CN115341113B - Method for synthesizing MAX phase metal ceramic material in situ - Google Patents
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- 238000000034 method Methods 0.000 title claims abstract description 29
- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 17
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 17
- 239000002184 metal Substances 0.000 title claims abstract description 17
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 16
- 230000002194 synthesizing effect Effects 0.000 title claims abstract description 11
- 239000000843 powder Substances 0.000 claims abstract description 31
- 239000000463 material Substances 0.000 claims abstract description 23
- 238000000227 grinding Methods 0.000 claims abstract description 21
- 238000005245 sintering Methods 0.000 claims abstract description 20
- 238000000498 ball milling Methods 0.000 claims abstract description 14
- 239000002994 raw material Substances 0.000 claims abstract description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 13
- 239000010439 graphite Substances 0.000 claims abstract description 13
- 238000010438 heat treatment Methods 0.000 claims abstract description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000011812 mixed powder Substances 0.000 claims abstract description 12
- 239000011268 mixed slurry Substances 0.000 claims abstract description 11
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 8
- 238000007731 hot pressing Methods 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 230000015572 biosynthetic process Effects 0.000 claims description 9
- 239000011195 cermet Substances 0.000 claims description 9
- 238000003786 synthesis reaction Methods 0.000 claims description 9
- 238000004321 preservation Methods 0.000 claims description 3
- 238000011049 filling Methods 0.000 claims description 2
- 238000005516 engineering process Methods 0.000 abstract description 4
- 230000007797 corrosion Effects 0.000 abstract description 3
- 238000005260 corrosion Methods 0.000 abstract description 3
- 239000013078 crystal Substances 0.000 abstract description 2
- 238000005728 strengthening Methods 0.000 abstract description 2
- 239000002131 composite material Substances 0.000 abstract 1
- 239000012071 phase Substances 0.000 description 24
- 238000002360 preparation method Methods 0.000 description 4
- 238000005452 bending Methods 0.000 description 3
- 238000005229 chemical vapour deposition Methods 0.000 description 3
- 238000009792 diffusion process Methods 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 238000001308 synthesis method Methods 0.000 description 2
- 229920002994 synthetic fiber Polymers 0.000 description 2
- 229910010038 TiAl Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000001010 compromised effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 230000000877 morphologic effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000001272 pressureless sintering Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000002490 spark plasma sintering Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 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
- C22C1/051—Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor
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- 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
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
-
- 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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
- C22C29/02—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides
- C22C29/06—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds
- C22C29/067—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds comprising a particular metallic binder
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
- C22C29/02—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides
- C22C29/06—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds
- C22C29/10—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds based on titanium carbide
-
- 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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
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Abstract
The invention discloses a method for synthesizing MAX phase metal ceramic material in situ, which comprises the steps of mixing Ti, si, tiC, al four kinds of powder according to 1:1.2: (2.0-2.4): mixing the mixed raw material powder, the alumina grinding ball and the absolute ethyl alcohol in a molar ratio of 0.3, putting the mixed raw material powder, the alumina grinding ball and the absolute ethyl alcohol into a grinding tank, putting the grinding tank into a planetary ball mill for ball milling to obtain mixed slurry, drying to obtain mixed powder, putting the mixed powder into a graphite mold, putting the graphite mold into a rapid hot pressing furnace, heating to 1250-1450 ℃, preserving heat, sintering for 5-15 minutes, and finally cooling along with the furnace to obtain the composite material. The material prepared by the method has the advantages of high strength, good toughness, good conductivity, excellent self-lubricating property, high temperature resistance, good corrosion resistance and the like, and can meet the application requirements under severe extreme environments. Compared with the traditional hot-pressed sintering technology, the method can effectively prevent the crystal grains from growing up, plays a role in strengthening fine grains, and improves the strength and toughness of the material.
Description
Technical Field
The invention belongs to the technical field of MAX phase synthesis, and particularly relates to a method for synthesizing MAX phase metal ceramic materials in situ.
Background
Ti 3 SiC 2 Ternary lamellar compounds are the most widely studied and most representative M n+1 AX n One of the phase materials (where M is a transition metal, A is a III or IV main group element, X is C or N) because of its unique propertiesBut are of interest to the materials community. Ti (Ti) 3 SiC 2 The ceramic material has excellent heat conductivity, electric conductivity and processability, and also has high yield strength, high melting point, high thermal stability and good oxidation resistance. Ti (Ti) 3 SiC 2 Also has very low friction coefficient, and can be matched with the existing lubricant graphite and MoS 2 Is comparable to, and Ti 3 SiC 2 The material has more excellent high temperature resistance, corrosion resistance, mechanical property and other properties, can meet the use requirements in harsh environments such as ultra-high temperature, supersonic speed, corrosive atmosphere and the like, and has wide application prospect in the field of self-lubricating materials.
Currently, for Ti 3 SiC 2 There are many reports on the preparation method of the metal ceramic. Chemical Vapor Deposition (CVD) is the earliest method for preparing Ti 3 SiC 2 But Ti prepared by CVD method 3 SiC 2 The purity of the material cannot be ensured, and only a thin layer of material can be prepared by depositing on the surface; hot pressed sintering is an effective method for preparing Ti 3 SiC 2 However, the hot-pressed sintering needs to rely on the diffusion synthesis of elements, so that the sintering time is longer, the cost is higher, the phenomenon of abnormal growth of grains due to overlong heat preservation time is easy to occur, and the prepared Ti is prepared 3 SiC 2 Performance is compromised; pre-pressed sintering is also a method for preparing Ti 3 SiC 2 The pressureless sintering also depends on diffusion bonding of elements for a long time, takes longer time and has lower efficiency when lacking pressure as sintering driving force; self-propagating sintering methods have also been reported for the preparation of Ti 3 SiC 2 The synthesis method has the advantages of high speed, short reaction time, energy conservation and high efficiency, but in the experimental process, the synthesis temperature is difficult to control, the reaction degree is difficult to grasp, and SiC, tiC and intermediate phase products are often associated, so that the purity of the synthesized materials is low. In conclusion, ti reported currently 3 SiC 2 In the synthesis process of (2), the problems of lower synthesis purity, higher cost and the like generally exist, so a rapid Ti synthesis method is developed 3 SiC 2 The preparation method of (2) is necessary.
Disclosure of Invention
The invention aims to solve the problems of Ti in the prior art 3 SiC 2 The defects in the synthesis process are overcome, and a method for synthesizing MAX phase metal ceramic material in situ is provided.
Technical proposal
A method for synthesizing MAX phase metal ceramic material in situ, comprising the following steps:
(1) Ti, si, tiC, al four powders were mixed according to 1:1.2: (2.0-2.4): mixing at a molar ratio of 0.3 to obtain mixed raw material powder, placing the mixed raw material powder, an alumina grinding ball and absolute ethyl alcohol into a grinding tank, and then placing the grinding tank into a planetary ball mill for ball milling to obtain mixed slurry;
(2) Drying the mixed slurry to obtain mixed powder;
(3) And (3) filling the mixed powder into a graphite mold, then placing the graphite mold into a rapid hot pressing furnace, heating to 1250-1450 ℃, preserving heat, sintering for 5-15 minutes, and then cooling along with the furnace to obtain the MAX phase metal ceramic material.
Further, in the step (1), the mass ratio of the mixed raw material powder, the alumina grinding ball and the absolute ethyl alcohol is 1:5 (5-10).
Further, in the step (1), the ball milling time is 240-480 minutes, and the rotating speed is 180-240 revolutions per minute.
Further, in the step (2), the drying temperature is 40-50 ℃.
Further, in the step (3), the temperature rising rate is 20 to 100 ℃/min.
Further, in the step (3), the sintering pressure is 10 to 30MPa.
The invention has the beneficial effects that:
1) The invention provides a method for synthesizing MAX phase metal ceramic material in situ, which adopts a small amount of Al powder as sintering aid, and the Al powder is changed into liquid phase at high temperature, so that the diffusion among elements is promoted by good fluidity and effectiveness, and the efficiency of in situ reaction is improved.
2) The invention adopts the rapid hot-pressing sintering technology, has lower sintering temperature and short heat preservation time, greatly shortens the production period,and can effectively inhibit Ti from being generated in the in-situ synthesis process 5 Si 3 、TiAl、Ti 3 Brittleness of Al and other impurities relative to mechanical properties of the synthetic material, and simultaneously ensures Ti 3 SiC 2 The material does not decompose at high temperatures.
3) Ti prepared by the method of the invention 3 SiC 2 The material has the advantages of high strength, good toughness, good conductivity, excellent self-lubricating property, high temperature resistance, good corrosion resistance and the like, and can meet the application requirements under severe extreme environments.
4) Compared with the spark plasma sintering technology, the method has the advantages that the cost is greatly reduced, and meanwhile, the high-efficiency production efficiency and the densification of the synthetic material can be ensured; compared with the traditional hot-pressed sintering technology, the method can effectively prevent the crystal grains from growing up, plays a role in strengthening fine grains, and improves the strength and toughness of the material.
5) The method has low cost and is expected to realize batch production of MAX phase materials.
Drawings
FIG. 1 is an XRD pattern of a MAX phase cermet material prepared in example 2;
FIG. 2 is a scanning electron microscope image of the MAX phase cermet material prepared in example 2.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings, and all other embodiments obtained by those skilled in the art without making any inventive effort are within the scope of the present invention.
Example 1
A method for synthesizing MAX phase metal ceramic material in situ, comprising the following steps:
(1) Mixing 11.18g of Ti powder, 3.91gSi powder, 13.97g of TiC powder and 0.94g of Al powder to obtain mixed raw material powder, putting the mixed raw material powder, 150g of alumina grinding balls and 150g of absolute ethyl alcohol into a grinding tank, putting the grinding tank into a planetary ball mill for ball milling, setting the ball milling speed to 240 r/min, and carrying out ball milling for 6 hours to obtain mixed slurry;
(2) Drying the mixed slurry at 50 ℃ until the absolute ethyl alcohol is completely volatilized, so as to obtain mixed powder;
(3) Putting the mixed powder into a graphite mould with the diameter of 45mm, then putting the graphite mould into a rapid hot pressing furnace, firstly raising the temperature to 1000 ℃ at the heating rate of 100 ℃/min, then raising the temperature to 1250 ℃ at the heating rate of 50 ℃/min, preserving the heat for 5 min, keeping the sintering pressure at 10MPa, starting a pressurizing program in the heating process, keeping the pressure for 5 min, and cooling along with the furnace after the heat-preserving pressurizing program is finished to obtain the MAX phase metal ceramic material Ti 3 SiC 2 。
The relative density, bending strength, fracture toughness and Vickers hardness of the MAX phase cermet material are measured to be 98.57 +/-0.24%, 1089.73 +/-52.72 MPa and 8.78+/-0.69 MPa-m respectively 1/2 ，801.12±24.38HV。
Example 2
A method for synthesizing MAX phase metal ceramic material in situ, comprising the following steps:
(1) Mixing 10.45g of Ti powder, 3.67g of gSi powder, 15.02g of TiC powder and 0.88g of Al powder to obtain mixed raw material powder, putting the mixed raw material powder, 150g of alumina grinding balls and 150g of absolute ethyl alcohol into a grinding tank, putting the grinding tank into a planetary ball mill for ball milling, setting the ball milling speed to 200 r/min, and carrying out ball milling for 8 hours to obtain mixed slurry;
(2) Drying the mixed slurry at 45 ℃ until the absolute ethyl alcohol is completely volatilized, so as to obtain mixed powder;
(3) Putting the mixed powder into a graphite mould with the diameter of 45mm, then putting the graphite mould into a rapid hot pressing furnace, firstly raising the temperature to 1000 ℃ at the heating rate of 100 ℃/min, then raising the temperature to 1350 ℃ at the heating rate of 50 ℃/min, preserving the heat for 5 min, keeping the sintering pressure at 30MPa, starting a pressurizing program in the heating process, maintaining the pressure for 10 min, and cooling along with the furnace after the heat-preserving pressurizing program is finished to obtain the MAX phase metal ceramic material Ti 3 SiC 2 。
The relative density, bending strength, fracture toughness and Vickers hardness of the MAX phase cermet material are respectively 99.27+/-0.14%, 1357.53 +/-78.39 MPa and 12.34+/-0.97 MPa-m 1/2 ，889.75±35.86HV。
FIG. 1 is a schematic illustration of the preparation of example 2XRD pattern of MAX phase cermet material. As can be seen from FIG. 1, in situ synthesized Ti 3 SiC 2 The material has very high purity, and almost no other impurity phases are detected in the sample after sintering.
FIG. 2 is a scanning electron microscope image of the MAX phase cermet material prepared in example 2. As can be seen from FIG. 2, the almost entire distribution of the cross section of the synthesized sample is lath-shaped grains, which are uniform and fine and conform to Ti 3 SiC 2 The morphological characteristics of the obtained product also show that the synthesized sample has high purity and mechanical properties.
Example 3
A method for synthesizing MAX phase metal ceramic material in situ, comprising the following steps:
(1) Mixing 10.01g of Ti powder, 3.50g gSi powder, 15.64g of TiC powder and 0.84g of Al powder to obtain mixed raw material powder, putting the mixed raw material powder, 150g of alumina grinding balls and 150g of absolute ethyl alcohol into a grinding tank, putting the grinding tank into a planetary ball mill for ball milling, setting the ball milling speed to be 200 r/min, and carrying out ball milling for 6 hours to obtain mixed slurry;
(2) Drying the mixed slurry at 50 ℃ until the absolute ethyl alcohol is completely volatilized, so as to obtain mixed powder;
(3) Putting the mixed powder into a graphite mould with the diameter of 45mm, then putting the graphite mould into a rapid hot pressing furnace, firstly raising the temperature to 1000 ℃ at the heating rate of 100 ℃/min, then raising the temperature to 1450 ℃ at the heating rate of 50 ℃/min, preserving the temperature for 10 min, keeping the sintering pressure at 20MPa, starting a pressurizing program in the heating process, keeping the pressure for 5 min, and cooling along with the furnace after the heat-preserving pressurizing program is finished to obtain the MAX phase metal ceramic material Ti 3 SiC 2 。
The relative density, bending strength, fracture toughness and Vickers hardness of the MAX phase cermet material are measured to be 98.12 +/-0.21%, 987.49 +/-74.43 MPa and 9.05+/-0.49 MPa-m respectively 1/2 ，721.13±64.39HV。
Claims (5)
1. A method for synthesizing MAX phase metal ceramic material in situ, which is characterized by comprising the following steps:
(1) Ti, si, tiC, al four powders were mixed according to 1:1.2: (2.0 to 2.4): mixing at a molar ratio of 0.3 to obtain mixed raw material powder, placing the mixed raw material powder, an alumina grinding ball and absolute ethyl alcohol into a grinding tank, and then placing the grinding tank into a planetary ball mill for ball milling to obtain mixed slurry;
(2) Drying the mixed slurry to obtain mixed powder;
(3) Filling the mixed powder into a graphite mold, then placing the graphite mold into a rapid hot pressing furnace, heating to 1250-1450 ℃, carrying out heat preservation and sintering for 5-15 minutes, and then cooling along with the furnace to obtain a MAX phase metal ceramic material;
in the step (3), the sintering pressure is 10-30 MPa.
2. The method of in-situ synthesis of MAX phase cermet material according to claim 1, wherein in step (1), the mass ratio of the mixed raw material powder, alumina grinding balls and absolute ethanol is 1:5 (5-10).
3. The method of in-situ synthesis of MAX phase cermet material according to claim 1, wherein in step (1), the ball milling time is 240-480 minutes and the rotational speed is 180-240 rpm.
4. The method of claim 1, wherein in step (2), the drying temperature is 40-50 ℃.
5. The method of claim 1, wherein in step (3), the heating rate is 20-100 ℃/min.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1800100A (en) * | 2006-01-12 | 2006-07-12 | 上海大学 | Ceramet Ti3SiC2 powder preparation method |
| JP2008213240A (en) * | 2007-03-01 | 2008-09-18 | National Institute Of Advanced Industrial & Technology | Manufacturing method of alumina ceramic sintered compact and alumina ceramic sintered compact |
| CN102992765A (en) * | 2012-11-09 | 2013-03-27 | 航天材料及工艺研究所 | Preparation method of tungsten-doped titanium-silicon-aluminum-carbon ceramic block body material |
| CN109666815A (en) * | 2018-12-28 | 2019-04-23 | 西安交通大学 | A kind of MAX phase enhances the preparation method and applications of nickel-base high-temperature lubricating composite |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1800100A (en) * | 2006-01-12 | 2006-07-12 | 上海大学 | Ceramet Ti3SiC2 powder preparation method |
| JP2008213240A (en) * | 2007-03-01 | 2008-09-18 | National Institute Of Advanced Industrial & Technology | Manufacturing method of alumina ceramic sintered compact and alumina ceramic sintered compact |
| CN102992765A (en) * | 2012-11-09 | 2013-03-27 | 航天材料及工艺研究所 | Preparation method of tungsten-doped titanium-silicon-aluminum-carbon ceramic block body material |
| CN109666815A (en) * | 2018-12-28 | 2019-04-23 | 西安交通大学 | A kind of MAX phase enhances the preparation method and applications of nickel-base high-temperature lubricating composite |
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