CN115627403B - High-toughness lubrication integrated high-entropy ceramic matrix composite material and preparation method thereof - Google Patents
High-toughness lubrication integrated high-entropy ceramic matrix composite material and preparation method thereof Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 48
- 239000011153 ceramic matrix composite Substances 0.000 title claims abstract description 23
- 238000005461 lubrication Methods 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000000919 ceramic Substances 0.000 claims description 26
- 238000005245 sintering Methods 0.000 claims description 22
- 239000000843 powder Substances 0.000 claims description 17
- 238000010438 heat treatment Methods 0.000 claims description 16
- 239000011812 mixed powder Substances 0.000 claims description 15
- 229910010293 ceramic material Inorganic materials 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 13
- 239000000203 mixture Substances 0.000 claims description 11
- 238000002156 mixing Methods 0.000 claims description 10
- 239000002994 raw material Substances 0.000 claims description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 229910002804 graphite Inorganic materials 0.000 claims description 6
- 239000010439 graphite Substances 0.000 claims description 6
- 239000011159 matrix material Substances 0.000 claims description 6
- 238000007873 sieving Methods 0.000 claims description 6
- 238000000713 high-energy ball milling Methods 0.000 claims description 3
- 238000002490 spark plasma sintering Methods 0.000 claims description 3
- 229910052715 tantalum Inorganic materials 0.000 claims description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 abstract description 10
- 239000004332 silver Substances 0.000 abstract description 10
- 229910052709 silver Inorganic materials 0.000 abstract description 10
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 abstract description 6
- 230000001050 lubricating effect Effects 0.000 abstract description 6
- 229910052750 molybdenum Inorganic materials 0.000 abstract description 6
- 239000011733 molybdenum Substances 0.000 abstract description 6
- 230000001105 regulatory effect Effects 0.000 abstract description 6
- 239000006104 solid solution Substances 0.000 abstract description 4
- 230000001276 controlling effect Effects 0.000 abstract description 3
- 239000002131 composite material Substances 0.000 abstract 1
- 238000012360 testing method Methods 0.000 description 6
- 238000001816 cooling Methods 0.000 description 4
- 238000011049 filling Methods 0.000 description 4
- 239000007787 solid Substances 0.000 description 3
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- OCKGFTQIICXDQW-ZEQRLZLVSA-N 5-[(1r)-1-hydroxy-2-[4-[(2r)-2-hydroxy-2-(4-methyl-1-oxo-3h-2-benzofuran-5-yl)ethyl]piperazin-1-yl]ethyl]-4-methyl-3h-2-benzofuran-1-one Chemical compound C1=C2C(=O)OCC2=C(C)C([C@@H](O)CN2CCN(CC2)C[C@H](O)C2=CC=C3C(=O)OCC3=C2C)=C1 OCKGFTQIICXDQW-ZEQRLZLVSA-N 0.000 description 1
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000007373 indentation Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
Classifications
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- 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
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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
- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
-
- 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
- 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
-
- 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
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
- B22F2003/1051—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding by electric discharge
-
- 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
Abstract
The invention relates to a high-toughness lubrication integrated high-entropy ceramic matrix composite material which is in a block shape and comprises (Hf) 0.2 Mo 0.4 Nb 0.2 Ta 0.2 Ti 0.2 ) C-xAg, x=3 to 22. The invention also discloses a preparation method of the composite material. The silver-containing high-entropy carbide ceramic matrix composite material with complete molybdenum solid solution is obtained by regulating and controlling material components, microstructure and preparation process based on the concept of high entropy, and the silver-containing high-entropy carbide ceramic matrix composite material has excellent fracture toughness and lubricating property in a wide temperature range and is particularly suitable for special workpieces requiring higher toughness under extremely severe working conditions such as high temperature and the like while maintaining lower friction and wear.
Description
Technical Field
The invention relates to the technical field of high-entropy materials, in particular to a high-toughness lubrication integrated high-entropy ceramic matrix composite material and a preparation method thereof.
Background
With the rapid development of tip technologies such as hypersonic aircrafts, aeroengines and the like in China, service conditions of hot-end moving parts are more and more severe, and development of solid lubricating materials with excellent mechanical properties and lubricating properties at high temperature is urgently needed. At present, although the traditional ceramic-based solid lubricating material can meet the use requirements under partial high-temperature working conditions, the bottleneck problems of high friction coefficient, high wear rate and poor fracture toughness are still faced. Therefore, the development of the high-toughness and lubrication integrated high-performance ceramic matrix composite material has important significance.
In recent years, high-entropy materials which are emerging due to novel 'high-entropy concept' are providing important scientific revenues for the leading edge field due to a plurality of novel characteristics. With the continuous and deep research on high-entropy materials, high-entropy carbide ceramics are favored by researchers due to the unique composition, microstructure, good mechanical properties and the like. At present, the high-entropy carbide ceramic is mainly researched on preparation, mechanical properties and thermophysical properties, and related tribological properties are rarely researched.
Disclosure of Invention
The invention aims to solve the technical problem of providing a high-toughness and lubrication integrated high-entropy ceramic matrix composite material with excellent fracture toughness and lubrication performance in a wide temperature range.
The invention aims to provide a preparation method of the high-toughness lubrication integrated high-entropy ceramic matrix composite.
In order to solve the problems, the high-toughness lubrication integrated high-entropy ceramic matrix composite material provided by the invention is characterized in that: the material is in the form of a block of the composition (Hf 0.2 Mo 0.4 Nb 0.2 Ta 0.2 Ti 0.2 )C- xAg，x=3~22。
The preparation method of the high-toughness lubrication integrated high-entropy ceramic matrix composite material is characterized by comprising the following steps of: the method comprises the steps of mixing 68.02-84.58% by mass of (Hf) 0.2 Mo 0.2 Nb 0.2 Ta 0.2 Ti 0.2 ) Placing the C high-entropy ceramic powder, 9.98-12.42% of Mo powder and 3-22% of Ag powder in a ball mill, adding absolute ethyl alcohol according to 10-50% of the mass of the mixed raw materials, uniformly mixing, drying, and sieving to obtain mixed powder with the particle size of 0.10-25 mu m; and filling the mixed powder into a graphite die, and sintering by spark plasma to obtain the high-toughness lubrication integrated high-entropy ceramic matrix material.
Said (Hf) 0.2 Mo 0.2 Nb 0.2 Ta 0.2 Ti 0.2 ) The high-entropy ceramic powder is prepared by the following steps: the weight percentage of the components is calculated according to the mass percentage,21.5% HfO 2 15.0% MoO 3 13.6% Nb 2 O 5 22.4% Ta 2 O 5 TiO 8.0% 2 Mixing with 19.5% of graphite powder uniformly, and sintering under the conditions that the vacuum degree is lower than 3 Pa, the average heating speed is 40-80 ℃/min, the sintering temperature is 1700 ℃, the pressure is 10 MPa, and the temperature is kept for 15 min to obtain a high-entropy ceramic material; the high-entropy ceramic material is prepared by high-energy ball milling (Hf) with the particle size of 0.10-3 mu m 0.2 Mo 0.2 Nb 0.2 Ta 0.2 Ti 0.2 ) And C, high-entropy ceramic powder.
The spark plasma sintering process is that mixed powder is heated to 1550-1650 ℃ at a faster rate, and is kept for 5-12 min under the pressure of 2-10 MPa; then rapidly heating to 1750-1900 ℃, and preserving heat for 5-15 min under the pressure of 10-20 MPa; the vacuum degree in the whole sintering process is lower than 1 Pa, and the average heating speed is 30-60 ℃/min.
Compared with the prior art, the invention has the following advantages:
1. the invention is based on the concept of high entropy, and by regulating and controlling the material components, the microstructure and the preparation process, on one hand, the fracture toughness can be improved by utilizing the added second phase, and on the other hand, the invention can realize cooperative lubrication by compounding with the self-lubricating property of the high entropy ceramic, thereby breaking through the performance bottleneck of the traditional ceramic matrix composite material and obtaining the high-toughness lubrication integrated high entropy ceramic matrix composite material.
2. According to the invention, the molybdenum and silver contents of the high-entropy ceramic material are regulated and controlled for the first time, and a proper preparation process is selected, so that the high-toughness lubrication integrated high-entropy ceramic matrix composite material is obtained through solid solution reaction in the high-temperature preparation process. As can be seen from FIG. 1, the high-entropy ceramic matrix composite material prepared by the invention consists of high-entropy ceramic and silver phases.
3. The invention is based on the fact that part of silver is dissolved in the high-entropy carbide ceramic in a solid way, and the controllable preparation of carbide high-entropy ceramic material with higher sintering temperature (the common sintering temperature is 2000 ℃ or even higher) doped with low-melting-point silver (the melting point is about 960 ℃) is realized for the first time, so that a new way is provided for preparing the material with larger difference of melting points of all components.
4. The invention can effectively refine grains by regulating the contents of molybdenum and silver (the invention is 1.0 mu m, compared with (Hf) 0.2 Mo 0.2 Nb 0.2 Ta 0.2 Ti 0.2 ) C is reduced by more than 5 times), and the prepared material has excellent fracture toughness and lubricating property in a wide temperature range. The fracture toughness can reach 4.9 Mpam at maximum 1/2 The wear rate is as low as 10 -7 mm 3 The Nm level, lubrication in a wide temperature range can be realized, and the friction coefficient is as low as about 0.35, so that the high-toughness lubrication integration of the high-entropy ceramic matrix composite material is realized.
[ Density and mechanical Properties ]
The density of the material was measured using archimedes principle. The test result shows that the relative density of the prepared block material is 98.0-99.4%.
The fracture toughness of the material is tested by adopting an indentation method, and the testing conditions are as follows: load 5 kg, load duration 10 s. Test results show that the fracture toughness of the prepared block material is 4.4-4.9 Mpam 1/2 。
[ atmospheric tribological Properties ]
The friction and wear test is evaluated by adopting an HT-1000 tester, and the dual ball is Al 2 O 3 The ceramic had a load of 5N, a sliding linear velocity of 0.10 m/s, a friction radius of 4 mm, a stroke of 200 m, a test temperature of 25 ℃, 300 ℃ and 600 ℃, and a coefficient of friction and wear rate of 3 test averages. Experimental results show that the prepared high-entropy ceramic material has excellent tribological properties in a wide temperature range: the coefficient of friction (as shown in Table 1) was as low as 0.35 over a wide temperature range with a wear rate of 10 -7 ~10 -6 mm 3 On the order of/Nm, in particular at 300℃compared with (Hf) 0.2 Mo 0.2 Nb 0.2 Ta 0.2 Ti 0.2 ) C, the friction coefficient of the high-entropy ceramic material prepared by the invention is reduced by 70%; the abrasion rate is reduced by more than 5 times.
Table 1: the high-entropy ceramic block material and Al of the invention 2 O 3 Coefficient of friction of ceramic ball pair
5. The invention can effectively reduce the sintering temperature and pressure of the high-entropy carbide ceramic material by regulating and controlling the content of molybdenum and silver, compared with (Hf) 0.2 Mo 0.2 Nb 0.2 Ta 0.2 Ti 0.2 ) The sintering temperature and the sintering pressure of the C high-entropy carbide ceramic material are respectively reduced by 100-250 ℃ and 20-30 MPa, so that the preparation of the carbide high-entropy carbide ceramic material at low temperature and low pressure is realized.
6. The preparation process is simple, the microstructure and the performance of the material can be regulated and controlled by adjusting the formula and the process parameters, and the obtained high-entropy material can be applied under extremely severe working conditions such as high temperature and the like.
Drawings
The following describes the embodiments of the present invention in further detail with reference to the drawings.
FIG. 1 shows the results of the process of example 1 and example 2 (Hf 0.2 Mo 0.4 Nb 0.2 Ta 0.2 Ti 0.2 ) C-3Ag and (Hf) 0.2 Mo 0.4 Nb 0.2 Ta 0.2 Ti 0.2 ) X-ray diffraction pattern of C-10 Ag.
FIG. 2 shows the composition of example 3 of the present invention (Hf 0.2 Mo 0.4 Nb 0.2 Ta 0.2 Ti 0.2 ) Fracture morphology of the C-22Ag high-entropy ceramic block.
FIG. 3 shows a sample of the composition (Hf) prepared in example 3 of the present invention 0.2 Mo 0.4 Nb 0.2 Ta 0.2 Ti 0.2 ) Coefficient of friction of C-22Ag at 300 ℃.
Detailed Description
A high-toughness lubricating integrated high-entropy ceramic matrix composite material is in the form of block and has the composition (Hf) 0.2 Mo 0.4 Nb 0.2 Ta 0.2 Ti 0.2 )C- xAg，x=3~22。
The preparation method comprises the following steps: 68.02 to 84.58 percent (Hf) of raw materials based on the mass percentage (g/g) 0.2 Mo 0.2 Nb 0.2 Ta 0.2 Ti 0.2 ) Placing C high-entropy ceramic powder, 9.98-12.42% of Mo powder and 3-22% of Ag powderAnd adding absolute ethyl alcohol in the ball mill according to 10-50% of the mass of the mixed raw materials, uniformly mixing, drying and sieving to obtain mixed powder with the particle size of 0.10-25 mu m. Filling the mixed powder into a graphite die for spark plasma sintering, and firstly heating the mixed powder to 1550-1650 ℃ at a relatively high speed, and preserving heat for 5-12 min under the pressure of 2-10 MPa; then rapidly heating to 1750-1900 ℃, and preserving heat for 5-15 min under the pressure of 10-20 MPa; the vacuum degree in the whole sintering process is lower than 1 Pa, and the average heating speed is 30-60 ℃/min. And cooling along with the furnace after the process is finished to obtain the high-toughness lubrication integrated high-entropy ceramic matrix block material.
Wherein: (Hf) 0.2 Mo 0.2 Nb 0.2 Ta 0.2 Ti 0.2 ) The high-entropy ceramic powder is prepared by the following steps: 21.5% HfO based on mass percent (g/g) 2 15.0% MoO 3 13.6% Nb 2 O 5 22.4% Ta 2 O 5 TiO 8.0% 2 Mixing with 19.5% of graphite powder uniformly, and sintering under the conditions that the vacuum degree is lower than 3 Pa, the average heating speed is 40-80 ℃/min, the sintering temperature is 1700 ℃, the pressure is 10 MPa, and the temperature is kept for 15 min to obtain a high-entropy ceramic material; the high-entropy ceramic material is prepared by high-energy ball milling (Hf) with the particle size of 0.10-3 mu m 0.2 Mo 0.2 Nb 0.2 Ta 0.2 Ti 0.2 ) And C, high-entropy ceramic powder.
Example 1A high-toughness lubrication-integrated high-entropy ceramic matrix composite, which is in the form of a block, having a composition of (Hf 0.2 Mo 0.4 Nb 0.2 Ta 0.2 Ti 0.2 )C- 3Ag。
The preparation method comprises the following steps: first, 84.58 g (Hf) 0.2 Mo 0.2 Nb 0.2 Ta 0.2 Ti 0.2 ) C,12.42 g Mo and 3 g Ag powder, and placing the raw materials into a ball mill; adding 10g of absolute ethyl alcohol into the mixed raw materials, uniformly mixing, and drying and sieving to obtain mixed powder with the particle size of 0.10-25 mu m; filling the mixed powder into a graphite mold, heating to 1650 ℃ in a discharge plasma sintering furnace at a high speed, and preserving heat for 5 min under the pressure of 10 MPa; then rapidly heating to 1900 ℃, and preserving heat for 5 min, wherein the pressure is 20 MPa. Finishing the wholeThe vacuum degree in the sintering process is lower than 1 Pa, and the average temperature rising speed is 60 ℃/min. And cooling along with the furnace to obtain the high-toughness lubrication integrated high-entropy ceramic matrix block material.
The phase composition of the material is shown in figure 1. As can be seen from fig. 1, the silver-containing high-entropy ceramic matrix composite material with complete molybdenum solid solution was successfully prepared.
Example 2A high-toughness lubrication-integrated high-entropy ceramic matrix composite, which is in the form of a block, having a composition of (Hf 0.2 Mo 0.4 Nb 0.2 Ta 0.2 Ti 0.2 )C-10Ag。
The preparation method comprises the following steps: first, 78.48 and g (Hf) 0.2 Mo 0.2 Nb 0.2 Ta 0.2 Ti 0.2 ) C,11.52 g of Mo and 10g of Ag powder, and placing the raw materials into a ball mill; adding 30g of absolute ethyl alcohol into the mixed raw materials, uniformly mixing, and drying and sieving to obtain mixed powder with the particle size of 0.10-25 mu m; filling the mixed powder into a graphite mold, heating to 1600 ℃ in a discharge plasma sintering furnace at a high speed, and preserving heat for 8 min under the pressure of 6 MPa; then rapidly heating to 1825 ℃, and preserving heat for 10 min, wherein the pressure is 15 MPa. The vacuum degree is lower than 1 Pa in the whole sintering process, and the average heating speed is 45 ℃/min. And cooling along with the furnace to obtain the high-toughness lubrication integrated high-entropy ceramic matrix block material.
The phase composition of the material is shown in figure 1. As can be seen from fig. 1, the silver-containing high-entropy ceramic matrix composite material with complete molybdenum solid solution was successfully prepared.
Example 3A high-toughness lubrication-Integrated high-entropy ceramic matrix composite, which is in the form of a block, having a composition of (Hf 0.2 Mo 0.4 Nb 0.2 Ta 0.2 Ti 0.2 )C-22Ag。
The preparation method comprises the following steps: first, 68.02 g (Hf) 0.2 Mo 0.2 Nb 0.2 Ta 0.2 Ti 0.2 ) C,9.98 g of Mo and 22 g of Ag powder, and placing the raw materials into a ball mill; adding 50g of absolute ethyl alcohol into the mixed raw materials, uniformly mixing, and drying and sieving to obtain mixed powder with the particle size of 0.10-25 mu m; the mixed powder is filled into a graphite mould and is quickly arranged in a discharge plasma sintering furnaceHeating to 1550 ℃ at a speed, and preserving heat for 12 min under a pressure of 2 MPa; then the temperature is quickly raised to 1750 ℃, the temperature is kept for 15 min, and the pressure is 10 MPa. The vacuum degree is lower than 1 Pa in the whole sintering process, and the average heating speed is 30 ℃/min. And cooling along with the furnace to obtain the high-toughness lubrication integrated high-entropy ceramic matrix block material.
The fracture morphology of the material is shown in figure 2. As can be seen from FIG. 2, the prepared high-entropy ceramic material has grains of uniform size, which are 1.0 μm on average, compared with (Hf 0.2 Mo 0.2 Nb 0.2 Ta 0.2 Ti 0.2 ) The grain size of the sample C is reduced by more than 5 times; at the same time, a high-density high-entropy ceramic block material without obvious air hole defects is obtained at a relatively low sintering temperature (1750 ℃) and pressure (10 MPa).
The friction coefficient curve of the material at 300 ℃ is shown in figure 3. It can be seen from fig. 3 that the material exhibits excellent self-lubricating properties, and the coefficient of friction is stabilized at about 0.35.
Claims (1)
1. A high-toughness lubrication integrated high-entropy ceramic matrix composite material is characterized in that: the material is in the form of a block of the composition (Hf 0.2 Mo 0.4 Nb 0.2 Ta 0.2 Ti 0.2 ) C-xAg, x=3 to 22; the preparation method of the material comprises the steps of preparing 68.02-84.58% of (Hf) by mass percent 0.2 Mo 0.2 Nb 0.2 Ta 0.2 Ti 0.2 ) Placing the C high-entropy ceramic powder, 9.98-12.42% of Mo powder and 3-22% of Ag powder in a ball mill, adding absolute ethyl alcohol according to 10-50% of the mass of the mixed raw materials, uniformly mixing, drying, and sieving to obtain mixed powder with the particle size of 0.10-25 mu m; the mixed powder is filled into a graphite mold, and is sintered by spark plasma to obtain the high-toughness lubrication integrated high-entropy ceramic matrix material; said (Hf) 0.2 Mo 0.2 Nb 0.2 Ta 0.2 Ti 0.2 ) The high-entropy ceramic powder is prepared by the following steps: 21.5% of HfO in mass percent 2 15.0% MoO 3 13.6% Nb 2 O 5 22.4% Ta 2 O 5 TiO 8.0% 2 And 19Uniformly mixing 5% of graphite powder, and sintering under the conditions that the vacuum degree is lower than 3 Pa, the average heating speed is 40-80 ℃/min, the sintering temperature is 1700 ℃, the pressure is 10 MPa, and the temperature is kept for 15 min to obtain a high-entropy ceramic material; the high-entropy ceramic material is prepared by high-energy ball milling (Hf) with the particle size of 0.10-3 mu m 0.2 Mo 0.2 Nb 0.2 Ta 0.2 Ti 0.2 ) C, high-entropy ceramic powder; the spark plasma sintering process is that mixed powder is heated to 1550-1650 ℃ at a faster rate, and is kept for 5-12 min under the pressure of 2-10 MPa; then rapidly heating to 1750-1900 ℃, and preserving heat for 5-15 min under the pressure of 10-20 MPa; the vacuum degree in the whole sintering process is lower than 1 Pa, and the average heating speed is 30-60 ℃/min.
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| CN113667938A (en) * | 2021-07-20 | 2021-11-19 | 南京航空航天大学 | Preparation method of super-hydrophilic metal/high-entropy ceramic composite antibacterial coating |
| CN114031406A (en) * | 2021-12-01 | 2022-02-11 | 中国科学院兰州化学物理研究所 | Easy-to-sinter wear-resistant antifriction high-entropy ceramic material and preparation method thereof |
| CN115287645A (en) * | 2022-08-25 | 2022-11-04 | 兰州空间技术物理研究所 | High-entropy alloy-based high-temperature solid lubricating coating and preparation method thereof |
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| JP2002173732A (en) * | 2000-11-29 | 2002-06-21 | Univ Qinghua | High entropy multicomponent alloy |
| CN111218603A (en) * | 2020-03-10 | 2020-06-02 | 中国科学院兰州化学物理研究所 | Preparation method of high-entropy alloy-based high-temperature solid lubricating composite material |
| CN113667938A (en) * | 2021-07-20 | 2021-11-19 | 南京航空航天大学 | Preparation method of super-hydrophilic metal/high-entropy ceramic composite antibacterial coating |
| CN114031406A (en) * | 2021-12-01 | 2022-02-11 | 中国科学院兰州化学物理研究所 | Easy-to-sinter wear-resistant antifriction high-entropy ceramic material and preparation method thereof |
| CN115287645A (en) * | 2022-08-25 | 2022-11-04 | 兰州空间技术物理研究所 | High-entropy alloy-based high-temperature solid lubricating coating and preparation method thereof |
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