CN114807725A - High-entropy alloy-based nano superhard composite material enhanced by inlaid particles and preparation method thereof - Google Patents

High-entropy alloy-based nano superhard composite material enhanced by inlaid particles and preparation method thereof Download PDF

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CN114807725A
CN114807725A CN202210609918.0A CN202210609918A CN114807725A CN 114807725 A CN114807725 A CN 114807725A CN 202210609918 A CN202210609918 A CN 202210609918A CN 114807725 A CN114807725 A CN 114807725A
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composite material
entropy alloy
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phase particles
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CN114807725B (en
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陈正
王汝江
赵李新
樊宇
许泉
刘猛
徐哲
蒋崴
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China University of Mining and Technology CUMT
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Abstract

The application discloses a particle-embedded reinforced high-entropy alloy-based nano superhard composite material and a preparation method thereof, and relates to the technical field of metal-based composite materials. The composite material comprises a high-entropy alloy matrix and reinforcing phase particles, wherein the reinforcing phase particles are dispersed in the high-entropy alloy matrix, the high-entropy alloy matrix comprises a base matrix and a reinforcing matrix, the base matrix comprises Al, Co, Cr, Fe, Ni and Mn, the reinforcing matrix comprises Mo, Nb and Zr, and the reinforcing phase particles comprise WC and TiC.

Description

High-entropy alloy-based nano superhard composite material enhanced by inlaid particles and preparation method thereof
Technical Field
The application relates to the technical field of metal matrix composite materials, in particular to a high-entropy alloy matrix nano superhard composite material enhanced by inlaid particles and a preparation method thereof.
Background
The traditional composite material usually uses single or binary metal as a matrix and adds a reinforcing phase to improve the strength and the hardness of the composite material, but the material prepared by the method has the defects of single performance and the like. For example, Fe-based composites have good corrosion resistance, but have limited hardness and wear resistance. In order to solve the problems, people use high-entropy alloy with good comprehensive mechanical properties as a base material and add a hard reinforcing phase to prepare a composite material, so that the wear resistance of the material is greatly enhanced. The research and development of the high-entropy alloy-based composite material meet the requirements under more severe working conditions, and the superposition of various properties improves the existing properties of the material or further obtains new characteristics.
The high-entropy alloy-based composite material has great potential in the aspects of being used as wear-resistant part materials and high-temperature structural member materials, integrates excellent performances of a reinforcing phase and a high-entropy alloy matrix, and has very wide application prospect. However, the high-entropy alloy-based composite material in the related art has the disadvantages of poor wettability of the reinforcing phase and the high-entropy alloy matrix and poor interface bonding property.
Disclosure of Invention
The present application is directed to solving at least one of the problems in the prior art. Therefore, one object of the present application is to provide a high-entropy alloy-based nano superhard composite material reinforced by inlaid particles, in which the wettability of the reinforcing phase particles and the high-entropy alloy matrix is good, and the composite material has good interface bonding, can improve the wear resistance of the composite material, and can effectively prevent the reinforcing phase particles from falling off in the friction process.
Another objective of the present application is to provide a method for preparing a high-entropy alloy-based nano superhard composite material reinforced by inlaid particles.
Still another object of the present application is to provide a high-entropy alloy-based nano superhard composite material reinforced by inlaid particles, which is prepared by the above preparation method.
In a first aspect, the present application provides a high entropy alloy based nano superhard composite material reinforced by inlaid particles, comprising: the high-entropy alloy comprises a high-entropy alloy matrix and reinforcing phase particles, wherein the reinforcing phase particles are dispersed in the high-entropy alloy matrix, the high-entropy alloy matrix comprises a base matrix and a reinforcing matrix, the base matrix comprises Al, Co, Cr, Fe, Ni and Mn, the reinforcing matrix comprises Mo, Nb and Zr, and the reinforcing phase particles comprise WC and TiC.
The particle-embedded reinforced high-entropy alloy-based nano superhard composite material has the advantages that the hardness of WC and TiC is high, the wear resistance of the composite material can be effectively improved, the atomic radius of nitrogen elements in reinforced phase particles of WC and TiC is small, a gap solid solution can be formed in the material, a solid solution strengthening effect is generated, and the deformation resistance of the composite material is improved. The nano-scale powder after ball milling and thinning is sintered, so that the reinforced phase particles WC and TiC in the material not only can play a bearing role, but also can block dislocation movement, reduce the growth rate of crystal grains, generate a nano fine crystal strengthening effect and a second phase synergistic strengthening effect, and greatly improve the wear resistance of the composite material. In addition, the reinforcing phase particles WC and TiC in the high-entropy alloy matrix have good wettability with metal elements such as Al, Co, Cr, Fe, Ni, Mn, Mo, Nb and Zr, the high-entropy alloy matrix is well combined with the reinforcing phase particles, the combination firmness of the reinforcing phase particles and the high-entropy alloy matrix can be effectively improved, and the phenomenon that the reinforcing phase particles fall off in the friction process to aggravate material abrasion in the use process of the composite material is avoided. In addition, in the friction and wear environment, the Al, Nb, Zr and Cr elements can form a continuous and compact oxide layer on the surface of the composite material through friction heating in the use process of the composite material, so that the friction coefficient between the composite material and a contact object can be effectively reduced, the wear loss of the composite material in the use process can be further reduced, the service life of the composite material is prolonged, and the use cost of the composite material is reduced.
In some embodiments herein, the mass fraction of reinforcing phase particles is greater than or equal to 5% and less than or equal to 30%
In some embodiments of the present application, the mass fractions of Al, Co, Cr, Fe, Ni, Mn are each greater than or equal to 10% in the high entropy alloy matrix.
In some embodiments of the present application, the mass fraction of the strengthening matrix in the high entropy alloy matrix is less than or equal to 5%. That is, the total mass fraction of Mo, Nb and Zr is 5% or less.
In a second aspect, the application provides a method for preparing a high-entropy alloy-based nano superhard composite material reinforced by inlaid particles, which comprises the following steps: weighing Al powder, Co powder, Cr powder, Fe powder, Ni powder, Mn powder, Mo powder, Nb powder, Zr powder, WC powder and TiC powder, and uniformly mixing to form composite material powder; performing ball milling treatment on the composite material powder to enable the composite material powder to be nanocrystallized to obtain nanocrystalline powder; and sintering the nanocrystalline powder to obtain the block composite material.
The preparation method takes Al, Co, Cr, Fe, Ni, Mn, Mo, Nb, Zr, WC, TiC and other powder as raw materials, and is prepared by combining a powder metallurgy method with a discharge plasma sintering technology, so that the powder is crushed, refined, uniformly dissolved and loaded into a graphite mold in a ball milling process, and is put into a furnace to be solidified into blocks at different sintering temperatures, and then a ball-disc reciprocating friction wear testing machine is used for testing the wear resistance. The composite material with the high-entropy alloy as the matrix has excellent comprehensive mechanical properties, and can meet the wear-resistant requirement under worse working conditions compared with the traditional metal matrix composite material. In the preparation method, the hardness and the strength of the matrix material are greatly improved by adding nitride reinforced phase particles such as WC, TiC and the like, and an oxide layer formed by Al, Nb, Zr and Cr elements in the friction and wear process has a lubricating effect, so that the friction coefficient is reduced, the wear loss is reduced, and the wear resistance of the composite material is effectively improved.
In some embodiments of the present application, the purity of Al powder, Co powder, Cr powder, Fe powder, Ni powder, Mn powder, Mo powder, Nb powder, Zr powder, WC powder, TiC powder is not less than 99.95%.
In some embodiments of the present application, the particle sizes of the Al powder, Co powder, Cr powder, Fe powder, Ni powder, Mn powder, Mo powder, Nb powder, Zr powder, WC powder, TiC powder are each greater than or equal to 30 μm and less than or equal to 50 μm.
In some embodiments of the present application, ball milling the composite powder to nanosize the composite powder comprises: and sealing the composite material powder and the dispersing agent into a ball milling tank for ball milling in an inert gas environment, wherein the rotating speed of the ball milling tank is 300r/min and the ball milling time is 15h in the ball milling process.
In some embodiments of the present application, the ball mill is paused for 20min to 30min every 30min of operation during the ball milling process.
In some embodiments of the present application, the nanocrystalline powder is subjected to a sintering process comprising: sintering the metal powder by using a discharge plasma sintering furnace, heating the temperature in the discharge plasma sintering furnace to 1050 +/-20 ℃, adding the pressure to 40MPa, preserving the temperature for 10min, and cooling to room temperature to obtain the massive composite material.
In a third aspect, the application provides a high-entropy alloy-based nano superhard composite material reinforced by inlaid particles, and the composite material is prepared by the preparation method in the second aspect.
Additional aspects and advantages of the present application will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the present application.
Drawings
The above and/or additional aspects and advantages of the present application will become apparent and readily appreciated from the following description of the embodiments, taken in conjunction with the accompanying drawings of which:
fig. 1 is a flow chart of a method of making a high entropy alloy based nano superhard composite material reinforced with inlaid particles provided by some embodiments herein;
fig. 2 is a scanning electron micrograph of a high-entropy alloy-based nano superhard composite material reinforced by inlaid particles according to some embodiments of the invention;
FIG. 3 is a scanning electron micrograph of a high-entropy alloy-based nano superhard composite material reinforced by inlaid particles according to other embodiments of the invention;
fig. 4 is a scanning electron micrograph of a high-entropy alloy-based nano superhard composite material reinforced by inlaid particles according to still other embodiments of the invention;
fig. 5 is a scanning electron micrograph of a high-entropy alloy-based nano superhard composite material reinforced by inlaid particles according to still other embodiments of the invention.
Detailed Description
Reference will now be made in detail to embodiments of the present application, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to the same or similar elements or elements having the same or similar function throughout. The embodiments described below with reference to the drawings are exemplary only for the purpose of explaining the present application and are not to be construed as limiting the present application.
The high entropy alloy-based nano superhard composite material reinforced by inlaid particles according to embodiments of the present application is described below. The composite material comprises: the high-entropy alloy comprises a high-entropy alloy matrix and reinforcing phase particles, wherein the reinforcing phase particles are dispersed in the high-entropy alloy matrix. Specifically, the reinforcing phase particles are uniformly dispersed in the high-entropy alloy matrix.
Specifically, the high-entropy alloy matrix comprises metal elements of Al (aluminum), Co (cobalt), Cr (chromium), Fe (iron), Ni (nickel), Mn (manganese), Mo (molybdenum), Nb (niobium) and Zr (zirconium), and the reinforced phase particles comprise WC (tungsten carbide) and TiC (titanium carbide). Wherein the composite material may be a block.
In some embodiments, the composite material may be prepared by sintering. Specifically, in the processing process, the composite material powder may be sintered to obtain a block-shaped composite material. In the sintering process, Mo, Nb and Zr elements of the reinforced matrix can reduce the surface tension between molten metal and reinforced phase particles in the sintering process, so that the reinforced phase particles are uniformly distributed, a certain interface reaction is introduced, and the strength of the composite material is improved.
In the composite material of the embodiment of the application, the hardness of WC and TiC is high, the wear resistance of the composite material can be effectively improved, the atomic radius of nitrogen elements in the reinforced phase grains of WC and TiC is small, a gap solid solution can be formed in the material, a solid solution strengthening effect is generated, and the deformation resistance of the composite material is improved. The nano-scale powder after ball milling and thinning is sintered, so that the reinforced phase particles WC and TiC in the material not only can play a bearing role, but also can block dislocation movement, reduce the growth rate of crystal grains, generate a nano fine crystal strengthening effect and a second phase synergistic strengthening effect, and greatly improve the wear resistance of the composite material. Meanwhile, in the processing process, the reinforced phase grains WC and TiC not only can play a bearing role, but also can block dislocation movement, so that fine crystal strengthening and second phase synergistic strengthening effects are generated, and the wear resistance of the composite material is greatly improved.
In addition, the reinforcing phase particles WC and TiC in the high-entropy alloy matrix have good wettability with metal elements such as Al, Co, Cr, Fe, Ni, Mn, Mo, Nb and Zr, the high-entropy alloy matrix is well combined with the reinforcing phase particles, the combination firmness of the reinforcing phase particles and the high-entropy alloy matrix can be effectively improved, and the phenomenon that the reinforcing phase particles fall off in the friction process to aggravate material abrasion in the use process of the composite material is avoided. .
In addition, by adding Al, Nb, Zr and Cr elements into the high-entropy alloy matrix, the Al, Nb, Zr and Cr elements can form a continuous and compact oxide layer on the surface of the composite material through friction heating in the use process of the composite material, so that the friction coefficient between the composite material and a contact object can be effectively reduced, the abrasion loss of the composite material in the use process can be further reduced, the service life of the composite material is prolonged, and the use cost of the composite material is reduced.
In some embodiments, the mass fraction of reinforcing phase particles is greater than or equal to 5% and less than or equal to 30%. That is, the total mass fraction of WC and TiC is 5% or more and 30% or less. Wherein the mass fraction of WC and the mass fraction of TiC may be equal.
Illustratively, the mass fraction of WC may be 2.5%, 3%, 3.5%, 4%, 4.5%, 5%, 5.5%, 6%, 6.5%, 7%, 7.5%, 8%, 8.5%, 9%, 9.5%, 10%, 11.5%, 12%, 12.5%, 13%, 13.5%, 14%, 14.5%, 15%, etc. The mass fraction of TiC may be 2.5%, 3%, 3.5%, 4%, 4.5%, 5%, 5.5%, 6%, 6.5%, 7%, 7.5%, 8%, 8.5%, 9%, 9.5%, 10%, 11.5%, 12%, 12.5%, 13%, 13.5%, 14%, 14.5%, 15%, etc.
When the mass fraction of the reinforcing phase particles is more than 30%, the reinforcing phase particles are easy to agglomerate in the high-entropy alloy matrix, so that the distribution of the reinforcing phase particles in the high-entropy alloy matrix is not uniform. When the mass fraction of the reinforcing phase particles is less than 5%, the purpose of enhancing the wear resistance of the composite material cannot be achieved. Therefore, the mass fraction of the reinforcing phase particles is controlled to be greater than or equal to 5% and less than or equal to 30%, so that the abrasive resistance of the composite material is enhanced, and the reinforcing phase particles are prevented from being agglomerated in the high-entropy alloy matrix, so that the reinforcing phase particles are more uniformly distributed in the high-entropy alloy matrix.
In some embodiments, the mass fraction of the Mo, Nb, Zr elements of the reinforcement matrix is less than or equal to 5%. Illustratively, the mass fraction of the strengthening matrix is 1%, 2%, 3%, 4%, or 5%. Optionally, the mass fractions of the Mo, Nb, and Zr elements are equal. Thus, in the sintering process, the Mo, Nb and Zr elements can reduce the surface tension between the molten metal and the reinforcing phase particles in the sintering process, so that the reinforcing phase particles are uniformly distributed. The interface reaction between the reinforcing phase particles and the matrix can ensure good combination between the reinforcing phase particles and the matrix. The using amount of Mo, Nb and Zr is less, and the cost of the composite material is reduced.
Illustratively, the mass fraction of Mo is 0.333%, 0.667%, 1%, 1.333%, or 1.667%. The mass fraction of Nb is 0.333%, 0.667%, 1%, 1.333%, or 1.667%. The mass fraction of Zr is 0.333%, 0.667%, 1%, 1.333%, or 1.667%.
In some embodiments, the mass fractions of Al, Co, Cr, Fe, Ni, Mn are all equal. For example, the mass fractions of Al, Co, Cr, Fe, Ni, and Mn are each 10% or more.
The preparation method of the high-entropy alloy-based nano superhard composite material reinforced by the inlaid particles provided by the embodiment of the application is described below with reference to fig. 1.
Referring to fig. 1, fig. 1 is a flow chart of a method for preparing a high-entropy alloy-based nano superhard composite material reinforced by inlaid particles according to some embodiments of the present application. The preparation method of the high-entropy alloy-based nano superhard composite material reinforced by inlaid particles comprises the following steps:
step S100: weighing Al powder, Co powder, Cr powder, Fe powder, Ni powder, Mn powder, Mo powder, Nb powder, Zr powder, WC powder and TiC powder, and uniformly mixing to form composite material powder;
specifically, the powder required by the composite material is weighed according to a certain proportion and uniformly mixed. Illustratively, the mass fraction of the reinforcing phase particles is 5% to 30%, the total mass fraction of the Mo powder, the Nb powder, and the Zr powder (i.e., the mass of the reinforcing matrix) is less than or equal to 5%, and the mass fractions of the Al powder, the Co powder, the Cr powder, the Fe powder, the Ni powder, and the Mn powder are each greater than or equal to 10%.
In some embodiments of the present application, the purity of Al powder, Co powder, Cr powder, Fe powder, Ni powder, Mn powder, Mo powder, Nb powder, Zr powder, WC powder, TiC powder is not less than 99.95%.
In some embodiments of the present application, the particle sizes of the Al powder, Co powder, Cr powder, Fe powder, Ni powder, Mn powder, Mo powder, Nb powder, Zr powder, WC powder, TiC powder are each greater than or equal to 30 μm and less than or equal to 50 μm. Illustratively, the particle size of the Al powder, Co powder, Cr powder, Fe powder, Ni powder, Mn powder, Mo powder, Nb powder, Zr powder, WC powder, TiC powder may be 30 μm, 35 μm, 45 μm, 50 μm, or the like.
Step S200: performing ball milling treatment on the composite material powder to nanocrystallize the composite material powder to obtain nanocrystalline powder;
in some embodiments of the present application, ball milling the composite powder to nanosize the composite powder comprises: and sealing the composite material powder and the dispersing agent into a ball milling tank for ball milling under an inert gas (such as argon), wherein the rotating speed of the ball mill is 300r/min and the ball milling time is 15h in the ball milling process. Therefore, the composite material powder can be made into a nanometer state, and the mixing uniformity of the enhanced phase particles and the high-entropy alloy matrix can be improved.
Further, in some embodiments of the present application, the ball mill is paused for 20min to 30min every 30min during the ball milling process. Thus, the temperature in the spherical tank can be prevented from being too high.
Step S300: and sintering the nanocrystalline powder to obtain the block composite material.
In some embodiments of the present application, the nanocrystalline powder is subjected to a sintering process comprising: sintering the metal powder by using a discharge plasma sintering furnace, putting the nanocrystalline powder into the discharge plasma sintering furnace, heating the temperature in the discharge plasma sintering furnace to 1050 +/-20 ℃, increasing the pressure to 40MPa, preserving the temperature for 10min, and cooling to room temperature to obtain the bulk composite material.
In the sintering process, after the nano-scale powder refined by ball milling is prepared by sintering, the toughness and the wear resistance of the material can be further ensured. In addition, because Mo, Nb and Zr elements are added into the high-entropy alloy matrix, the surface tension between molten metal and the reinforced phase particles in the sintering process can be reduced, the reinforced phase particles are uniformly distributed, a certain interface reaction is introduced, and the strength of the composite material is improved.
The preparation method of the particle-embedded reinforced high-entropy alloy-based nano superhard composite material provided by the embodiment of the application has the following advantages:
(1) the components of the high-entropy alloy matrix comprise Al, Co, Cr, Fe, Ni, Mn, Mo, Nb and Zr, and all selected elements have good wettability with reinforcing phase particles WC and TiC, so that the high-entropy alloy matrix of the composite material can be well combined with the reinforcing phase particles to form better interface combination. In addition, carbide is decomposed in the sintering process and combined with Fe and Cr elements to generate carbide, so that the hardness of the material is improved, and the aim of improving the wear resistance of the material is fulfilled.
(2) In the friction heating process of the composite material, Al, Nb, Zr and Cr elements can form a continuous and compact oxide layer. The oxide layer formed by Al, Nb, Zr and Cr elements in the friction and wear process has the function of lubrication, so that the friction coefficient of the composite material is reduced, the wear loss is reduced, and the wear resistance of the composite material is effectively improved. Meanwhile, the existence of WC and TiC reinforced phase particles can improve the strength and hardness of the material, further improve the frictional wear performance of the composite material and improve the wear resistance of the composite material.
(3) The metal powder is refined by a mechanical alloying method, and the nano-scale powder is sintered into a solid by a discharge plasma sintering technology. The process enables the sintered powder particles to generate plasma under the action of pulse current of 5000-8000A, can quickly realize densification within 1-3 min, and the prepared material has fine and uniform tissue, good toughness, effectively saves production time and improves preparation efficiency.
(4) The addition of a small amount of Mo, Nb and Zr elements reduces the surface tension of molten metal and a reinforcing phase in the sintering process, so that particles are uniformly distributed, a certain interface reaction is introduced, and the strength of the composite material is improved.
(5) According to the method, the content of the reinforcing phase particles is regulated and controlled to obtain the composite material with different reinforcing phase particle contents, the materials are prepared at different sintering temperatures, the organization structure of the materials is researched and analyzed, and the optimal proportion and process are finally obtained through performance comparison.
The embodiment of the application also provides a high-entropy alloy-based nano superhard composite material enhanced by inlaid particles, and the composite material is prepared by the preparation method.
The present application is further illustrated by the following specific examples.
Example 1
A high-entropy alloy-based nano superhard composite material reinforced by inlaid particles comprises a high-entropy alloy matrix component including Al, Co, Cr, Fe, Ni, Mn, Mo, Nb and Zr, and reinforcing phase particles including WC and TiC. The mass fraction of the reinforced phase particles is 5%, the total mass fraction of Mo, Nb and Zr is less than or equal to 5%, and the mass fractions of Al, Co, Cr, Fe, Ni and Mn elements are all more than 10%.
In this embodiment, the preparation method of the grain-embedded reinforced high-entropy alloy-based nano superhard composite material comprises the following steps:
(1) weighing metal powder required by preparing the composite material according to the determined proportion;
(2) sealing metal powder and a dispersant (alcohol) into a ball milling tank under an inert gas (argon) environment;
(3) putting a ball milling tank into a ball mill to perform ball milling refinement on the powder, setting the ball milling rotation speed to be 300r/min, setting the time to be 15h, pausing for 30min every time the ball mill runs for 30min, putting the taken wet powder into a vacuum drying oven to be dried after the ball milling is finished, setting the temperature to be 65 ℃ and the time to be 6h, and taking the wet powder out after the drying is finished;
(4) and (2) putting the metal powder into a graphite die, putting the graphite die into a discharge plasma sintering furnace for sintering, setting the sintering temperature to be 1050 +/-20 ℃, applying the pressure to be 40MPa, preserving the temperature for 10min, and cooling to room temperature to obtain the block composite material.
Fig. 2 is a scanning electron micrograph of the high-entropy alloy-based nano superhard composite material reinforced by the inlaid particles prepared in example 1. As can be seen from fig. 2, the white reinforcing phase particles in this example are uniformly distributed on the high-entropy alloy matrix.
Example 2
A high-entropy alloy-based nano superhard composite material reinforced by inlaid particles comprises a high-entropy alloy matrix component including Al, Co, Cr, Fe, Ni, Mn, Mo, Nb and Zr, and reinforcing phase particles including WC and TiC. The mass fraction of the reinforced phase particles is 10 percent, the total mass fraction of Mo, Nb and Zr is less than or equal to 5 percent, and the mass fractions of Al, Co, Cr, Fe, Ni and Mn elements are all more than 10 percent.
In this embodiment, the preparation method of the grain-embedded reinforced high-entropy alloy-based nano superhard composite material comprises the following steps:
(1) weighing metal powder required by preparing the composite material according to the determined proportion;
(2) sealing metal powder and a dispersant (alcohol) into a ball milling tank under an inert gas (argon) environment;
(3) putting a ball milling tank into a ball mill to perform ball milling refinement on the powder, setting the ball milling rotation speed to be 300r/min, setting the time to be 15h, pausing for 30min every time the ball mill runs for 30min, putting the taken wet powder into a vacuum drying oven to be dried after the ball milling is finished, setting the temperature to be 65 ℃ and the time to be 6h, and taking the wet powder out after the drying is finished;
(4) and (2) putting the metal powder into a graphite die, putting the graphite die into a discharge plasma sintering furnace for sintering, setting the sintering temperature to be 1050 +/-20 ℃, applying the pressure to be 40MPa, preserving the temperature for 10min, and cooling to room temperature to obtain the block composite material.
Fig. 3 is a scanning electron micrograph of the high-entropy alloy-based nano superhard composite material reinforced by the inlaid particles prepared in example 2. As can be seen from fig. 3, the white reinforcing phase particles in this example are uniformly distributed on the high-entropy alloy matrix.
Example 3
A high-entropy alloy-based nano superhard composite material reinforced by inlaid particles comprises a high-entropy alloy matrix component including Al, Co, Cr, Fe, Ni, Mn, Mo, Nb and Zr, and reinforcing phase particles including WC and TiC. The mass fraction of the reinforced phase particles is 15 percent, the total mass fraction of Mo, Nb and Zr is less than or equal to 5 percent, and the mass fractions of Al, Co, Cr, Fe, Ni and Mn elements are all more than 10 percent.
In this embodiment, the preparation method of the grain-embedded reinforced high-entropy alloy-based nano superhard composite material comprises the following steps:
(1) weighing metal powder required by preparing the composite material according to the determined proportion;
(2) sealing metal powder and a dispersant (alcohol) into a ball milling tank under an inert gas (argon) environment;
(3) putting a ball milling tank into a ball mill to perform ball milling refinement on the powder, setting the ball milling rotation speed to be 300r/min, setting the time to be 15h, pausing for 30min every time the ball mill runs for 30min, putting the taken wet powder into a vacuum drying oven to be dried after the ball milling is finished, setting the temperature to be 65 ℃ and the time to be 6h, and taking the wet powder out after the drying is finished;
(4) and (2) putting the metal powder into a graphite die, putting the graphite die into a discharge plasma sintering furnace for sintering, setting the sintering temperature to be 1050 +/-20 ℃, applying the pressure to be 40MPa, preserving the temperature for 10min, and cooling to room temperature to obtain the block composite material.
Fig. 4 is a scanning electron micrograph of the inlaid particle reinforced high-entropy alloy-based superhard nanocomposite prepared in example 3. As can be seen from fig. 4, the white reinforcing phase particles in this example are uniformly distributed on the high-entropy alloy matrix.
Example 4
A high-entropy alloy-based nano superhard composite material reinforced by inlaid particles comprises a high-entropy alloy matrix component including Al, Co, Cr, Fe, Ni, Mn, Mo, Nb and Zr, and reinforcing phase particles including WC and TiC. The mass fraction of the reinforced phase particles is 30 percent, the total mass fraction of Mo, Nb and Zr is less than or equal to 5 percent, and the mass fractions of Al, Co, Cr, Fe, Ni and Mn elements are all more than 10 percent.
In this embodiment, the preparation method of the grain-embedded reinforced high-entropy alloy-based nano superhard composite material comprises the following steps:
(1) weighing metal powder required by preparing the composite material according to the determined proportion;
(2) sealing metal powder and a dispersing agent (alcohol) into a ball milling tank under an inert gas (argon) environment;
(3) putting a ball milling tank into a ball mill to perform ball milling refinement on the powder, setting the ball milling rotation speed to be 300r/min, setting the time to be 15h, pausing for 30min every time the ball mill runs for 30min, putting the taken wet powder into a vacuum drying oven to be dried after the ball milling is finished, setting the temperature to be 65 ℃ and the time to be 6h, and taking the wet powder out after the drying is finished;
(4) and (2) putting the metal powder into a graphite die, putting the graphite die into a discharge plasma sintering furnace for sintering, setting the sintering temperature to be 1050 +/-20 ℃, applying the pressure to be 40MPa, preserving the temperature for 10min, and cooling to room temperature to obtain the block composite material.
Fig. 5 is a scanning electron micrograph of the inlaid particle reinforced high-entropy alloy-based superhard nanocomposite prepared in example 4. As can be seen from fig. 5, the white reinforcing phase particles in this example are uniformly distributed on the high-entropy alloy matrix.
In addition, the results of the mechanical property tests of the composite materials of examples 1 to 4 are shown in table 1.
TABLE 1 mechanical Properties of the composites of examples 1-4
Figure BDA0003672867210000091
As can be seen from table 1, the composite material in the present application exhibits extremely excellent mechanical properties. Specifically, the composite material of example 1 had a hardness of 996.3HV, a compressive strength of 1414.8MPa, and an abrasion loss of 427299.36 μm 3 The coefficient of friction was 0.35. The composite material of example 2 had a hardness of 1164.3HV, a compressive strength of 1565.4MPa, and an abrasion loss of 442170.16 μm 3 The coefficient of friction was 0.32. The composite material of example 3 had a hardness of 1531.7HV, a compressive strength of 1395.1MPa, and an abrasion loss of 250740.32 μm 3 The coefficient of friction was 0.37. The composite material of example 4 had a hardness of 1392.0HV, a compressive strength of 995.7MPa, and an abrasion loss of 287661.44 μm 3 The coefficient of friction was 0.39.
In addition, as can be seen from table 1, the hardness and the compressive strength of the composite material tend to increase and decrease with the increase of the mass fraction of WC and TiC, the abrasion loss and the friction coefficient tend to increase after decreasing, and the performance of the composite material is the best when 10 to 11 wt% of reinforcing phase particles are added.
In addition, compared with a composite material which is not added with reinforcing phase particles and only comprises a high-entropy alloy matrix, the friction coefficient of the composite material of the embodiment of the application is reduced by more than 74%, and the abrasion loss is reduced by more than 60%.
In the description herein, reference to the description of the terms "one embodiment," "some embodiments," "an illustrative embodiment," "an example," "a specific example," or "some examples" or the like means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the application. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
While embodiments of the present application have been shown and described, it will be understood by those of ordinary skill in the art that: various changes, modifications, substitutions and alterations can be made to the embodiments without departing from the principles and spirit of the application, the scope of which is defined by the claims and their equivalents.

Claims (9)

1. A high-entropy alloy-based nano superhard composite material reinforced by inlaid particles is characterized by comprising the following components in percentage by weight: the high-entropy alloy comprises a high-entropy alloy matrix and reinforcing phase particles, wherein the reinforcing phase particles are dispersed in the high-entropy alloy matrix, the high-entropy alloy matrix comprises a base matrix and a reinforcing matrix, the base matrix comprises Al, Co, Cr, Fe, Ni and Mn, the reinforcing matrix comprises Mo, Nb and Zr, and the reinforcing phase particles comprise WC and TiC.
2. Composite material according to claim 1, characterized in that the mass fraction of the reinforcing phase particles is greater than or equal to 5% and less than or equal to 30%.
3. Composite material according to claim 1 or 2, characterized in that the reinforcing matrix mass fraction is less than or equal to 5%.
4. A method of producing a high entropy alloy based nano ultra hard composite material reinforced with mosaic particles according to any one of claims 1 to 3, comprising:
weighing Al powder, Co powder, Cr powder, Fe powder, Ni powder, Mn powder, Mo powder, Nb powder, Zr powder, WC powder and TiC powder according to a proportion, and uniformly mixing to form composite material powder;
performing ball milling treatment on the composite material powder to enable the composite material powder to be nano-sized to obtain nanocrystalline powder;
and sintering the nanocrystalline powder to obtain the block composite material.
5. The production method according to claim 4, wherein the particle sizes of the Al powder, the Co powder, the Cr powder, the Fe powder, the Ni powder, the Mn powder, the Mo powder, the Nb powder, the Zr powder, the WC powder, and the TiC powder are each 30 μm or more and 50 μm or less.
6. The method according to claim 4, wherein the ball-milling of the composite powder to form the composite powder into a nano-size comprises:
and sealing the composite material powder and the dispersing agent into a ball milling tank for ball milling under an inert gas environment, wherein the rotating speed of the ball mill is 300r/min and the ball milling time is 15h in the ball milling process.
7. The preparation method according to claim 6, wherein the ball mill is paused for 20min to 30min every 30min of operation during the ball milling process.
8. The production method according to any one of claims 4 to 7, wherein the nanocrystalline powder is subjected to a sintering process including: sintering the metal powder by using a discharge plasma sintering furnace, heating the temperature in the discharge plasma sintering furnace to 1050 +/-20 ℃, adding the pressure to 40MPa, preserving the temperature for 10min, and cooling to room temperature to obtain the massive composite material.
9. A high-entropy alloy-based nano superhard composite material reinforced by inlaid particles, prepared by the preparation method according to any one of claims 4 to 8.
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