcements.
The invention relates to a high-flux preparation device for a metal matrix composite, which consists of a lifting rod 1, an exhaust tube 2, a furnace body 3, a preheating zone 4, a smelting zone 5, a grid type crucible 6, an inflation tube 7, a preform mounting disc 9, a plurality of preforms 10, a heat insulation plate 11 and a crucible heating zone 13;
the furnace body 3 is a sealed cavity body, a horizontal annular heat insulation plate 11 is arranged in the middle of the inside of the furnace body 3, the annular heat insulation plate 11 is fixedly connected with the inner wall of the furnace body 3, the upper part of the annular heat insulation plate 11 in the furnace body 3 is a preheating zone 4, the lower part of the annular heat insulation plate 11 in the furnace body 3 is a smelting zone 5, the bottom of the smelting zone 5 is a crucible heating zone 13, and electric heating elements are respectively arranged at the position, close to the inner wall of the furnace body 3, in the preheating zone 4, at the position, close to the inner wall of the furnace body 3; the upper part of the furnace body 3 is provided with an exhaust tube 2 and an inflation tube 7 which are communicated with the inside of the furnace body 3; one end of the lifting rod 1 is arranged in the furnace body 3, the lower end of the lifting rod is fixedly connected with a horizontally arranged prefabricated body mounting disc 9, and the other end of the lifting rod 1 extends out of the furnace body 3 from a through hole at the top of the furnace body 3; the lower surface of the prefabricated body mounting plate 9 is hung with a plurality of same prefabricated bodies 10, the arrangement form of the prefabricated bodies 10 is concentric ring-shaped, the prefabricated body mounting plate 9 and the prefabricated bodies 10 are arranged in the preheating zone 4, the grid type crucible 6 is arranged in the smelting zone 5 between the prefabricated bodies 10 and the crucible heating zone 13, the grid type crucible 6 is cylindrical, and a crucible chamber 61 corresponding to the arrangement position of each prefabricated body 10 is arranged in the grid type crucible 6;
wherein the heat insulation plate 11 can separate the temperature fields of the furnace body 3 and the preheating zone 4 so as to ensure that the temperatures of the smelting zone 5 and the preheating zone 4 are different.
The high-flux preparation method of the metal matrix composite material by using the high-flux preparation device of the metal matrix composite material comprises the following steps:
first, prepare
Respectively hoisting prefabricated bodies 10 on the lower surface of a prefabricated body mounting plate 9 in a concentric ring manner, arranging the prefabricated bodies 10 in a concentric ring manner, placing a grid type crucible 6 in a smelting zone 5 between the prefabricated bodies 10 and a crucible heating zone 13, and filling different crucible chambers 61 with base metals with different components;
second, removing the adhesive of the prefabricated body
Sealing the gas filling pipe 7, connecting the exhaust pipe 2 with a vacuumizing device to vacuumize the furnace body 3, and simultaneously heating the prefabricated body 10 by using an electric heating element in the preheating zone 4 to remove the adhesive in the prefabricated body 10;
third, atmosphere protection
Sealing the exhaust tube 2, filling inert gas into the furnace body 3 through the inflation tube 7 for protection, and simultaneously heating the smelting zone 5 and the crucible heating zone 13 to heat the base metals with different components filled in different crucible chambers 61 to a temperature 20-350 ℃ above the melting point of the base metal with the highest melting point and preserving heat for 0.1-3 h to obtain liquid base metal; heating the preheating zone 4 to heat the preform 10 to a temperature 20-50 ℃ below the melting point of the matrix metal with the lowest melting point, and keeping the temperature for 0.1-3 h;
fourthly, vacuum degassing
Sealing the gas filling pipe 7, connecting the gas pumping pipe 2 with a vacuumizing device to vacuumize the furnace body 3 so as to remove the matrix metal in the crucible chamber 61 and the inclusion gas in the preform 10, stopping heating the smelting zone 5, the crucible heating zone 13 and the preheating zone 4, and lowering the lifting rod 1 so that the preform mounting plate 9 and the preform 10 pass through the heat insulation plate 11 until the preform 10 is completely immersed below the liquid matrix metal in the crucible chamber 61;
fifth, air pressure infiltration
Injecting high-pressure inert gas into the furnace body 3 through the gas filling pipe 7 and maintaining the pressure to obtain a metal matrix composite material;
wherein, the impregnation of the liquid matrix on the prefabricated part 10 is realized by injecting inert gas into the furnace body 3 and maintaining the pressure, so as to obtain the metal matrix composite material;
sixthly, forming
Lifting the prefabricated body installation disc 9 to the prefabricated body 10 through the lifting rod 1, completely separating the prefabricated body 10 from the liquid base metal in the crucible chamber 61, alternately opening the exhaust tube 2 and the gas filling tube 7 to replace hot gas until the temperature of the metal-based composite material is reduced to 100-150 ℃, and finally unloading the metal-based composite material from the prefabricated body installation disc 9 and cooling to room temperature to finish the process;
the invention has the following beneficial effects: 1. according to the invention, through the design innovation of the grid type crucible, the metal matrix composite materials with different material matrixes are prepared at one time in a high flux manner in the same furnace, so that the interface wetting and interface reaction behaviors of the composite materials can be efficiently researched, and the aims of halving the cost, halving the period and quickly responding in the process of developing the metal matrix composite materials are supported; 2. according to the invention, the metal matrix composite materials with different matrixes are prepared by adopting air pressure infiltration, so that the equal pressure of each prefabricated part in the infiltration process can be ensured, and the mutual contrast of the infiltration results of different liquid metals on the reinforcement body is strong; 3. the invention adopts the lifting infiltration, which can accurately control the infiltration time; meanwhile, the prefabricated body is separated from the liquid metal after being impregnated with the liquid metal, so that the prefabricated body is prevented from being embedded in a solidified metal matrix, the sampling time can be shortened, and a sample can be quickly obtained; the crucible does not need to be damaged in the sampling process, the damage to the crucible is avoided, and the cost is saved.
The other metal matrix composite high-flux preparation device is composed of a lifting rod 1, an exhaust tube 2, a furnace body 3, a preheating zone 4, a smelting zone 5, a crucible 6, an inflation tube 7, a preform mounting disc 9, a plurality of preforms 10, a heat insulation plate 11 and a crucible heating zone 13;
the furnace body 3 is a sealed cavity body, a horizontal annular heat insulation plate 11 is arranged in the middle of the inside of the furnace body 3, the annular heat insulation plate 11 is fixedly connected with the inner wall of the furnace body 3, the upper part of the annular heat insulation plate 11 in the furnace body 3 is a preheating zone 4, the lower part of the annular heat insulation plate 11 in the furnace body 3 is a smelting zone 5, the bottom of the smelting zone 5 is a crucible heating zone 13, and electric heating elements are respectively arranged at the position, close to the inner wall of the furnace body 3, in the preheating zone 4, at the position, close to the inner wall of the furnace body 3; the upper part of the furnace body 3 is provided with an exhaust tube 2 and an inflation tube 7 which are communicated with the inside of the furnace body 3; one end of the lifting rod 1 is arranged in the furnace body 3, the lower end of the lifting rod is fixedly connected with a horizontally arranged prefabricated body mounting disc 9, and the other end of the lifting rod 1 extends out of the furnace body 3 from a through hole at the top of the furnace body 3; a plurality of prefabricated bodies 10 are hung on the lower surface of the prefabricated body mounting disc 9, the prefabricated bodies 10 are arranged in a concentric ring shape, the prefabricated body mounting disc 9 and the prefabricated bodies 10 are arranged in the preheating zone 4, the crucible 6 is arranged in the smelting zone 5 between the prefabricated bodies 10 and the crucible heating zone 13, and the crucible 6 is cylindrical; the electric heating element is a silicon-carbon rod, a silicon-molybdenum rod or an electrode graphite rod.
The method for preparing the metal matrix composite material with high flux by using the metal matrix composite material high flux preparation device comprises the following steps:
first, prepare
Hoisting a preform 10 on the lower surface of a preform mounting plate 9 in a concentric ring shape, placing a crucible 6 in a smelting zone 5 between the preform 10 and a crucible heating zone 13, and filling matrix metal in the crucible 6;
the prefabricated body 10 is composed of a mould and a composite reinforcement filled in the mould, the composite reinforcement is formed by bonding the reinforcement and an adhesive, and the composite reinforcement in the mould of each prefabricated body 10 is different;
the die is a hollow cylinder, the bottom of the die is sealed, and the side wall of the die is provided with a plurality of through holes; the aperture of the through hole is 0.5-3 mm;
the reinforcement is a particle reinforcement, a nanowire reinforcement, a nanotube reinforcement, a fiber reinforcement or a two-dimensional nanomaterial reinforcement; the material of the reinforcement body is one or more of carbide, oxide, boride, nitride, intermetallic compound and carbon material; the average particle diameter of the particle reinforcement is 50 nm-250 mu m; the average diameter of the nanowire reinforcement is 5-250 nm, and the average length of the nanowire reinforcement is 5-100 mu m; the average diameter of the nanotube reinforcement is 1-50 nm, and the average length of the nanotube reinforcement is 1-50 μm; the average fiber diameter of the fiber reinforcement body is 1-20 mu m; the average thickness of the two-dimensional nano material reinforcement is 0.34-20 nm, and the sheet diameter is 0.5-30 μm;
the number of the prefabricated bodies 10 is 30-1000;
the base metal is aluminum, aluminum alloy, copper alloy, magnesium alloy, iron alloy, titanium alloy, zinc alloy, nickel alloy, zirconium alloy, silver alloy, gold alloy, cobalt alloy, chromium alloy, tin or tin alloy;
second, removing the adhesive of the prefabricated body
Sealing the gas filling pipe 7, connecting the exhaust pipe 2 with a vacuumizing device to vacuumize the furnace body 3, and simultaneously heating the prefabricated body 10 by using an electric heating element in the preheating zone 4 to remove the adhesive in the prefabricated body 10;
the exhaust pipe 2 is connected with a vacuumizing device to vacuumize the furnace body 3 until the vacuum degree is 10-1000 Pa;
third, atmosphere protection
Sealing the exhaust tube 2, filling inert gas into the furnace body 3 through the gas filling tube 7 for protection, simultaneously heating the melting zone 5 and the crucible heating zone 13 to heat the base metal in the crucible 6 to 20-350 ℃ above the melting point of the base metal, and preserving heat for 0.1-3 h; the heating preheating zone 4 heats the prefabricated body 10 to 20-50 ℃ below the melting point of the matrix metal and keeps the temperature for 0.1-3 h;
fourthly, vacuum degassing
Sealing the gas filling pipe 7, connecting the gas pumping pipe 2 with a vacuumizing device to vacuumize the furnace body 3 so as to remove the matrix metal in the crucible 6 and the inclusion gas in the preform 10, stopping heating the smelting zone 5, the crucible heating zone 13 and the preheating zone 4, and lowering the lifting rod 1 to enable the preform mounting disc 9 and the preform 10 to pass through the heat insulation plate 11 until the preform 10 is completely immersed below the liquid level of the liquid matrix metal in the crucible 6;
fifth, air pressure infiltration
Injecting high-pressure inert gas into the furnace body 3 through the gas-filled pipe 7, carrying out air pressure infiltration and maintaining pressure; impregnating the prefabricated part 10 by a liquid matrix after injecting inert gas into the furnace body 3 to obtain a metal matrix composite material;
sixthly, forming
Lifting the prefabricated body installation disc 9 to the prefabricated body 10 through the lifting rod 1, enabling the prefabricated body 10 to be completely separated from the liquid base metal in the crucible 6, opening the air exhaust pipe 2 and the air charging pipe 7 in turn to replace hot gas until the temperature of the metal-based composite material is reduced to 100-150 ℃, and finally unloading the metal-based composite material from the prefabricated body installation disc 9 and cooling to room temperature to complete the process.
The principle and the beneficial effects of the invention are as follows: 1. according to the invention, the parallel type prefabricated body mold is designed and innovated, the metal matrix composite material of different reinforcements can be prepared at one time in a high flux manner in the same furnace, and samples of different reinforcements and liquid metal after infiltration at a set temperature can be obtained at a high flux, so that the interface wetting and interface reaction behaviors of the composite material can be efficiently researched, and the aims of cost halving, cycle halving and quick response in the process of developing the metal matrix composite material are supported; 2. according to the invention, the metal-based composite material of different reinforcements is prepared by adopting air pressure infiltration, so that the pressure of each prefabricated part is equal in the infiltration process, and the mutual contrast of the infiltration results of the liquid metal to the different reinforcements is strong; 3. the invention adopts the lifting infiltration, which can accurately control the infiltration time; meanwhile, the prefabricated body is separated from the liquid metal after being impregnated with the liquid metal, so that the prefabricated body is prevented from being embedded in a solidified metal matrix, the sampling time can be shortened, and a sample can be quickly obtained; the crucible does not need to be damaged in the sampling process, the damage to the crucible is avoided, and the cost is saved.
Drawings
FIG. 1 is a schematic structural diagram of a high-throughput metal matrix composite manufacturing apparatus according to a first embodiment;
FIG. 2 is a schematic diagram illustrating the distribution positions of a plurality of preforms 10 on the lower surface of a preform mounting plate 9 according to the first embodiment;
FIG. 3 is a schematic structural diagram of an eighteen embodiment of a high-throughput metal-based composite manufacturing apparatus;
FIG. 4 is a schematic diagram showing the distribution positions of the preforms 10 on the lower surface of the preform mounting tray 9 in the eighteenth embodiment;
the specific implementation mode is as follows:
the technical scheme of the invention is not limited to the specific embodiments listed below, and any reasonable combination of the specific embodiments is included.
The first embodiment is as follows: the embodiment is described with reference to fig. 1 and 2, and the high-throughput preparation device for metal matrix composites of the embodiment is composed of a lifting rod 1, an exhaust tube 2, a furnace body 3, a preheating zone 4, a smelting zone 5, a grid type crucible 6, an inflation tube 7, a preform mounting plate 9, a plurality of same preforms 10, a heat insulation plate 11 and a crucible heating zone 13;
the furnace body 3 is a sealed cavity body, a horizontal annular heat insulation plate 11 is arranged in the middle of the inside of the furnace body 3, the annular heat insulation plate 11 is fixedly connected with the inner wall of the furnace body 3, the upper part of the annular heat insulation plate 11 in the furnace body 3 is a preheating zone 4, the lower part of the annular heat insulation plate 11 in the furnace body 3 is a smelting zone 5, the bottom of the smelting zone 5 is a crucible heating zone 13, and electric heating elements are respectively arranged at the position, close to the inner wall of the furnace body 3, in the preheating zone 4, at the position, close to the inner wall of the furnace body 3; the upper part of the furnace body 3 is provided with an exhaust tube 2 and an inflation tube 7 which are communicated with the inside of the furnace body 3; one end of the lifting rod 1 is arranged in the furnace body 3, the lower end of the lifting rod is fixedly connected with a horizontally arranged prefabricated body mounting disc 9, and the other end of the lifting rod 1 extends out of the furnace body 3 from a through hole at the top of the furnace body 3; the lower surface of the prefabricated body mounting plate 9 is hung with a plurality of same prefabricated bodies 10, the arrangement form of the prefabricated bodies 10 is concentric ring-shaped, the prefabricated body mounting plate 9 and the prefabricated bodies 10 are arranged in the preheating zone 4, the grid type crucible 6 is arranged in the smelting zone 5 between the prefabricated bodies 10 and the crucible heating zone 13, the grid type crucible 6 is cylindrical, and a crucible chamber 61 corresponding to the arrangement position of each prefabricated body 10 is arranged in the grid type crucible 6;
the number of the crucible chambers 61 is 30-1000;
the prefabricated part 10 consists of a mould and a reinforcement filled in the mould, and the reinforcement is formed by bonding reinforcement particles with an adhesive;
the mould is a hollow cylinder, the bottom of the mould is sealed, the side wall of the mould is provided with a plurality of through holes, and the through holes on the side wall of the mould are used as passages for the base body to enter the mould.
The embodiment has the following beneficial effects:
1. the embodiment prepares the metal matrix composite material with different material matrixes in one step at high flux in the same furnace through the design innovation of the grid type crucible, thereby efficiently researching the interface wetting and interface reaction behaviors of the composite material and supporting the aims of halving the cost, halving the period and quickly responding in the process of developing the metal matrix composite material;
2. the embodiment adopts the air pressure infiltration to prepare the metal matrix composite materials with different matrixes, so that the equal pressure of each prefabricated part can be ensured in the infiltration process, and the mutual contrast of the infiltration results of different liquid metals on the reinforcement body is strong;
3. the embodiment adopts the lifting infiltration, so that the infiltration time can be accurately controlled; meanwhile, the prefabricated body is separated from the liquid metal after being impregnated with the liquid metal, so that the prefabricated body is prevented from being embedded in a solidified metal matrix, the sampling time can be shortened, and a sample can be quickly obtained; the crucible does not need to be damaged in the sampling process, the damage to the crucible is avoided, and the cost is saved.
The second embodiment is as follows: the first difference between the present embodiment and the specific embodiment is: the electric heating element is a silicon-carbon rod, a silicon-molybdenum rod or an electrode graphite rod.
The third concrete implementation mode: the first difference between the present embodiment and the specific embodiment is: the adhesive is polyvinyl alcohol.
The fourth concrete implementation mode: the first difference between the present embodiment and the specific embodiment is: the aperture of the through hole on the side wall of the die is 0.5-3 mm.
The fifth concrete implementation mode: the first difference between the present embodiment and the specific embodiment is: the material of the mould is ceramic, graphite or metal which is not melted with the base metal.
The sixth specific implementation mode: the embodiment of the invention provides a high-flux preparation method of a metal matrix composite material by using a high-flux preparation device of the metal matrix composite material, which comprises the following steps:
first, prepare
Respectively hoisting prefabricated bodies 10 on the lower surface of a prefabricated body mounting plate 9 in a concentric ring manner, arranging the prefabricated bodies 10 in a concentric ring manner, placing a grid type crucible 6 in a smelting zone 5 between the prefabricated bodies 10 and a crucible heating zone 13, and filling different crucible chambers 61 with base metals with different components;
the types of the base metal are 30-1000; the material of each base metal is aluminum, aluminum alloy, copper alloy, magnesium alloy, iron alloy, titanium alloy, zinc alloy, nickel alloy, zirconium alloy, silver alloy, gold alloy, cobalt alloy, chromium alloy, tin alloy, tungsten or tungsten alloy;
the matrix metal is in the form of one or a mixture of two of metal block bodies and metal powder in any proportion; the particle size of the metal powder is 1-250 μm, and the particle size of the metal block is 300-1000 μm;
the prefabricated part 10 consists of a mould and a reinforcement filled in the mould, and the reinforcement is formed by bonding reinforcement particles with an adhesive;
the reinforcement is made of carbide, oxide, nitride, boride, intermetallic compound, carbon material or boron material;
the particle size range of the reinforcing body particles is 1-200 mu m.
Second, removing the adhesive of the prefabricated body
Sealing the gas filling pipe 7, connecting the exhaust pipe 2 with a vacuumizing device to vacuumize the furnace body 3, and simultaneously heating the prefabricated body 10 by using an electric heating element in the preheating zone 4 to remove the adhesive in the prefabricated body 10;
third, atmosphere protection
Sealing the exhaust tube 2, filling inert gas into the furnace body 3 through the inflation tube 7 for protection, and simultaneously heating the smelting zone 5 and the crucible heating zone 13 to heat the base metals with different components filled in different crucible chambers 61 to a temperature 20-350 ℃ above the melting point of the base metal with the highest melting point and preserving heat for 0.1-3 h to obtain liquid base metal; heating the preheating zone 4 to heat the preform 10 to a temperature 20-50 ℃ below the melting point of the matrix metal with the lowest melting point, and keeping the temperature for 0.1-3 h;
fourthly, vacuum degassing
Sealing the gas filling pipe 7, connecting the gas pumping pipe 2 with a vacuumizing device to vacuumize the furnace body 3 so as to remove the matrix metal in the crucible chamber 61 and the inclusion gas in the preform 10, stopping heating the smelting zone 5, the crucible heating zone 13 and the preheating zone 4, and lowering the lifting rod 1 so that the preform mounting plate 9 and the preform 10 pass through the heat insulation plate 11 until the preform 10 is completely immersed below the liquid matrix metal in the crucible chamber 61;
fifth, air pressure infiltration
Injecting high-pressure inert gas into the furnace body 3 through the gas filling pipe 7 and maintaining the pressure to obtain a metal matrix composite material;
sixthly, forming
Lifting the prefabricated body installation disc 9 to the prefabricated body 10 through the lifting rod 1, completely separating the prefabricated body 10 from the liquid base metal in the crucible chamber 61, alternately opening the exhaust tube 2 and the gas filling tube 7 to replace hot gas until the temperature of the metal-based composite material is reduced to 100-150 ℃, and finally unloading the metal-based composite material from the prefabricated body installation disc 9 and cooling to room temperature to finish the process.
1. The embodiment prepares the metal matrix composite material with different material matrixes in one step at high flux in the same furnace through the design innovation of the grid type crucible, thereby efficiently researching the interface wetting and interface reaction behaviors of the composite material and supporting the aims of halving the cost, halving the period and quickly responding in the process of developing the metal matrix composite material;
2. the embodiment adopts the air pressure infiltration to prepare the metal matrix composite materials with different matrixes, so that the equal pressure of each prefabricated part can be ensured in the infiltration process, and the mutual contrast of the infiltration results of different liquid metals on the reinforcement body is strong;
3. the embodiment adopts the lifting infiltration, so that the infiltration time can be accurately controlled; meanwhile, the prefabricated body is separated from the liquid metal after being impregnated with the liquid metal, so that the prefabricated body is prevented from being embedded in a solidified metal matrix, the sampling time can be shortened, and a sample can be quickly obtained; the crucible does not need to be damaged in the sampling process, the damage to the crucible is avoided, and the cost is saved.
The seventh embodiment: the sixth embodiment is different from the sixth embodiment in that: step one, the grid type crucible 6 is made of ceramic or graphite. The grid type crucible is made of a material which is not melted with the matrix component, and has high temperature resistance, high air tightness and high strength.
The specific implementation mode is eight: the sixth embodiment is different from the sixth embodiment in that: step one, the adhesive is polyvinyl alcohol.
The specific implementation method nine: the sixth embodiment is different from the sixth embodiment in that: step one, the mass ratio of the reinforcing body particles to the adhesive is 1 (0.05-0.1).
The detailed implementation mode is ten: the sixth embodiment is different from the sixth embodiment in that: step one the difference in melting points of the base metal filled in the different crucible chambers 61 is less than 150 ℃. The melting point difference of the base bodies is less than 150 ℃, so that the different base bodies can be completely melted, and the problem that the accuracy of components is influenced due to serious volatilization of volatile elements in the alloy with a lower melting point can be avoided.
The concrete implementation mode eleven: the sixth embodiment is different from the sixth embodiment in that: and fourthly, the descending speed of the lifting rod 1 is 0.01 mm/s-2.0 mm/s.
The specific implementation mode twelve: the sixth embodiment is different from the sixth embodiment in that: and step four, connecting the exhaust pipe 2 with a vacuumizing device to vacuumize the furnace body 3 until the vacuum degree is 10-1000 Pa.
The specific implementation mode is thirteen: the sixth embodiment is different from the sixth embodiment in that: and fifthly, the inert gas is nitrogen, argon or helium.
The specific implementation mode is fourteen: the sixth embodiment is different from the sixth embodiment in that: fifthly, the pressure of the inert gas is 0.1-10 MPa.
The concrete implementation mode is fifteen: the sixth embodiment is different from the sixth embodiment in that: and step five, the pressure maintaining time is 1-60 min.
The specific implementation mode is sixteen: the sixth embodiment is different from the sixth embodiment in that: and sixthly, the lifting speed of the prefabricated body mounting disc 9 is 0.1-10 mm/s.
Seventeenth embodiment: the sixth embodiment is different from the sixth embodiment in that: and step two, connecting the exhaust pipe 2 with a vacuumizing device to vacuumize the furnace body 3 until the vacuum degree is 10-1000 Pa.
The specific implementation mode is eighteen: the embodiment is described with reference to fig. 3 and 4, and the high-throughput preparation device of metal matrix composite material of the embodiment is composed of a lifting rod 1, an exhaust tube 2, a furnace body 3, a preheating zone 4, a smelting zone 5, a crucible 6, an inflation tube 7, a preform mounting plate 9, a plurality of preforms 10, a heat insulation plate 11 and a crucible heating zone 13;
the furnace body 3 is a sealed cavity body, a horizontal annular heat insulation plate 11 is arranged in the middle of the inside of the furnace body 3, the annular heat insulation plate 11 is fixedly connected with the inner wall of the furnace body 3, the upper part of the annular heat insulation plate 11 in the furnace body 3 is a preheating zone 4, the lower part of the annular heat insulation plate 11 in the furnace body 3 is a smelting zone 5, the bottom of the smelting zone 5 is a crucible heating zone 13, and electric heating elements are respectively arranged at the position, close to the inner wall of the furnace body 3, in the preheating zone 4, at the position, close to the inner wall of the furnace body 3; the upper part of the furnace body 3 is provided with an exhaust tube 2 and an inflation tube 7 which are communicated with the inside of the furnace body 3; one end of the lifting rod 1 is arranged in the furnace body 3, the lower end of the lifting rod is fixedly connected with a horizontally arranged prefabricated body mounting disc 9, and the other end of the lifting rod 1 extends out of the furnace body 3 from a through hole at the top of the furnace body 3; a plurality of prefabricated bodies 10 are hung on the lower surface of the prefabricated body mounting disc 9, the prefabricated bodies 10 are arranged in a concentric ring shape, the prefabricated body mounting disc 9 and the prefabricated bodies 10 are arranged in the preheating zone 4, the crucible 6 is arranged in the smelting zone 5 between the prefabricated bodies 10 and the crucible heating zone 13, and the crucible 6 is cylindrical;
the electric heating element is a silicon-carbon rod, a silicon-molybdenum rod or an electrode graphite rod.
1. The embodiment realizes the one-time high-flux preparation of the metal-based composite materials of different reinforcements in the same furnace through the design innovation of a parallel type prefabricated body mold, and can obtain samples of different reinforcements and liquid metal infiltrated at a set temperature in a high-flux manner, so that the interface wetting and interface reaction behaviors of the composite materials can be efficiently researched, and the aims of cost halving, cycle halving and quick response in the process of developing the metal-based composite materials are supported;
2. in the embodiment, the metal-based composite material of different reinforcements is prepared by adopting air pressure infiltration, so that the pressure of each prefabricated part is equal in the infiltration process, and the mutual contrast of the infiltration results of the liquid metal to the different reinforcements is strong;
3. the embodiment adopts the lifting infiltration, so that the infiltration time can be accurately controlled; meanwhile, the prefabricated body is separated from the liquid metal after being impregnated with the liquid metal, so that the prefabricated body is prevented from being embedded in a solidified metal matrix, the sampling time can be shortened, and a sample can be quickly obtained; the crucible does not need to be damaged in the sampling process, the damage to the crucible is avoided, and the cost is saved.
The detailed embodiment is nineteen: the method for preparing the metal matrix composite material with high flux by using the metal matrix composite material high flux preparation device in the embodiment comprises the following steps:
first, prepare
Hoisting a preform 10 on the lower surface of a preform mounting plate 9 in a concentric ring shape, placing a crucible 6 in a smelting zone 5 between the preform 10 and a crucible heating zone 13, and filling matrix metal in the crucible 6;
the prefabricated body 10 is composed of a mould and a composite reinforcement filled in the mould, the composite reinforcement is formed by bonding the reinforcement and an adhesive, and the composite reinforcement in the mould of each prefabricated body 10 is different;
the die is a hollow cylinder, the bottom of the die is sealed, and the side wall of the die is provided with a plurality of through holes; the aperture of the through hole is 0.5-3 mm;
the reinforcement is a particle reinforcement, a nanowire reinforcement, a nanotube reinforcement, a fiber reinforcement or a two-dimensional nanomaterial reinforcement; the material of the reinforcement body is one or more of carbide, oxide, boride, nitride, intermetallic compound and carbon material; the average particle diameter of the particle reinforcement is 50 nm-250 mu m; the average diameter of the nanowire reinforcement is 5-250 nm, and the average length of the nanowire reinforcement is 5-100 mu m; the average diameter of the nanotube reinforcement is 1-50 nm, and the average length of the nanotube reinforcement is 1-50 μm; the average fiber diameter of the fiber reinforcement body is 1-20 mu m; the average thickness of the two-dimensional nano material reinforcement is 0.34-20 nm, and the sheet diameter is 0.5-30 μm;
the number of the prefabricated bodies 10 is 30-1000;
the matrix metal is aluminum, aluminum alloy, copper alloy, magnesium alloy, iron alloy, titanium alloy, zinc alloy, nickel alloy, zirconium alloy, silver alloy, gold alloy, cobalt alloy, chromium alloy, tin or tin;
second, removing the adhesive of the prefabricated body
Sealing the gas filling pipe 7, connecting the exhaust pipe 2 with a vacuumizing device to vacuumize the furnace body 3, and simultaneously heating the prefabricated body 10 by using an electric heating element in the preheating zone 4 to remove the adhesive in the prefabricated body 10;
the exhaust pipe 2 is connected with a vacuumizing device to vacuumize the furnace body 3 until the vacuum degree is 10-1000 Pa;
third, atmosphere protection
Sealing the exhaust tube 2, filling inert gas into the furnace body 3 through the gas filling tube 7 for protection, simultaneously heating the melting zone 5 and the crucible heating zone 13 to heat the base metal in the crucible 6 to 20-350 ℃ above the melting point of the base metal, and preserving heat for 0.1-3 h; the heating preheating zone 4 heats the prefabricated body 10 to 20-50 ℃ below the melting point of the matrix metal and keeps the temperature for 0.1-3 h;
fourthly, vacuum degassing
Sealing the gas filling pipe 7, connecting the gas pumping pipe 2 with a vacuumizing device to vacuumize the furnace body 3 so as to remove the matrix metal in the crucible 6 and the inclusion gas in the preform 10, stopping heating the smelting zone 5, the crucible heating zone 13 and the preheating zone 4, and lowering the lifting rod 1 to enable the preform mounting disc 9 and the preform 10 to pass through the heat insulation plate 11 until the preform 10 is completely immersed below the liquid level of the liquid matrix metal in the crucible 6;
fifth, air pressure infiltration
Injecting high-pressure inert gas into the furnace body 3 through the gas-filled pipe 7, carrying out air pressure infiltration and maintaining pressure; impregnating the prefabricated part 10 by a liquid matrix after injecting inert gas into the furnace body 3 to obtain a metal matrix composite material;
sixthly, forming
Lifting the prefabricated body installation disc 9 to the prefabricated body 10 through the lifting rod 1, enabling the prefabricated body 10 to be completely separated from the liquid base metal in the crucible 6, opening the air exhaust pipe 2 and the air charging pipe 7 in turn to replace hot gas until the temperature of the metal-based composite material is reduced to 100-150 ℃, and finally unloading the metal-based composite material from the prefabricated body installation disc 9 and cooling to room temperature to complete the process.
The principle and the beneficial effects of the implementation mode are as follows:
1. the embodiment realizes the one-time high-flux preparation of the metal-based composite materials of different reinforcements in the same furnace through the design innovation of a parallel type prefabricated body mold, and can obtain samples of different reinforcements and liquid metal infiltrated at a set temperature in a high-flux manner, so that the interface wetting and interface reaction behaviors of the composite materials can be efficiently researched, and the aims of cost halving, cycle halving and quick response in the process of developing the metal-based composite materials are supported;
2. in the embodiment, the metal-based composite material of different reinforcements is prepared by adopting air pressure infiltration, so that the pressure of each prefabricated part is equal in the infiltration process, and the mutual contrast of the infiltration results of the liquid metal to the different reinforcements is strong;
3. the embodiment adopts the lifting infiltration, so that the infiltration time can be accurately controlled; meanwhile, the prefabricated body is separated from the liquid metal after being impregnated with the liquid metal, so that the prefabricated body is prevented from being embedded in a solidified metal matrix, the sampling time can be shortened, and a sample can be quickly obtained; the crucible does not need to be damaged in the sampling process, the damage to the crucible is avoided, and the cost is saved.
The specific implementation mode twenty: this embodiment differs from the nineteenth embodiment in that: step one, the adhesive is polyvinyl alcohol.
The specific implementation mode is twenty one: this embodiment differs from the nineteenth embodiment in that: step one, the mass ratio of the reinforcement to the adhesive is 1 (0.05-0.1).
Specific embodiment twenty-two: this embodiment differs from the nineteenth embodiment in that: step one, the material of the mould is ceramic, graphite or metal which is not melted with base metal.
Specific embodiment twenty-three: this embodiment differs from the nineteenth embodiment in that: step one, the two-dimensional nanomaterial reinforcement is graphene.
Twenty-four specific embodiments: this embodiment differs from the nineteenth embodiment in that: step one, the prefabricated body installation disc 9 is made of graphite, carbon/carbon composite materials or heat-resistant steel. The graphite, carbon/carbon composite material or heat-resistant steel and other materials are not melted with the matrix components, and have high temperature resistance, high air tightness and high strength.
The specific implementation mode is twenty five: this embodiment differs from the nineteenth embodiment in that: step one the crucible 6 is a cylindrical crucible.
The specific implementation mode is twenty-six: this embodiment differs from the nineteenth embodiment in that: step one, the crucible 6 is made of ceramic or graphite. The crucible 6 is made of a material which is not melted with the matrix component, and has high temperature resistance, high air tightness and high strength.
The specific implementation mode is twenty-seven: this embodiment differs from the nineteenth embodiment in that: and step four, connecting the exhaust pipe 2 with a vacuumizing device to vacuumize the furnace body 3 until the vacuum degree is 10-1000 Pa.
The specific implementation mode is twenty-eight: this embodiment differs from the nineteenth embodiment in that: and fourthly, the descending speed of the lifting rod 1 is 0.01 mm/s-2.0 mm/s.
The specific implementation mode is twenty-nine: this embodiment differs from the nineteenth embodiment in that: and fifthly, the inert gas is nitrogen, argon or helium.
The specific implementation mode is thirty: this embodiment differs from the nineteenth embodiment in that: fifthly, the pressure of the inert gas is 0.1-10 MPa.
The specific implementation mode is thirty-one: this embodiment differs from the nineteenth embodiment in that: and step five, the pressure maintaining time is 1-60 min.
The specific implementation mode is thirty-two: this embodiment differs from the nineteenth embodiment in that: and sixthly, the lifting speed of the prefabricated body mounting disc 9 is 0.1-10 mm/s.
The following examples were used to demonstrate the beneficial effects of the present invention:
example 1:
the metal matrix composite high-throughput preparation device of the embodiment comprises a lifting rod 1, an exhaust tube 2, a furnace body 3, a preheating zone 4, a smelting zone 5, a grid type crucible 6, an inflation tube 7, a preform mounting disc 9, 1000 preforms 10, a heat insulation plate 11 and a crucible heating zone 13;
the furnace body 3 is a sealed cavity body, a horizontal annular heat insulation plate 11 is arranged in the middle of the inside of the furnace body 3, the annular heat insulation plate 11 is fixedly connected with the inner wall of the furnace body 3, the upper part of the annular heat insulation plate 11 in the furnace body 3 is a preheating zone 4, the lower part of the annular heat insulation plate 11 in the furnace body 3 is a smelting zone 5, the bottom of the smelting zone 5 is a crucible heating zone 13, and electric heating elements are respectively arranged at the position, close to the inner wall of the furnace body 3, in the preheating zone 4, at the position, close to the inner wall of the furnace body 3; the upper part of the furnace body 3 is provided with an exhaust tube 2 and an inflation tube 7 which are communicated with the inside of the furnace body 3; one end of the lifting rod 1 is arranged in the furnace body 3, the lower end of the lifting rod is fixedly connected with a horizontally arranged prefabricated body mounting disc 9, and the other end of the lifting rod 1 extends out of the furnace body 3 from a through hole at the top of the furnace body 3; 1000 same preforms 10 are hung on the lower surface of the preform mounting disc 9, the arrangement forms of the preforms 10 are concentric rings, the preform mounting disc 9 and the preforms 10 are arranged in the preheating zone 4, the grid type crucible 6 is arranged in the smelting zone 5 between the preforms 10 and the crucible heating zone 13, the grid type crucible 6 is cylindrical, and a crucible chamber 61 corresponding to the arrangement position of each preform 10 is arranged in the grid type crucible 6.
The electric heating element is a silicon carbide rod;
the prefabricated part 10 consists of a mould and a reinforcement filled in the mould, and the reinforcement is formed by bonding reinforcement particles with an adhesive;
the adhesive is polyvinyl alcohol;
the die is a hollow cylinder, the bottom of the die is sealed, and the side wall of the die is provided with a plurality of through holes; wherein, the through hole of the side wall of the mould is used as a channel for the substrate to enter the mould;
the aperture of the through hole on the side wall of the die is 0.5 mm;
the material of the mould is alumina ceramic;
the high-flux preparation method of the metal matrix composite material by using the high-flux preparation device of the metal matrix composite material comprises the following steps:
first, prepare
Respectively hoisting prefabricated bodies 10 on the lower surface of a prefabricated body mounting plate 9 in a concentric ring manner, arranging the prefabricated bodies 10 in a concentric ring manner, placing a grid type crucible 6 in a smelting zone 5 between the prefabricated bodies 10 and a crucible heating zone 13, and filling different crucible chambers 61 with base metals with different components;
the prefabricated part 10 consists of a mould and a reinforcement filled in the mould; the adhesive is polyvinyl alcohol; the reinforcement is SiC ceramic particles with the particle size of 10 mu m; the mass ratio of the reinforcing body particles to the adhesive is 1: 0.1;
the die is a hollow cylinder, the bottom of the die is sealed, and the side wall of the die is provided with a plurality of through holes; the aperture of the through hole is 0.5 mm; the through hole on the side wall of the mold is used as a passage for the matrix to enter the mold;
the material of the mould is alumina ceramic;
the grid type crucible 6 is made of high-purity graphite;
the components of the matrix metal filled in each crucible chamber are different;
the number of the base metal species is 1000; the matrix metal is Al-Mg-Si alloy; in different Al-Mg-Si alloys: the Mg element component accounts for 0.2-8.0% of the mass fraction, and the mass fraction interval of the Mg element is 0.2%; the Si element component accounts for 0.5-12.5% of the mass fraction and the mass fraction interval of the Si element is 0.5%;
the melting points of the matrixes with different components filled in the different crucible chambers 61 are 660 ℃ at most, 577 ℃ at least and 83 ℃ in difference;
the matrix metal is a mixture of pure Al block, pure Mg powder and pure Si powder; the grain size of the pure Al block is 300-400 mu m;
second, removing the adhesive of the prefabricated body
Sealing the gas filling pipe 7, connecting the exhaust pipe 2 with a vacuumizing device to vacuumize the furnace body 3, and simultaneously heating the prefabricated body 10 by using an electric heating element in the preheating zone 4 to remove the adhesive in the prefabricated body 10;
the exhaust pipe 2 is connected with a vacuumizing device to vacuumize the furnace body 3 until the vacuum degree is 1000 Pa;
third, atmosphere protection
The extraction pipe 2 is closed, inert gas is filled into the furnace body 3 through the inflation pipe 7 for protection, and meanwhile, the smelting zone 5 and the crucible heating zone 13 are heated, so that the base metals with different components filled in different crucible chambers 61 are heated to 340 ℃ (namely 1000 ℃) above the melting point of the base metal with the highest melting point, and heat preservation is carried out for 3 hours, and liquid base metal is obtained; heating the preheating zone 4 to heat the preform 10 to 50 ℃ (i.e. 527 ℃) below the melting point of the base metal with the lowest melting point and keeping the temperature for 3 hours; the inert gas is nitrogen;
fourthly, vacuum degassing
Sealing the gas filling pipe 7, connecting the gas pumping pipe 2 with a vacuumizing device to vacuumize the furnace body 3 so as to remove the matrix metal in the crucible chamber 61 and the inclusion gas in the preform 10, stopping heating the smelting zone 5, the crucible heating zone 13 and the preheating zone 4, and lowering the lifting rod 1 so that the preform mounting plate 9 and the preform 10 pass through the heat insulation plate 11 until the preform 10 is completely immersed below the liquid matrix metal in the crucible chamber 61;
the descending speed of the lifting rod 1 is 0.01 mm/s;
and the exhaust pipe 2 is connected with a vacuumizing device to vacuumize the furnace body 3 until the vacuum degree is 1000 Pa.
Fifth, air pressure infiltration
Injecting high-pressure inert gas into the furnace body 3 through the gas filling pipe 7 and maintaining the pressure to obtain a metal matrix composite material;
the inert gas is nitrogen;
the pressure of the inert gas is 0.1 MPa;
the pressure maintaining time is 60 min;
sixthly, forming
Lifting the prefabricated body installation disc 9 to the prefabricated body 10 through the lifting rod 1, completely separating the prefabricated body 10 from the liquid base metal in the crucible chamber 61, alternately opening the exhaust tube 2 and the gas filling tube 7 to replace hot gas until the temperature of the metal-based composite material is reduced to 150 ℃, and finally unloading the metal-based composite material from the prefabricated body installation disc 9 and cooling to room temperature to finish the process;
sixthly, the lifting speed of the prefabricated body mounting disc 9 is 0.1 mm/s;
example 1 microscopic Structure Observation results:
example 1 a metal matrix composite of 10 μm silicon carbide particles with 1000 Al-Mg-Si alloys was obtained under the same infiltration pressure conditions of 0.1 MPa. Experiments show that under the infiltration pressure of 0.1MPa, when the Mg content is less than or equal to 5.4 percent, the Al-Mg-Si alloy can not fully infiltrate the SiC preform, and when the Mg content is less than or equal to 5.4 percent>5.4 percent, the Al-Mg-Si alloy can fully infiltrate the SiC prefabricated body; when the Si content is less than or equal to 7.5 percent, SiC can generate a harmful interface reaction product with the aluminum matrix to generate Al4C3When the content of Si is>When the silicon carbide content is 7.5 percent, SiC can not generate interface reaction with an aluminum matrix; if the traditional one-time and sequential iteration mode is adopted for research, hundreds of tests or even 1000 tests are needed, and by adopting the scheme, the interface wetting and interface reaction behaviors of the SiC reinforced Al-Mg-Si composite material can be efficiently researched only by one test.
Example 2:
the metal matrix composite high-throughput preparation device of the embodiment comprises a lifting rod 1, an exhaust tube 2, a furnace body 3, a preheating zone 4, a smelting zone 5, a grid type crucible 6, an inflation tube 7, a preform mounting disc 9, 40 preforms 10, a heat insulation plate 11 and a crucible heating zone 13;
the furnace body 3 is a sealed cavity body, a horizontal annular heat insulation plate 11 is arranged in the middle of the inside of the furnace body 3, the annular heat insulation plate 11 is fixedly connected with the inner wall of the furnace body 3, the upper part of the annular heat insulation plate 11 in the furnace body 3 is a preheating zone 4, the lower part of the annular heat insulation plate 11 in the furnace body 3 is a smelting zone 5, the bottom of the smelting zone 5 is a crucible heating zone 13, and electric heating elements are respectively arranged at the position, close to the inner wall of the furnace body 3, in the preheating zone 4, at the position, close to the inner wall of the furnace body 3; the upper part of the furnace body 3 is provided with an exhaust tube 2 and an inflation tube 7 which are communicated with the inside of the furnace body 3; one end of the lifting rod 1 is arranged in the furnace body 3, the lower end of the lifting rod is fixedly connected with a horizontally arranged prefabricated body mounting disc 9, and the other end of the lifting rod 1 extends out of the furnace body 3 from a through hole at the top of the furnace body 3; the lower surface of the prefabricated body mounting plate 9 is hung with 40 same prefabricated bodies 10, the arrangement form of the prefabricated bodies 10 is concentric ring-shaped, the prefabricated body mounting plate 9 and the prefabricated bodies 10 are arranged in the preheating zone 4, the grid type crucible 6 is arranged in the smelting zone 5 between the prefabricated bodies 10 and the crucible heating zone 13, the grid type crucible 6 is cylindrical, and a crucible chamber 61 corresponding to the arrangement position of each prefabricated body 10 is arranged in the grid type crucible 6.
The electric heating element is an electrode graphite rod;
the prefabricated part 10 consists of a mould and a reinforcement filled in the mould, and the reinforcement is formed by bonding reinforcement particles with an adhesive;
the adhesive is polyvinyl alcohol;
the die is a hollow cylinder, the bottom of the die is sealed, and the side wall of the die is provided with a plurality of through holes; wherein, the through hole of the side wall of the mould is used as a channel for the substrate to enter the mould;
the aperture of the through hole on the side wall of the die is 3 mm;
the material of the mould is high-purity graphite;
the high-flux preparation method of the metal matrix composite material by using the high-flux preparation device of the metal matrix composite material comprises the following steps:
first, prepare
Respectively hoisting prefabricated bodies 10 on the lower surface of a prefabricated body mounting plate 9 in a concentric ring manner, arranging the prefabricated bodies 10 in a concentric ring manner, placing a grid type crucible 6 in a smelting zone 5 between the prefabricated bodies 10 and a crucible heating zone 13, and filling different crucible chambers 61 with base metals with different components;
the prefabricated part 10 consists of a mould and a reinforcement filled in the mould; the adhesive is polyvinyl alcohol; the reinforcing body is diamond particles with the particle size of 200 mu m; the mass ratio of the reinforcing body particles to the adhesive is 1: 0.08;
the die is a hollow cylinder, the bottom of the die is sealed, and the side wall of the die is provided with a plurality of through holes; the aperture of the through hole is 3 mm; the through hole on the side wall of the mold is used as a passage for the matrix to enter the mold;
the material of the mould is high-purity graphite;
the grid type crucible 6 is made of high-purity graphite;
the components of the matrix metal filled in each crucible chamber are different;
the number of the base metal species is 40; the base metal is Cu-Zr alloy; wherein, the Zr element component accounts for 0.5 to 20 percent of the mass fraction, and the component intervals are all 0.5 percent;
the melting points of the matrixes with different components filled in the different crucible chambers 61 are 1115 ℃ at most, 972 ℃ at least and 143 ℃ in difference;
the matrix metal is a mixture of pure Cu powder and pure Zr powder; the grain size of the pure Cu powder is 100 mu m, and the grain size of the pure Zr powder is 100 mu m;
second, removing the adhesive of the prefabricated body
Sealing the gas filling pipe 7, connecting the exhaust pipe 2 with a vacuumizing device to vacuumize the furnace body 3, and simultaneously heating the prefabricated body 10 by using an electric heating element in the preheating zone 4 to remove the adhesive in the prefabricated body 10;
the exhaust pipe 2 is connected with a vacuumizing device to vacuumize the furnace body 3 until the vacuum degree is 10 Pa;
third, atmosphere protection
The extraction tube 2 is closed, inert gas is filled into the furnace body 3 through the inflation tube 7 for protection, and meanwhile, the smelting zone 5 and the crucible heating zone 13 are heated, so that the base metals with different components filled in different crucible chambers 61 are heated to 40 ℃ above the melting point of the base metal with the highest melting point (namely 1155 ℃) and are kept warm for 0.1h, and liquid base metal is obtained; heating the preheating zone 4 to heat the preform 10 to 20 ℃ (952 ℃) below the melting point of the lowest melting point base metal and keeping the temperature for 0.1 h; the inert gas is nitrogen;
fourthly, vacuum degassing
Sealing the gas filling pipe 7, connecting the gas pumping pipe 2 with a vacuumizing device to vacuumize the furnace body 3 so as to remove the matrix metal in the crucible chamber 61 and the inclusion gas in the preform 10, stopping heating the smelting zone 5, the crucible heating zone 13 and the preheating zone 4, and lowering the lifting rod 1 so that the preform mounting plate 9 and the preform 10 pass through the heat insulation plate 11 until the preform 10 is completely immersed below the liquid matrix metal in the crucible chamber 61;
the descending speed of the lifting rod 1 is 0.1 mm/s;
and the exhaust pipe 2 is connected with a vacuumizing device to vacuumize the furnace body 3 until the vacuum degree is 10 Pa.
Fifth, air pressure infiltration
Injecting high-pressure inert gas into the furnace body 3 through the gas filling pipe 7 and maintaining the pressure to obtain a metal matrix composite material;
the inert gas is nitrogen;
the pressure of the inert gas is 10 MPa;
the pressure maintaining time is 2 min;
sixthly, forming
Lifting the prefabricated body installation disc 9 to the prefabricated body 10 through the lifting rod 1, completely separating the prefabricated body 10 from the liquid base metal in the crucible chamber 61, alternately opening the exhaust tube 2 and the gas filling tube 7 to replace hot gas until the temperature of the metal-based composite material is reduced to 110 ℃, and finally unloading the metal-based composite material from the prefabricated body installation disc 9 and cooling to room temperature to finish the process;
sixthly, the lifting speed of the prefabricated body mounting disc 9 is 10 mm/s;
example 2 microscopic structure observation results:
example 2 a metal matrix composite of 200 μm diamond particles with 40 Cu-Zr alloys was obtained under the same 10MPa infiltration pressure conditions. Experiments show that under the infiltration pressure of 10MPa, when the Zr content is 8 to 12 percent, the Cu-Zr alloy can fully infiltrate the diamond preform, and when the Zr content is 8 to 12 percent<8% or>At 12%, the Cu — Zr alloy cannot sufficiently infiltrate into the diamond preform; when the Zr content is less than or equal to 1 percent, the diamond particles do not generate interface reaction with the Cu-Zr alloy, and when the Zr content is between 1 and 18.5 percent, Cu can be separated out from the interface of the diamond and the Cu-Zr alloy9Zr2And when the Zr content is 18.5-20%, Cu can be precipitated on the interface of diamond and Cu-Zr alloy9Zr2And Cu51Zr14。
If the traditional one-time and sequential iteration mode is adopted for research, 40 times of tests are needed, and by adopting the scheme, the interface wetting and interface reaction behaviors of the diamond reinforced Cu-Zr composite material can be efficiently researched only by one test.
Example 3:
the metal matrix composite high-throughput preparation device of the embodiment comprises a lifting rod 1, an exhaust tube 2, a furnace body 3, a preheating zone 4, a smelting zone 5, a grid type crucible 6, an inflation tube 7, a preform mounting disc 9, 40 preforms 10, a heat insulation plate 11 and a crucible heating zone 13;
the furnace body 3 is a sealed cavity body, a horizontal annular heat insulation plate 11 is arranged in the middle of the inside of the furnace body 3, the annular heat insulation plate 11 is fixedly connected with the inner wall of the furnace body 3, the upper part of the annular heat insulation plate 11 in the furnace body 3 is a preheating zone 4, the lower part of the annular heat insulation plate 11 in the furnace body 3 is a smelting zone 5, the bottom of the smelting zone 5 is a crucible heating zone 13, and electric heating elements are respectively arranged at the position, close to the inner wall of the furnace body 3, in the preheating zone 4, at the position, close to the inner wall of the furnace body 3; the upper part of the furnace body 3 is provided with an exhaust tube 2 and an inflation tube 7 which are communicated with the inside of the furnace body 3; one end of the lifting rod 1 is arranged in the furnace body 3, the lower end of the lifting rod is fixedly connected with a horizontally arranged prefabricated body mounting disc 9, and the other end of the lifting rod 1 extends out of the furnace body 3 from a through hole at the top of the furnace body 3; 500 same prefabricated bodies 10 are hung on the lower surface of the prefabricated body mounting plate 9, the arrangement forms of the prefabricated bodies 10 are concentric rings, the prefabricated body mounting plate 9 and the prefabricated bodies 10 are arranged in the preheating zone 4, the grid type crucible 6 is arranged in the smelting zone 5 between the prefabricated bodies 10 and the crucible heating zone 13, the grid type crucible 6 is cylindrical, and a crucible chamber 61 corresponding to the arrangement position of each prefabricated body 10 is arranged in the grid type crucible 6.
The electric heating element is a silicon-molybdenum rod;
the prefabricated part 10 consists of a mould and a reinforcement filled in the mould, and the reinforcement is formed by bonding reinforcement particles with an adhesive;
the adhesive is polyvinyl alcohol;
the die is a hollow cylinder, the bottom of the die is sealed, and the side wall of the die is provided with a plurality of through holes; wherein, the through hole of the side wall of the mould is used as a channel for the substrate to enter the mould;
the aperture of the through hole on the side wall of the die is 1.5 mm;
the material of the mould is high-purity graphite;
the high-flux preparation method of the metal matrix composite material by using the high-flux preparation device of the metal matrix composite material comprises the following steps:
first, prepare
Respectively hoisting prefabricated bodies 10 on the lower surface of a prefabricated body mounting plate 9 in a concentric ring manner, arranging the prefabricated bodies 10 in a concentric ring manner, placing a grid type crucible 6 in a smelting zone 5 between the prefabricated bodies 10 and a crucible heating zone 13, and filling different crucible chambers 61 with base metals with different components;
the prefabricated part 10 consists of a mould and a reinforcement filled in the mould; the adhesive is polyvinyl alcohol; the reinforcement is B with the grain diameter of 50 mu m4C, particles; the mass ratio of the reinforcing body particles to the adhesive is 1: 0.05;
the die is a hollow cylinder, the bottom of the die is sealed, and the side wall of the die is provided with a plurality of through holes; the aperture of the through hole is 1.5 mm; the through hole on the side wall of the mold is used as a passage for the matrix to enter the mold;
the material of the mould is high-purity graphite;
the grid type crucible 6 is made of high-purity graphite;
the components of the matrix metal filled in each crucible chamber are different;
the number of the base metal species is 500; the matrix metal is Ti-Nb alloy; wherein the Nb element accounts for 0.05-25 percent of the mass fraction, and the component intervals are all 0.05 percent;
the melting points of the matrixes with different components filled in the different crucible chambers 61 are 1800 ℃ at most, 1670 ℃ at least and 130 ℃ in difference;
the matrix metal is a mixture of pure Ti powder and pure Nb powder; the grain size of the pure Ti powder is 250 mu m, and the grain size of the pure Nb powder is 250 mu m;
second, removing the adhesive of the prefabricated body
Sealing the gas filling pipe 7, connecting the exhaust pipe 2 with a vacuumizing device to vacuumize the furnace body 3, and simultaneously heating the prefabricated body 10 by using an electric heating element in the preheating zone 4 to remove the adhesive in the prefabricated body 10;
the exhaust pipe 2 is connected with a vacuumizing device to vacuumize the furnace body 3 until the vacuum degree is 500 Pa;
third, atmosphere protection
The extraction tube 2 is closed, inert gas is filled into the furnace body 3 through the inflation tube 7 for protection, and meanwhile, the smelting zone 5 and the crucible heating zone 13 are heated, so that the base metals with different components filled in different crucible chambers 61 are heated to be 200 ℃ above the melting point of the base metal with the highest melting point (namely 2000 ℃) and are kept warm for 1.5 hours, and liquid base metals are obtained; heating the preheating zone 4 to heat the preform 10 to 40 ℃ (1630 ℃) below the melting point of the lowest melting point base metal and keeping the temperature for 1.5 h; the inert gas is nitrogen;
fourthly, vacuum degassing
Sealing the gas filling pipe 7, connecting the gas pumping pipe 2 with a vacuumizing device to vacuumize the furnace body 3 so as to remove the matrix metal in the crucible chamber 61 and the inclusion gas in the preform 10, stopping heating the smelting zone 5, the crucible heating zone 13 and the preheating zone 4, and lowering the lifting rod 1 so that the preform mounting plate 9 and the preform 10 pass through the heat insulation plate 11 until the preform 10 is completely immersed below the liquid matrix metal in the crucible chamber 61;
the descending speed of the lifting rod 1 is 0.01 mm/s;
and the exhaust pipe 2 is connected with a vacuumizing device to vacuumize the furnace body 3 until the vacuum degree is 500 Pa.
Fifth, air pressure infiltration
Injecting high-pressure inert gas into the furnace body 3 through the gas filling pipe 7 and maintaining the pressure to obtain a metal matrix composite material;
the inert gas is nitrogen;
the pressure of the inert gas is 5 MPa;
the pressure maintaining time is 30 min;
sixthly, forming
Lifting the prefabricated body installation disc 9 to the prefabricated body 10 through the lifting rod 1, completely separating the prefabricated body 10 from the liquid base metal in the crucible chamber 61, alternately opening the exhaust tube 2 and the gas filling tube 7 to replace hot gas until the temperature of the metal-based composite material is reduced to 130 ℃, and finally unloading the metal-based composite material from the prefabricated body installation disc 9 and cooling to room temperature to finish the process;
sixthly, the lifting speed of the prefabricated body mounting disc 9 is 4 mm/s;
example 3 microscopic structure observation results:
example 3B of 50 μm was obtained under the same 5MPa infiltration pressure4C particles and 500 Ti-Nb alloys. Experiments show that under the impregnation pressure of 5MPa, when the Nb content is less than or equal to 11.5 percent, the Ti-Nb alloy can fully impregnate B4C preform, when Nb content>At 11.5%, the Ti-Nb alloy cannot be sufficiently impregnated into B4C, prefabricating a body; when the Nb content is less than or equal to 8 percent, B4The C particles and Ti-Nb alloy generate TiB through interface reaction2And TiC, when Nb is contained>At 8%, B4The C particles and Ti-Nb alloy are subjected to interface reaction to generate NbB2And TiC.
If the traditional one-time same and sequential iteration mode is adopted for research, 500 times of tests are needed, and by adopting the scheme, the B can be efficiently researched by only one test4C granuleThe interfacial wetting and interfacial reaction behavior of the grain reinforced Ti-Nb composite material.
Example 4:
the high-throughput preparation device for the metal matrix composite material comprises a lifting rod 1, an exhaust tube 2, a furnace body 3, a preheating zone 4, a smelting zone 5, a crucible 6, an inflation tube 7, a preform mounting plate 9, a 552 preform 10, a heat insulation plate 11 and a crucible heating zone 13;
the furnace body 3 is a sealed cavity body, a horizontal annular heat insulation plate 11 is arranged in the middle of the inside of the furnace body 3, the annular heat insulation plate 11 is fixedly connected with the inner wall of the furnace body 3, the upper part of the annular heat insulation plate 11 in the furnace body 3 is a preheating zone 4, the lower part of the annular heat insulation plate 11 in the furnace body 3 is a smelting zone 5, the bottom of the smelting zone 5 is a crucible heating zone 13, and electric heating elements are respectively arranged at the position, close to the inner wall of the furnace body 3, in the preheating zone 4, at the position, close to the inner wall of the furnace body 3; the upper part of the furnace body 3 is provided with an exhaust tube 2 and an inflation tube 7 which are communicated with the inside of the furnace body 3; one end of the lifting rod 1 is arranged in the furnace body 3, the lower end of the lifting rod is fixedly connected with a horizontally arranged prefabricated body mounting disc 9, and the other end of the lifting rod 1 extends out of the furnace body 3 from a through hole at the top of the furnace body 3; 552 prefabricated bodies 10 are hung on the lower surface of the prefabricated body mounting disc 9, the arrangement form of the prefabricated bodies 10 is concentric and annular, the prefabricated body mounting disc 9 and the prefabricated bodies 10 are arranged in the preheating zone 4, the crucible 6 is arranged in the smelting zone 5 between the prefabricated bodies 10 and the crucible heating zone 13, and the crucible 6 is cylindrical; the electric heating element is a silicon-molybdenum rod;
the method for preparing the metal matrix composite material with high flux by using the metal matrix composite material high flux preparation device comprises the following steps:
first, prepare
Hoisting a preform 10 on the lower surface of a preform mounting plate 9 in a concentric ring shape, placing a crucible 6 in a smelting zone 5 between the preform 10 and a crucible heating zone 13, and filling matrix metal in the crucible 6;
step one, the prefabricated part 10 is composed of a mold and a composite reinforcement filled in the mold, the composite reinforcement is formed by bonding the reinforcement and an adhesive, and the composite reinforcement in the mold of the prefabricated part 10 is different;
the adhesive is polyvinyl alcohol;
the mass ratio of the reinforcement to the adhesive is 1: 0.1;
the reinforcement body is a particle reinforcement body, a SiC nanowire reinforcement body, a carbon nanotube reinforcement body and a carbon fiber reinforcement body. The material of the particle reinforcement is SiC and B respectively4C、Al2O3、TiB2AlN and TiAl3;
The average particle diameter of the SiC particle reinforcement is 50 nm-250 mu m; wherein when the average diameter is 50 nm-1 μm, the diameter interval is 50 nm; when the average diameter is 1-20 μm, the diameter interval is 0.5 μm; when the average diameter is 20-250 μm, the diameter interval is 5 μm;
b is4The average diameter of the particle diameter of the C particle reinforcement body is 1-200 mu m; when the average diameter is 1-20 μm, the diameter interval is 1 μm; when the average diameter is 20-200 μm, the diameter interval is 5 μm;
the Al is2O3The average diameter of the particle reinforcement is 50 nm-250 mu m; wherein when the average diameter is 50 nm-1 μm, the diameter interval is 50 nm; when the average diameter is 1-20 μm, the diameter interval is 0.5 μm; when the average diameter is 20-250 μm, the diameter interval is 5 μm;
the TiB2The average diameter of the particle reinforcement is 1-200 mu m; when the average diameter is 1-20 μm, the diameter interval is 1 μm; when the average diameter is 20-200 μm, the diameter interval is 5 μm;
the average particle diameter of the AlN particle reinforcement body is 50 nm-250 mu m; wherein when the average diameter is 50 nm-1 μm, the diameter interval is 50 nm; when the average diameter is 1-20 μm, the diameter interval is 0.5 μm; when the average diameter is 20-250 μm, the diameter interval is 5 μm;
the TiAl3The average diameter of the particle reinforcement is 1-200 mu m; when the average diameter is 1-20 μm, the diameter interval is 1 μm; when the average diameter is 20-200 μm, the diameter interval is 5 μm;
the SiC nanowire reinforcement has an average diameter of 5-250 nm and an average length of 5-100 mu m; wherein when the average diameter is 5 nm-50 nm, the diameter interval is 5 nm; when the average diameter is 50 nm-250 nm, the diameter interval is 10 nm;
the carbon nano tube reinforcement has the average diameter of 1nm, 5nm, 10nm, 15nm, 20nm, 25nm, 30nm, 35nm, 40nm, 45nm and 50nm, and the average length of 1-50 mu m;
the carbon fiber reinforcement has an average diameter of 7 μm;
the die is a hollow cylinder, the bottom of the die is sealed, and the side wall of the die is provided with a plurality of through holes; the aperture of the through hole is 0.5 mm;
the mould is made of ceramics;
step one, the number of the prefabricated bodies 10 is 552;
step one, the base metal is a pure Al alloy (1199 alloy); step one, the prefabricated body installation disc 9 is made of heat-resistant steel;
step one, the crucible 6 is a cylindrical crucible;
firstly, the crucible 6 is made of graphite;
second, removing the adhesive of the prefabricated body
Sealing the gas filling pipe 7, connecting the exhaust pipe 2 with a vacuumizing device to vacuumize the furnace body 3, and simultaneously heating the prefabricated body 10 by using an electric heating element in the preheating zone 4 to remove the adhesive in the prefabricated body 10;
secondly, connecting the exhaust pipe 2 with a vacuumizing device to vacuumize the furnace body 3 until the vacuum degree is 1000 Pa;
third, atmosphere protection
The extraction tube 2 is closed, inert gas is filled into the furnace body 3 through the inflation tube 7 for protection, and simultaneously the melting zone 5 and the crucible heating zone 13 are heated to heat the base metal in the crucible 6 to 300 ℃ above the melting point of the base metal and the temperature is kept for 1 h; the preheating zone 4 is heated to 40 ℃ below the melting point of the matrix metal and the temperature is kept for 1 h; the inert gas is nitrogen;
fourthly, vacuum degassing
Sealing the gas filling pipe 7, connecting the gas pumping pipe 2 with a vacuumizing device to vacuumize the furnace body 3 so as to remove the matrix metal in the crucible 6 and the inclusion gas in the preform 10, stopping heating the smelting zone 5, the crucible heating zone 13 and the preheating zone 4, and lowering the lifting rod 1 to enable the preform mounting disc 9 and the preform 10 to pass through the heat insulation plate 11 until the preform 10 is completely immersed below the liquid level of the liquid matrix metal in the crucible 6;
fourthly, the descending speed of the lifting rod 1 is 0.01 mm/s;
fourthly, connecting the exhaust pipe 2 with a vacuumizing device to vacuumize the furnace body 3 until the vacuum degree is 1000 Pa;
fifth, air pressure infiltration
Injecting high-pressure inert gas into the furnace body 3 through the gas-filled pipe 7, carrying out air pressure infiltration and maintaining pressure; impregnating the prefabricated part 10 by a liquid matrix after injecting inert gas into the furnace body 3 to obtain a metal matrix composite material;
fifthly, the inert gas is nitrogen;
fifthly, the pressure of the inert gas is 5 MPa;
fifthly, the pressure maintaining time is 1 min;
sixthly, forming
Lifting the prefabricated body mounting disc 9 to the prefabricated body 10 through the lifting rod 1, enabling the prefabricated body 10 to be completely separated from the liquid base metal in the crucible 6, alternately opening the exhaust tube 2 and the gas filling tube 7 to replace hot gas until the temperature of the metal-based composite material is reduced to 100 ℃, and finally unloading the metal-based composite material from the prefabricated body mounting disc 9 and cooling to room temperature to finish the process;
and sixthly, the lifting speed of the prefabricated body mounting disc 9 is 10 mm/s.
1. In the embodiment, the parallel-type prefabricated part mold is designed and innovated, the metal-based composite material of different reinforcements can be prepared at one time in a high flux in the same furnace, and samples of different reinforcements and liquid metal infiltrated at a set temperature can be obtained at a high flux, so that the interface wetting and interface reaction behaviors of the composite material can be efficiently researched, and the aims of halving the cost, halving the period and quickly responding in the process of developing the metal-based composite material are supported; 2. in the embodiment, the metal-based composite material of different reinforcements is prepared by adopting air pressure infiltration, so that the pressure of each prefabricated part is equal in the infiltration process, and the infiltration results of the liquid metal to the different reinforcements are strong in mutual contrast; 3. in the embodiment, the lifting infiltration is adopted, so that the infiltration time can be accurately controlled; meanwhile, the prefabricated body is separated from the liquid metal after being impregnated with the liquid metal, so that the prefabricated body is prevented from being embedded in a solidified metal matrix, the sampling time can be shortened, and a sample can be quickly obtained; the crucible does not need to be damaged in the sampling process, the damage to the crucible is avoided, and the cost is saved.
Example 4 metal matrix composites of pure aluminum matrix and 552 reinforcements of different shapes, types and sizes can be obtained under the same infiltration pressure condition of 5 MPa. Experiments show that under the impregnation pressure of 5MPa, when the average diameter of SiC particles is more than or equal to 35 mu m, the SiC particle preform can be fully impregnated by the pure aluminum alloy; when the average diameter of the SiC particles>When the grain size is 250nm and less than 35 mu m, the pure aluminum alloy can be partially impregnated with the SiC grain prefabricated body; when the average diameter of the SiC particles is less than or equal to 250nm, the pure aluminum alloy can not infiltrate the SiC particle preform; when B is present4When the average diameter of the C particles is more than or equal to 45 mu m, the pure aluminum alloy can fully infiltrate the B4C, preparing a particle prefabricated body; when Al is present2O3When the average diameter of the particles is more than or equal to 10 mu m, the pure aluminum alloy can fully infiltrate Al2O3A particle preform; when TiB2When the average diameter of the particles is more than or equal to 50 mu m, the pure aluminum alloy can fully infiltrate the TiB2A particle preform; when the average diameter of the AlN particles is more than or equal to 15 mu m, the pure aluminum alloy can fully infiltrate the AlN particle prefabricated body; when TiAl3When the average diameter of the particles is more than or equal to 25 mu m, the pure aluminum alloy can fully infiltrate TiAl3A particle preform; the infiltration of the particle reinforcement with the pure Al matrix is therefore ordered to Al2O3>AlN>TiAl3>SiC>B4C>TiB2;
When the average diameter of the SiC nanowire is larger than 130nm, the SiC nanowire preform can be fully impregnated by the pure aluminum alloy; when the average diameter of the carbon nano tube is more than 40nm, the pure aluminum alloy can fully infiltrate the carbon nano tube prefabricated body; the 7 mu m carbon fiber reinforcement body can be fully impregnated by pure aluminum alloy;
meanwhile, when the average diameter of the SiC particles is less than or equal to 350nm or the average diameter of the SiC nanowires<At 80nm, SiC and pureThe interface reaction of Al is stronger, and Al is generated4C3(ii) a Diameter of carbon nanotube<At 25nm, the interface reaction between the carbon nanotube and pure Al is stronger, and Al is generated4C3;
If the traditional one-time and sequential iteration mode is adopted for research, 552 tests are needed, and by adopting the scheme, the interface wetting and interface reaction behaviors of different types of reinforcement-enhanced pure Al composite materials can be efficiently researched only by one test.