CN110983209A - Preparation method of high-strength porous three-dimensional ceramic matrix metal composite material - Google Patents
Preparation method of high-strength porous three-dimensional ceramic matrix metal composite material Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C47/00—Making alloys containing metallic or non-metallic fibres or filaments
- C22C47/02—Pretreatment of the fibres or filaments
- C22C47/06—Pretreatment of the fibres or filaments by forming the fibres or filaments into a preformed structure, e.g. using a temporary binder to form a mat-like element
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D18/00—Pressure casting; Vacuum casting
- B22D18/02—Pressure casting making use of mechanical pressure devices, e.g. cast-forging
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D19/00—Casting in, on, or around objects which form part of the product
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C47/00—Making alloys containing metallic or non-metallic fibres or filaments
- C22C47/08—Making alloys containing metallic or non-metallic fibres or filaments by contacting the fibres or filaments with molten metal, e.g. by infiltrating the fibres or filaments placed in a mould
- C22C47/12—Infiltration or casting under mechanical pressure
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C49/00—Alloys containing metallic or non-metallic fibres or filaments
- C22C49/02—Alloys containing metallic or non-metallic fibres or filaments characterised by the matrix material
- C22C49/04—Light metals
- C22C49/06—Aluminium
Abstract
The invention provides a preparation method of a high-strength porous three-dimensional ceramic matrix metal composite, which relates to the technical field of composite materials and comprises the following steps: after carbon fibers are pretreated, the carbon fibers are made into a prefabricated part with a three-dimensional structure by using 3D printing equipment; depositing SiC on the surface of the prefabricated part, washing the prefabricated part with water to be neutral, and drying the prefabricated part to obtain a blank; fixing the blank in a casting mold by using a metal support, preheating to the temperature of 550-.
Description
Technical Field
The invention relates to the technical field of composite materials, in particular to a preparation method of a high-strength porous three-dimensional ceramic matrix metal composite material.
Background
The ceramic matrix composite is a composite material compounded with various metal materials by taking ceramic as a matrix. The ceramic matrix can be high temperature structural ceramic such as silicon nitride, silicon carbide, etc. These advanced ceramics have excellent properties of high temperature resistance, high strength and rigidity, relatively light weight, corrosion resistance and the like, and have the fatal weakness of brittleness, and when in a stress state, the advanced ceramics can generate cracks and even break to cause material failure. The adoption of high-strength and high-elasticity fiber and matrix composite is an effective method for improving the toughness and reliability of the ceramic. The fiber can prevent the crack from expanding, thereby obtaining the fiber reinforced ceramic matrix composite material with excellent toughness. The ceramic matrix composite material has been used as a liquid rocket engine nozzle, a missile radome, a nose cone of a space shuttle, a brake disc of an airplane, a brake disc of a high-grade automobile and the like, and becomes an important branch of a high-technology new material.
The three-dimensional ceramic-based metal composite material in the ceramic-based composite material is a structural form of a ceramic/metal composite material developed in the 80 s of the 20 th century, namely, a ceramic reinforcement is continuous in a three-dimensional space, a metal matrix is continuous in the three-dimensional space, and the reinforcement and the matrix form a network structure in the space. Because the network ceramic framework is three-dimensionally continuous with the metal, each phase can exert unique performance. Therefore, the three-dimensional continuous network ceramic reinforced metal matrix composite material has high strength, high hardness, good abrasion resistance and thermal shock resistance, higher thermal conductivity and lower thermal expansion coefficient, and shows wide application prospects in the industrial fields of aerospace, automobiles, electronics, mechanical manufacturing and the like.
Chinese patent CN 108315629A discloses a preparation method of an Al/SiC metal ceramic composite material, belonging to the technical field of metal ceramic composite material preparation. The method comprises the following specific steps: weighing aluminum powder and silicon carbide powder respectively, placing the aluminum powder and the silicon carbide powder in a grinding body, carrying out ball milling on the mixed material by adopting a planetary ball mill, drying the ball-milled material in a vacuum drying box, and grinding the dried material to enable all powder to pass through a 100-mesh sieve for later use; and placing the ground material into a graphite die for spark plasma sintering to be sintered. The invention utilizes the discharge plasma sintering technology to prepare the Al/SiC metal ceramic composite material at high temperature and high pressure, and breaks through the traditional preparation method of the Al/SiC metal ceramic composite material; compared with aluminum-based metal, the prepared Al/SiC metal ceramic composite material system has higher use temperature, and aluminum/silicon carbide has better wear resistance, fracture toughness and corrosion resistance, thereby widening the application range of the aluminum/silicon carbide.
Chinese patent CN 106756388A discloses a preparation process of a toughened Ti (C, N) -based metal ceramic composite material, which comprises the following steps: firstly, weighing carbon nano tubes in proportion, putting the carbon nano tubes into a glow discharge plasma furnace for discharge treatment to obtain modified carbon nano tubes; putting the modified carbon nano tube into a polar solvent, and putting 1-5 per mill of sorbitan tristearate into the polar solvent to be used as a surface dispersant; preparing a fully dispersed solvent containing carbon nano tubes and metal ceramic composite powder to form a mixture, putting the mixture into a planetary ball mill for ball milling to form a ball-milled mixture, wherein the ball-to-material ratio is 5: 1-8: 1; the prepared mixture after ball milling is dried, mixed with a forming agent and pressed into a blank, and the blank is sintered in a vacuum sintering furnace. The hardness of the toughened Ti (C, N) -based metal ceramic composite material obtained by the preparation process is increased by 0.1-0.3HRA, the bending strength (sigma b) is increased by 10-20%, and the fracture toughness (KIC) is increased by 15-25%.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides a preparation method of a high-strength porous three-dimensional ceramic matrix metal composite material.
(II) technical scheme
In order to achieve the purpose, the invention is realized by the following technical scheme:
a preparation method of a high-strength porous three-dimensional ceramic matrix metal composite material comprises the following steps:
(1) putting carbon fibers into an acetone solution, carrying out ultrasonic cleaning for 30-50min, filtering, transferring the carbon fibers into a muffle furnace, heating to 450-plus-500 ℃ for high-temperature treatment for 3-6h, cooling to room temperature along with the furnace, adding the carbon fibers into a mixed acid solution, carrying out immersion treatment for 10-15min, filtering, washing with water to be neutral, carrying out immersion treatment for 1-3h by using an ammonium persulfate solution, filtering again, carrying out elution by using deionized water for 3 times, drying at 70-90 ℃, and preparing the carbon fibers into a prefabricated member with a three-dimensional structure by using 3D printing equipment;
(2) pulverizing mesophase pitch particles, adding into deionized water, stirring, adding polyethylene glycol 6000 distearate, stirring to obtain uniform liquid, soaking the prefabricated member, ultrasonic treating for 5-10min, taking out, transferring into a container, transferring the container into a high-pressure reaction kettle, replacing air in the kettle with nitrogen, continuously introducing nitrogen to ensure that the pressure in the kettle is 5-8MPa, hermetically heating to 480-plus-500 ℃, carrying out heat preservation reaction for 2-5h, transferring into a carbonization furnace, heating to 1000-plus-1020 ℃ under the protection of nitrogen, treating for 2-5h, transferring into a vacuum sintering furnace, adding a proper amount of silicon powder, heating to 1500-plus-1550 ℃ under the protection of nitrogen, carrying out heat preservation reaction for 5-10min, soaking in a mixed solution of hydrofluoric acid and nitric acid for 5-10min, washing with water to neutrality, and drying to obtain a blank;
(3) fixing the blank in a casting mold by using a metal support, preheating to the temperature of 550-600 ℃, then pouring molten high-temperature alloy liquid into the mold, allowing the alloy liquid to permeate into the blank under the action of natural gravity, wherein the pouring temperature of the alloy liquid is 750-770 ℃, the internal pressure of the mold is 20-25MPa, the pressure maintaining time is 30-40s, placing the composite material into a muffle furnace after demolding, heating to the temperature of 400-450 ℃, preserving heat for 2-5h, and cooling to room temperature along with the furnace.
Preferably, the mixed acid solution in the step (1) is a mixed solution of concentrated nitric acid and concentrated sulfuric acid, and the volume ratio of the two is 1-5: 1-5.
Preferably, the mass concentration of the ammonium persulfate solution in the step (1) is 18-25%.
Preferably, the particle size of the mesophase pitch particles after being crushed in the step (2) is less than or equal to 15 mu m.
Preferably, the mass ratio of the mesophase pitch particles, the polyethylene glycol 6000 distearate and the deionized water in the step (2) is 20-30: 5-10: 50-80.
Preferably, the temperature rising speed of the high-pressure reaction kettle in the step (2) is 3-5 ℃/min.
Preferably, the temperature rising speed of the carbonization furnace in the step (2) is 1-2 ℃/min.
Preferably, the temperature rising speed of the vacuum sintering furnace in the step (2) is 10-20 ℃/min.
Preferably, the volume ratio of the hydrofluoric acid to the nitric acid in the mixed solution in the step (2) is 40-50: 1.
Preferably, the alloy liquid in the step (3) comprises the following elements in percentage by weight: 0.1 to 0.18 percent of Si, 0.16 to 0.32 percent of Fe0.1 to 2.5 percent of Cu, 0.02 to 0.08 percent of Mg, 0.38 to 0.5 percent of Cr, 0.3 to 0.86 percent of Mn, 0.12 to 0.24 percent of Zn, 0.16 to 0.33 percent of Ti, 0.05 to 0.13 percent of Ce and the balance of Al.
(III) advantageous effects
The invention provides a preparation method of a high-strength porous three-dimensional ceramic matrix metal composite material, which has the following beneficial effects:
the carbon fiber can increase the number of active functional groups-COOH and-OH on the surface of the carbon fiber and improve the binding force with SiC on the one hand through mixed acid treatment, on the other hand, the colloid on the surface of the carbon fiber can be washed away, the formation of grooves and micropores on the surface of the carbon fiber is promoted, the adhesive force of SiC is promoted, the ammonium persulfate solution is used as a coarsening agent to form a rough microscopic surface on the surface of the carbon fiber and promote the settlement and adhesion of SiC in the sintering process, mesophase pitch is attached to the surface of a carbon fiber prefabricated part with a three-dimensional structure through impregnation, high-temperature reaction is carried out in a high-pressure reaction kettle to obtain carbon foam, the carbon foam and silicon powder react at high temperature in a vacuum sintering furnace to generate SiC which is coated on the surface of the carbon fiber prefabricated part to play a supporting role, the carbon fiber prefabricated part, by utilizing the extrusion casting process, the alloy liquid and SiC can have good compatibility and bonding performance and compact structure, and the ceramic matrix metal composite material has excellent performances and meets the use requirements of modern industry.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
a preparation method of a high-strength porous three-dimensional ceramic matrix metal composite material comprises the following steps:
(1) putting the carbon fibers into an acetone solution, carrying out ultrasonic cleaning for 32min, filtering, transferring to a muffle furnace, heating to 480 ℃, carrying out high-temperature treatment for 5h, cooling to room temperature along with the furnace, and adding the mixture to a reaction kettle with a volume ratio of 1: 5, soaking for 12min in mixed acid solution consisting of concentrated nitric acid and concentrated sulfuric acid, filtering, washing to be neutral, soaking for 2h by using ammonium persulfate solution with the mass concentration of 22%, filtering again, rinsing for 3 times by using deionized water, drying at 75 ℃, and preparing the carbon fibers into prefabricated members with three-dimensional structures by using 3D printing equipment;
(2) crushing the intermediate phase asphalt particles to a particle size of less than or equal to 15 microns, adding the crushed intermediate phase asphalt particles into deionized water, stirring, adding polyethylene glycol 6000 distearate, wherein the mass ratio of the intermediate phase asphalt particles to the polyethylene glycol 6000 distearate to the deionized water is 25: 5: 60, continuously stirring to obtain uniform liquid, immersing the prefabricated part, performing ultrasonic treatment for 7min, taking out and transferring the prefabricated part into a container, transferring the container into a high-pressure reaction kettle, replacing air in the kettle with nitrogen, continuously introducing nitrogen, keeping the pressure in the kettle at 6MPa, sealing and heating to 490 ℃, heating at a speed of 5 ℃/min, performing heat preservation reaction for 2h, transferring into a carbonization furnace, heating to 1005 ℃ under the protection of nitrogen, performing treatment for 2h, heating at a speed of 1.2 ℃/min, transferring into a vacuum sintering furnace, heating at a speed of 10 ℃/min, adding a proper amount of silicon powder, performing heat preservation reaction for 5-10h, immersing into a hydrofluoric acid-nitric acid mixed solution with a volume ratio of 45:1, performing immersion treatment for 8min, washing with water to neutrality, and drying to obtain a blank;
(3) fixing the blank in a casting mould by using a metal bracket, preheating to 570 ℃, and then pouring molten high-temperature alloy liquid into the mould, wherein the alloy liquid comprises the following elements in percentage by weight: 0.13% of Si, 0.22% of Fe, 2.4% of Cu2, 0.06% of Mg, 0.39% of Cr, 0.35% of Mn, 0.18% of Zn, 0.26% of Ti, 0.10% of Ce and the balance of Al, wherein the alloy liquid permeates into the blank under the action of natural gravity, the pouring temperature of the alloy liquid is 755 ℃, the internal pressure of a mold is 24MPa, the pressure maintaining time is 36s, the composite material is placed into a muffle furnace after being demoulded, the temperature is raised to 420 ℃, the temperature is kept for 5h, and the composite material is air-cooled to room temperature along with the furnace.
Example 2:
a preparation method of a high-strength porous three-dimensional ceramic matrix metal composite material comprises the following steps:
(1) putting the carbon fibers into an acetone solution, carrying out ultrasonic cleaning for 50min, filtering, transferring to a muffle furnace, heating to 470 ℃, carrying out high-temperature treatment for 5h, cooling to room temperature along with the furnace, and adding the mixture to a reaction kettle according to a volume ratio of 5: 2, soaking for 15min in a mixed acid solution consisting of concentrated nitric acid and concentrated sulfuric acid, filtering, washing to be neutral, soaking for 1h by using an ammonium persulfate solution with the mass concentration of 20%, filtering again, rinsing for 3 times by using deionized water, drying at 75 ℃, and preparing the carbon fibers into a prefabricated member with a three-dimensional structure by using 3D printing equipment;
(2) crushing the intermediate phase asphalt particles to a particle size of less than or equal to 15 microns, adding the crushed intermediate phase asphalt particles into deionized water, stirring, adding polyethylene glycol 6000 distearate, wherein the mass ratio of the intermediate phase asphalt particles to the polyethylene glycol 6000 distearate to the deionized water is 30: 8: 55, continuously stirring to obtain uniform liquid, immersing the prefabricated part, performing ultrasonic treatment for 10min, taking out and transferring the prefabricated part into a container, transferring the container into a high-pressure reaction kettle, replacing air in the kettle with nitrogen, continuously introducing the nitrogen to ensure that the pressure in the kettle is 8MPa, sealing and heating to 485 ℃, the heating rate is 5 ℃/min, performing heat preservation reaction for 5h, transferring into a carbonization furnace, heating to 1010 ℃ under the protection of the nitrogen, performing treatment for 5h, the heating rate is 1 ℃/min, transferring into a vacuum sintering furnace, the heating rate is 15 ℃/min, adding a proper amount of silicon powder, performing heat preservation reaction for 10h under the protection of the nitrogen, immersing into a hydrofluoric acid-nitric acid mixed solution with the volume ratio of 48:1, performing immersion treatment for 10min, washing with water to neutrality, and drying to obtain a blank;
(3) fixing the blank in a casting mold by using a metal support, preheating to 600 ℃, and then pouring molten high-temperature alloy liquid into the mold, wherein the alloy liquid comprises the following elements in percentage by weight: 0.18% of Si, 0.25% of Fe, 2.1% of Cu2, 0.05% of Mg, 0.46% of Cr, 0.55% of Mn, 0.18% of Zn, 0.26% of Ti, 0.11% of Ce and the balance of Al, wherein the alloy liquid permeates into the blank under the action of natural gravity, the pouring temperature of the alloy liquid is 750 ℃, the internal pressure of a mold is 22MPa, the pressure maintaining time is 30s, the composite material is placed into a muffle furnace after being demoulded, the temperature is raised to 420 ℃, the temperature is kept for 3h, and the composite material is air-cooled to room temperature along with the furnace.
Example 3:
a preparation method of a high-strength porous three-dimensional ceramic matrix metal composite material comprises the following steps:
(1) putting the carbon fibers into an acetone solution, carrying out ultrasonic cleaning for 30min, filtering, transferring to a muffle furnace, heating to 450 ℃, carrying out high-temperature treatment for 3h, cooling to room temperature along with the furnace, and adding the mixture to a reaction kettle with a volume ratio of 1: 1, soaking in a mixed acid solution consisting of concentrated nitric acid and concentrated sulfuric acid for 10min, filtering, washing to be neutral, soaking for 1h by using an ammonium persulfate solution with the mass concentration of 18%, filtering again, rinsing for 3 times by using deionized water, drying at 70 ℃, and preparing the carbon fibers into a prefabricated member with a three-dimensional structure by using 3D printing equipment;
(2) crushing the intermediate phase asphalt particles to the particle size of less than or equal to 15 microns, adding the crushed intermediate phase asphalt particles into deionized water, stirring, adding polyethylene glycol 6000 distearate, wherein the mass ratio of the intermediate phase asphalt particles to the polyethylene glycol 6000 distearate to the deionized water is 20: 5: 50, continuously stirring to obtain uniform liquid, immersing the prefabricated part, performing ultrasonic treatment for 5min, taking out and transferring the prefabricated part into a container, transferring the container into a high-pressure reaction kettle, replacing air in the kettle with nitrogen, continuously introducing nitrogen to ensure that the pressure in the kettle is 5MPa, hermetically heating to 480 ℃, the heating speed is 3 ℃/min, performing heat preservation reaction for 2h, transferring into a carbonization furnace, heating to 1000 ℃ under the protection of nitrogen, performing treatment for 2h, the heating speed is 1 ℃/min, transferring into a vacuum sintering furnace, heating to 10 ℃/min, adding a proper amount of silicon powder, performing heat preservation reaction for 5h under the protection of nitrogen, immersing into a hydrofluoric acid-nitric acid mixed solution with the volume ratio of 40:1, performing immersion treatment for 5min, washing with water to neutrality, and drying to obtain a blank;
(3) fixing the blank in a casting mold by using a metal bracket, preheating to 550 ℃, and then pouring molten high-temperature alloy liquid into the mold, wherein the alloy liquid comprises the following elements in percentage by weight: 0.1% of Si, 0.16% of Fe, 2.1% of Cu2, 0.02% of Mg, 0.38% of Cr, 0.3% of Mn, 0.12% of Zn, 0.16% of Ti, 0.05% of Ce and the balance of Al, wherein the alloy liquid permeates into the blank under the action of natural gravity, the pouring temperature of the alloy liquid is 750 ℃, the internal pressure of a mold is 20MPa, the pressure maintaining time is 30s, the composite material is placed into a muffle furnace after being demoulded, the temperature is raised to 400 ℃, the temperature is kept for 2h, and the composite material is air-cooled to the room temperature along with the furnace.
Example 4:
a preparation method of a high-strength porous three-dimensional ceramic matrix metal composite material comprises the following steps:
(1) putting the carbon fibers into an acetone solution, carrying out ultrasonic cleaning for 50min, filtering, transferring to a muffle furnace, heating to 500 ℃, carrying out high-temperature treatment for 6h, cooling to room temperature along with the furnace, and adding the carbon fibers to a solution with a volume ratio of 5:1, soaking for 15min in a mixed acid solution consisting of concentrated nitric acid and concentrated sulfuric acid, filtering, washing to be neutral, soaking for 3h by using an ammonium persulfate solution with the mass concentration of 25%, filtering again, rinsing for 3 times by using deionized water, drying at 90 ℃, and preparing the carbon fibers into a prefabricated member with a three-dimensional structure by using 3D printing equipment;
(2) crushing the intermediate phase asphalt particles to a particle size of less than or equal to 15 microns, adding the crushed intermediate phase asphalt particles into deionized water, stirring, adding polyethylene glycol 6000 distearate, wherein the mass ratio of the intermediate phase asphalt particles to the polyethylene glycol 6000 distearate to the deionized water is 30: 10: 80, continuously stirring to obtain uniform liquid, immersing the prefabricated part, performing ultrasonic treatment for 10min, taking out and transferring the prefabricated part into a container, transferring the container into a high-pressure reaction kettle, replacing air in the kettle with nitrogen, continuously introducing the nitrogen to ensure that the pressure in the kettle is 8MPa, hermetically heating to 500 ℃, the heating speed is 5 ℃/min, performing heat preservation reaction for 5h, transferring into a carbonization furnace, heating to 1020 ℃ under the protection of the nitrogen, performing treatment for 5h, the heating speed is 2 ℃/min, transferring into a vacuum sintering furnace, heating to 20 ℃/min, adding a proper amount of silicon powder, performing heat preservation reaction for 10h under the protection of the nitrogen, immersing into a hydrofluoric acid-nitric acid mixed solution with the volume ratio of 50:1, performing immersion treatment for 10min, washing with water to neutrality, and drying to obtain a blank;
(3) fixing the blank in a casting mold by using a metal support, preheating to 600 ℃, and then pouring molten high-temperature alloy liquid into the mold, wherein the alloy liquid comprises the following elements in percentage by weight: 0.18% of Si, 0.32% of Fe, 2.5% of Cu2, 0.08% of Mg, 0.5% of Cr, 0.86% of Mn, 0.24% of Zn, 0.33% of Ti, 0.13% of Ce and the balance of Al, wherein the alloy liquid permeates into the blank under the action of natural gravity, the pouring temperature of the alloy liquid is 770 ℃, the internal pressure of a mold is 25MPa, the pressure maintaining time is 40s, the composite material is placed into a muffle furnace after being demoulded, the temperature is raised to 450 ℃, the temperature is kept for 5h, and the composite material is air-cooled to room temperature along with the furnace.
Example 5:
a preparation method of a high-strength porous three-dimensional ceramic matrix metal composite material comprises the following steps:
(1) putting the carbon fiber into an acetone solution, carrying out ultrasonic cleaning for 40min, filtering, transferring to a muffle furnace, heating to 470 ℃, carrying out high-temperature treatment for 4h, cooling to room temperature along with the furnace, and adding the carbon fiber into the muffle furnace according to a volume ratio of 2: 3, dipping for 12min in a mixed acid solution consisting of concentrated nitric acid and concentrated sulfuric acid, filtering, washing to be neutral, dipping for 2.5h by using an ammonium persulfate solution with the mass concentration of 20%, filtering again, rinsing for 3 times by using deionized water, drying at 80 ℃, and preparing the carbon fibers into a prefabricated member with a three-dimensional structure by using 3D printing equipment;
(2) crushing the intermediate phase asphalt particles to the particle size of less than or equal to 15 microns, adding the crushed intermediate phase asphalt particles into deionized water, stirring, adding polyethylene glycol 6000 distearate, wherein the mass ratio of the intermediate phase asphalt particles to the polyethylene glycol 6000 distearate to the deionized water is 28: 5: 70, continuously stirring to obtain uniform liquid, immersing the prefabricated part, performing ultrasonic treatment for 10min, taking out and transferring the prefabricated part into a container, transferring the container into a high-pressure reaction kettle, replacing air in the kettle with nitrogen, continuously introducing the nitrogen to ensure that the pressure in the kettle is 5MPa, hermetically heating to 500 ℃, the heating speed is 4 ℃/min, performing heat preservation reaction for 4h, transferring into a carbonization furnace, heating to 1020 ℃ under the protection of the nitrogen, performing treatment for 5h, the heating speed is 2 ℃/min, transferring into a vacuum sintering furnace, heating to 20 ℃/min, adding a proper amount of silicon powder, performing heat preservation reaction for 6h under the protection of the nitrogen, immersing into a hydrofluoric acid-nitric acid mixed solution with the volume ratio of 50:1, performing immersion treatment for 8min, washing to neutrality, and drying to obtain a blank;
(3) fixing the blank in a casting mould by using a metal bracket, preheating to 570 ℃, and then pouring molten high-temperature alloy liquid into the mould, wherein the alloy liquid comprises the following elements in percentage by weight: 0.6% of Si, 0.22% of Fe, 2.3% of Cu2, 0.02% of Mg, 0.5% of Cr, 0.3% of Mn, 0.24% of Zn, 0.16% of Ti, 0.08% of Ce and the balance of Al, wherein the alloy liquid permeates into the blank under the action of natural gravity, the pouring temperature of the alloy liquid is 760 ℃, the internal pressure of a mold is 22MPa, the pressure maintaining time is 40s, the composite material is placed into a muffle furnace after being demoulded, the temperature is raised to 440 ℃, the temperature is kept for 4h, and the composite material is air-cooled to room temperature along with the furnace.
Example 6:
a preparation method of a high-strength porous three-dimensional ceramic matrix metal composite material comprises the following steps:
(1) putting the carbon fibers into an acetone solution, carrying out ultrasonic cleaning for 50min, filtering, transferring to a muffle furnace, heating to 480 ℃, carrying out high-temperature treatment for 5h, cooling to room temperature along with the furnace, and adding the carbon fibers to a reaction kettle according to a volume ratio of 5: 3, dipping for 12min in a mixed acid solution consisting of concentrated nitric acid and concentrated sulfuric acid, filtering, washing to be neutral, dipping for 2h by using an ammonium persulfate solution with the mass concentration of 25%, filtering again, rinsing for 3 times by using deionized water, drying at 75 ℃, and preparing the carbon fibers into a prefabricated member with a three-dimensional structure by using 3D printing equipment;
(2) crushing the intermediate phase asphalt particles to a particle size of less than or equal to 15 microns, adding the crushed intermediate phase asphalt particles into deionized water, stirring, adding polyethylene glycol 6000 distearate, wherein the mass ratio of the intermediate phase asphalt particles to the polyethylene glycol 6000 distearate to the deionized water is 30: 8: 60, continuously stirring to obtain uniform liquid, immersing the prefabricated part, performing ultrasonic treatment for 10min, taking out and transferring the prefabricated part into a container, transferring the container into a high-pressure reaction kettle, replacing air in the kettle with nitrogen, continuously introducing the nitrogen to ensure that the pressure in the kettle is 7MPa, hermetically heating to 500 ℃, the heating speed is 4 ℃/min, performing heat preservation reaction for 3h, transferring into a carbonization furnace, heating to 1020 ℃ under the protection of the nitrogen, performing treatment for 4h, the heating speed is 1 ℃/min, transferring into a vacuum sintering furnace, heating to 10 ℃/min, adding a proper amount of silicon powder, performing heat preservation reaction for 8h under the protection of the nitrogen, immersing into a hydrofluoric acid-nitric acid mixed solution with the volume ratio of 48:1, performing immersion treatment for 10min, washing with water to neutrality, and drying to obtain a blank;
(3) fixing the blank in a casting mould by using a metal bracket, preheating to 570 ℃, and then pouring molten high-temperature alloy liquid into the mould, wherein the alloy liquid comprises the following elements in percentage by weight: 0.12% of Si, 0.18% of Fe, 2.3% of Cu2, 0.06% of Mg, 0.45% of Cr, 0.36% of Mn, 0.14% of Zn, 0.20% of Ti, 0.07% of Ce and the balance of Al, wherein the alloy liquid permeates into the blank under the action of natural gravity, the pouring temperature of the alloy liquid is 755 ℃, the internal pressure of a mold is 22MPa, the pressure maintaining time is 40s, the composite material is placed into a muffle furnace after being demoulded, the temperature is raised to 420 ℃, the temperature is kept for 3h, and the composite material is air-cooled to room temperature along with the furnace.
Example 7:
a preparation method of a high-strength porous three-dimensional ceramic matrix metal composite material comprises the following steps:
(1) putting the carbon fiber into an acetone solution, carrying out ultrasonic cleaning for 30min, filtering, transferring to a muffle furnace, heating to 500 ℃, carrying out high-temperature treatment for 3h, cooling to room temperature along with the furnace, and adding the carbon fiber to the muffle furnace according to a volume ratio of 2: 3, soaking for 15min in a mixed acid solution consisting of concentrated nitric acid and concentrated sulfuric acid, filtering, washing to be neutral, soaking for 3h by using an ammonium persulfate solution with the mass concentration of 18%, filtering again, rinsing for 3 times by using deionized water, drying at 70 ℃, and preparing the carbon fibers into a prefabricated member with a three-dimensional structure by using 3D printing equipment;
(2) crushing the intermediate phase asphalt particles to a particle size of less than or equal to 15 microns, adding the crushed intermediate phase asphalt particles into deionized water, stirring, adding polyethylene glycol 6000 distearate, wherein the mass ratio of the intermediate phase asphalt particles to the polyethylene glycol 6000 distearate to the deionized water is 30: 5: 80, continuously stirring to obtain uniform liquid, immersing the prefabricated part, performing ultrasonic treatment for 5min, taking out and transferring the prefabricated part into a container, transferring the container into a high-pressure reaction kettle, replacing air in the kettle with nitrogen, continuously introducing the nitrogen to ensure that the pressure in the kettle is 8MPa, hermetically heating to 480 ℃, the heating speed is 5 ℃/min, performing heat preservation reaction for 2h, transferring into a carbonization furnace, heating to 1020 ℃ under the protection of the nitrogen, performing treatment for 2h, heating at the speed of 2 ℃/min, transferring into a vacuum sintering furnace, heating at the speed of 10 ℃/min, adding a proper amount of silicon powder, performing heat preservation reaction for 5h under the protection of the nitrogen, immersing into a hydrofluoric acid-nitric acid mixed solution with the volume ratio of 50:1, performing soaking treatment for 5min, washing with water to neutrality, and drying to obtain a blank;
(3) fixing the blank in a casting mold by using a metal support, preheating to 600 ℃, and then pouring molten high-temperature alloy liquid into the mold, wherein the alloy liquid comprises the following elements in percentage by weight: 0.1% of Si, 0.32% of Fe, 2.1% of Cu2, 0.08% of Mg, 0.38% of Cr, 0.86% of Mn, 0.12% of Zn, 0.33% of Ti, 0.05% of Ce and the balance of Al, wherein the alloy liquid permeates into the blank under the action of natural gravity, the pouring temperature of the alloy liquid is 770 ℃, the internal pressure of a mold is 20MPa, the pressure maintaining time is 40s, the composite material is placed into a muffle furnace after being demoulded, the temperature is raised to 400 ℃, the temperature is kept for 5h, and the composite material is air-cooled to the room temperature along with the furnace.
Example 8:
a preparation method of a high-strength porous three-dimensional ceramic matrix metal composite material comprises the following steps:
(1) putting the carbon fiber into an acetone solution, carrying out ultrasonic cleaning for 50min, filtering, transferring to a muffle furnace, heating to 450 ℃, carrying out high-temperature treatment for 6h, cooling to room temperature along with the furnace, and adding the carbon fiber to a solution with a volume ratio of 2: 5, soaking in a mixed acid solution consisting of concentrated nitric acid and concentrated sulfuric acid for 10min, filtering, washing to be neutral, soaking for 1h by using an ammonium persulfate solution with the mass concentration of 25%, filtering again, rinsing for 3 times by using deionized water, drying at 90 ℃, and preparing the carbon fibers into a prefabricated member with a three-dimensional structure by using 3D printing equipment;
(2) crushing the intermediate phase asphalt particles to the particle size of less than or equal to 15 microns, adding the crushed intermediate phase asphalt particles into deionized water, stirring, adding polyethylene glycol 6000 distearate, wherein the mass ratio of the intermediate phase asphalt particles to the polyethylene glycol 6000 distearate to the deionized water is 20: 10: 50, continuously stirring to obtain uniform liquid, immersing the prefabricated part, performing ultrasonic treatment for 10min, taking out and transferring the prefabricated part into a container, transferring the container into a high-pressure reaction kettle, replacing air in the kettle with nitrogen, continuously introducing nitrogen to ensure that the pressure in the kettle is 5MPa, hermetically heating to 500 ℃, the heating speed is 3 ℃/min, performing heat preservation reaction for 5h, transferring into a carbonization furnace, heating to 1000 ℃ under the protection of nitrogen, performing treatment for 5h, the heating speed is 1 ℃/min, transferring into a vacuum sintering furnace, heating at the heating speed of 20 ℃/min, adding a proper amount of silicon powder, performing heat preservation reaction for 10h under the protection of nitrogen, immersing into a hydrofluoric acid-nitric acid mixed solution with the volume ratio of 40:1, performing immersion treatment for 10min, washing with water to neutrality, and drying to obtain a blank;
(3) fixing the blank in a casting mold by using a metal bracket, preheating to 550 ℃, and then pouring molten high-temperature alloy liquid into the mold, wherein the alloy liquid comprises the following elements in percentage by weight: 0.18% of Si, 0.16% of Fe, 2.5% of Cu2, 0.02% of Mg, 0.5% of Cr, 0.3% of Mn, 0.24% of Zn, 0.16% of Ti, 0.13% of Ce and the balance of Al, wherein the alloy liquid permeates into the blank under the action of natural gravity, the pouring temperature of the alloy liquid is 750 ℃, the internal pressure of a mold is 25MPa, the pressure maintaining time is 30s, the composite material is placed into a muffle furnace after being demoulded, the temperature is increased to 450 ℃, the temperature is kept for 2h, and the composite material is air-cooled to the room temperature along with the furnace.
And (3) performance testing:
table 1 below shows the results of the performance tests of the composites prepared in examples 1 to 3 according to the invention:
table 1:
as can be seen from the above Table 1, the ceramic-based metal composite material of the present invention has excellent properties and meets the requirements of modern industrial use.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other identical elements in a process, method, article, or apparatus that comprises the element.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (10)
1. The preparation method of the high-strength porous three-dimensional ceramic matrix metal composite material is characterized by comprising the following steps of:
(1) putting carbon fibers into an acetone solution, carrying out ultrasonic cleaning for 30-50min, filtering, transferring the carbon fibers into a muffle furnace, heating to 450-plus-500 ℃ for high-temperature treatment for 3-6h, cooling to room temperature along with the furnace, adding the carbon fibers into a mixed acid solution, carrying out immersion treatment for 10-15min, filtering, washing with water to neutrality, carrying out immersion treatment for 1-3h by using an ammonium persulfate solution, filtering again, carrying out elution for 3 times by using deionized water, drying at 70-90 ℃, and preparing the carbon fibers into a prefabricated member with a three-dimensional structure by using 3D printing equipment;
(2) pulverizing mesophase pitch particles, adding into deionized water, stirring, adding polyethylene glycol 6000 distearate, stirring to obtain uniform liquid, soaking the prefabricated member, ultrasonic treating for 5-10min, taking out, transferring into a container, transferring the container into a high-pressure reaction kettle, replacing air in the kettle with nitrogen, continuously introducing nitrogen to ensure that the pressure in the kettle is 5-8MPa, hermetically heating to 480-plus-500 ℃, carrying out heat preservation reaction for 2-5h, transferring into a carbonization furnace, heating to 1000-plus-1020 ℃ under the protection of nitrogen, treating for 2-5h, transferring into a vacuum sintering furnace, adding a proper amount of silicon powder, heating to 1500-plus-1550 ℃ under the protection of nitrogen, carrying out heat preservation reaction for 5-10h, soaking in a mixed solution of hydrofluoric acid and nitric acid for 5-10min, washing with water to neutrality, and drying to obtain a blank;
(3) fixing the blank in a casting mold by using a metal support, preheating to the temperature of 550-600 ℃, then pouring molten high-temperature alloy liquid into the mold, allowing the alloy liquid to permeate into the blank under the action of natural gravity, wherein the pouring temperature of the alloy liquid is 750-770 ℃, the internal pressure of the mold is 20-25MPa, the pressure maintaining time is 30-40s, placing the composite material into a muffle furnace after demolding, heating to the temperature of 400-450 ℃, preserving heat for 2-5h, and cooling to room temperature along with the furnace.
2. The method for preparing a high-strength porous three-dimensional ceramic matrix metal composite material according to claim 1, wherein the mixed acid solution in the step (1) is a mixed solution of concentrated nitric acid and concentrated sulfuric acid, and the volume ratio of the two is 1-5: 1-5.
3. The method for preparing a high-strength porous three-dimensional ceramic-based metal composite material according to claim 1, wherein the mass concentration of the ammonium persulfate solution in the step (1) is 18-25%.
4. The method according to claim 1, wherein the size of the pulverized mesophase pitch particles in step (2) is less than or equal to 15 μm.
5. The method for preparing a high-strength porous three-dimensional ceramic-based metal composite material according to claim 1, wherein the mass ratio of the mesophase pitch particles, the polyethylene glycol 6000 distearate and the deionized water in the step (2) is 20-30: 5-10: 50-80.
6. The method for preparing a high-strength porous three-dimensional ceramic matrix metal composite material according to claim 1, wherein the temperature rise rate of the high-pressure reaction kettle in the step (2) is 3-5 ℃/min.
7. The method for preparing a high strength porous three dimensional ceramic matrix metal composite material according to claim 1, wherein the temperature rise rate of the carbonization furnace in step (2) is 1-2 ℃/min.
8. The method for preparing a high strength porous three dimensional ceramic matrix metal composite material according to claim 1, wherein the temperature rise rate of the vacuum sintering furnace in step (2) is 10-20 ℃/min.
9. The method for preparing a high strength porous three dimensional ceramic matrix metal composite according to claim 1, wherein the volume ratio of hydrofluoric acid to nitric acid in the mixed solution of step (2) is 40-50: 1.
10. The method for preparing a high-strength porous three-dimensional ceramic matrix metal composite material according to claim 1, wherein the alloy liquid in the step (3) comprises the following elements in percentage by weight: 0.1 to 0.18 percent of Si, 0.16 to 0.32 percent of Fe, 2.1 to 2.5 percent of Cu2, 0.02 to 0.08 percent of Mg, 0.38 to 0.5 percent of Cr0, 0.3 to 0.86 percent of Mn, 0.12 to 0.24 percent of Zn, 0.16 to 0.33 percent of Ti, 0.05 to 0.13 percent of Ce and the balance of Al.
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