CN117300125A - Preparation method of dense and high-hardness carbon-rich high-entropy alloy or carbon-rich high-entropy alloy-high-entropy ceramic composite material - Google Patents
Preparation method of dense and high-hardness carbon-rich high-entropy alloy or carbon-rich high-entropy alloy-high-entropy ceramic composite material Download PDFInfo
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Abstract
The invention discloses a preparation method of a compact and high-hardness carbon-rich high-entropy alloy or carbon-rich high-entropy alloy-high-entropy ceramic composite material, which comprises the following steps: taking metal oxide powder and a carbon source as raw materials, weighing according to a designed proportion, adding an organic solvent, fully mixing, and then carrying out rotary evaporation drying; and (3) pressing and forming the dried powder by using a die, and performing pressureless sintering in a vacuum state after forming to obtain the compact and high-hardness carbon-rich high-entropy alloy. The invention takes metal oxide powder as raw material, and adopts a pressureless reaction sintering one-step method to successfully prepare the carbon-rich high-entropy alloy or the carbon-rich high-entropy alloy-high-entropy ceramic composite material, thereby not only greatly reducing the production cost, but also being expected to prepare the successfully-configured parts with complex structures.
Description
Technical Field
The invention belongs to the technical field of alloy and alloy-ceramic composite material preparation, and particularly relates to a preparation method of a compact and high-hardness carbon-rich high-entropy alloy or carbon-rich high-entropy alloy-high-entropy ceramic composite material.
Background
High-entropy alloys have been attracting attention since their first proposal in 1995 by scholars She Junwei as novel high-performance structural materials. The unique multi-main element composition ensures that the composite has excellent mechanical property and high-temperature stability [ Journal of Alloys and Compounds,549 (2013): 195-199]. The characteristics of high hardness, high strength and wear resistance lead the alloy to be widely used for machine tools, hard cutter coatings, motors and the like; at the same time, the stability and excellent oxidation resistance at high temperatures make it attractive for components for extreme environments (engine blades, jet engines, nuclear fusion) [ International Journal of Refractory Metals and Hard Materials,105 (2022): 105836]. Therefore, the high-entropy alloy material has wide application, and subsequent development and observability.
Subsequently, researchers have conducted long and intensive research into methods of preparing high-entropy alloys. The most used preparation method comprises the following steps: resistance induction melting, vacuum arc melting, mechanical alloying, powder metallurgy, laser coagulation, and the like. Patent number CN 111206174A discloses the preparation of (Fe 50Mn30Cr10Co 10) 100-XAlX (x=8-20) high entropy alloy with a mechanical alloying combined with spark plasma sintering two-step method, with a compressive strength of 1916MPa and a hardness of 614Hv; patent number CN 108531799A discloses that the press button ingot of the TiAlNbVMo master alloy is obtained by arc melting, and the compression strength measured by post-processing is 1000Mpa. The existing high-entropy alloy preparation process mostly uses high-purity metal powder as a raw material, and has the problems that the raw material powder is high in price, easy to oxidize and complex in process operation. The alloy is limited by the preparation process, and the obtained alloy can not meet the requirements of the metal structural material on parts with complex structures in engineering application. Meanwhile, the performance of the material in mechanical properties is also bad.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention takes the cheap metal oxide powder as the raw material through the design components, adds a certain amount of carbon source, prepares compact and high-hardness carbon-rich high-entropy alloy or carbon-rich high-entropy alloy-high-entropy ceramic complex phase material through pressureless reaction sintering, and can greatly reduce the production cost of the high-entropy alloy.
In order to achieve the above purpose, the present invention is realized by the following technical scheme:
in one aspect, the invention provides a method for preparing a dense and high-hardness carbon-rich high-entropy alloy, comprising the following steps:
taking metal oxide powder and a carbon source as raw materials, weighing according to a designed proportion, adding an organic solvent, fully mixing, and then carrying out rotary evaporation drying; and (3) pressing and forming the dried powder by using a die, and performing pressureless sintering in a vacuum state after forming to obtain the compact and high-hardness carbon-rich high-entropy alloy.
Preferably, the metal elements in the metal oxide are Cr, V, W and Mo, the atomic ratio of Cr, V, W, mo to C is 1:1:1:1:0.53-0.61, and the carbon-rich high-entropy alloy is BCC-phase carbon-rich high-entropy alloy.
Preferably, the metal elements in the metal oxide are Cr, V, W and Me, wherein me=ti, zr or Hf, the atomic ratio of Cr, V, W, me to C is 1:1:1:1:1:0.54-0.82, and the carbon-rich high-entropy alloy is composed of a BCC-phase carbon-rich high-entropy alloy and a HCP-phase carbon-rich high-entropy alloy.
Preferably, the metal elements in the metal oxide are Cr, mo, V, W and Me, wherein me=ti, zr, hf or Nb, the atomic ratio of Cr, mo, V, W, me to C is 1:1:1:1:1:0.42-0.66, and the carbon-rich high entropy alloy material is composed of a BCC phase carbon-rich high entropy alloy and a HCP phase carbon-rich high entropy alloy.
Preferably, the step of pressureless sintering is specifically: raising the temperature to 700 ℃ at 8 ℃/min, then adjusting the temperature raising rate to 5 ℃/min, respectively preserving heat for 10-30min at 900-950 ℃, 1100-1300 ℃ and 1600 ℃ until the temperature is 1650-1900 ℃, preserving heat for 1-2h, and naturally cooling to room temperature along with the furnace body.
Preferably, the dried powder is subjected to cold isostatic pressing treatment after preliminary compression molding, and then subjected to carbothermic reduction reaction in a vacuum state.
Preferably, the carbon source is selected from graphite or carbon black powder.
A preparation method of a compact and high-hardness carbon-rich high-entropy alloy-high-entropy ceramic complex phase material comprises the following steps:
taking metal oxide powder and a carbon source as raw materials, weighing according to a designed proportion, adding an organic solvent, fully mixing, and then carrying out rotary evaporation drying; and (3) pressing and forming the dried powder by using a die, and performing pressureless sintering in a vacuum state after forming to obtain the compact and high-hardness carbon-rich high-entropy alloy-high-entropy ceramic composite material.
Preferably, the metal elements in the metal oxide are Cr, V, W and Mo, and when the atomic ratio of Cr, V, W, mo to C is 1:1:1:1:0.62-0.82, the carbon-rich high-entropy alloy-high-entropy ceramic composite material is composed of HCP-phase carbon-rich high-entropy alloy and FCC-phase high-entropy ceramic.
Preferably, the step of pressureless sintering is specifically: heating to 700 ℃ at 8 ℃/min, then adjusting the heating rate to 5 ℃/min, respectively preserving heat at 950 ℃ and 1100 ℃ and 1300-1400 ℃ for 10-30min until the temperature rises to 1450-1900 ℃, preserving heat for 1-2h, and naturally cooling the sample to room temperature along with the furnace body.
The technical scheme provided by the invention has the following beneficial effects:
according to the invention, the preparation of the carbon-rich high-entropy alloy or the carbon-rich high-entropy alloy-high-entropy ceramic composite material by using the cheap metal oxide powder as a raw material and adding a certain amount of graphite or carbon black through carbothermic reduction reaction is realized by designing components, so that the production cost of the high-entropy alloy is greatly reduced.
The invention adopts the pressureless reaction one-step sintering method to prepare the compact carbon-rich high-entropy alloy or carbon-rich high-entropy alloy-high-entropy ceramic composite material, thereby simplifying the problems of complex operation and high energy consumption of the prior art.
The invention adopts pressureless reaction sintering, the configuration of the sintered part is not limited, and parts with different configurations can be prepared according to the requirements in the early stage of sample preparation, so that the limitation of the configuration of the part caused by pressure sintering is avoided.
The carbon-rich high-entropy alloy with compactness and high hardness, which is prepared by the invention, has the hardness of 730-1230Hv 3 The bending strength is 330-550MPa, the compression strength is 2.0-2.9GPa, and the Young's modulus is 200-310GPa.
The invention can prepare the carbon-rich high-entropy alloy-high-entropy ceramic composite material with different phases, compactness and high hardness by regulating and controlling the types of metal oxides and the content of carbon atoms in the raw materials, and the hardness of the carbon-rich high-entropy alloy-high-entropy ceramic composite material can reach 610-1130Hv 3 The bending strength is 200-550MPa, the compression strength is 1.9-2.9GPa, and the Young's modulus is 200-310GPa.
Carbon can be combined with most metal oxides as a gap element, and finally exists in a carbon compound form as a strengthening phase, so that the carbon-containing high-entropy alloy is universally applicable to the preparation of carbon-containing high-entropy alloy by using a carbothermic reduction method, and the carbon-containing high-entropy alloy has great significance in the aspect of method innovation and wide application prospect.
Drawings
FIG. 1 is a preparation process flow of a carbon-rich high-entropy alloy or a carbon-rich high-entropy alloy-high-entropy ceramic composite material according to the invention;
FIG. 2 is an XRD diffraction pattern of the carbon-rich high-entropy alloy and the carbon-rich high-entropy alloy-high-entropy ceramic composite material prepared in examples 1-4 of the present invention;
FIG. 3 is an SEM image of polished surfaces of the carbon-rich high-entropy alloy and the carbon-rich high-entropy alloy-high-entropy ceramic composite material obtained in examples 1 and 2 of the present invention;
FIG. 4 is a compressive stress strain curve of the carbon-rich high-entropy alloy-high-entropy ceramic composite material obtained in example 1 of the present invention;
fig. 5 is an XRD diffractogram of the CrMoVW high entropy ceramic material prepared in comparative examples 1 and 2.
Fig. 6 is an SEM image of polished surfaces of CrMoVW high entropy ceramic materials prepared in comparative examples 1 (fig. a) and 2 (fig. B).
Detailed Description
In order that those skilled in the art will better understand the technical solution of the present invention, preferred embodiments of the present invention will be described below with reference to specific examples, but the present invention should not be construed as being limited thereto, but only by way of example.
The test methods or test methods described in the following examples are all conventional methods unless otherwise specified; the reagents and materials, unless otherwise specified, are obtained from conventional commercial sources or prepared in conventional manner.
The invention is described in further detail below with reference to the drawings.
Example 1
As shown in FIG. 1, cr is selected 2 O 3 、MoO 3 、V 2 O 5 、WO 3 Powder and graphite or carbon black are used as raw materials, the atomic ratio of Cr, mo, V, W, C in the high-entropy alloy is 1:1:1:1:0.53-0.61, and the high-density carbon-rich high-entropy alloy-high-entropy ceramic complex phase material is prepared by adopting carbothermal reduction and pressureless sintering in one step; wherein the raw material only contains Cr, mo, V, W, C, O element; the particle size of the metal oxide powder is 0.2 mu m, and the particle size of the graphite or carbon black powder is 2 mu m; the preparation method comprises the following steps:
s1, mixing: high-purity (purity is more than or equal to 99.9%) Cr 2 O 3 、MoO 3 、V 2 O 5 、WO 3 Mixing with graphite or carbon black according to the molar ratio of 0.5:1:0.5:1:7.42-8.54, then adding a certain amount of ethanol, and fully mixing for 16-24h on a roll mixer at the rotating speed of 80-120 r/min;
s2, drying: carrying out rotary evaporation on the mixed powder by using a rotary evaporator at 50 ℃ and under vacuum, and then drying the evaporated powder in an oven at 60 ℃ for 8 hours, so as to remove redundant ethanol;
s3, sintering: after passing through a 80-mesh sieve, the dried powder is pressed into a wafer with the diameter phi 30 by using a die, after preliminary molding, the wafer is cold isostatic pressed for 10 minutes under the condition of 200MPa, and then carbothermic reduction reaction is carried out under the vacuum state, the sintering process is that the temperature is increased to 700 ℃ at 8 ℃/min, then the temperature increasing rate is regulated to 5 ℃/min, and the temperature is respectively kept at 950 ℃ and 1100 ℃ and 1300 ℃ for 10-30min until the temperature is increased to 1450-1800 ℃, and the temperature is kept for 1.5h, thus the sintering process is finishedAnd after the process is finished, naturally cooling the sample to room temperature along with the furnace body. XRD phase analysis and polished-surface SEM showed that the material prepared at this time was a dense BCC phase carbon-rich high entropy alloy (as shown in fig. 2 and 3). The mechanical characterization result shows that the Vickers hardness of the material is 730-820Hv 3 The bending strength is 470-550MPa, the compressive strength is 2.3-2.9GPa (the compressive stress strain curve is shown in figure 4), and the Young's modulus is 260-310GPa.
Example 2
As shown in FIG. 1, cr is selected 2 O 3 、V 2 O 5 、WO 3 And MoO 3 And graphite or carbon black is used as a raw material, wherein the atomic ratio of Cr, V, W, me to carbon in the high-entropy alloy is 1:1:1:0.62-0.82, and the carbon-thermal reduction and pressureless sintering are combined to prepare the highly compact carbon-rich high-entropy alloy-high-entropy ceramic complex phase material in one step; wherein the raw materials only contain Cr, V, W, mo, C and O elements; the particle size of the metal oxide powder is 0.2 mu m, and the particle size of the graphite or carbon black powder is 2 mu m; the preparation method comprises the following steps:
s1, mixing: high-purity (purity is more than or equal to 99.9%) Cr 2 O 3 、V 2 O 5 、WO 3 、MoO 3 Mixing with graphite or carbon black according to the molar ratio of 0.5:0.5:1:1:8.68-11.48, then adding a certain amount of ethanol, and fully mixing for 16-24 hours on a mixer at the rotating speed of 80-120 r/min;
s2, drying: performing rotary evaporation on the mixed powder at 50 ℃ and in a vacuum state by using a rotary evaporator to remove ethanol, and then placing the powder in a baking oven at 60 ℃ for 8 hours to remove redundant ethanol;
s3, sintering: after the dried powder is sieved by a 80-mesh sieve, the powder is pressed into a circular sheet with the diameter phi 30 by using a die, after preliminary molding, the circular sheet is subjected to cold isostatic pressing for 10 minutes under the condition of 200MPa, then carbothermic reduction reaction is carried out under the vacuum state, the temperature is increased to 700 ℃ at 8 ℃/min, the temperature rising rate is regulated to 5 ℃/min, the temperature is respectively kept at 950 ℃ and 1100 ℃ and 1400 ℃ for 10 minutes until the temperature is increased to 1750 ℃ to 1900 ℃, and after the temperature is kept for 1.5 hours, the sample is naturally cooled to the room temperature along with a furnace body. XRD phase analysis and polished surface SEM showed that the material prepared at this time was such thatDense HCP phase carbon-rich high entropy alloys and FCC phase high entropy ceramic composites (as shown in fig. 2 and 3). The mechanical characterization result shows that the Vickers hardness of the material is 833-1023Hv 3 The bending strength is 200-380MPa, the compression strength is 2.1-2.5GPa, and the Young's modulus is 200-270GPa.
Example 3
As shown in FIG. 1, cr is selected 2 O 3 、V 2 O 5 、WO 3 And Me (me=tio 2 、ZrO 2 Or HfO 2 ) And graphite or carbon black is used as a raw material, wherein the atomic ratio of Cr, V, W, me to carbon in the high-entropy alloy is 1:1:1:0.54-0.82, and the carbon-rich high-entropy alloy-high-entropy ceramic complex phase material with high compactness is prepared by adopting carbothermal reduction and pressureless sintering in one step; wherein the raw materials only contain Cr, V, W, me, C and O elements; the particle size of the metal oxide powder is 0.2 mu m, and the particle size of the graphite or carbon black powder is 2 mu m; the preparation method comprises the following steps:
s1, mixing: high-purity (purity is more than or equal to 99.9%) Cr 2 O 3 、V 2 O 5 、WO 3 Mixing Me and graphite or carbon black according to the molar ratio of 0.5:1:0.5:1:7.02-10.52, then adding a certain amount of ethanol, and fully mixing for 16-24h on a mixer at the rotating speed of 80-120 r/min;
s2, drying: performing rotary evaporation on the mixed powder at 50 ℃ and in a vacuum state by using a rotary evaporator to remove ethanol, and then placing the powder in a baking oven at 60 ℃ for 8 hours to remove redundant ethanol;
s3, sintering: after the dried powder is sieved by a 80-mesh sieve, the powder is pressed into a circular sheet with the diameter phi 30 by using a die, after preliminary molding, the circular sheet is subjected to cold isostatic pressing for 10 minutes under the condition of 200MPa, then carbothermic reduction reaction is carried out under the vacuum state, the temperature is increased to 700 ℃ at 8 ℃/min, the temperature rising rate is regulated to 5 ℃/min, the temperature is respectively kept at 950 ℃ and 1100 ℃ and 1400 ℃ for 10 minutes until the temperature is increased to 1750 ℃ to 1900 ℃, and after the temperature is kept for 1.5 hours, the sample is naturally cooled to the room temperature along with a furnace body. XRD phase analysis shows that the prepared materials are compact BCC phase carbon-rich high-entropy alloy and HCP phase carbon-rich high-entropy alloy (shown in figure 2). Mechanical characterization result display material dimensionHardness of 610-1130Hv 3 The bending strength is 250-400MPa, the compression strength is 1.9-2.5GPa, and the Young's modulus is 260-290GPa.
Example 4
As shown in FIG. 1, cr is selected 2 O 3 、MoO 3 、V 2 O 5 、WO 3 、Me(Me＝TiO 2 、ZrO 2 、HfO 2 Or Nb (Nb) 2 O 5 ) Powder and graphite or carbon black are used as raw materials, the atomic ratio of Cr, mo, V, W, me, C in the raw materials is 1:1:1:1:0.42-0.66, and the high-density carbon-rich high-entropy alloy is prepared by combining carbothermal reduction and pressureless sintering in one step; wherein the raw materials only contain Cr, mo, V, W, me, C and O elements; the particle size of the metal oxide powder is 0.2 mu m, and the particle size of the graphite or carbon black powder is 2 mu m; the preparation method comprises the following steps:
s1, mixing: high-purity (purity is more than or equal to 99.9%) metal oxide powder Cr 2 O 3 、MoO 3 、V 2 O 5 、WO 3 Mixing Me and graphite or carbon black according to a molar ratio of 0.5:1:0.5:1:1 or 0.5:7.0-10.0, adding a certain amount of ethanol, and fully mixing for 16-24h on a mixer at a rotating speed of 80-120 r/min;
s2, drying: performing rotary evaporation on the mixed powder at 50 ℃ and in a vacuum state by using a rotary evaporator to remove ethanol, and then placing the powder in a baking oven at 60 ℃ for 8 hours to remove redundant ethanol;
s3, sintering: after the dried powder is sieved by a 80-mesh sieve, the powder is pressed into a circular sheet with the diameter phi 30 by using a die, after preliminary molding, the circular sheet is subjected to cold isostatic pressing for 10 minutes under the condition of 200MPa, then carbothermic reduction reaction is carried out under the vacuum state, the temperature is increased to 700 ℃ at 8 ℃/min, the heating rate is regulated to 5 ℃/min, and the temperature is respectively kept at 900-950 ℃, 1100-1300 ℃ and 1600 ℃ for 10-30min until the temperature is increased to 1650-1900 ℃, and the furnace body is naturally cooled to room temperature after the temperature is kept for 1-2 h. XRD phase analysis showed that the material prepared at this time was a dense carbon-rich high entropy alloy of BCC and HCP phases (as shown in FIG. 2). The mechanical characterization result shows that the Vickers hardness of the material is 820-1230Hv 3 Bending strength of 330-490MPa, compressive strength of 2.0-2.6GPa and Young's modulus of 200-270GPa.
Comparative example 1
The procedure for preparing the high-entropy alloy material was the same as in example 1, except that high-purity Cr was used 2 O 3 、MoO 3 、V 2 O 5 、WO 3 And graphite or carbon black are mixed according to the molar ratio of 0.5:1:0.5:1:11.48, and the atomic ratio of Cr, mo, V, W to C in the material is 1:1:1:1:1:0.82. In the sintered sample, XRD diffraction shows that the FCC phase is the main phase (as shown in figures 5 and 6) and the relative density is only 92%, the hardness is improved, but the brittleness is large, the main phase is a high-entropy ceramic phase, no high-entropy alloy phase exists, and the mechanical characterization result shows that the Vickers hardness of the material is 1312Hv 3 The bending strength was 230MPa, the compressive strength was 2.5GPa, and the Young's modulus was 276GPa.
Comparative example 2
The preparation steps of the high-entropy alloy material are the same as those of the embodiment 1, except that high-purity chromium oxide, molybdenum oxide, vanadium pentoxide, tungsten oxide and carbon are mixed according to the molar ratio of 0.5:1:0.5:1:11.6-14.0, and the atomic ratio of chromium, molybdenum, vanadium, tungsten and carbon in the material is 1:1:1:1:1:0.83-1.0. The sintered sample showed an FCC phase (as shown in fig. 5 and 6) with increased hardness by XRD diffractometry, but was brittle, the main phase was a ceramic phase, no alloy phase, and the relative density was only 58.5-86.7%, and the mechanical properties could not be characterized.
The invention adopts a carbothermic reduction one-step method and pressureless sintering preparation conditions, has simple process and strong operability, and can realize the preparation of complex components; in addition, the high-entropy alloy is formed and the interstitial element carbon is introduced, so that the hardness of the alloy material is remarkably improved through solid solution strengthening while the plasticity of the alloy is maintained.
The foregoing is merely a preferred embodiment of the present invention, and it should be noted that the above-mentioned preferred embodiment should not be construed as limiting the invention, and the scope of the invention should be defined by the appended claims. It will be apparent to those skilled in the art that various modifications and adaptations can be made without departing from the spirit and scope of the invention, and such modifications and adaptations are intended to be comprehended within the scope of the invention.
Claims (10)
1. A method for preparing a dense and high-hardness carbon-rich high-entropy alloy, which is characterized by comprising the following steps:
taking metal oxide powder and a carbon source as raw materials, weighing according to a designed proportion, adding an organic solvent, fully mixing, and then carrying out rotary evaporation drying; and (3) pressing and forming the dried powder by using a die, and performing pressureless sintering in a vacuum state after forming to obtain the compact and high-hardness carbon-rich high-entropy alloy.
2. The method for preparing a dense and high-hardness carbon-rich high-entropy alloy according to claim 1, wherein the metal elements in the metal oxide are Cr, V, W and Mo, the atomic ratio of Cr, V, W, mo to C is 1:1:1:1:0.53-0.61, and the carbon-rich high-entropy alloy is a BCC phase carbon-rich high-entropy alloy.
3. The method for preparing a dense and high-hardness carbon-rich high-entropy alloy according to claim 1, wherein the metal elements in the metal oxide are Cr, V, W and Me, wherein me=ti, zr or Hf, the atomic ratio of Cr, V, W, me to C is 1:1:1:1:1:0.54-0.82, and the carbon-rich high-entropy alloy is composed of a BCC phase carbon-rich high-entropy alloy and a HCP phase carbon-rich high-entropy alloy.
4. The method for preparing a dense and high-hardness carbon-rich high-entropy alloy according to claim 1, wherein the metal elements in the metal oxide are Cr, mo, V, W and Me, wherein me=ti, zr, hf or Nb, the atomic ratio of Cr, mo, V, W, me to C is 1:1:1:1:1:0.42-0.66, and the carbon-rich high-entropy alloy material is composed of a BCC phase carbon-rich high-entropy alloy and a HCP phase carbon-rich high-entropy alloy.
5. The method for producing a dense and high-hardness carbon-rich high-entropy alloy according to claim 1, wherein the dried powder is subjected to cold isostatic pressing after preliminary press forming, and then subjected to carbothermic reduction under vacuum.
6. The method of producing a dense and high hardness carbon-rich high entropy alloy according to claim 1, wherein the carbon source is selected from graphite or carbon black powder.
7. The method for producing a dense and high-hardness carbon-rich high-entropy alloy according to any one of claims 1 to 6, wherein the step of pressureless sintering is specifically: raising the temperature to 700 ℃ at 8 ℃/min, then adjusting the temperature raising rate to 5 ℃/min, respectively preserving heat for 10-30min at 900-950 ℃, 1100-1300 ℃ and 1600 ℃ until the temperature is 1650-1900 ℃, preserving heat for 1-2h, and naturally cooling to room temperature along with the furnace body.
8. The preparation method of the compact and high-hardness carbon-rich high-entropy alloy-high-entropy ceramic complex phase material is characterized by comprising the following steps of:
taking metal oxide powder and a carbon source as raw materials, weighing according to a designed proportion, adding an organic solvent, fully mixing, and then carrying out rotary evaporation drying; and (3) pressing and forming the dried powder by using a die, and performing pressureless sintering in a vacuum state after forming to obtain the compact and high-hardness carbon-rich high-entropy alloy-high-entropy ceramic composite material.
9. The method for preparing a dense and high-hardness carbon-rich high-entropy alloy-high-entropy ceramic composite material according to claim 8, wherein when the metal elements in the metal oxide are Cr, V, W and Mo and the atomic ratio of Cr, V, W, mo to C is 1:1:1:1:0.62-0.82, the carbon-rich high-entropy alloy-high-entropy ceramic composite material is composed of HCP-phase carbon-rich high-entropy alloy and FCC-phase high-entropy ceramic.
10. The method for preparing a dense and high-hardness carbon-rich high-entropy alloy-high-entropy ceramic composite material according to claim 8 or 9, wherein the step of pressureless sintering is specifically: heating to 700 ℃ at 8 ℃/min, then adjusting the heating rate to 5 ℃/min, respectively preserving heat at 950 ℃ and 1100 ℃ and 1300-1400 ℃ for 10-30min until the temperature rises to 1450-1900 ℃, preserving heat for 1-2h, and naturally cooling the sample to room temperature along with the furnace body.
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| KR20180035750A (en) * | 2018-03-22 | 2018-04-06 | 한국과학기술원 | In-situ strengthened high entropy powder, alloy thereof and method of manufacturing the same |
| CN110078512A (en) * | 2019-05-17 | 2019-08-02 | 淄博星澳新材料研究院有限公司 | High entropy carbide powder of superhigh temperature and preparation method thereof |
| CN110423930A (en) * | 2019-08-21 | 2019-11-08 | 福建工程学院 | A kind of high entropy ceramic-metal composite of Ultra-fine Grained and preparation method thereof |
-
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- 2023-09-05 CN CN202311134519.4A patent/CN117300125A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20180035750A (en) * | 2018-03-22 | 2018-04-06 | 한국과학기술원 | In-situ strengthened high entropy powder, alloy thereof and method of manufacturing the same |
| CN110078512A (en) * | 2019-05-17 | 2019-08-02 | 淄博星澳新材料研究院有限公司 | High entropy carbide powder of superhigh temperature and preparation method thereof |
| CN110423930A (en) * | 2019-08-21 | 2019-11-08 | 福建工程学院 | A kind of high entropy ceramic-metal composite of Ultra-fine Grained and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| 谭红: "粉末冶金法制备CoCrFeNi系含碳高熵合金及其摩擦学性能研究", 中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑, 15 August 2021 (2021-08-15), pages 21 - 23 * |
| 黄颖: "(TiVNbTaCrW)C6高熵碳化物陶瓷的制备与组织性能的研究", 中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑, 15 March 2022 (2022-03-15), pages 14 - 15 * |
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