CN116144968B - Ti with excellent room temperature plasticity2Preparation method of AlNb-based composite material - Google Patents

Ti with excellent room temperature plasticity2Preparation method of AlNb-based composite material Download PDF

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CN116144968B
CN116144968B CN202310150011.7A CN202310150011A CN116144968B CN 116144968 B CN116144968 B CN 116144968B CN 202310150011 A CN202310150011 A CN 202310150011A CN 116144968 B CN116144968 B CN 116144968B
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alnb
powder
composite material
based composite
ball milling
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CN116144968A (en
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张宇
黄陆军
张雪
贾自远
喻启元
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Harbin Institute of Technology
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C14/00Alloys based on titanium
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10Sintering only
    • B22F3/1039Sintering only by reaction
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/12Both compacting and sintering
    • B22F3/14Both compacting and sintering simultaneously
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/04Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C32/00Non-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
    • C22C32/0047Non-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
    • C22C32/0073Non-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 only borides
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/04Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • B22F2009/043Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/25Process efficiency

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Ceramic Products (AREA)

Abstract

A preparation method of a Ti 2 AlNb-based composite material with excellent room temperature plasticity relates to a preparation method of a Ti 2 AlNb-based composite material. The invention aims to solve the technical problems that the discontinuous reinforced titanium-based composite material has poor reinforcing effect and high room temperature brittleness, and the traditional smelting technology has serious segregation and poor tissue uniformity. According to the invention, a low-energy ball milling method is adopted, so that TiB 2 powder is uniformly adhered to the surfaces of Ti 2 AlNb prealloy powder particles, and reasonable ball milling parameters are selected, so that the Ti 2 AlNb powder maintains good sphericity in the powder mixing process; then in-situ autogenous reaction promotes TiBw to grow near the surface of the spherical matrix alloy in the hot-press sintering process, so that further growth of crystal grains can be limited, a uniform network structure can be obtained, and the network structure can inhibit growth of the crystal grains in the sintering process, so that the Ti 2 AlNb-based composite material with excellent room temperature performance is obtained.

Description

Preparation method of Ti 2 AlNb-based composite material with excellent room temperature plasticity
Technical Field
The invention relates to a preparation method of a Ti 2 AlNb-based composite material.
Background
The new generation of aircraft has higher thrust-weight ratio of engines, and meets the requirement of long-time high-temperature environment service, while the Ti 2 AlNb alloy has excellent high-temperature performance, higher specific strength and good room-temperature plasticity, and is mainly applied to high-temperature parts on the engines of aerospace aircrafts. However, as an intermetallic compound, the plasticity of the Ti 2 ainb alloy cannot meet the requirements of the new generation of aircrafts, which also limits the wide application of the Ti 2 ainb alloy in the fields of aerospace and automobile engines. In order to further improve the room temperature performance of the Ti 2 AlNb alloy, the ceramic reinforcing phase can be introduced into the matrix alloy by utilizing the characteristics of high strength and high rigidity of the ceramic material through an in-situ autogenous or externally-added method, so that the Ti 2 AlNb-based composite material with excellent performance is obtained.
The discontinuous reinforced metal matrix composite material has the advantages of higher specific strength, higher specific rigidity, higher heat resistance limit and the like compared with the matrix alloy. Japanese scholars Emura et al first introduced in-situ authigenic boride reinforcing phases into Ti 2 AlNb alloys to prepare discontinuous reinforced Ti 2 AlNb-based composites. The reinforcing phase has a very good reinforcing effect, and the high-temperature mechanical property of the Ti 2 AlNb-based composite material is obviously improved; in the research process of reinforcing Ti 2 AlNb-based composite materials by boride, american scholars Cowen and the like find that reducing the size of a reinforcing phase and improving the compactness of the materials are key for improving the comprehensive mechanical properties of the composite materials. However, according to the conventional studies, the strength of the Ti 2 ainb alloy was greatly increased by introducing a high-strength reinforcing phase, and the plasticity was greatly lowered.
Because the difference of melting points of Ti, al and Nb is large, the boiling point of Al element is far lower than that of Nb element, and the phenomena of serious volatilization of Al element (the mass fraction of volatilized burning loss reaches 5% -10%) and serious segregation of Nb element occur in the Ti 2 AlNb-based alloy in the smelting and casting process, the indexes such as the accuracy of the final alloy components, the uniformity of the structure, the compactness of the alloy cast ingot and the like are difficult to ensure. Compared with the traditional smelting method, the powder metallurgy method can obtain a uniform microstructure without segregation phenomenon.
Disclosure of Invention
The invention aims to solve the technical problems of poor reinforcing effect and high room temperature brittleness of a discontinuous reinforced titanium-based composite material, serious segregation and poor tissue uniformity of the traditional smelting technology, and provides a preparation method of a Ti 2 AlNb-based composite material with excellent room temperature plasticity.
The preparation method of the Ti 2 AlNb-based composite material with excellent room temperature plasticity is carried out according to the following steps:
TiB 2 particle powder is used as a reinforcing phase, ti 2 AlNb prealloy powder is used as a matrix alloy, tiB 2 particle powder and Ti 2 AlNb prealloy powder are poured into a ball milling tank together for ball milling and mixing, the mixed powder is packaged in a graphite mold after ball milling is finished, then the graphite mold is placed into a vacuum hot-pressing sintering furnace for vacuumizing to avoid powder oxidation pollution caused by contact with air, sintering is carried out for 1h to 5h under the conditions that the sintering temperature is 1250 ℃ to 1330 ℃ and the sintering pressure is 30MPa to 45MPa, and the TiBw/Ti 2 AlNb-based composite material is obtained after the sintering is finished and then cooled along with the furnace;
The mass of the TiB 2 particle powder is 0.1-0.2% of the sum of the mass of the TiB 2 particle powder and the mass of the Ti 2 AlNb pre-alloy powder.
The TiBw/Ti 2 AlNb-based composite material with excellent room temperature plasticity is prepared by adopting a preparation method of low-energy ball milling and vacuum hot-pressing sintering and combining an in-situ self-generating reaction technology. The formula of in-situ autogenous reaction of Ti and TiB 2 is Ti+TiB 2 =2TiB, firstly, a low-energy ball milling method is adopted to ensure that TiB 2 powder is uniformly adhered on the surfaces of Ti 2 AlNb prealloy powder particles, and reasonable ball milling parameters are selected to ensure that the Ti 2 AlNb powder is not deformed in the powder mixing process, so that better sphericity is maintained; then in-situ self-generating reaction promotes TiBw (TiB whisker) to grow near the surface of the spherical matrix alloy in the hot-press sintering process, so that further growth of crystal grains can be limited, a uniform three-dimensional reticular structure is obtained, the reticular structure has a very good grain boundary strengthening effect, and the TiBw strengthening phase of in-situ self-generating reaction can be connected with adjacent titanium crystal grains like pins to coordinate integral deformation of the material, and can effectively improve the plasticity and toughness of the composite material; the mesh structure can inhibit the growth of crystal grains in the sintering process; the three-dimensional network structure has the characteristic of introducing a ceramic phase into a grain boundary, can achieve the aim of improving the room temperature plasticity of the composite material, and obtains the TiBw/Ti 2 AlNb-based composite material with excellent room temperature performance, wherein the tensile strength is more than 1050MPa, and the elongation is more than 12%.
The invention is based on the design principle of damage tolerance, and improves the room temperature plasticity of the Ti 2 AlNb-based composite material as much as possible while maintaining the same strength, thus obtaining the Ti 2 AlNb-based composite material with excellent strong plasticity matching.
Drawings
FIG. 1 is a low magnification SEM image of a mixed powder (before sintering) after testing a ball mill;
FIG. 2 is a high magnification SEM image of the mixed powder (before sintering) after testing a ball mill;
FIG. 3 is a low magnification SEM image of a TiBw/Ti 2 AlNb-based composite material obtained after completion of test-A sintering;
FIG. 4 is a high magnification SEM image of a TiBw/Ti 2 AlNb-based composite material obtained after completion of test-A sintering;
FIG. 5 is a graph showing the tensile stress-strain at room temperature of TiBw/Ti 2 AlNb-based composite material obtained after completion of the test.
Detailed Description
The first embodiment is as follows: the embodiment is a preparation method of a Ti 2 AlNb-based composite material with excellent room temperature plasticity, which comprises the following steps:
TiB 2 particle powder is used as a reinforcing phase, ti 2 AlNb prealloy powder is used as a matrix alloy, tiB 2 particle powder and Ti 2 AlNb prealloy powder are poured into a ball milling tank together for ball milling and mixing, the mixed powder is packaged in a graphite mold after ball milling is finished, then the graphite mold is placed into a vacuum hot-pressing sintering furnace for vacuumizing to avoid powder oxidation pollution caused by contact with air, sintering is carried out for 1h to 5h under the conditions that the sintering temperature is 1250 ℃ to 1330 ℃ and the sintering pressure is 30MPa to 45MPa, and the TiBw/Ti 2 AlNb-based composite material is obtained after the sintering is finished and then cooled along with the furnace;
The mass of the TiB 2 particle powder is 0.1-0.2% of the sum of the mass of the TiB 2 particle powder and the mass of the Ti 2 AlNb pre-alloy powder.
The second embodiment is as follows: the first difference between this embodiment and the specific embodiment is that: the purity of the TiB 2 granule powder is more than 99.5%. The other is the same as in the first embodiment.
And a third specific embodiment: this embodiment differs from the first or second embodiment in that: the ball milling is carried out on a planetary ball mill. The other embodiments are the same as those of the first or second embodiment.
The specific embodiment IV is as follows: this embodiment differs from one of the first to third embodiments in that: the ball milling rotation speed is 200 rpm-240 rpm. The other is the same as in one of the first to third embodiments.
Fifth embodiment: the fourth difference between this embodiment and the third embodiment is that: the mass ratio of the ball materials is (2-4) 1 during ball milling. The other is the same as in the fourth embodiment.
Specific embodiment six: the fifth difference between this embodiment and the third embodiment is that: the ball milling time is 3-6 h. The other is the same as in the fifth embodiment.
Seventh embodiment: the sixth embodiment differs from the first embodiment in that: the mass of the TiB 2 particle powder is 0.125 percent of the sum of the mass of the TiB 2 particle powder and the mass of the Ti 2 AlNb prealloy powder. The other is the same as in the sixth embodiment.
Eighth embodiment: the present embodiment is different from the seventh embodiment in that: vacuum was applied to a vacuum of 10 - 2 Pa. The other is the same as in the seventh embodiment.
Detailed description nine: this embodiment differs from the eighth embodiment in that: the sintering temperature is 1300 ℃, and the heat preservation time is 2 hours. The other is the same as in the eighth embodiment.
Detailed description ten: this embodiment differs from the ninth embodiment in that: the sintering pressure was 35MPa. The other steps are the same as those in the embodiment nine.
The invention was verified with the following test:
test one: the test is a preparation method of a Ti 2 AlNb-based composite material with excellent room temperature plasticity, and specifically comprises the following steps:
TiB 2 particle powder is used as a reinforcing phase, ti 2 AlNb prealloy powder is used as a matrix alloy, tiB 2 particle powder and Ti 2 AlNb prealloy powder are poured into a ball milling tank together for ball milling and mixing, the mixed powder is packaged in a graphite mold after ball milling is finished, then the graphite mold is placed into a vacuum hot-pressing sintering furnace for vacuumizing to avoid powder oxidation pollution caused by contact with air, sintering is carried out for 2 hours under the conditions of 1300 ℃ and 35MPa of sintering pressure, and cooling is carried out along with the furnace after sintering is finished, so that TiBw/Ti 2 AlNb-based composite material is obtained;
The purity of the TiB 2 granule powder is more than 99.5%, and the average grain diameter is less than or equal to 10 mu m;
The grain diameter of the Ti 2 AlNb pre-alloy powder ranges from 75 mu m to 125 mu m;
The mass of the TiB 2 particle powder is 0.125% of the sum of the mass of the TiB 2 particle powder and the mass of the Ti 2 AlNb pre-alloy powder;
The ball milling rotating speed is 220rpm, the ball milling time is 5h, and the mass ratio of the ball materials is 3:1.
Fig. 1 is a low-magnification SEM image of the mixed powder (before sintering) after ball milling, and fig. 2 is a high-magnification SEM image of the mixed powder (before sintering) after ball milling, from which it can be seen that TiB 2 powder is uniformly adhered to Ti 2 ainb prealloy powder, so that the surface of Ti 2 ainb prealloy powder is no longer smooth, no scattered powder particles are around, the morphology of most Ti 2 ainb powder particles is not changed in the process of low-energy powder mixing, and the nearly spherical morphology is still maintained, so that the ideal mixing effect is achieved.
FIG. 3 is a low-magnification SEM image of a TiBw/Ti 2 AlNb-based composite material obtained after the completion of the test, and FIG. 4 is a high-magnification SEM image of a TiBw/Ti 2 AlNb-based composite material obtained after the completion of the test, wherein the design of a three-dimensional quasi-continuous network structure of the composite material is realized by adopting a preparation method of low-energy ball milling and vacuum hot-pressing sintering to form honeycomb arrangement can be seen from the image; secondly, in-situ autogenous reaction promotes TiBw to grow near the surface of the spherical matrix alloy in the hot-press sintering process, so that further growth of crystal grains can be limited, tiBw at a crystal boundary can be promoted to grow inwards from the crystal boundary, adjacent matrix particles are connected like pins, deformation of all parts is coordinated, and the purpose of improving the room-temperature plasticity of the TiBw/Ti 2 AlNb matrix composite is achieved.
Fig. 5 is a room temperature tensile stress-strain curve of the TiBw/Ti 2 ainb-based composite material obtained after the sintering is completed, and an experiment of room temperature stretching is performed on electronic universal tester equipment, so that the tensile strength of the TiBw/Ti 2 ainb-based composite material is 1055MPa, the plasticity is 14.7%, and the comprehensive improvement of the room temperature tensile strength and the plasticity of the Ti 2 ainb-based composite material is realized.
And (2) testing II: the first difference between this test and the test is: the mass of the TiB 2 particle powder is 0.15 percent of the sum of the mass of the TiB 2 particle powder and the mass of the Ti 2 AlNb prealloy powder. The others are the same as in test one.
The room temperature tensile strength of the obtained network structure TiBw/Ti 2 AlNb-based composite material is 1100MPa, and the elongation rate can reach 13.8%.
And (3) test III: the first difference between this test and the test is: sintering for 2h at 1330 ℃ and 45 MPa. The others are the same as in test one.
The room temperature tensile strength of the obtained network structure TiBw/Ti 2 AlNb-based composite material is 1085MPa, and the elongation rate can reach 15.7%.

Claims (1)

1. A preparation method of a Ti 2 AlNb-based composite material with excellent room temperature plasticity is characterized in that the preparation method of the Ti 2 AlNb-based composite material with excellent room temperature plasticity is carried out according to the following steps:
TiB 2 particle powder is used as a reinforcing phase, ti 2 AlNb prealloy powder is used as a matrix alloy, tiB 2 particle powder and Ti 2 AlNb prealloy powder are poured into a ball milling tank together for ball milling and mixing, the mixed powder is packaged in a graphite mold after ball milling is finished, then the graphite mold is placed into a vacuum hot-pressing sintering furnace for vacuumizing to avoid powder oxidation pollution caused by contact with air, sintering is carried out for 2 hours under the conditions of the sintering temperature of 1330 ℃ and the sintering pressure of 45MPa, and cooling is carried out along with the furnace after sintering is finished, so that TiBw/Ti 2 AlNb-based composite material is obtained;
The room-temperature tensile strength of the TiBw/Ti 2 AlNb-based composite material is 1085MPa, and the elongation is 15.7%;
The purity of the TiB 2 granule powder is more than 99.5%, and the average grain diameter is less than or equal to 10 mu m;
The grain diameter of the Ti 2 AlNb pre-alloy powder ranges from 75 mu m to 125 mu m;
The mass of the TiB 2 particle powder is 0.125% of the sum of the mass of the TiB 2 particle powder and the mass of the Ti 2 AlNb pre-alloy powder;
The ball milling rotating speed is 220rpm, the ball milling time is 5h, and the mass ratio of the ball materials is 3:1.
CN202310150011.7A 2023-02-22 2023-02-22 Ti with excellent room temperature plasticity2Preparation method of AlNb-based composite material Active CN116144968B (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101333607A (en) * 2008-07-31 2008-12-31 哈尔滨工业大学 Process for preparing TiBw/Ti alloy-based composite material
CN109759665A (en) * 2019-03-22 2019-05-17 中山大学 A kind of ceramic/metal connector preparation method of the TiB whisker reinforcement with three-dimensional netted distribution
CN114150238A (en) * 2021-11-26 2022-03-08 中国航发北京航空材料研究院 Ti-Al-Nb-based composite material and preparation method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101333607A (en) * 2008-07-31 2008-12-31 哈尔滨工业大学 Process for preparing TiBw/Ti alloy-based composite material
CN109759665A (en) * 2019-03-22 2019-05-17 中山大学 A kind of ceramic/metal connector preparation method of the TiB whisker reinforcement with three-dimensional netted distribution
CN114150238A (en) * 2021-11-26 2022-03-08 中国航发北京航空材料研究院 Ti-Al-Nb-based composite material and preparation method thereof

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