CN109457132B - TiC prepared through in-situ reactionxMethod for particle-reinforcing Ni (Si) composite material - Google Patents
TiC prepared through in-situ reactionxMethod for particle-reinforcing Ni (Si) composite material Download PDFInfo
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- CN109457132B CN109457132B CN201811519172.4A CN201811519172A CN109457132B CN 109457132 B CN109457132 B CN 109457132B CN 201811519172 A CN201811519172 A CN 201811519172A CN 109457132 B CN109457132 B CN 109457132B
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- 239000002131 composite material Substances 0.000 title claims abstract description 31
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 20
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 52
- 238000000034 method Methods 0.000 claims abstract description 25
- 239000000919 ceramic Substances 0.000 claims abstract description 23
- 229910009817 Ti3SiC2 Inorganic materials 0.000 claims abstract description 22
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000006243 chemical reaction Methods 0.000 claims abstract description 18
- 239000002245 particle Substances 0.000 claims abstract description 18
- 238000010438 heat treatment Methods 0.000 claims abstract description 12
- 238000007731 hot pressing Methods 0.000 claims abstract description 12
- 229910052786 argon Inorganic materials 0.000 claims abstract description 9
- 238000004381 surface treatment Methods 0.000 claims abstract description 3
- 239000002184 metal Substances 0.000 claims description 12
- 229910052751 metal Inorganic materials 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 10
- 230000003014 reinforcing effect Effects 0.000 claims description 8
- 229910052759 nickel Inorganic materials 0.000 claims description 3
- 238000011068 loading method Methods 0.000 claims description 2
- 230000002787 reinforcement Effects 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 10
- 238000002360 preparation method Methods 0.000 abstract description 8
- 239000011156 metal matrix composite Substances 0.000 abstract description 4
- 238000000227 grinding Methods 0.000 abstract description 3
- 238000004140 cleaning Methods 0.000 abstract 1
- 239000000956 alloy Substances 0.000 description 8
- 229910045601 alloy Inorganic materials 0.000 description 8
- 244000137852 Petrea volubilis Species 0.000 description 5
- 239000011159 matrix material Substances 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 239000002243 precursor Substances 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000000280 densification Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000005452 bending Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 238000005049 combustion synthesis Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 230000016507 interphase Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000004506 ultrasonic cleaning Methods 0.000 description 1
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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
- C22C1/058—Mixtures of metal powder with non-metallic powder by reaction sintering (i.e. gasless reaction starting from a mixture of solid metal compounds)
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C19/00—Alloys based on nickel or cobalt
- C22C19/03—Alloys based on nickel or cobalt based on nickel
-
- 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
- C22C32/0052—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 only carbides
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Manufacture Of Alloys Or Alloy Compounds (AREA)
- Ceramic Products (AREA)
Abstract
The invention discloses a method for preparing TiC through in-situ reactionxA method for particle reinforced Ni (Si) composite material, belonging to the technical field of metal matrix composite material preparation. The method first adds Ti3SiC2Grinding and ultrasonically cleaning the ceramic and the metallic nickel, and then carrying out surface treatment on the Ti3SiC2Placing the ceramic and the metallic nickel in a hot pressing furnace, and vacuumizing or protecting the hot pressing furnace by argon; under the vacuum state, the vacuum degree in the hot pressing furnace reaches 10‑2Heating at Pa, heating at a heating rate of 10-15 deg.C/min at a temperature not lower than 1300 deg.C and under a pressure of 0-10MPa for 30-120min to obtain Ti3SiC2TiC prepared by ceramic and metallic nickel in-situ reactionxThe particles reinforce the Ni (Si) composite. The method has simple process and convenient operation, and the TiC prepared by the method isxThe particle reinforced Ni (Si) composite material has the characteristics of high purity, high density and the like.
Description
The technical field is as follows:
the invention belongs to the technical field of metal matrix composite preparation, and particularly relates to TiC prepared through in-situ reactionxA method of particle reinforcing a Ni (Si) composite.
Background art:
TiC has the characteristics of high hardness (32GPa), high melting point (3065 ℃), low density (4.93g/cm3) and the like, and is often used as a reinforcing phase of a metal matrix composite material. The TiC reinforced Ni-based alloy composite material has excellent performanceIs receiving extensive attention from researchers. In the TiC reinforced Ni-based alloy composite material generated in situ, the TiC of a reinforcing phase is firmly combined with a Ni matrix interface, and the particles of the reinforcing phase are fine and are uniformly distributed in the matrix. Many researchers have used different methods to prepare in-situ TiC-Ni based alloy composites. Document 1(mater.sci.eng.a,2010,527:3898) prepares an in-situ 20% TiC-Ni based alloy composite material by a medium frequency induction casting method; document 2(mater.sci.eng.a,2000,280:328) prepares an in-situ TiC-Ni-based alloy composite material by a combustion synthesis method. In addition to the synthesis of TiC reinforced Ni-based alloy composites by in-situ reaction by addition of Ti and C powders, document 3(j. alloy company, 2014,602:53) prepares non-stoichiometric TiC by topological reaction of MAX phase materialsxA reinforced metal matrix composite. However, the above methods all adopt powder materials as precursors, which causes difficulty in eliminating adsorbed gases, requires high-pressure forming in the preparation process, and has lower material density compared with cast alloys. Therefore, a TiC with simple process, convenient operation and high compactness is soughtxThe preparation method of the particle reinforced Ni (Si) composite material has important practical significance.
The invention content is as follows:
the invention aims to provide an in-situ reaction TiC prepared by easy control of process conditions, short reaction time, high purity and high densityxA method of particle reinforcing a Ni (Si) composite. The invention uses bulk Ti3SiC2Ceramic and metallic nickel are used as precursors; prepared TiCxParticle reinforced Ni (Si) composite TiCxVolume of (2)<50％，TiCxThe content of (A) can be determined from Ti in the original proportion3SiC2The contents of ceramic and Ni.
The invention provides a method for preparing TiC through in-situ reactionxThe specific steps of the method for particle-reinforced Ni (Si) composite material are as follows:
(1) the bulk Ti3SiC2Carrying out surface treatment on the ceramic and the metallic nickel, and then treating the treated bulk Ti3SiC2The ceramic and the metallic nickel are arranged in a hot pressing furnace, and the hot pressing furnace is vacuumizedOr argon protection; the bulk Ti3SiC2The volume of the ceramic is less than or equal to the volume of the metallic nickel.
(2) The vacuum degree in the hot pressing furnace reaches 10-2Heating at Pa or under the protection of argon, and keeping the temperature at 1300 ℃ and the pressure of 0-10MPa for 30-120min to ensure that the block Ti3SiC2TiC prepared by ceramic and metal nickel in-situ reactionxThe particles reinforce the Ni (Si) composite.
(3) After the reaction is finished, cooling the autoclave to 200 ℃ under the original vacuum condition or under the protection of argon, and then naturally cooling.
In the step (2), heating to 1300 ℃ at a heating rate of 10-15 ℃/min, and preserving heat for 30-120 min; pressurizing to be within 10MPa at a loading rate of 0.2 kN/min.
Compared with the prior art, the invention has the following technical effects.
1. The raw materials adopted by the invention are simple and need block Ti3SiC2Compared with powder materials, the raw materials of ceramics and commercial metal Ni are cheap and easy to obtain.
2. Simple process and low cost. The invention adopts a block material as a precursor, the preparation process is prepared by in-situ diffusion reaction, and the densification and the reaction process are carried out simultaneously. Compared with the preparation of composite materials from powder materials, the preparation method reduces the processes of powdering, mixing and the like, requires small pressure during densification, and has simple process flow and cost saving.
3. The prepared material has high density and excellent performance. The block material is selected as a precursor, the prepared composite material can reach theoretical density, and the matrix and the reinforced interphase interface are clean, good in wettability and firm in interface combinationxThe particle reinforced Ni (Si) composite material has hardness reaching HV663 and bending strength reaching 1234 MPa.
Description of the drawings:
FIG. 1 shows Ti in the process of the present invention3SiC2TiC prepared under the conditions of the volume ratio of the TiC to Ni being 1:1, the temperature being 1300 ℃, the pressure being 5MPa and the heat preservation being 120minxParticle reinforcementScanning electron microscope photograph of Ni (Si) composite material.
FIG. 2 is TiC prepared by the method of the present inventionxParticle-reinforced ni (si) composite X-ray diffraction patterns.
The specific implementation mode is as follows:
example 1: selecting bulk Ti3SiC2The volume ratio of the ceramic to the metal Ni is 1:1, and the bulk Ti3SiC21000 for ceramic and metal Ni#And (4) after the SiC sand paper is ground and ultrasonically cleaned, putting the mixture into a high-temperature hot pressing furnace, and vacuumizing. When the vacuum degree reaches 5 multiplied by 10-2At Pa, the pressure was increased to 5MPa at a rate of 0.2kN/min while heating at a temperature rise rate of 15 ℃/min. Keeping the temperature at 1300 deg.C and pressure at 5MPa for 120min, cooling to 200 deg.C in the original vacuum condition, and naturally cooling. In-situ reaction to produce compact TiCxThe particles reinforce the Ni (Si) composite.
Example 2: selecting bulk Ti3SiC2The volume ratio of the ceramic to the metal Ni is 1:1, adding Ti3SiC21000 for ceramic and metal Ni#And (3) after grinding and ultrasonic cleaning of SiC sand paper, putting the SiC sand paper into a high-temperature hot pressing furnace, and protecting the SiC sand paper by using argon. Heating at a temperature rise rate of 15 ℃/min while pressurizing to 1MPa at a rate of 0.2 kN/min. Keeping the temperature at 1300 deg.C and pressure at 1MPa for 120min, cooling to 200 deg.C under the protection of argon, and naturally cooling. Preparing compact TiCxThe particles reinforce the Ni (Si) composite.
Example 3: selecting bulk Ti3SiC2The volume ratio of the ceramic to the metal Ni is 1:2, adding Ti3SiC21000 for ceramic and metal Ni#And (4) after the SiC sand paper is ground and the sample is ultrasonically cleaned, putting the sample into a high-temperature hot pressing furnace, and vacuumizing the furnace. When the vacuum degree reaches 5 multiplied by 10-2At Pa, the pressure was increased to 5MPa at a rate of 0.2kN/min while heating at a temperature rise rate of 15 ℃/min. Keeping the temperature at 1300 deg.C and 5MPa for 90min, cooling to 200 deg.C in the original vacuum condition, and naturally cooling. Obtaining compact TiCxThe particles reinforce the Ni (Si) composite.
FIG. 1 is Ti3SiC2The volume ratio of the ceramic to the metal Ni is 1:1, and the scanning electron microscope picture of the composite material is prepared by in-situ reaction under the vacuum conditions of 1300 ℃, 120min and 5 MPa. In the figure, black is the reinforcing phase and white is the matrix, on which a large number of fine, granular reinforcing phases are also distributed. FIG. 2 is Ti3SiC2And the X-ray diffraction spectrum of the composite material prepared when the volume ratio of the ceramic to the metal Ni is 1: 1. Except for Ni and TiCxNo other diffraction peak was observed except for the diffraction peak, and no other reaction phase was formed in the figure.
As can be seen from examples 1, 2 and 3, the present invention utilizes Ti3SiC2Topological reaction between ceramic and metal Ni, in-situ TiC preparationxThe particles reinforce the Ni (Si) composite. The invention has the advantages of simple required equipment, small applied pressure, simple process and easy control.
Claims (2)
1. TiC prepared through in-situ reactionxThe method for particle reinforcement of the Ni (Si) composite material is characterized by comprising the following specific steps:
(1) the bulk Ti3SiC2Carrying out surface treatment on the ceramic and the metallic nickel, and then treating the treated bulk Ti3SiC2The ceramic and the metal nickel are arranged in a hot pressing furnace, and the hot pressing furnace is vacuumized or protected by argon; the bulk Ti3SiC2The volume of the ceramic is less than that of the metallic nickel;
(2) the vacuum degree in the hot pressing furnace reaches 10-2Heating at Pa or under the protection of argon, heating to 1300 ℃ at the heating rate of 10-15 ℃/min, and keeping the temperature at 1300 ℃ and the pressure of 0-10MPa for 30-120min to ensure that the bulk Ti3SiC2The ceramic reacts with the metallic nickel in situ to prepare a TiCx particle reinforced Ni (Si) composite material;
(3) after the reaction is finished, cooling the autoclave to 200 ℃ under the original vacuum condition or under the protection of argon, and then naturally cooling.
2. The method of claim 1TiC prepared through in-situ reactionxA method of particle reinforcing a ni (si) composite characterised in that in step (2) the pressure is increased to within 10MPa at a loading rate of 0.2 kN/min.
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| CN201811519172.4A CN109457132B (en) | 2018-12-12 | 2018-12-12 | TiC prepared through in-situ reactionxMethod for particle-reinforcing Ni (Si) composite material |
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| CN201811519172.4A CN109457132B (en) | 2018-12-12 | 2018-12-12 | TiC prepared through in-situ reactionxMethod for particle-reinforcing Ni (Si) composite material |
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| CN109457132B true CN109457132B (en) | 2021-01-29 |
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Non-Patent Citations (4)
| Title |
|---|
| Cr3C2-Ni-Ti3SiC2 新型减摩复合材料的高温摩擦学行为;李立鑫等;《中国有色金属学报》;20140228;第24卷(第2期);第424-430页 * |
| Microstructure and mechanical strength of diffusion-bonded Ti3SiC2/Ni joints;X.H YIN et al.;《J. Mater. Res》;20060930;第21卷(第9期);第2415-2421页 * |
| Nickel assisted sintering of Ti3SiC2 powder under pressureless conditions;Bharat Bhooshan Panigrahia，et al.;《Journal of Alloys and Compounds》;20101231(第505期);第337-342页 * |
| Processing and microstructure of Ti3SiC2 /M (M=Ni or Co) composites;H.Li et al.;《Materials letters》;20051231(第59期);第2647-2649页 * |
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