CN115747610A - SiC-doped high-entropy alloy and preparation method and application thereof - Google Patents
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- 239000000956 alloy Substances 0.000 title claims abstract description 77
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 76
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000011159 matrix material Substances 0.000 claims abstract description 11
- 239000005543 nano-size silicon particle Substances 0.000 claims abstract description 8
- 238000000498 ball milling Methods 0.000 claims description 26
- 238000005245 sintering Methods 0.000 claims description 20
- 238000007731 hot pressing Methods 0.000 claims description 18
- 238000002156 mixing Methods 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 10
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Abstract
The invention provides a SiC doped high-entropy alloy and a preparation method and application thereof, belonging to the technical field of high-entropy alloys. The high-entropy alloy is SiC-doped FeNiCoCr high-entropy alloy, and consists of a disordered FCC matrix (face-centered cubic) and a large number of regular cubic forms L1 in the matrix on a nano scale 2 Type Ni 3 Si nanoparticles precipitate out the phase composition, realizing the rule L1 2 Type Ni 3 And (3) a strengthening design of the Si nanoparticle strengthened FeNiCoCr high-entropy alloy. Wherein a large amount of Ni 3 The Si nano precipitation has obvious effect on improving the yield strength of the alloy, and is due to precipitationPhase Ni 3 The mismatching degree of the Si and the substrate interface is low, the premature instability caused by stress concentration can be avoided, and the brittleness L2 is avoided 1 Type Ni 2 The precipitation of AlTi can improve the yield strength and maintain good plasticity.
Description
Technical Field
The invention relates to the technical field of high-entropy alloys, in particular to a SiC doped high-entropy alloy and a preparation method and application thereof.
Background
High Entropy Alloys (HEAs) due to flexible composition and microstructure control space, often can achieve mechanical and physical properties such as good low temperature fracture resistance, excellent strength-ductility combinations, wear resistance, oxidation resistance, and corrosion resistance that are difficult to achieve with traditional alloy materials. However, there are some problems that restrict the development of high-entropy alloys, such as that having a single-phase face-centered cubic solid solution structure, which generally exhibits good plasticity but low strength. FeNiCoCrHEAs are typical Face Centered Cubic (FCC) alloys that have desirable plasticity at room temperature, but low yield strength. How to improve the yield strength of FeNiCoCr HEAs becomes a focus of attention of researchers.
Disclosure of Invention
The invention aims to provide a SiC doped high-entropy alloy, a preparation method and application thereof.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a SiC doped high-entropy alloy with a chemical general formula of Fe a Ni b Co c Cr d (SiC) e Wherein a is more than or equal to 20 percent and less than or equal to25 percent, more than or equal to 20 percent and less than or equal to 25 percent of b, more than or equal to 20 percent and less than or equal to 25 percent of c, more than or equal to 20 percent and less than or equal to 25 percent of d, more than or equal to 3.5 percent and less than or equal to 13.5 percent of e, wherein a + b + c + d + e =100 percent, and a, b, c, d and e respectively correspond to the mole percent of each element.
Preferably, the SiC doped high-entropy alloy consists of a disordered face-centered cubic matrix and a regular cubic form L1 positioned in the face-centered cubic matrix 2 Type Ni 3 Si nanoparticles.
The invention provides a preparation method of the SiC doped high-entropy alloy, which comprises the following steps:
and (3) performing ball milling and mixing on Fe, ni, co, cr and SiC according to a ratio, and performing vacuum hot-pressing sintering to obtain the SiC-doped high-entropy alloy.
Preferably, the purity of the Fe, the Ni, the Co and the Cr is more than or equal to 99.9 percent, and the average grain size is less than or equal to 20 mu m; the purity of the SiC is more than or equal to 99.9 percent, and the average particle size is less than or equal to 1 mu m.
Preferably, the ball milling medium used for ball milling and mixing is stainless steel balls, the ball material ratio of the ball milling and mixing is 5-10.
Preferably, before the vacuum hot-pressing sintering is carried out, the vacuum degree is reduced to less than 1 × 10 -1 Pa。
Preferably, the temperature of the vacuum hot-pressing sintering is 900-1000 ℃, the pressure is 12-20 MPa, and the heat preservation time is 0.5-1 h.
Preferably, the heating rate from room temperature to the temperature of the vacuum hot-pressing sintering is 8-10 ℃/min.
The invention provides application of the SiC doped high-entropy alloy in the technical scheme or the SiC doped high-entropy alloy prepared by the preparation method in the technical scheme in the field of engineering structures.
The invention provides a SiC doped high-entropy alloy with a chemical general formula of Fe a Ni b Co c Cr d (SiC) e Wherein a is more than or equal to 20% and less than or equal to 25%, b is more than or equal to 20% and less than or equal to 25%, c is more than or equal to 20% and less than or equal to 25%, d is more than or equal to 20% and less than or equal to 25%, e is more than or equal to 3.5% and less than or equal to 13.5%, and a + b + c + d + e =100%, and a, b, c, d and e respectively correspond to the mole percentage of each element. The inventionThe high-entropy alloy is SiC-doped FeNiCoCr high-entropy alloy, and consists of an unordered FCC matrix (face-centered cubic) and a large number of regular cubic forms L1 in the matrix on a nanometer scale 2 Type Ni 3 Si nanoparticles precipitate out the phase composition, realizing the rule L1 2 Type Ni 3 And (3) a strengthening design of the Si nanoparticle strengthened FeNiCoCr high-entropy alloy. Wherein a large amount of Ni 3 Si nano precipitation has obvious effect on improving the yield strength of the alloy, and Ni is precipitated 3 The mismatching degree of the Si and the substrate interface is low, premature instability caused by stress concentration can be avoided, and good plasticity is kept while the yield strength is improved.
Furthermore, ni 3 Si has a high melting point, high-temperature thermal stability and R effect (a phenomenon that the strength increases with the temperature rise), and can be well adapted to a high-temperature environment. L1 provided by the invention 2 Type Ni 3 The FeNiCoCr high-entropy alloy reinforced by Si nano-particles has the room-temperature yield strength of more than 890MPa, can replace nickel-based high-temperature alloy to be used in high-temperature service environment, and has wide application prospect in the field of engineering structures.
The high-entropy alloy of the invention uses Ni 3 Substitution of Si precipitate phase for Ni 3 (Al, ti) is used as an FCC high-entropy alloy strengthening phase, and Al and Ti elements are not added in the alloy, so that brittleness L2 is avoided 1 Type Ni 2 And the precipitation of AlTi ensures the good plasticity of the high-entropy alloy. The high-entropy alloy disclosed by the invention not only shows excellent yield strength and good plasticity, but also has a potential application prospect of a high-temperature structural material.
Furthermore, the SiC doped high-entropy alloy is prepared by adopting vacuum hot-pressing sintering, the control of the reaction process is realized by regulating and controlling key parameters such as SiC doping proportion, sintering temperature, heating rate, heat preservation time, pressure and the like, the selective reaction of SiC, cr and Ni elements is promoted, and a large amount of Ni is formed 3 Si nanometer precipitates phases, and the yield strength of the high-entropy alloy is improved.
Drawings
FIG. 1 shows Fe prepared in example 1 22.45 Ni 22.45 Co 22.45 Cr 22.45 (SiC) 10.2 A microstructure diagram of a high-entropy alloy sintered state;
FIG. 2 shows Fe prepared in example 1 22.45 Ni 22.45 Co 22.45 Cr 22.45 (SiC) 10.2 Scanning an element distribution diagram of an EDS surface of a high-entropy alloy sintered state;
FIG. 3 is Fe prepared in example 1 22.45 Ni 22.45 Co 22.45 Cr 22.45 (SiC) 10.2 HRTEM of the high-entropy alloy in a sintered state and diffraction spots after Fourier transform;
FIG. 4 shows Fe after SiC addition in example 1 22.45 Ni 22.45 Co 22.45 Cr 22.45 (SiC) 10.2 High entropy alloy and Fe without SiC in comparative example 1 25 Ni 25 Co 25 Cr 25 A compression true stress-strain curve diagram of the high-entropy alloy under the room temperature condition;
FIG. 5 is Fe prepared in example 2 23.25 Ni 23.25 Co 23.25 Cr 23.25 (SiC) 7 High entropy alloy and Fe without SiC in comparative example 1 25 Ni 25 Co 25 Cr 25 Compression true stress-strain curves of high entropy alloys at room temperature.
Detailed Description
The invention provides a SiC doped high-entropy alloy with a chemical general formula of Fe a Ni b Co c Cr d (SiC) e Wherein a is more than or equal to 20% and less than or equal to 25%, b is more than or equal to 20% and less than or equal to 25%, c is more than or equal to 20% and less than or equal to 25%, d is more than or equal to 20% and less than or equal to 25%, e is more than or equal to 3.5% and less than or equal to 13.5%, and a + b + c + d + e =100%, and a, b, c, d and e respectively correspond to the mole percentage of each element.
In the present invention, a is preferably =22.45 to 23.25% >; b preferably =22.45 to 23.25%%; c is preferably = 22.45-23.25%; d preferably =22.45 to 23.25%%; e preferably =7 to 12%.
In the invention, the SiC doped high-entropy alloy consists of a disordered face-centered cubic matrix and a regular cubic form L1 positioned in the face-centered cubic matrix 2 Type Ni 3 Si nanoparticles.
The invention provides a preparation method of the SiC doped high-entropy alloy, which comprises the following steps:
and (3) performing ball milling and mixing on Fe, ni, co, cr and SiC according to a ratio, and performing vacuum hot-pressing sintering to obtain the SiC-doped high-entropy alloy.
In the present invention, unless otherwise specified, all the starting materials required for the preparation are commercially available products well known to those skilled in the art.
In the invention, the purity of the Fe, ni, co and Cr (all metallic simple substances) is preferably more than or equal to 99.9 percent, and the average particle size is preferably less than or equal to 20 mu m; the purity of the SiC is preferably equal to or more than 99.9%, and the average particle size is preferably equal to or less than 1 μm, and more preferably 0.6 μm.
The method preferably comprises the steps of putting Fe, ni, co, cr and SiC into a stainless steel ball milling tank, and carrying out ball milling and mixing by adopting a planetary ball mill; the ball milling medium used for ball milling and mixing is preferably a stainless steel ball milling ball, and the ball milling and mixing mode is preferably dry mixing; the ball-milling mixing ball-material ratio is preferably 5-10, the rotating speed is preferably 120-200 r/min, and more preferably 150r/min; the time is preferably 3 to 5 hours, more preferably 4 hours.
After the ball milling and mixing are finished, the obtained mixed material is preferably loaded into a graphite die for vacuum hot-pressing sintering; before the vacuum hot-pressing sintering is carried out, the invention preferably carries out vacuum pumping until the vacuum degree is less than 1 multiplied by 10 -1 Pa. The graphite mold is not particularly limited in the present invention, and may be a corresponding mold well known in the art.
In the invention, the temperature of the vacuum hot pressing sintering is preferably 900-1000 ℃, and more preferably 950 ℃; the pressure is preferably 12 to 20MPa, more preferably 12.5 to 15MPa; the heat preservation time is preferably 0.5-1 h, and more preferably 0.75h; the heating rate from room temperature to the temperature of the vacuum hot-pressing sintering is preferably 8-10 ℃/min. In the vacuum hot-pressing sintering process, siC reacts with Cr and Ni elements to generate Cr 7 C 3 、Ni 3 Si, thereby forming an integral high entropy alloy.
After the vacuum hot-pressing sintering is finished, the SiC doped high-entropy alloy is obtained by preferably cooling along with the furnace.
The invention provides application of the SiC doped high-entropy alloy in the technical scheme or the SiC doped high-entropy alloy prepared by the preparation method in the technical scheme in the field of engineering structures. The method of the present invention is not particularly limited, and the method may be applied according to a method known in the art.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
Example 1
The general formula of the high-entropy alloy is Fe 22.45 Ni 22.45 Co 22.45 Cr 22.45 (SiC) 10.2 。
Fe. The purity of the Ni, co and Cr powder is 99.9 percent, and the average particle size is 20 mu m; the purity of the SiC powder was 99.9%, and the average particle size was 0.6. Mu.m;
weighing the powder according to a chemical ratio, and then loading the powder into a stainless steel ball milling tank, wherein the ball milling medium is stainless steel balls, and the ball-material ratio is 5; dry-mixing for 4h at 150r/min by using a planetary ball mill, loading into a graphite mold after ball milling, and vacuumizing until the vacuum degree is less than 1 × 10 -1 Pa, performing vacuum hot-pressing sintering: heating from room temperature to 900 ℃ at the heating rate of 10 ℃/min, adjusting the pressure to be 12.5MPa, preserving heat for 0.5h, and cooling along with the furnace after the heat preservation is finished to obtain the high-entropy alloy.
Example 2
The general formula of the high-entropy alloy is Fe 23.25 Ni 23.25 Co 23.25 Cr 23.25 (SiC) 7 。
Fe. The purity of the Ni, co and Cr powder is 99.9 percent, and the average particle size is 20 mu m; the purity of the SiC powder was 99.9%, and the average particle size was 0.6. Mu.m.
Weighing the powder according to the chemical proportion, then loading the powder into a stainless steel ball milling tank, wherein the ball milling medium is stainless steel grinding balls, the ball-material ratio is 5, dry-mixing is carried out for 4h at the rotating speed of 150r/min by adopting a planetary ball mill, loading the powder into a graphite mold after the ball milling is finished, and vacuumizing the graphite mold until the vacuum degree is less than 1 multiplied by 10 -1 Pa, carrying out vacuum hot-pressing sintering:heating from room temperature to 900 ℃ at the heating rate of 10 ℃/min, adjusting the pressure to be 12.5MPa, preserving heat for 0.5h, and cooling along with the furnace after the heat preservation is finished to obtain the high-entropy alloy.
Comparative example 1
The general formula of the high-entropy alloy is Fe 25 Ni 25 Co 25 Cr 25 。
Fe. The purity of the Ni, co and Cr powder is 99.9 percent, and the average particle size is 20 mu m;
weighing powder according to a chemical ratio, and then loading the powder into a stainless steel ball milling tank, wherein a ball milling medium is a stainless steel ball, and the ball material ratio is 5; dry-mixing for 4h at 150r/min by using a planetary ball mill, loading into a graphite mold after ball milling, and vacuumizing until the vacuum degree is less than 1 × 10 -1 Pa, performing vacuum hot-pressing sintering: heating from room temperature to 900 ℃ at the heating rate of 10 ℃/min, adjusting the pressure to be 12.5MPa, keeping the temperature for 0.5h, and cooling along with the furnace after the heat preservation is finished to obtain the high-entropy alloy.
Characterization and Performance testing
FIG. 1 shows Fe prepared in example 1 22.45 Ni 22.45 Co 22.45 Cr 22.45 (SiC) 10.2 The microstructure diagram of the sintered HAADF of the high-entropy alloy is shown in FIG. 1, and the high-entropy alloy presents a large amount of dispersed and distributed regular cubic nanometer precipitated phases.
FIG. 2 shows Fe prepared in example 1 22.45 Ni 22.45 Co 22.45 Cr 22.45 (SiC) 10.2 The EDS surface scanning element distribution diagram of the sintered high-entropy alloy is shown in FIG. 2, and the high-entropy alloy is in a Ni-Si element-rich nano precipitated phase.
FIG. 3 is Fe prepared in example 1 22.45 Ni 22.45 Co 22.45 Cr 22.45 (SiC) 10.2 HRTEM of the high-entropy alloy in a sintered state and diffraction spots after Fourier transformation show that the high-entropy alloy Ni 3 The Si precipitated region (FIG. 3 (a)) is composed of a matrix of FCC disordered structure (FIG. 3 (b)) and FCC ordered structure (L1) 2 Structure) (fig. 3 (c)) of Ni 3 Si precipitated phase composition.
FIG. 4 shows Fe after addition of SiC prepared in example 1 22.45 Ni 22.45 Co 22.45 Cr 22.45 (SiC) 10.2 High entropy alloy and Fe without SiC in comparative example 1 25 Ni 25 Co 25 Cr 25 Compression true stress-strain curves of high entropy alloys at room temperature. As can be seen from FIG. 4, fe without SiC addition (before SiC addition) 25 Ni 25 Co 25 Cr 25 The yield strength of the high-entropy alloy is only 475MPa, and the strain reaches 74%; fe after SiC addition 22.45 Ni 22.45 Co 22.45 Cr 22.45 (SiC) 10.2 The yield strength of the high-entropy alloy is improved to 891MPa, and the strain of 28 percent is maintained. Namely, the yield strength is improved while the good plasticity is kept, so that the method has great application prospect in the field of engineering application.
FIG. 5 shows Fe after SiC addition prepared in example 2 23.25 Ni 23.25 Co 23.25 Cr 23.25 (SiC) 7 High entropy alloy and Fe without SiC in comparative example 1 25 Ni 25 Co 25 Cr 25 Compression true stress-strain curves of high entropy alloys at room temperature. As can be seen from FIG. 5, fe before SiC addition 25 Ni 25 Co 25 Cr 25 The yield strength of the high-entropy alloy is only 475MPa, and the strain reaches 74%; fe after SiC addition 23.25 Ni 23.25 Co 23.25 Cr 23.25 (SiC) 7 The yield strength of the high-entropy alloy is improved to 515MPa, and 56% of strain is maintained. Namely, the yield strength is improved while the good plasticity is kept, so that the method has great application prospect in the field of engineering application.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and amendments can be made without departing from the principle of the present invention, and these modifications and amendments should also be considered as the protection scope of the present invention.
Claims (9)
1. The SiC doped high-entropy alloy is characterized in that the chemical general formula is Fe a Ni b Co c Cr d (SiC) e Wherein a is more than or equal to 20 percent and less than or equal to 25 percent, b is more than or equal to 20 percent and less than or equal to 25 percent, c is more than or equal to 20 percent and less than or equal to 25 percent,D is more than or equal to 20 percent and less than or equal to 25 percent, e is more than or equal to 3.5 percent and less than or equal to 13.5 percent, a + b + c + d + e =100 percent, and a, b, c, d and e respectively correspond to the mole percent of each element.
2. The SiC doped high entropy alloy of claim 1, wherein the SiC doped high entropy alloy consists of a disordered face centered cubic matrix and a regular cubic morphology L1 located inside the face centered cubic matrix 2 Type Ni 3 Si nanoparticles.
3. A method for preparing the SiC-doped high-entropy alloy of claim 1 or 2, characterized by comprising the steps of:
and (3) performing ball milling and mixing on Fe, ni, co, cr and SiC according to the proportion, and performing vacuum hot-pressing sintering to obtain the SiC-doped high-entropy alloy.
4. The preparation method according to claim 3, wherein the purity of Fe, ni, co and Cr is more than or equal to 99.9%, and the average particle size is less than or equal to 20 μm; the purity of the SiC is more than or equal to 99.9 percent, and the average particle size is less than or equal to 1 mu m.
5. The preparation method according to claim 3, wherein the ball milling medium used for ball milling and mixing is stainless steel balls, the ball-material ratio of the ball milling and mixing is 5-1, the rotating speed is 120-200 r/min, and the time is 3-5 h.
6. The method according to claim 3, wherein before the vacuum hot pressing sintering, the vacuum is performed until the vacuum degree is less than 1 x 10 -1 Pa。
7. The preparation method according to claim 3 or 6, wherein the temperature of the vacuum hot-pressing sintering is 900-1000 ℃, the pressure is 12-20 MPa, and the holding time is 0.5-1 h.
8. The method according to claim 7, wherein a temperature rise rate from room temperature to the temperature of the vacuum hot press sintering is 8 to 10 ℃/min.
9. The SiC doped high-entropy alloy of claim 1 or 2 or the SiC doped high-entropy alloy prepared by the preparation method of any one of claims 3 to 8 is applied to the field of engineering structures.
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