CN111910114A - Endogenous nano carbide reinforced multi-scale FCC high-entropy alloy-based composite material and preparation method thereof - Google Patents
Endogenous nano carbide reinforced multi-scale FCC high-entropy alloy-based composite material and preparation method thereof Download PDFInfo
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- 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
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- C22C32/0047—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents
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Abstract
The invention discloses an endogenic nano-carbide reinforced multi-scale FCC high-entropy alloy-based composite material and a preparation method thereof. The composite composition (at.%): 10-35% of Fe, 10-35% of Co, 10-35% of Ni, 0-25% of Cu, 0-25% of Mn, 5-15% of Nb, 5-15% of Ti or 5-25% of Nb and Ti, and a C source (not more than 15 at.%) introduced by a process control agent. The preparation method comprises the following steps: uniformly mixing the element (or alloy) powder; preparing high-entropy alloy powder by adopting a mechanical alloying method; sintering to obtain the block composite material. The microstructure of the composite material is composed of nano carbide and a multi-scale FCC high-entropy alloy solid solution phase, the strength of the material is effectively improved by the multi-scale microstructure, good plasticity can be kept, and the urgent requirements of high strength and high toughness of advanced structural materials are met. The method has the characteristics of short flow, low energy consumption and the like.
Description
Technical Field
The invention belongs to the technical field of preparation of high-entropy alloys and composites thereof, and particularly relates to an endogenous nano carbide reinforced multi-scale FCC (fluid catalytic cracking) high-entropy alloy-based composite and a preparation method thereof.
Background
The high-entropy alloy is a novel solid solution alloy, generally contains more than 4 main elements, and the configuration entropy change satisfies deltaS conf More than or equal to 1.5R. The alloy is characterized in that the 'high entropy effect' caused by the multi-principal element characteristic can inhibit the alloy system from forming complex intermetallic compounds, thereby forming simple solid solution phases, namely FCC (face centered cubic) phase, BCC (body centered cubic) phase, HCP (hexagonal close packed) phase or the composite of the FCC (face centered cubic) phase, the BCC (body centered cubic) phase and the HCP (hexagonal close packed) phase. The single-phase FCC high-entropy alloy has excellent plasticity, and is relatively lower in price compared with BCC and HCP high-entropy alloys containing alloy elements such as Zr, Ta, W, Hf and Dy. However, the lower yield strength (mostly in the range of 130-450 MPa) of the FCC high-entropy alloy becomes one of the key factors restricting the large-scale application of the FCC high-entropy alloy in the engineering field.
Most conventional strengthening methods (such as grain refinement) inevitably lose plasticity while improving strength. In contrast, in the literature (Evan Ma, Ting Zhu, "Materials structure and microstructure in metals", Materials Today, 2017, 20(6): 323-331), it is pointed out that after the multi-scale microstructure is introduced, the strength of the alloy is greatly improved and good plasticity is retained, so that the high-strength and high-toughness metal structural material can be obtained. However, in the existing research, a casting method and subsequent hot working are mostly used for introducing a multi-scale microstructure into an alloy, which requires a severe deformation (such as a rolling deformation amount exceeding 75%) and a precise heat treatment process, and has the disadvantages of long process flow, poor controllability and high energy consumption.
Research shows that the multi-scale FCC high-entropy alloy can be prepared by adopting the short-flow process of mechanical alloying and Spark Plasma Sintering (SPS). Namely, FCC high-entropy alloy nanocrystalline powder is obtained through mechanical alloying, and then SPS is adopted to sinter into a block high-entropy alloy. The local overheating phenomenon generated in the SPS sintering process is utilized to quickly grow the crystal grains in the local area, so that the multi-scale microstructure is obtained. However, depending only on the temperature gradient caused by local overheating, a multi-scale microstructure with large grain size difference is often not obtained.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention aims to provide an endogenous nano carbide reinforced multi-scale FCC high-entropy alloy-based composite material and a preparation method thereof.
The invention aims to provide an endogenetic nano carbide reinforced multi-scale FCC high-entropy alloy-based composite material and a preparation method thereof through a process of mechanical alloying and spark plasma sintering, so as to realize the preparation of a block composite material with short flow, low energy consumption, ultrahigh strength and good plasticity.
The invention discovers that in the SPS sintering process, the added carbon element and the C source generated by the decomposition of the process control agent can generate in-situ self-generated reaction to form endogenous nano carbide which is uniformly distributed in an FCC matrix. By utilizing the pinning effect of the endogenous nano carbide on the grain boundary, the asynchronous growth of grains can be further promoted, so that a multi-scale microstructure with larger grain size difference is formed. The cooperative reinforcement of the endogenous nano carbide (dispersion reinforcement) and the multi-scale microstructure can obviously improve the strength of the high-entropy alloy-based composite material, and simultaneously, the good plasticity is kept. Therefore, the invention provides an endogenous nano carbide reinforced multi-scale FCC high-entropy alloy-based composite material with a microstructure composed of nano carbide and a multi-scale FCC high-entropy alloy solid solution phase, so as to meet the urgent requirements of high strength and high toughness of advanced structural materials.
The purpose of the invention is realized by at least one of the following technical solutions.
The invention provides an endogenic nano-carbide reinforced multi-scale FCC high-entropy alloy-based composite material, which comprises the following components in atomic percentage (at.%):
Fe 10-35 at.%；
Co10-35 at.%；
Ni 10-35 at.%；
Cu 0-25 at.%；
Mn 0-25 at.%；
Nb0-15at.%；
Ti0-15at.%；
C0-15 at.%。
further, the material comprises the following components in atomic percentage:
Fe 10-35 at.%；
Co10-35 at.%；
Ni 10-35 at.%；
Cu 0-25 at.%；
Mn 0-25 at.%；
Nb5-15at.%；
C0-15 at.%。
further, the material comprises the following components in atomic percentage:
Fe 10-35 at.%；
Co10-35 at.%；
Ni 10-35 at.%；
Cu 0-25 at.%；
Mn 0-25 at.%；
Ti5-15at.%；
C0-15 at.%。
further, the sum of the atomic percentages of Nb and Ti is 5-25% by atomic percentage.
The endogenous nano carbide reinforced multi-scale FCC high-entropy alloy-based composite material provided by the invention contains C element introduced by a process control agent in the preparation method.
Furthermore, in the material, the grain size of the FCC high-entropy alloy matrix presents gradient distribution, and the average size of endogenous nano-carbides does not exceed 100 nm.
The invention provides a method for preparing an endogenous nano carbide reinforced multi-scale FCC high-entropy alloy-based composite material, which comprises the following steps:
(1) preparing a powder mixture by adopting element powder or alloy powder according to the atomic percentage: mixing Fe, Co, Ni, Cu, Mn, Nb and Ti element powder or alloy powder to obtain a mixture;
(2) putting the mixture obtained in the step (1) into a powder mixer, and uniformly mixing to obtain mixed powder;
(3) putting the mixed powder obtained in the step (2) into a stainless steel vacuum ball-milling tank, filling argon for protection, and carrying out wet milling under argon atmosphere to obtain high-entropy alloy powder;
(4) and (3) placing the high-entropy alloy powder obtained in the step (3) into a vacuum drying oven for drying treatment, then placing the high-entropy alloy powder into a graphite sintering mold, and heating by adopting a discharge plasma system for sintering treatment to obtain the endogenous nano carbide reinforced multi-scale FCC high-entropy alloy-based composite material (block composite material).
Further, the mixing time of the step (2) is 4-8 hours.
Further, the wet grinding time in the step (3) is 20-60 hours; the process control agent for wet grinding is an alkane organic solvent, preferably cyclohexane (C)6H12) (ii) a The wet grinding rotating speed is more than or equal to 200 rpm; the material ratio (mass ratio) of the wet-grinding balls is 10:1-20: 1.
Further, the temperature rise in the step (4) is a step-type temperature rise, the temperature rise is carried out at a speed of 50-200 ℃/min when the temperature is lower than 1000 ℃, and the temperature rise is carried out at a speed of 10-50 ℃/min when the temperature is higher than 1000 ℃; the sintering temperature is 900-1250 ℃; the sintering treatment time is 10-60 min; the pressure of the sintering treatment is 30-100 MPa; the vacuum degree of the sintering treatment is less than 8 Pa.
The preparation method provided by the invention adopts the process of mechanical alloying and spark plasma sintering to obtain the high-strength and high-toughness FCC high-entropy alloy-based composite material. The gradient FCC high-entropy alloy-based composite material enhanced by the endogenous nano carbides is obtained through spark plasma sintering, the microstructure of the composite material is a nano carbide and multi-scale FCC high-entropy alloy solid solution phase, and the composite material has excellent mechanical properties.
The microscopic structure of the endogenous nano carbide reinforced multi-scale FCC high-entropy alloy-based composite material provided by the invention is composed of a nano carbide and a multi-scale FCC high-entropy alloy solid solution phase, wherein the grain size of an FCC high-entropy alloy matrix is in gradient distribution, the average size of the endogenous nano carbide is not more than 100nm, and the endogenous nano carbide is uniformly distributed in the FCC high-entropy alloy matrix. Compared with the complex process for preparing the multi-scale FCC high-entropy alloy by the casting method and the subsequent hot working, the process of mechanical alloying and spark plasma sintering adopted by the invention has the characteristics of short flow, low energy consumption and the like.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) according to the preparation method provided by the invention, a C source generated by decomposing a process control agent in SPS sintering and Nb or Ti or Nb and Ti elements are subjected to in-situ self-generation reaction to form endogenous nano carbides (the average size is less than 100 nm), and the endogenous nano carbides are uniformly distributed in an FCC high-entropy alloy matrix to generate a remarkable dispersion strengthening effect and improve the material strength;
(2) according to the preparation method provided by the invention, a multi-scale microstructure is introduced into the alloy by utilizing local overheating (temperature gradient) generated in SPS sintering and the pinning effect of endogenous nano carbide, so that the strength is remarkably improved and good plasticity is maintained; compared with the traditional method of introducing a multi-scale microstructure through severe plastic deformation (such as rolling and high-pressure torsion) and subsequent precise heat treatment, the method has the advantages of simple preparation process, short flow, low energy consumption and good development prospect;
(3) the microstructure of the prepared endogenous nano carbide reinforced multi-scale FCC high-entropy alloy-based composite material is composed of an endogenous nano carbide and a multi-scale FCC high-entropy alloy solid solution phase, and the average size of the endogenous nano carbide is not more than 100 nm; the room temperature tensile yield strength is 900-1250MPa, the tensile strength is 1050-1450MPa, and the tensile breaking strain is 4-13%, so that the requirements of high strength and high toughness of the advanced structural material are met.
Drawings
FIG. 1 is an XRD pattern of an endogenetic nano-carbide enhanced multi-scale FCC high-entropy alloy-based composite prepared in example 1;
fig. 2 and 3 are Transmission Electron Microscope (TEM) images of the endogenic nanocarbide-reinforced multi-scale FCC high-entropy alloy-based composite prepared in example 1 at low power and high power, respectively;
FIG. 4 is a room temperature tensile stress-strain curve of the endogenetic nanocarbide enhanced multi-scale FCC high entropy alloy based composite prepared in example 1;
FIG. 5 is an XRD pattern of the endogenetic nanocarbide enhanced multi-scale FCC high-entropy alloy-based composite prepared in example 3;
fig. 6 and 7 are Transmission Electron Microscope (TEM) images of low power and high power, respectively, of the endogenic nanocarbide-reinforced multi-scale FCC high-entropy alloy-based composite prepared in example 3;
fig. 8 is a room temperature tensile stress-strain curve of the endogenetic nanocarbide enhanced multi-scale FCC high-entropy alloy-based composite prepared in example 3.
Detailed Description
The following examples are presented to further illustrate the practice of the invention, but the practice and protection of the invention is not limited thereto. It is noted that the processes described below, if not specifically described in detail, are all realizable or understandable by those skilled in the art with reference to the prior art. The reagents or apparatus used are not indicated to the manufacturer, and are considered to be conventional products available by commercial purchase.
Example 1
The preparation method of the endogenous nano carbide reinforced multi-scale FCC high-entropy alloy-based composite material specifically comprises the following steps:
(1) preparing element powder into mixed powder according to the following atomic percentages: 25% of Fe, 35% of Co, 25% of Ni and 15% of Nb, wherein the average grain diameter of each element powder is less than or equal to 45 mu m, and the purity is more than or equal to 99.7 wt.%;
(2) placing the prepared mixed powder into a powder mixer to be mixed for 6 hours, and uniformly mixing;
(3) and (3) putting the uniformly mixed powder into a stainless steel vacuum ball-milling tank, filling argon gas into the ball-milling tank for protection, and wet-milling for 60 hours to obtain the high-entropy alloy powder. The process control agent is cyclohexane (C)6H12) The ball milling rotating speed is 300rpm, and the ball material ratio (mass ratio) is 10: 1;
(4) putting the wet-milled high-entropy alloy powder into a vacuum drying oven for drying, putting 80g of the dried high-entropy alloy powder into a graphite sintering die with the diameter of phi 40mm, and sintering by adopting discharge plasma to form a block composite material; the sintering process parameters are as follows:
sintering temperature: 1050 ℃;
the heating rate is as follows: the temperature of the room temperature to 1000 ℃ is 80 ℃/min, and the temperature of the room temperature to 1050 ℃ is 10 ℃/min;
and (3) heat preservation time: 30 min; sintering pressure: 50 MPa; sintering vacuum degree: 8 Pa.
The phase composition of the nano-carbide reinforced multi-scale FCC high-entropy alloy-based composite material prepared by the embodiment is shown in figure 1, the picture of a microstructure transmission electron microscope is shown in figures 2 and 3, the material is composed of nano NbC and a multi-scale FCC high-entropy alloy solid solution phase, wherein the grain size of an FCC matrix presents gradient distribution (composed of micron crystal and ultra-fine crystal), the average grain size is 428nm, and the average size of endogenous nano NbC particles is 72 nm; the mechanical properties of the material are shown in figure 4, the room-temperature tensile yield strength, tensile strength and tensile breaking strain are 1127MPa, 1138MPa and 7.0 percent respectively, and the mechanical properties are excellent.
Example 2
The preparation method of the endogenous nano carbide reinforced multi-scale FCC high-entropy alloy-based composite material specifically comprises the following steps:
(1) preparing element powder into mixed powder according to the following atomic percentages: 35% of Fe, 24% of Co, 26% of Ni and 15% of Ti, wherein the average grain diameter of each element powder is less than or equal to 45 mu m, and the purity is more than or equal to 99.7 wt%;
(2) placing the prepared mixed powder into a powder mixer, mixing for 5 hours, and uniformly mixing;
(3) and (3) putting the uniformly mixed powder into a stainless steel vacuum ball-milling tank, filling argon gas into the ball-milling tank for protection, and then carrying out wet milling for 40h to obtain the high-entropy alloy powder. The process control agent is cyclohexane (C)6H12) The ball milling rotating speed is 300rpm, and the ball material ratio (mass ratio) is 15: 1;
(4) putting the wet-milled high-entropy alloy powder into a vacuum drying oven for drying, putting 80g of the dried high-entropy alloy powder into a graphite sintering die with the diameter of phi 40mm, and sintering by adopting discharge plasma to form a block composite material; the sintering process parameters are as follows:
sintering temperature: 1100 ℃;
the heating rate is as follows: room temperature to 1000 ℃ is 100 ℃/min, 1000 ℃ to 1100 ℃ is 25 ℃/min;
and (3) heat preservation time: 20 min; sintering pressure: 80 MPa; sintering vacuum degree: 8 Pa.
In the nano-carbide reinforced multi-scale FCC high-entropy alloy-based composite material prepared by the embodiment, the microstructure is composed of a nano TiC + multi-scale FCC high-entropy alloy solid solution phase, wherein the grain size of the FCC matrix is in gradient distribution (composed of a micron crystal and a superfine crystal), the average grain size is 461nm, and the average size of endogenous nano TiC particles is 77 nm; the room-temperature tensile yield strength, the tensile strength and the tensile breaking strain are 1121MPa, 1450MPa and 11.4 percent respectively, and the mechanical property is excellent.
Example 3
The preparation method of the endogenous nano carbide reinforced multi-scale FCC high-entropy alloy-based composite material specifically comprises the following steps:
(1) preparing element powder into mixed powder according to the following atomic percentages: 10% of Fe, 28% of Co, 32% of Ni, 25% of Mn and 5% of Nb, wherein the average grain diameter of each element powder is less than or equal to 45 mu m, and the purity is more than or equal to 99.7 wt%;
(2) putting the prepared mixed powder into a powder mixer, mixing for 8 hours, and uniformly mixing;
(3) loading the uniformly mixed powder into a containerAnd in a stainless steel vacuum ball milling tank, filling argon for protection, and then carrying out wet milling for 60h to obtain the high-entropy alloy powder. The process control agent is an alkane organic solvent-n-heptane (C)7H16) The ball milling rotating speed is 250rpm, and the ball material ratio (mass ratio) is 20: 1;
(4) putting the wet-milled high-entropy alloy powder into a vacuum drying oven for drying, putting 80g of the dried high-entropy alloy powder into a graphite sintering die with the diameter of phi 40mm, and sintering by adopting discharge plasma to form a block composite material; the sintering process parameters are as follows:
sintering temperature: 1250 ℃;
the heating rate is as follows: the temperature of room temperature to 1000 ℃ is 200 ℃/min, and the temperature of 1000 ℃ to 1250 ℃ is 50 ℃/min;
and (3) heat preservation time: 10 min; sintering pressure: 30 MPa; sintering vacuum degree: 8 Pa.
The phase composition of the nano-carbide reinforced multi-scale FCC high-entropy alloy-based composite material prepared by the embodiment is shown in a figure 5, the picture of a microstructure transmission electron microscope is shown in a figure 6 and a figure 7, the material is composed of a nano NbC + multi-scale FCC high-entropy alloy solid solution phase, the grain size of an FCC matrix is in gradient distribution (composed of micron crystals and ultra-fine crystals), the average grain size is 800nm, and the average size of endogenous nano NbC particles is 97 nm; the mechanical properties of the material are shown in figure 8, the room-temperature tensile yield strength, tensile strength and tensile breaking strain are 900MPa, 1139MPa and 13 percent respectively, and the mechanical properties are excellent.
Example 4
The preparation method of the endogenous nano carbide reinforced multi-scale FCC high-entropy alloy-based composite material specifically comprises the following steps:
(1) preparing element powder into mixed powder according to the following atomic percentages: 25% of Fe, 10% of Co, 35% of Ni, 25% of Cu and 5% of Ti, wherein the average grain diameter of each element powder is less than or equal to 45 mu m, and the purity is more than or equal to 99.7 wt.%;
(2) placing the prepared mixed powder into a powder mixer to be mixed for 4 hours, and uniformly mixing;
(3) putting the uniformly mixed powder into a stainless steel vacuum ball milling tank, and filling argon into the ball milling tank for protectionAnd then wet grinding for 40h to obtain the high-entropy alloy powder. The process control agent is cyclohexane (C)6H12) The ball milling rotating speed is 350rpm, and the ball material ratio (mass ratio) is 20: 1;
(4) putting the wet-milled high-entropy alloy powder into a vacuum drying oven for drying, putting 80g of the dried high-entropy alloy powder into a graphite sintering die with the diameter of phi 40mm, and sintering by adopting discharge plasma to form a block composite material; the sintering process parameters are as follows:
sintering temperature: 1200 ℃;
the heating rate is as follows: 125 ℃/min between room temperature and 1000 ℃, and 20 ℃/min between 1000 ℃ and 1200 ℃;
and (3) heat preservation time: 40 min; sintering pressure: 50 MPa; sintering vacuum degree: 8 Pa.
In the nano-carbide reinforced multi-scale FCC high-entropy alloy-based composite material prepared by the embodiment, a microstructure consists of a nano TiC + multi-scale FCC high-entropy alloy solid solution phase, wherein the grain size of an FCC matrix is in gradient distribution (consisting of micron crystals and superfine crystals), the average grain size is 709nm, and the average size of endogenous nano TiC particles is 89 nm; the room temperature tensile yield strength, tensile strength and tensile breaking strain are 916MPa, 1050MPa and 12.1 percent respectively, and the mechanical property is excellent.
Example 5
The preparation method of the endogenous nano carbide reinforced multi-scale FCC high-entropy alloy-based composite material specifically comprises the following steps:
(1) preparing element powder into mixed powder according to atomic percent: 30% of Fe, 25% of Co, 10% of Ni, 15% of Cu, 15% of Mn, 4% of Ti, 1% of Nb, wherein the average grain diameter of each element powder is less than or equal to 45 mu m, and the purity is more than or equal to 99.7 wt%;
(2) placing the prepared mixed powder into a powder mixer, mixing for 7 hours, and uniformly mixing;
(3) and (3) putting the uniformly mixed powder into a stainless steel vacuum ball-milling tank, filling argon gas into the ball-milling tank for protection, and then carrying out wet milling for 50h to obtain the high-entropy alloy powder. The process control agent is cyclohexane (C)6H12) The ball milling rotating speed is 200rpm, and the ball material ratio (mass ratio) is 20: 1;
(4) putting the wet-milled high-entropy alloy powder into a vacuum drying oven for drying, putting 80g of the dried high-entropy alloy powder into a graphite sintering die with the diameter of phi 40mm, and sintering by adopting discharge plasma to form a block composite material; the sintering process parameters are as follows:
sintering temperature: 900 ℃;
the heating rate is as follows: the temperature is 50 ℃/min from room temperature to 900 ℃;
and (3) heat preservation time: 60 min; sintering pressure: 100 MPa; sintering vacuum degree: 8 Pa.
In the nano-carbide-reinforced multi-scale FCC high-entropy alloy-based composite material prepared in this embodiment, the microstructure is composed of a "nano (Ti, Nb) C + multi-scale FCC high-entropy alloy solid solution phase", wherein the size of the FCC matrix crystal grains is in gradient distribution (composed of "micro crystal + ultra-fine crystal"), the average size of the crystal grains is 300nm, and the average size of endogenous nano (Ti, Nb) C particles is 65 nm; the room temperature tensile yield strength, tensile strength and tensile breaking strain are 1250MPa, 1261MPa and 4.0% respectively, and the mechanical property is excellent.
Example 6
The preparation method of the endogenous nano carbide reinforced multi-scale FCC high-entropy alloy-based composite material specifically comprises the following steps:
(1) according to atomic percentage, the content of the prepared mixed powder is as follows: 25% of Fe, 25% of Co, 25% of Ni, 12.5% of Nb and 12.5% of Ti, wherein the Fe-Ni, Nb-Ti, Fe, Ti and Co powders are prepared, the average grain diameter of each powder is less than or equal to 45 mu m, and the purity is more than or equal to 99.7 wt%;
(2) placing the prepared mixed powder into a powder mixer to be mixed for 6 hours, and uniformly mixing;
(3) and (3) putting the uniformly mixed powder into a stainless steel vacuum ball-milling tank, filling argon gas into the ball-milling tank for protection, and wet-milling for 60 hours to obtain the high-entropy alloy powder. The process control agent is cyclohexane (C)6H12) The ball milling rotating speed is 300rpm, and the ball material ratio (mass ratio) is 10: 1;
(4) putting the wet-milled high-entropy alloy powder into a vacuum drying oven for drying, putting 80g of the dried high-entropy alloy powder into a graphite sintering die with the diameter of phi 40mm, and sintering by adopting discharge plasma to form a block composite material; the sintering process parameters are as follows:
sintering temperature: 1000 ℃;
the heating rate is as follows: the temperature of the room temperature to 1000 ℃ is 125 ℃/min;
and (3) heat preservation time: 45 min; sintering pressure: 60 MPa; sintering vacuum degree: 8 Pa.
In the nano-carbide-reinforced multi-scale FCC high-entropy alloy-based composite material prepared in this embodiment, the microstructure is composed of a "nano (Ti, Nb) C + multi-scale FCC high-entropy alloy solid solution phase", wherein the size of the FCC matrix crystal grain presents a gradient distribution (composed of "micro crystal + ultra-fine crystal"), the average crystal grain size is 382nm, and the average size of endogenous nano (Ti, Nb) C particles is 69 nm; the room-temperature tensile yield strength, the tensile strength and the tensile breaking strain are 1183MPa, 1206MPa and 6.2 percent respectively, and the mechanical property is excellent.
The above examples are only preferred embodiments of the present invention, which are intended to be illustrative and not limiting, and those skilled in the art should understand that they can make various changes, substitutions and alterations without departing from the spirit and scope of the invention.
Claims (10)
1. An endogenic nano-carbide reinforced multi-scale FCC high-entropy alloy-based composite material is characterized by comprising the following components in atomic percentage:
Fe 10-35 at.%；
Co 10-35 at.%；
Ni 10-35 at.%；
Cu 0-25 at.%；
Mn 0-25 at.%；
Nb 0-15at.%；
Ti 0-15at.%；
C 0-15 at.%。
2. the endogenic nanocarbide-reinforced multi-scale FCC high-entropy alloy-based composite material according to claim 1, characterized in that the material comprises the following components in atomic percent:
Fe 10-35 at.%；
Co 10-35 at.%；
Ni 10-35 at.%；
Cu 0-25 at.%；
Mn 0-25 at.%；
Nb 5-15at.%；
C 0-15 at.%。
3. the endogenic nanocarbide-reinforced multi-scale FCC high-entropy alloy-based composite material according to claim 1, characterized in that the material comprises the following components in atomic percent:
Fe 10-35 at.%；
Co 10-35 at.%；
Ni 10-35 at.%；
Cu 0-25 at.%；
Mn 0-25 at.%；
Ti 5-15at.%；
C 0-15 at.%。
4. the endogenic nanocarbide-reinforced multi-scale FCC high-entropy alloy-based composite material of claim 1, wherein the sum of the atomic percentages of Nb and Ti is 5-25% in terms of atomic percentage.
5. The endogenic nanocarbide-reinforced multi-scale FCC high-entropy alloy-based composite material according to claim 1, wherein the grain size of the FCC high-entropy alloy matrix exhibits a gradient distribution, and the average size of the endogenic nanocarbides does not exceed 100 nm.
6. A method for preparing the endogenous nanocarbide reinforced multi-scale FCC high-entropy alloy-based composite material according to any one of claims 1 to 5, comprising the following steps:
(1) mixing Fe, Co, Ni, Cu, Mn, Nb and Ti element powder or alloy powder to obtain a mixture;
(2) putting the mixture obtained in the step (1) into a powder mixer, and uniformly mixing to obtain mixed powder;
(3) wet-grinding the mixed powder obtained in the step (2) in an argon atmosphere to obtain high-entropy alloy powder;
(4) and (4) drying the high-entropy alloy powder obtained in the step (3), and then heating for sintering to obtain the endogenous nano carbide reinforced multi-scale FCC high-entropy alloy-based composite material.
7. The method for preparing the endogenic nanocarbide-reinforced multi-scale FCC high-entropy alloy-based composite material according to claim 6, wherein the mixing time of step (2) is 4 to 8 hours.
8. The method for preparing the endogenic nanocarbide-reinforced multi-scale FCC high-entropy alloy-based composite material according to claim 6, wherein the wet milling time of step (3) is 20 to 60 hours; the process control agent adopted in wet grinding is an alkane organic solvent; the wet grinding rotating speed is more than or equal to 200 rpm; the wet grinding ball material ratio is 10:1-20: 1.
9. The method for preparing the endogenic nanocarbide-reinforced multi-scale FCC high-entropy alloy-based composite material according to claim 8, wherein the process control agent used for wet milling is cyclohexane.
10. The preparation method of the endogenic nanocarbide-reinforced multi-scale FCC high-entropy alloy-based composite material according to claim 6, wherein the temperature rise in the step (4) is a step-type temperature rise, and the temperature rise is performed at a rate of 50-200 ℃/min when the temperature is lower than 1000 ℃ and at a rate of 10-50 ℃/min when the temperature is higher than 1000 ℃; the sintering temperature is 900-1250 ℃; the sintering treatment time is 10-60 min; the pressure of the sintering treatment is 30-100 MPa; the vacuum degree of the sintering treatment is less than 8 Pa.
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| CN113337746B (en) * | 2021-05-31 | 2022-03-15 | 上海大学 | Preparation method of carbide-reinforced high-entropy alloy composite material |
| CN113444956A (en) * | 2021-06-11 | 2021-09-28 | 西安工业大学 | Ceramic particle in-situ reinforced high-entropy alloy and preparation method thereof |
| CN113751707A (en) * | 2021-09-14 | 2021-12-07 | 郑州磨料磨具磨削研究所有限公司 | Method for preparing nano carbide particle dispersion strengthening alloy powder |
| CN113751707B (en) * | 2021-09-14 | 2023-08-22 | 郑州磨料磨具磨削研究所有限公司 | Method for preparing nano carbide particle dispersion strengthening alloy powder |
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| WO2023104780A1 (en) * | 2021-12-07 | 2023-06-15 | Vulkam | Metallic glasses made of ni-nb-cu alloy |
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