CN107475596B - High-entropy intermetallic compound - Google Patents

High-entropy intermetallic compound Download PDF

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CN107475596B
CN107475596B CN201710681712.8A CN201710681712A CN107475596B CN 107475596 B CN107475596 B CN 107475596B CN 201710681712 A CN201710681712 A CN 201710681712A CN 107475596 B CN107475596 B CN 107475596B
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intermetallic compound
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CN107475596A (en
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孔凡涛
陈玉勇
王晓鹏
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Harbin Institute of Technology
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    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
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    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/0433—Nickel- or cobalt-based alloys
    • C22C1/0441—Alloys based on intermetallic compounds of the type rare earth - Co, Ni
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/045—Alloys based on refractory metals
    • C22C1/0458—Alloys based on titanium, zirconium or hafnium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/047—Making non-ferrous alloys by powder metallurgy comprising intermetallic compounds
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C14/00—Alloys based on titanium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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Abstract

The invention discloses a high-entropy intermetallic compound, relates to the field of novel metal material preparation, and particularly relates to a high-entropy intermetallic compound. The invention aims to obtain a novel metal material which has the characteristics of a highly ordered crystal structure of an intermetallic compound and high-entropy alloy multi-principal element. One high entropy intermetallic compound is a binary intermetallic compound or a ternary intermetallic compound; the chemical formula of the binary intermetallic compound is MN, MN 2、M 3N、M 5N 3Or M 6N 7(ii) a The chemical formula of the ternary intermetallic compound is ABC and ABC 2、ABC 3、AB 2C 3、AB 2C 2、ABC 4、AB 2C 4. The high-entropy intermetallic compound is used in the fields of aviation, aerospace, military, civil use and the like.

Description

High-entropy intermetallic compound
Technical Field
The invention relates to the field of metal material preparation, in particular to a high-entropy intermetallic compound.
Background
At present, the field of metal materials is mainly classified into pure metals, traditional alloys, amorphous alloys, high-entropy alloys, intermetallic compounds, metal matrix composites and the like.
The high-entropy alloy is a multi-principal element disordered solid solution alloy different from other types of alloys. The multi-principal element solid solution alloy is an alloy with more than five metal elements as main elements, the ratio of the mole number of each main metal element to the total mole number of the alloy is between 5 at.% and 30 at.%, solute and solvent components cannot be distinguished, simple BCC, FCC and BCC + FCC solid solution phases are formed, and the formation of intermetallic compounds is inhibited. As no element with the content exceeding 30 at.% is used as a main element, the characteristics of the high-entropy alloy are led by all main elements collectively, so that the mixed entropy of the alloy is remarkably increased, and a high-entropy effect, a delayed diffusion effect, a lattice distortion effect and a cocktail effect are generated, so that the material has excellent comprehensive properties. And the intermetallic compound is a kind of ordered metal material completely different from the high-entropy alloy. Unlike other types of metallic materials, such materials are compounds of metals and metals or metals and metalloids (e.g., silicon, arsenic, tellurium), having long-range ordered crystal structures and metallic fundamental properties different from their constituent elements. The main element atoms are mainly combined by covalent bonds and are a compound, and the main element atoms are highly ordered in arrangement. Due to the existence of covalent bonds, the intermetallic compound has unique materials with high strength, high hardness, high melting point, high creep resistance, low plasticity, special electrical, magnetic and acoustic properties and the like. Both high-entropy alloy and intermetallic compound are metal materials which are mainly developed at home and abroad at present.
Therefore, the high-entropy alloy is a multi-principal solid solution and is required to suppress the formation of intermetallic compounds, which are materials mainly composed of intermetallic compounds and are generally required to suppress the formation of solid solutions. Currently, high entropy alloys add elements in a near equimolar ratio, while intermetallic compounds add small amounts of alloying elements (similar to conventional metallic materials) based on the primary elements forming the compound.
Disclosure of Invention
The invention aims to obtain a metal material which has the characteristics of a highly ordered crystal structure of an intermetallic compound and high-entropy alloy multi-principal elements, and provides a high-entropy intermetallic compound.
One high entropy intermetallic compound is a binary intermetallic compound or a ternary intermetallic compound; the chemical formula of the binary intermetallic compound is MN, MN 2、M 3N、M 5N 3Or M 6N 7(ii) a The chemical formula of the ternary intermetallic compound is ABC and ABC 2、ABC 3、AB 2C 3、AB 2C 2、ABC 4、AB 2C 4(ii) a A binary intermetallic compound containing 5 to 16 elements, which is composed of M representing 1 to 8 elements and N representing 1 to 8 elements; a ternary intermetallic compound containing 5 to 24 elements, which is composed of A representing 1 to 8 elements, B representing 1 to 8 elements and C representing 1 to 8 elements; a, B, C, M and N are selected from Ti, Ni, Co, Nb, Ta, W, Zr, Mo, Cr, Mn, Fe, Al, V, Sc, Hf, RuElements selected from Ga, Ge, Cu, Sn, Li, Pd, Pt, Ir, Si, C, B and rare earth elements; the atomic percentage of each element in the binary intermetallic compound is 1.5 to 77 percent; the atomic percentage of each element in the ternary intermetallic compound is 1.5 to 77 percent; m and N are not the same element, and A, B and C are not the same element; the high-entropy intermetallic compound contains 0.00001 to 20 volume percent of solid solution, nonmetal compound or intermetallic compound with other crystal structures.
The invention has the beneficial effects that:
the high-entropy intermetallic compound obtained by the invention combines the characteristics of the intermetallic compound and the high-entropy alloy, and on the basis of the intermetallic compound, elements which form the intermetallic compound and have nearly equal molar ratio are added, and the main elements are five or more, so that a metal material which has a highly ordered crystal structure of the intermetallic compound and the characteristics of multiple principal elements of the high-entropy alloy is formed. The high-entropy intermetallic compound obtained by the invention is still an intermetallic compound, and different types of atoms have strong bonding, so that the crystal structure is more stable, the mobility of atoms and dislocation of the high-entropy intermetallic compound is reduced at high temperature, and compared with a high-entropy alloy and a traditional metal material, the high-entropy alloy has more excellent hardness, strength and thermal stability and better high-temperature resistance, and is more suitable for being used as a high-temperature structural material; compared with the traditional intermetallic compound, part of the high-entropy intermetallic compound has good room-temperature plasticity due to the high-entropy effect brought by the multiple principal elements. For example, compared with high-entropy alloy and traditional metal materials, the use temperature of the high-entropy intermetallic compound can be increased by 200-400 ℃; and M 3Partial M compared to the lower room temperature plasticity (less than 5%) of N-type intermetallics 3The room temperature plasticity of the N-type high-entropy intermetallic compound can be improved by more than 30 percent, and the strength can also be improved by more than one time. High entropy intermetallic formationThe compound has the characteristics, so that the compound has wide application prospect in the fields of aviation, aerospace, military, civil use and the like, and has important commercial value.
Drawings
FIG. 1 is an X-ray diffraction pattern of a binary high-entropy intermetallic compound obtained in example one;
FIG. 2 is an X-ray diffraction pattern of the binary high-entropy intermetallic compound obtained in example two;
FIG. 3 is an X-ray diffraction pattern of the ternary high-entropy intermetallic compound obtained in example III.
Detailed Description
The first embodiment is as follows: the high-entropy intermetallic compound according to the present embodiment is a binary intermetallic compound or a ternary intermetallic compound; the chemical formula of the binary intermetallic compound is MN, MN 2、M 3N、M 5N 3Or M 6N 7(ii) a The chemical formula of the ternary intermetallic compound is ABC and ABC 2、ABC 3、AB 2C 3、AB 2C 2、ABC 4、AB 2C 4(ii) a A binary intermetallic compound containing 5 to 16 elements, which is composed of M representing 1 to 8 elements and N representing 1 to 8 elements; a ternary intermetallic compound containing 5 to 24 elements, which is composed of A representing 1 to 8 elements, B representing 1 to 8 elements and C representing 1 to 8 elements; a, B, C, M and N are selected from Ti, Ni, Co, Nb, Ta, W, Zr, Mo, Cr, Mn, Fe, Al, V, Sc, Hf, Ru, Ga, Ge, Cu, Sn, Li, Pd, Pt, Ir, Si, C, B and rare earth elements; the atomic percentage of each element in the binary intermetallic compound is 1.5 to 77 percent; the atomic percentage of each element in the ternary intermetallic compound is 1.5 to 77 percent; m and N are not the same element, and A, B and C are not the same element; the high-entropy intermetallic compound contains 0.00001 to 20 volume percent of solid solution, nonmetal compound or other compoundsAn intermetallic compound of a crystal structure.
The solid solution or the nonmetal compound according to the present embodiment means other crystalline substances having a crystal structure different from that of the intermetallic compound having another crystal structure and the high-entropy intermetallic compound to be finally formed; the various elements are melted together and solidify, possibly producing a small amount of a second phase, which may be a solid solution or other non-compound material.
The second embodiment is as follows: the first difference between the present embodiment and the specific embodiment is: the principle of selecting elements in the binary intermetallic compound is that at least three intermetallic compounds exist in a compound formed by the reaction of any one of 1 to 8 elements represented by M and one of 1 to 8 elements represented by N, the chemical formula types and the crystal structures of the intermetallic compounds formed by the reaction are the same, and the elements in the intermetallic compounds are selected as the elements of the binary intermetallic compound. The rest is the same as the first embodiment.
The same crystal structure in this embodiment means: the most basic structural features of the metal crystal are the same with the regular arrangement that its internal atoms are three-dimensionally periodic in space.
The third concrete implementation mode: the present embodiment differs from the first or second embodiment in that: when M is composed of two or more elements, the molar ratio between the respective elements provided by M in the binary intermetallic compound is the same; when N is composed of two or more elements, the molar ratio between the respective elements provided by N in the binary intermetallic compound is the same. The others are the same as in the first or second embodiment.
The fourth concrete implementation mode: the difference between this embodiment mode and one of the first to third embodiment modes is: the selection principle of the elements in the ternary intermetallic compound is that at least two intermetallic compounds exist in a compound formed by the reaction of any one of A representing 1-8 elements, any one of B representing 1-8 elements and any one of C representing 1-8 elements in the selected elements, and the chemical formula types and the crystal structures of the intermetallic compounds formed by the reaction are the same, so that the elements in the intermetallic compound are selected as the elements of the ternary intermetallic compound. The rest is the same as one of the first to third embodiments.
The same crystal structure in this embodiment means: the most basic structural features of the metal crystal are the same with the regular arrangement that its internal atoms are three-dimensionally periodic in space.
The fifth concrete implementation mode: the difference between this embodiment and one of the first to fourth embodiments is: when a is composed of two or more elements, the molar ratio between the respective elements provided by a in the ternary intermetallic compound is the same, when B is composed of two or more elements, the molar ratio between the respective elements provided by B in the ternary intermetallic compound is the same, and when C is composed of two or more elements, the molar ratio between the respective elements provided by C in the ternary intermetallic compound is the same. The rest is the same as one of the first to fourth embodiments.
The sixth specific implementation mode: the difference between this embodiment and one of the first to fifth embodiments is: the high-entropy intermetallic compound is prepared by a fusion casting method, a rapid solidification method or a rapid solidification method combined with a powder metallurgy method. The rest is the same as one of the first to fifth embodiments.
The seventh embodiment: the difference between this embodiment and one of the first to sixth embodiments is: the casting method comprises the steps of weighing and uniformly mixing all elements according to a molar ratio, smelting by adopting an electric arc furnace or an induction smelting furnace, and pouring alloy into a casting mold to obtain a high-entropy intermetallic compound ingot or casting. The rest is the same as one of the first to sixth embodiments.
The specific implementation mode is eight: the present embodiment differs from one of the first to seventh embodiments in that: the rapid solidification method is to prepare the high-entropy intermetallic compound in the shape of powder, thin slice or strip by a mold cooling technology, an atomization technology and a surface melting and deposition technology. The rest is the same as one of the first to seventh embodiments.
The specific implementation method nine: the present embodiment differs from the first to eighth embodiments in that: the rapid solidification method is combined with a powder metallurgy method, powder, thin slices or strip-shaped high-entropy intermetallic compounds obtained by the rapid solidification method are sintered under the conditions of high temperature or high temperature and high pressure or are printed by a metal 3D printer, and high-entropy intermetallic compound block materials or components are obtained. The rest is the same as the first to eighth embodiments.
The following examples were used to demonstrate the beneficial effects of the present invention:
the first embodiment is as follows: a high-entropy intermetallic compound is a binary high-entropy intermetallic compound with a chemical formula of M 3N, wherein M is Ni element and Co element, and N is Al element, Si element and Ti element; m reacts with N to form Ni 3Al、Co 3Ti、Ni 3Si and Co 3Al four intermetallic compounds with crystal structures of L1 2The molar ratios of the elements provided by M in the binary intermetallic compound are the same, the molar ratios of the elements provided by N in the binary intermetallic compound are the same, and the molar fractions of the Ni element, the Co element, the Al element, the Si element and the Ti element in the binary high-entropy intermetallic compound are 37.55%, 8.3% and 8.3% in sequence.
The preparation method comprises the following steps: the raw materials of Ni element, Co element, Al element, Si element and Ti element are all simple substances (purity)>99.5 wt.%), then putting the ingredients into a vacuum arc furnace, vacuumizing the vacuum arc furnace, flushing the vacuum arc furnace with high-purity argon, smelting the raw materials under the condition of argon protection, repeatedly smelting for 5 times, and smelting after turning the cast ingot 180 degrees after finishing smelting each time; cooling the cast ingot obtained by the last smelting and solidification, and taking out the cast ingot from the vacuum electric arc furnace to obtain the binary M 3An N-type high entropy intermetallic compound.
This binary M 3The N-type high-entropy intermetallic compound can also be prepared by adopting a rapid solidification technology (such as a mold cooling technology, an atomization technology and a surface melting and deposition technology) to prepare powder, thin slice or strip-shaped binary M 3An N-type high entropy intermetallic compound. Binary M 3The N-type high-entropy intermetallic compound can also be prepared by powder metallurgyThe preparation method comprises the following steps: preparing powder, slice or strip binary M by adopting rapid solidification technology or mechanical alloying technology 3N-type high entropy intermetallic compound, binary M in the form of powder, flakes or strips 3Sintering the N-type high-entropy intermetallic compound under the conditions of high temperature or high temperature and high pressure or printing by using a metal 3D printer to obtain the binary M 3An N-type high entropy intermetallic bulk material or component.
FIG. 1 is an X-ray diffraction pattern of the binary high-entropy intermetallic compound obtained in example one, from which it can be seen that the binary M finally obtained 3The crystal structure of the N-type high-entropy intermetallic compound is still mainly L1 2The volume fraction of solid solution or non-metallic compound or intermetallic compound with other crystal structure is only 5-10%; example one binary high entropy intermetallic Compound with Ni 3Al、Co 3Ti、Ni 3Si、Co 3Compared with four intermetallic compounds of Al, the binary M 3The N-type high-entropy intermetallic compound has excellent mechanical property, and the yield strength and plasticity at room temperature can be improved by more than one time.
Example two: the high-entropy intermetallic compound is a binary high-entropy intermetallic compound, the type of a chemical formula is MN, wherein M is Co element, Fe element, Ni element and Ti element, and N is Al element; the reaction of M and N can form four intermetallic compounds of CoAl, FeAl, NiAl and FeTi, the crystal structure is B2, the molar ratio of each element provided by M in the binary intermetallic compound is the same, and the molar fractions of Co element, Fe element, Ni element, Ti element and Al element in the binary high-entropy intermetallic compound are 12.5%, 12.5% and 50.0% in sequence.
The preparation method comprises the following steps: mixing the raw materials of Co element, Fe element, Ni element, Ti element and Al element according to the molar fraction ratio, wherein the raw materials are all simple substances (the purity is more than 99.5 wt.%), then putting the mixture into a vacuum electric arc furnace, vacuumizing and flushing the vacuum electric arc furnace with high-purity argon, smelting the raw materials under the condition of argon protection, repeatedly smelting for 5 times, and smelting after turning an ingot by 180 degrees every time when smelting is finished; and cooling the cast ingot obtained by the last smelting and solidification, and taking out the cast ingot from the vacuum electric arc furnace to obtain the binary MN-type high-entropy intermetallic compound.
The binary MN type high-entropy intermetallic compound can also be prepared by adopting a rapid solidification technology (such as a mold cooling technology, an atomization technology and a surface melting and deposition technology) to prepare the binary MN type high-entropy intermetallic compound in the form of powder, thin slices or strips. The binary MN type high-entropy intermetallic compound can also be prepared by adopting a powder metallurgy technology: the powder, slice or strip binary MN type high-entropy intermetallic compound is prepared by adopting a rapid solidification technology or a mechanical alloying technology, and is sintered under the conditions of high temperature or high temperature and high pressure or is printed by a metal 3D printer to obtain the binary MN type high-entropy intermetallic compound block material or component.
The crystal structure of the finally obtained binary MN type high-entropy intermetallic compound is still mainly B2, the volume fraction of the solid solution or the nonmetal compound or the intermetallic compound with other crystal structures is only 8-15%, and FIG. 2 is an X-ray diffraction diagram of the binary high-entropy intermetallic compound obtained in example II, so that the crystal structure of the finally obtained binary MN type high-entropy intermetallic compound is still mainly B2, and the volume fraction of the solid solution or the intermetallic compound with the nonmetal compound or the intermetallic compound with other crystal structures is only 8-15%; compared with four intermetallic compounds, namely CoAl, FeAl, NiAl and FeTi, the binary MN type high-entropy intermetallic compound obtained in the second embodiment has excellent mechanical properties, and the room temperature hardness can be improved by more than one time.
Example three: a high-entropy intermetallic compound is a ternary high-entropy intermetallic compound with a chemical formula of A 2BC, wherein A is Ti element, B is Al element, and C is Nb element, Mo element and Zr element; A. the reaction of B and C can form Ti 2AlNb、Ti 2The crystal structures of two intermetallic compounds AlMo are both B2, the molar ratios of the elements provided by C in the ternary intermetallic compound are the same, and the Ti element, the Al element, the Nb element, the Mo element and the Zr element in the ternary high-entropy intermetallic compound are sameThe mole fractions of (A) are 50%, 24.8%, 8.4% in sequence.
The preparation method comprises the following steps: the raw materials of Ti element, Al element, Nb element, Mo element and Zr element are all simple substances (purity)>99.5 wt.%), then putting the ingredients into a vacuum arc furnace, vacuumizing the vacuum arc furnace, flushing the vacuum arc furnace with high-purity argon, smelting the raw materials under the condition of argon protection, repeatedly smelting for 5 times, and smelting after turning the cast ingot 180 degrees after finishing smelting each time; cooling the cast ingot obtained by the last smelting and solidification, and taking out the cast ingot from the vacuum electric arc furnace to obtain the ternary A material 2BC type high entropy intermetallic compound.
This ternary A 2The BC type high-entropy intermetallic compound can also be prepared by adopting a rapid solidification technology (such as a mold cooling technology, an atomization technology and a surface melting and deposition technology) to prepare ternary A in the form of powder, thin slices or strips 2BC type high entropy intermetallic compound. Ternary A 2The BC type high-entropy intermetallic compound can also be prepared by adopting a powder metallurgy technology: preparing ternary A in the form of powder, thin slice or strip by adopting rapid solidification technology or mechanical alloying technology 2BC type high entropy intermetallic compound, ternary A in the form of powder, flake or ribbon 2Sintering the BC type high-entropy intermetallic compound under the conditions of high temperature or high temperature and high pressure or printing by using a metal 3D printer to obtain the ternary A 2BC type high entropy intermetallic compound bulk material or member.
The final ternary A 2The crystal structure of the BC type high-entropy intermetallic compound is still mainly B2, the volume fraction of solid solution or nonmetal compound or intermetallic compound with other crystal structure is only 4-8%, FIG. 3 is the X-ray diffraction pattern of the ternary high-entropy intermetallic compound obtained in the third embodiment, and the ternary A finally obtained can be seen from the pattern 2The crystal structure of the BC type high-entropy intermetallic compound is still mainly B2, and the volume fraction of solid solution or nonmetal compounds or intermetallic compounds with other crystal structures is only 4-8%; ternary high entropy intermetallic Compound obtained in example III and Ti 2AlNb、Ti 2Between two metals of AlMoThe compound is compared with the ternary A 2The BC type high-entropy intermetallic compound has excellent mechanical property, and the yield strength and the hardness at room temperature can be improved by more than 30%.
In addition to the above-mentioned embodiments, all the high-entropy intermetallic compounds with different compositions obtained by the design method according to the present invention, and the modifications or variations based on the present invention are included in the scope of the present invention.

Claims (2)

1. A high-entropy intermetallic compound is characterized in that the high-entropy intermetallic compound is a binary high-entropy intermetallic compound with a chemical formula of M 3N, wherein M is Ni element and Co element, and N is Al element, Si element and Ti element; m reacts with N to form Ni 3Al、Co 3Ti、Ni 3Si and Co 3Al four intermetallic compounds with crystal structures of L1 2The molar ratios of the elements provided by M in the binary high-entropy intermetallic compound are the same, the molar ratios of the elements provided by N in the binary high-entropy intermetallic compound are the same, and the molar fractions of the Ni element, the Co element, the Al element, the Si element and the Ti element in the binary high-entropy intermetallic compound are 37.55%, 8.3% and 8.3% in sequence.
2. A high entropy intermetallic compound according to claim 1, characterized in that the process for the preparation of the high entropy intermetallic compound is carried out by the following steps: mixing the materials according to the proportion that the mole fractions of Ni element, Co element, Al element, Si element and Ti element are 37.55%, 8.3% and 8.3% in sequence, wherein the raw materials of Ni element, Co element, Al element, Si element and Ti element are all purity>99.5 wt.% of simple substance, then putting the ingredients into a vacuum arc furnace, vacuumizing the vacuum arc furnace, flushing the vacuum arc furnace with high-purity argon, smelting the raw materials under the condition of argon protection, repeatedly smelting for 5 times, and smelting after turning the cast ingot 180 degrees after finishing smelting each time; cooling the ingot obtained by the last smelting and solidification, and taking out the ingot from the vacuum electric arc furnace to obtain a binary materialM 3An N-type high entropy intermetallic compound.
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CN115976391B (en) * 2022-12-07 2023-10-20 哈尔滨工业大学 High-temperature-resistant multi-principal-element intermetallic compound and preparation method thereof

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