CN114250379B - Preparation method of in-situ particle reinforced metal matrix composite material - Google Patents

Preparation method of in-situ particle reinforced metal matrix composite material Download PDF

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CN114250379B
CN114250379B CN202111542459.0A CN202111542459A CN114250379B CN 114250379 B CN114250379 B CN 114250379B CN 202111542459 A CN202111542459 A CN 202111542459A CN 114250379 B CN114250379 B CN 114250379B
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powder
sintering
metal matrix
matrix composite
composite material
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CN114250379A (en
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杨芳
郭丽丽
郭志猛
陈存广
隋延力
杨松
李延丽
李泽北
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University of Science and Technology Beijing USTB
Shunde Graduate School of USTB
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Shunde Graduate School of USTB
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/05—Mixtures of metal powder with non-metallic powder
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/02—Compacting only
    • B22F3/04—Compacting only by applying fluid pressure, e.g. by cold isostatic pressing [CIP]
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10—Sintering only
    • B22F3/1003—Use of special medium during sintering, e.g. sintering aid
    • B22F3/1007—Atmosphere
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10—Sintering only
    • B22F3/1017—Multiple heating or additional steps
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10—Sintering only
    • B22F3/1039—Sintering only by reaction
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C14/00—Alloys based on titanium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
    • C22C32/0047—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/25—Process efficiency

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
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Abstract

A method for preparing an in-situ particle reinforced metal matrix composite material, belonging to the field of powder metallurgy. The invention mixes titanium powder, reinforcement X and adhesive M according to a certain proportion, after pressing and forming, adopts two-step sintering process of nitrogen sintering and high temperature sintering to obtain the high-performance in-situ particle reinforced metal matrix composite material. In the invention, titanium powder and nitrogen, C, B or B are utilized4C to generate fine and uniform TiC, TiB, TiN or Ti (C, N) reinforced phase particles. Meanwhile, Fe, Ni and Co are used as binders to increase the wettability between the strengthening phase and the binder phase and realize the metallurgical bonding of the strengthening particles and the metal matrix, so that the toughness of the metal matrix composite material is improved, full compactness is realized and residual pores are eliminated. The metal matrix composite material is prepared by a powder metallurgy process, in-situ particle strengthening can be realized, the process is simple, the utilization rate of raw materials is high, the shape of the material is complex and changeable, the production efficiency is high, and the method is suitable for large-scale industrial production.

Description

Preparation method of in-situ particle reinforced metal matrix composite material
Technical Field
The invention belongs to the field of powder metallurgy, and provides a preparation method of an in-situ particle reinforced metal matrix composite.
Background
In recent years, with the rapid development of modern manufacturing industries, metal matrix composites have become indispensable new materials. Metal base in the metal base composite material as base body, TiB2、Ti(C,N)、B4C. TiN and Si3N4And ceramic particles as a reinforcing phase. The ceramic particles of TiN, TiC, TiB, Ti (C, N) and the like have the advantages of high melting point, high hardness, good corrosion resistance and oxidation resistance and the like, have good thermal conductivity, electrical conductivity and chemical stability, and are suitable for a plurality of fields of cutter and die manufacturing, aerospace and the like. Generally, TiN, TiC, TiB and Ti (C, N) ceramic particles are prepared by a high-temperature solid solution method, a high-temperature nitridation method, a sol-gel method, an ammonolysis method, a high-temperature self-propagating reaction method, a high-energy ball milling method and an in-situ synthesis method, wherein the in-situ synthesis method can effectively solve the interface reaction between a reinforcement material and a substrate, further improves the hardness, strength, wear resistance, creep resistance, high-cycle fatigue resistance and the like of the material, and can simultaneously keep the surface of the reinforcement body free of pollution.
The powder metallurgy process mixes the metal and the reinforcement powder, forms and sinters the metal and the reinforcement powder to prepare the metal matrix composite material, and the reinforcement and the matrix particles can be aggregated and bonded to form a bonding surface through the powder sintering process, so that the size and the number of gaps among the particles are greatly reduced, and the densification of the metal matrix composite material is realized. Meanwhile, different powder metallurgy processes provide good premise for preparing metal-based materials with different strengthening modes and different properties, and have the advantages of low production cost, complex and changeable material shapes, high production efficiency, simple production process and the like. By adopting the powder metallurgy process, the method has very important significance on how to obtain the fully-compact metal matrix composite material reinforced by the in-situ particles.
Disclosure of Invention
The invention aims to provide a preparation method of an in-situ particle reinforced metal matrix composite. The method selects titanium powder as matrix powder, uniformly mixes the titanium powder with the reinforcement X and the binder M according to a certain proportion, presses and forms the mixture, and obtains the high-performance in-situ particle reinforced metal matrix composite material after two-step sintering. On one hand, in the primary sintering, in the nitrogen sintering process at the sintering temperature of 1100-1250 ℃, titanium powder and nitrogen are subjected to nitridation reaction to generate TiN enhanced particles, and the primary sintering shrinkage of a blank can be realized by using the sintering activity of the titanium powder; at the same time, the reinforcement C, B or B4The C particles and titanium powder can generate TiC, TiB and Ti (C, N) strengthening phase particles in situ under the nitrogen atmosphere, so that the mechanical property of the material is improved; on the other hand, in the high-temperature sintering process with the sintering temperature of 1300-1500 ℃, the binders Fe, Ni and Co can increase the wettability between the strengthening phase and the binder phase, realize the metallurgical bonding of the strengthening particles and the metal matrix, prevent the strengthening phase from aggregating and growing up, and make the distribution of the strengthening phase more uniform, thereby improving the toughness of the metal matrix composite material, realizing full compactness and eliminating residual pores. In addition, the metal matrix composite material is prepared by a powder metallurgy process, in-situ particle strengthening can be realized, the process is simple, the utilization rate of raw materials is high, the shape of the material is complex and changeable, the production efficiency is high, and the method is suitable for large-scale industrial production.
In order to obtain the preparation method of the in-situ particle reinforced metal matrix composite, the preparation method is characterized in that the metal matrix composite is prepared by adopting a powder metallurgy technology and a two-step sintering process, and the preparation method comprises the following specific steps:
(1) weighing titanium powder, a reinforcement body X and a binder M according to a certain proportion, then loading the titanium powder, the reinforcement body X and the binder M into a mixing tank for mixing for 1-4h to obtain uniform mixed powder;
(2) filling the mixed powder in the step (1) into a cold isostatic pressing sheath, compacting, then strictly sealing the cold isostatic pressing sheath, and carrying out cold isostatic pressing forming under 200-400MPa for 30-120s to obtain a pressed sample;
(3) and (3) performing primary sintering, namely putting the pressed blank sample in the step (2) into a sintering furnace for nitrogen sintering, wherein the sintering temperature is 1100-1250 ℃, and the heat preservation time is 2-4 h, so as to obtain the titanium-based sintered blank.
(4) And (4) high-temperature sintering, namely sintering the titanium-based sintered blank in the step (3) in a sintering furnace at high temperature to finally obtain the high-performance in-situ particle reinforced metal-based composite material.
Further, the titanium powder in the step (1) is irregular pure titanium powder which is sold in the market, the particle size of the powder is less than or equal to 100 mu m, and the oxygen content is less than 0.2 wt.%.
Further, the reinforcement X in the step (1) is C, B or B which is commercially available4One or more of C powder with particle size not more than 10 μm and purity more than 99.9%.
Furthermore, the binder M in the step (1) is commercially available iron powder, nickel powder or cobalt powder, the particle size of the powder is less than or equal to 150 mu M, and the purity is more than 99.9%.
Further, in the mixed powder in the step (1), the content of the reinforcement X is 2-10 wt.%, the content of the binder M is 15-40 wt.%, and the balance is titanium powder.
Further, in the step (3), the sintering temperature is 1100-1250 ℃, the heat preservation time is 2-4 h, and the density of the titanium-based sintered blank is not less than 70%.
Further, the high-temperature sintering in the step (4) is carried out, wherein the sintering temperature is 1300-1500 ℃, the heat preservation time is 2-4 h, the sintering atmosphere is nitrogen, argon or vacuum, and the vacuum degree is 10-2-10Pa。
Further, the particle size of the hard phase in the in-situ particle reinforced metal matrix composite material in the step (4) is 0.1-5 μm.
The key points of the technology of the invention are as follows: (1) and a secondary sintering process is adopted. During nitrogen sintering, the reinforcement C, B or B4The C particles react with the titanium powder to generate fine and uniform TiC, TiB, TiN and Ti (C, N) strengthening phase particles in situ, so that the size and the number of gaps among the particles are continuously reduced, and the strength and the hardness of the material are greatly improved. (2) By utilizing the mutual reaction between titanium powder and nitrogen, nitrogen sintering is proposed, not only can the titanium powder be completely nitrided to generate fine and uniform TiN reinforced particles in situ, but also the titanium powder is utilizedAnd sintering activity is realized, primary sintering of the green body is realized, the purpose of partial shrinkage is achieved, and the partially sintered particle reinforced metal matrix composite material is obtained. (3) In the high-temperature sintering process at 1300-1500 ℃, the molten Fe, Ni and Co can increase the wettability between the strengthening phase and the binding phase, and can refine the crystal grains of the hard phase, so that the metallurgical bonding of the material is improved; meanwhile, the hardness and the toughness of the material are improved, and the full compactness of the material is realized. (4) In order to match the proportion of TiN or Ti (C, N) particles generated in situ in the nitrogen sintering process, the weight percentages of the titanium powder, the reinforcement body X and the binder M in the raw material powder are obtained through a large number of experimental verifications and are matched with the nitrogen sintering temperature and the sintering compactness.
The invention has the advantages that:
1. the method is not only suitable for preparing the metal-based composite material by cold isostatic pressing, but also suitable for preparing the metal-based composite material with a complex shape by gel injection molding and injection molding, and has universality.
2. Reinforcement C, B or B by powder metallurgy4The C particles are introduced into the titanium powder matrix to generate TiC, TiB, TiN and Ti (C, N) reinforced phase particles in situ, the distribution is fine and uniform, and the mechanical property of the metal matrix composite material is effectively improved.
3. The Fe, Ni and Co can increase the wettability between the strengthening phase and the binding phase in the high-temperature sintering process, realize the metallurgical bonding of the materials, ensure that the metal matrix composite material has high strength and high hardness, and can realize full compactness.
4. The in-situ particle reinforced metal matrix composite prepared by the method can solve the problems of pollution, poor wettability, serious interface reaction and the like of an externally added reinforcement body in the traditional external addition method.
5. The powder metallurgy method can realize the preparation of parts with complex shapes, the design is more free and flexible, and simultaneously, the content and the distribution of the reinforcement body are easy to control, and the near-net forming can be realized.
Detailed Description
Example 1:
a preparation method of an in-situ particle reinforced metal matrix composite material comprises the following specific preparation steps:
(1) weighing 55 wt.% of titanium powder, 10wt.% of carbon powder and 35 wt.% of iron powder according to a ratio, then filling the materials into a mixing tank for mixing, and obtaining uniform mixed powder after mixing for 2 hours;
(2) filling the mixed powder in the step (1) into a cold isostatic pressing sheath, compacting, strictly sealing the cold isostatic pressing sheath, and carrying out cold isostatic pressing under 200MPa for 120s to obtain a pressed compact sample;
(3) and (3) putting the pressed compact sample in the step (2) into a sintering furnace for nitrogen sintering, wherein the sintering temperature is 1250 ℃, and the heat preservation time is 2 hours, so as to obtain the titanium-based sintered compact.
(4) Carrying out vacuum sintering on the titanium-based sintering blank in the step (3) in a vacuum sintering furnace, wherein the sintering temperature is 1350 ℃, and the vacuum degree is 10-2Pa, keeping the temperature for 4h, and finally obtaining the high-performance in-situ TiC/Ti (C, N) particle reinforced metal matrix composite material.
Example 2:
a preparation method of an in-situ particle reinforced metal matrix composite material comprises the following specific preparation steps:
(1) weighing 75 wt.% of titanium powder, 5 wt.% of boron powder and 20 wt.% of nickel powder according to a ratio, then filling the materials into a mixing tank for mixing, and mixing for 2 hours to obtain uniform mixed powder;
(2) filling the mixed powder in the step (1) into a cold isostatic pressing sheath, compacting, strictly sealing the cold isostatic pressing sheath, and carrying out cold isostatic pressing forming under 300MPa for 100s to obtain a pressed compact sample;
(3) and (3) putting the pressed compact sample in the step (2) into a sintering furnace for nitrogen sintering at the sintering temperature of 1200 ℃ for 3h to obtain the titanium-based sintered compact.
(4) And (4) sintering the titanium-based sintered blank in the step (3) in a tubular furnace by nitrogen at the sintering temperature of 1450 ℃ for 3h to finally obtain the high-performance in-situ TiN/TiB particle reinforced metal-based composite material.
Example 3:
a preparation method of an in-situ particle reinforced metal matrix composite material comprises the following specific preparation steps:
(1) 70 wt.% of titanium powder and 10wt.% of B4Weighing the C powder and 20 wt.% of cobalt powder according to a ratio, then filling the mixture into a mixing tank for mixing for 2 hours to obtain uniform mixed powder
(2) Filling the mixed powder in the step (1) into a cold isostatic pressing sheath, compacting, strictly sealing the cold isostatic pressing sheath, and carrying out cold isostatic pressing under 400MPa for 120s to obtain a pressed compact sample;
(3) and (3) putting the pressed compact sample in the step (2) into a sintering furnace for nitrogen sintering, wherein the sintering temperature is 1100 ℃, and the heat preservation time is 2 hours, so as to obtain the titanium-based sintered compact.
(4) And (4) sintering the titanium-based sintered blank in the step (3) in a tubular furnace by argon gas at the sintering temperature of 1500 ℃ for 4 hours to finally obtain the high-performance in-situ TiB/Ti (C, N)/TiN particle reinforced metal-based composite material.

Claims (2)

1. The preparation method of the in-situ particle reinforced metal matrix composite is characterized in that the metal matrix composite is prepared by adopting a powder metallurgy technology and a two-step sintering process, and the preparation method comprises the following specific steps:
(1) weighing titanium powder, a reinforcement body X and a binder M according to a certain proportion, then loading the titanium powder, the reinforcement body X and the binder M into a mixing tank for mixing for 1-4h to obtain uniform mixed powder;
(2) filling the mixed powder in the step (1) into a cold isostatic pressing sheath, compacting, strictly sealing the cold isostatic pressing sheath, and carrying out cold isostatic pressing under the pressure of 200-400MPa for 30-120s to obtain a pressed compact sample;
(3) primary sintering, namely putting the pressed compact sample obtained in the step (2) into a sintering furnace for nitrogen sintering to obtain a titanium-based sintered compact;
(4) high-temperature sintering, namely sintering the titanium-based sintered blank in the step (3) in a sintering furnace at high temperature to finally obtain the high-performance in-situ particle reinforced metal-based composite material;
the titanium powder in the step (1) is commercially available irregular pure titanium powder, the particle size of the powder is less than or equal to 100 microns, and the oxygen content is less than 0.2 wt%;
the reinforcement X in the step (1) is C, B or B which is commercially available4One or more of C powder, the particle size of the powder is less than or equal to 10 mu m, and the purity is more than 99.9 percent;
the binder M in the step (1) is commercially available iron powder, nickel powder or cobalt powder, the particle size of the powder is less than or equal to 150 mu M, and the purity is more than 99.9 percent;
in the mixed powder in the step (1), the content of the reinforcement X is 2-10 wt.%, the content of the binder M is 15-40 wt.%, and the balance is titanium powder;
in the step (3), the primary sintering temperature is 1100-1250 ℃, the heat preservation time is 2-4 h, and the density of the titanium-based sintered blank is more than or equal to 70%;
sintering at the high temperature in the step (4), wherein the sintering temperature is 1300-1500 ℃, the heat preservation time is 2-4 hours, the sintering atmosphere is nitrogen, argon or vacuum, and the vacuum degree is 10-2-10Pa。
2. The method of claim 1, wherein the method comprises: the particle size of the hard phase in the in-situ particle reinforced metal matrix composite material in the step (4) is 0.1-5 mu m.
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US5137565A (en) * 1990-12-21 1992-08-11 Sandvik Ab Method of making an extremely fine-grained titanium-based carbonitride alloy
CN109554567A (en) * 2018-12-20 2019-04-02 广东省材料与加工研究所 A kind of Ti-Fe alloy based composites and preparation method thereof
CN110791682A (en) * 2019-12-16 2020-02-14 泉州市派腾新材料科技有限公司 Preparation method of powder metallurgy titanium alloy
CN113373335A (en) * 2021-05-28 2021-09-10 北京科技大学 Preparation method of high-strength titanium-based composite material

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Publication number Priority date Publication date Assignee Title
US5137565A (en) * 1990-12-21 1992-08-11 Sandvik Ab Method of making an extremely fine-grained titanium-based carbonitride alloy
CN109554567A (en) * 2018-12-20 2019-04-02 广东省材料与加工研究所 A kind of Ti-Fe alloy based composites and preparation method thereof
CN110791682A (en) * 2019-12-16 2020-02-14 泉州市派腾新材料科技有限公司 Preparation method of powder metallurgy titanium alloy
CN113373335A (en) * 2021-05-28 2021-09-10 北京科技大学 Preparation method of high-strength titanium-based composite material

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