CN117385297A - Fiber reinforced metal matrix composite material and normal pressure preparation process thereof - Google Patents

Fiber reinforced metal matrix composite material and normal pressure preparation process thereof Download PDF

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Publication number
CN117385297A
CN117385297A CN202311301087.1A CN202311301087A CN117385297A CN 117385297 A CN117385297 A CN 117385297A CN 202311301087 A CN202311301087 A CN 202311301087A CN 117385297 A CN117385297 A CN 117385297A
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China
Prior art keywords
composite material
temperature
cooling
matrix
fiber
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CN202311301087.1A
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张健
朱敏
蒋世权
马小民
马晓东
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Guozhuang New Material Technology Jiangsu Co ltd
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Guozhuang New Material Technology Jiangsu Co ltd
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C47/00Making alloys containing metallic or non-metallic fibres or filaments
    • C22C47/08Making 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
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C49/00Alloys containing metallic or non-metallic fibres or filaments
    • C22C49/02Alloys containing metallic or non-metallic fibres or filaments characterised by the matrix material
    • C22C49/04Light metals
    • C22C49/06Aluminium
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C49/00Alloys containing metallic or non-metallic fibres or filaments
    • C22C49/14Alloys containing metallic or non-metallic fibres or filaments characterised by the fibres or filaments

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Manufacture Of Alloys Or Alloy Compounds (AREA)

Abstract

The invention belongs to the technical field of preparation of special composite materials, and relates to a fiber reinforced metal matrix composite material and a normal pressure preparation process thereof. Adding a metal alloy matrix into an induction furnace, heating to fully melt, and then cooling to a solid-liquid mixed state; cutting after coating the surface of the alumina fiber, putting the alumina fiber into an induction furnace, and mechanically stirring and fully and uniformly mixing the alumina fiber; heating and preserving heat to perform matrix alloying, pouring into a mould, compacting and performing programmed cooling operation; and (3) raising the temperature for the second time, preserving heat, performing subsequent aging treatment, and naturally cooling to room temperature to obtain the product. Can solve the technical dilemma that large-scale equipment is needed for preparing the alumina composite material, refine grains and improve the strength and the compactness of the composite material. The fiber content is controllable, and the composite configuration of particles and short, medium and long fibers is realized. The process provided by the invention has the advantages of simple operation, low preparation cost and no need of special atmosphere protection.

Description

Fiber reinforced metal matrix composite material and normal pressure preparation process thereof
Technical Field
The invention belongs to the technical field of preparation of special composite materials, and relates to a fiber reinforced metal matrix composite material and a normal pressure preparation process thereof.
Background
Al 2 O 3 The fiber reinforced metal matrix composite has the characteristics of high hardness, tensile strength, compression resistance and the like, and has wide application prospects in the aspects of aviation, aerospace structural members, automobile members and the like. Currently, there are various methods for preparing metal matrix composite materials, such as a common solid phase method, a liquid phase method, and an in situ generation method. Among them, the problem of wettability between the fiber and the matrix is a difficulty in all the methods.
The patent CN 111218579B adopts the steps that SiC particles are subjected to surface pretreatment, then a semi-solid stirring process is matched with an ultrasonic auxiliary process to jointly prepare a metal composite material, finally technological parameters are set to forge the composite material, the process needs atmosphere protection in the preparation process, certain requirements are met on equipment, and the preparation period is relatively long. The process provided in patent CN 109022859B is divided into four steps: smelting a matrix alloy and preheating reinforcement nano titanium particles; semi-solid stirring; performing ultrasonic treatment; and (5) die casting and forming. The process adopts differential forward and reverse stirring and slow rotating crucible ultrasonic treatment to prepare the nano titanium particle reinforced high-strength magnesium-based composite material, the magnesium-based substrate alloy is heated and cooled to form a semi-solid state, then the preheated nano titanium particles are added into a semi-solid melt, the differential forward and reverse stirring is carried out, the mixed melt is heated to a liquid state after the stirring is finished, the slow rotating crucible ultrasonic treatment is carried out, and finally the cast magnesium-based composite material is prepared by die casting. The process has simple steps, but has certain requirements on the form of the reinforcement and has poor universality. The process of patent CN 104805318B is divided into five steps: preheating TC4 particles; semi-solid stirring; performing ultrasonic treatment; self-settling; and (5) cooling. The scheme avoids the problem of poor wettability in the preparation of the metal matrix composite material by the semi-solid stirring technology, but selects the semi-solid stirring preparation technology aiming at the relation of good wettability of TC4 particles and magnesium alloy, so that the method has no universal applicability. The patent CN 115491568B has the specific steps: (1) subjecting SiC particles to an oxidation pretreatment; (2) Laying a piece of magnesium alloy on the bottom, then laying a layer of SiC particles, repeating the operation of a layer of magnesium alloy and a layer of SiC particles until all the magnesium alloy and the SiC particles are laid, introducing inert gas, heating to melt, and slagging off; (4) Cooling to the semi-solid temperature of the magnesium alloy, performing semi-solid mechanical stirring, heating, and performing mechanical stirring again; (5) cooling to semi-solid temperature again, and casting into a blank; (6) And heating the blank again to the semi-solid temperature and extruding to obtain the magnesium-based composite material. The process can only be used for manufacturing composite materials by using particles, and the defect of non-wetting between ceramic particles and metal is not considered.
Disclosure of Invention
The invention aims at the traditional Al 2 O 3 The problems existing in the preparation of the fiber reinforced metal matrix composite material provide a novel fiber reinforced metal matrix composite material and a normal pressure preparation process thereof.
In order to achieve the above purpose, the invention is realized by adopting the following technical scheme:
a normal pressure preparation process of a fiber reinforced metal matrix composite material comprises the following steps:
(1) Adding a metal alloy matrix into an induction furnace, heating to fully melt, and then cooling to a solid-liquid mixed state.
(2) Cutting after coating the surface of the alumina fiber, putting the alumina fiber into the induction furnace of the step (1), and mechanically stirring and fully and uniformly mixing the alumina fiber.
(3) Heating and preserving heat to alloy the matrix, pouring the matrix into a die, compacting the matrix, and performing programmed cooling operation.
(4) And (3) raising the temperature for the second time, preserving heat, performing subsequent aging treatment, and naturally cooling to room temperature to obtain the product.
The invention provides a process for preparing a reinforced body fiber, which is characterized in that a continuous alumina fiber produced by a national new material technology (Jiangsu) limited company is adopted, after the surface of the fiber is metallized, the fiber is sheared into a required length, an intermediate frequency induction furnace is used for setting the temperature to be 200 ℃ higher than the melting point, a metal block is put into the furnace, the temperature is reduced to 10 ℃ below the melting point after the metal block is fully melted, at the moment, the prepared fiber is added in a small amount successively, mechanical stirring is used for a certain time, after the metal block is fully melted, the temperature is raised to 200 ℃ above the melting point of the metal, the temperature is kept for a period of time, the solution is poured into a die, and the die is compacted, and cooling parameters are set: cooling at a cooling rate of 20-50 ℃/h to 200 ℃, and performing effective treatment after that: heating to 450-500 ℃, heating at a speed of 30-60 ℃/h, maintaining for 2-6h, and then air cooling to room temperature to obtain the metal matrix composite material with a certain mass fraction.
Preferably, the continuous alumina fibers in step (1) are numbered 735, 857, 996, etc.; the fiber surface metallization treatment comprises, but is not limited to, electroless plating, vapor deposition and plasma spraying; cut lengths include, but are not limited to, pellets, 3-5mm staple fibers, and long fibers; the fiber surface metallization component includes but is not limited to copper, nickel, silver; the metal alloy matrix is any one of aluminum magnesium alloy, aluminum copper alloy and aluminum silicon alloy; the stirring time in the step (2) comprises, but is not limited to, 10-20min; the incubation time in step (3) includes, but is not limited to, 10min-20min.
In principle, the fiber surface after the fiber surface metallization treatment in the process provided by the invention has a uniform metal coating, and the metal can be effectively compounded at a certain temperature to play a role of an intermediate bridge; the temperature of the induction furnace is set to 200 ℃ higher than the melting point of the alloy matrix for the first time, so that the matrix metal can be melted, and the aim of alloying uniformity is fulfilled. Then the temperature is reduced to 10 ℃ below the melting point of the alloy matrix, so that the target metal can be in a semi-solid state, and the fiber with the metal coating can be compounded due to the self viscosity during mechanical stirring. And the temperature is raised to 200 ℃ above the metal melting point again, and the matrix can be alloyed after the heat preservation is carried out for a period of time, so that the wettability between the fiber and the matrix is improved. The invention can control the cooling speed of the composite material to ensure that atoms have enough energy and time migration. If cooled rapidly, the energy of the atoms and their migration time are reduced and the grain growth process is inhibited. The post-treatment aims at eliminating residual stress of composite materials and stabilizing tissues and sizes.
Compared with the prior art, the invention has the advantages and positive effects that:
1. normal pressure preparation combined with cooling control can solve the problems of Al preparation 2 O 3f @Al composite materialThe technology dilemma of large-scale equipment is needed, grains are refined, and the strength and the compactness of the composite material are improved.
2. The content of the alumina fiber is controllable, and the composite configuration of the particles and the short, medium and long fibers is realized.
3. The matrix alloy element component has no specific requirement, and can be widely applied to the preparation of various metal matrix composite materials taking aluminum and aluminum alloy as matrixes.
4. The process provided by the invention has the advantages of simple operation, low preparation cost and no need of special atmosphere protection.
Detailed Description
In order that the above objects, features and advantages of the invention will be more clearly understood, a further description of the invention will be provided with reference to specific examples. It should be noted that, in the case of no conflict, the embodiments of the present application and the features in the embodiments may be combined with each other.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, however, the present invention may be practiced otherwise than as described herein, and therefore the present invention is not limited to the specific embodiments of the disclosure that follow.
Example 1
In the embodiment, aluminum oxide fiber (99% aluminum oxide and 1% silicon dioxide) with the trademark of 996 is produced by national material technology (Jiangsu) limited company, the surface of the fiber is plated with copper (the thickness of the coating is about 1 micrometer) by an electroless plating technology, and the fiber is naturally dried and cut into 3-5mm for standby; the matrix is aluminum magnesium alloy (the matrix alloy adopted in the embodiment and the following embodiments is conventional commercial alloy, and the temperature is raised by fine adjustment according to the melting point of the matrix alloy, wherein the mass percentage of the aluminum magnesium alloy in the embodiment is about 4%). Setting the temperature of the medium-frequency induction furnace to 800 ℃, adding 90g of matrix, heating to 850 ℃, keeping the temperature for 10min after the matrix is fully melted, cooling to 640 ℃, adding 10g of copper-plated aluminum oxide fiber, stirring for 15min at the rotation speed of 200 r/min, heating to 850 ℃ again, keeping the temperature for 10min, and stirring for 10min at the rotation speed of 200 r/min; preparing a graphite mold, pouring composite aluminum liquid into the mold, compacting, and setting cooling parameters: cooling at a cooling rate of 20 ℃/h, cooling to 200 ℃, and performing effect treatment after that: heating to 450 ℃, heating at a speed of 30 ℃/h, preserving heat for 2h, and then air-cooling to room temperature to obtain the aluminum-based composite material with the mass fraction of 10%.
Example 2
Selecting 857 alumina fiber (85% alumina and 15% silica), plating copper on the surface of the fiber (the thickness of the coating is about 1 micron) by chemical vapor deposition technology, naturally airing, and grinding into particles for standby; the matrix is made of aluminum copper alloy (the weight percentage of copper is about 9%). Setting the temperature of the medium frequency induction furnace to 840 ℃, adding 90g of matrix, cooling to 630 ℃ after the matrix is fully melted and insulated for 10min, adding 10g of alumina particles at the moment, stirring for 10min, heating to 840 ℃ again, insulating for 15min, and stirring for 15min; preparing a graphite mold, pouring composite aluminum liquid into the mold, compacting, and setting cooling parameters: cooling at a cooling rate of 30 ℃/h, cooling to 200 ℃, and performing effect treatment after that: heating to 470 ℃, heating at a speed of 45 ℃/h, preserving heat for 4h, and then air-cooling to room temperature to obtain the aluminum-based composite material with the mass fraction of 10%.
Example 3
Alumina fiber (73% alumina and 25% silica) with the brand number of 735 is selected, copper plating treatment is carried out on the surface of the fiber by a plasma spraying technology, and the fiber is kept in an original state for standby after natural airing; the matrix is made of aluminum-silicon alloy (the silicon mass percentage is about 10 percent); setting the temperature of the medium frequency induction furnace to 780 ℃, adding 90g of matrix, cooling to 570 ℃ after the matrix is fully melted and insulated for 20min, adding 10g of alumina fiber, stirring for 20min, heating to 780 ℃ again, insulating for 20min, and stirring for 20min; preparing a graphite mold, pouring composite aluminum liquid into the mold, compacting, and setting cooling parameters: cooling at a cooling rate of 50 ℃/h, cooling to 200 ℃, and performing effect treatment after that: heating to 500 ℃, heating at a speed of 60 ℃/h, preserving heat for 6h, and then air-cooling to room temperature to obtain the aluminum-based composite material with the mass fraction of 10%.
Comparative example 1
Setting the temperature of the intermediate frequency induction furnace in the comparative example to 900 ℃, adding a matrix, preserving heat for 30min after the matrix is fully melted, cooling to 640 ℃, adding alumina fibers at the moment, stirring for 8min, heating to 900 ℃ again, preserving heat for 15min, and stirring for 30min; the remaining process conditions and material amounts were identical to those of example 1. And obtaining the aluminum-based composite material with the mass fraction of 10%.
Comparative example 2
This comparative example did not employ a cooling procedure, but instead employed a room temperature natural cooling process, the remaining operating steps remained the same as in example 1. And obtaining the aluminum-based composite material with the mass fraction of 10%.
Comparative example 3
In this comparative example, the fiber was not subjected to surface modification treatment, and the rest of the procedure was the same as in example 1, to obtain an aluminum-based composite material having a mass fraction of 10%.
Comparative example 4
In this comparative example, the mechanical stirring step was omitted, and the rest of the steps were the same as in example 1, to obtain an aluminum-based composite material having a mass fraction of 10%.
Comparative example 5
In this comparative example, the compacting step was omitted, and the rest of the steps were the same as in example 1, to obtain an aluminum-based composite material having a mass fraction of 10%.
The mechanical properties of the aluminum-based composites prepared in comparative examples 1 to 3 and comparative examples 1 to 5 were tested, and the specific test results are shown in Table 1.
TABLE 1 results of mechanical Properties test of aluminum-based composite materials
The hardness and the tensile strength of the composite material are determined by the wettability of the material, the fibers and the matrix can be well combined under the condition of good wettability, and external load can be transmitted to the matrix through the fibers, so that the hardness and the tensile strength of the composite material are improved, and under the condition of poor wettability, the external load cannot be transmitted to the matrix through the fibers, so that the performance is reduced and the compactness is poor. As can be seen from Table 1, the aluminum-based composite materials prepared in examples 1 to 3 have excellent hardness and tensile strength, and thus the material prepared in the present invention has excellent wettability. As can be seen from the data of comparative example 1, the hardness and tensile strength of the material are reduced to some extent by changing the process parameters proposed in the present invention. As can be seen from the test results of comparative example 2, compared with the cooling procedure proposed by the present invention, the hardness and tensile strength of the material after natural cooling are both significantly reduced, and the hardness of the material is significantly reduced, because the atoms can possess sufficient energy and time migration by controlling the cooling rate of the composite material. If rapidly cooled, the energy of the atoms and its migration time are reduced and the grain growth process is inhibited, thereby affecting the hardness and strength of the material. Comparative examples 3 to 5, in which the fiber surface modification step, the mechanical stirring step and the compaction step of the material in the mold were omitted, respectively, showed that the hardness and tensile strength of the final product were significantly reduced from the results of the test, indicating that the fiber surface modification step, the mechanical stirring step and the compaction step of the material in the mold were key steps in the process step of the present invention.
The invention adopts normal pressure to prepare the metal-based composite material, has the advantages of simple process, lower cost than a solid phase method and a traditional liquid phase method, and the like, and can utilize a material design method to design the final required composite material performance and interface structure, so the invention is a preparation process of the metal-based composite material with very good development prospect.
The present invention is not limited to the above-mentioned embodiments, and any equivalent embodiments which can be changed or modified by the technical content disclosed above can be applied to other fields, but any simple modification, equivalent changes and modification made to the above-mentioned embodiments according to the technical substance of the present invention without departing from the technical content of the present invention still belong to the protection scope of the technical solution of the present invention.

Claims (6)

1. The normal pressure preparation process of the fiber reinforced metal matrix composite material is characterized by comprising the following steps:
(1) Adding a metal alloy matrix into an induction furnace, heating to fully melt, and then cooling to a solid-liquid mixed state;
(2) Cutting after coating the surface of the alumina fiber, putting the alumina fiber into an induction furnace in the step (1), and mechanically stirring the alumina fiber until the alumina fiber is fully and uniformly mixed;
(3) Heating and preserving heat to perform matrix alloying, pouring into a mould, compacting and performing programmed cooling operation;
(4) And (3) raising the temperature for the second time, preserving heat, performing subsequent aging treatment, and naturally cooling to room temperature to obtain the product.
2. The normal pressure preparation process of the fiber reinforced metal matrix composite material according to claim 1, wherein in the step (1), the metal alloy matrix is any one of aluminum magnesium alloy, aluminum copper alloy and aluminum silicon alloy, the temperature rise temperature is 200 ℃ higher than the melting point of the metal alloy matrix, and the temperature drop temperature is 10 ℃ lower than the melting point of the metal alloy matrix.
3. The process for preparing a fiber reinforced metal matrix composite at normal pressure according to claim 1, wherein the alumina fiber surface coating in step (2) is cut and then placed into the induction furnace a small number of times.
4. The normal pressure preparation process of the fiber reinforced metal matrix composite material according to claim 1, wherein the temperature rise in the step (3) is 200 ℃ higher than the melting point of the metal alloy matrix, and the heat preservation time is 10-20min; the cooling process is that the cooling rate is 20-50 ℃/h, and the temperature is cooled to 200 ℃.
5. The normal pressure preparation process of the fiber reinforced metal matrix composite according to claim 1, wherein the secondary temperature rise temperature in the step (4) is 450-500 ℃, the temperature rise rate is 30-60 ℃/h, and the heat preservation time is 2-6h.
6. A fibre reinforced metal matrix composite prepared by the process of any one of claims 1 to 5.
CN202311301087.1A 2023-10-10 2023-10-10 Fiber reinforced metal matrix composite material and normal pressure preparation process thereof Pending CN117385297A (en)

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CN202311301087.1A CN117385297A (en) 2023-10-10 2023-10-10 Fiber reinforced metal matrix composite material and normal pressure preparation process thereof

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Application Number Priority Date Filing Date Title
CN202311301087.1A CN117385297A (en) 2023-10-10 2023-10-10 Fiber reinforced metal matrix composite material and normal pressure preparation process thereof

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CN117385297A true CN117385297A (en) 2024-01-12

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