CN108642399B - Basal high-entropy alloy and preparation method thereof - Google Patents

Basal high-entropy alloy and preparation method thereof Download PDF

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CN108642399B
CN108642399B CN201810478103.7A CN201810478103A CN108642399B CN 108642399 B CN108642399 B CN 108642399B CN 201810478103 A CN201810478103 A CN 201810478103A CN 108642399 B CN108642399 B CN 108642399B
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李邦盛
周扬
晋玺
张璐
杜兴宇
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Harbin Institute of Technology
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Abstract

A basal high-entropy alloy and a preparation method thereof, which relate to a high-entropy alloy and a preparation method thereof. The invention aims to solve the problems that the existing high-entropy alloy has poor mechanical property, and the high-entropy alloy contains massive brittle intermetallic compound phases and has poor plasticity. The high-entropy alloy with base is prepared from 50-90% of alloy matrix and 10-50% of alloying elements by mass percent. The method comprises the following steps: firstly, preparing raw materials; and secondly, smelting the raw materials of the base high-entropy alloy weighed in the step one by adopting an arc smelting method or an induction smelting method to obtain the base high-entropy alloy. The yield strength of the basal high-entropy alloy prepared by the invention is 1000MPa to 2000MPa, the breaking strength is 2000MPa to 4000MPa, and the ultimate strain epsilonp(%) is 20-70%. The invention can obtain the high-entropy alloy with the base.

Description

Basal high-entropy alloy and preparation method thereof
Technical Field
The invention relates to a high-entropy alloy and a preparation method thereof.
Background
In the field of traditional alloy material design, one or two alloy elements are often used as a matrix, and a small amount of other elements are added as alloying elements, so that the mechanical properties such as hardness and strength of the matrix alloy are improved, and the physical properties such as magnetic property, electrical property and the like of the alloy material are improved, such as various steel, aluminum alloy, titanium alloy, nickel-based high-temperature alloy materials, and intermetallic compound materials such as Ti-Al, Ni-Al and the like.
In 2004, Taiwan scholars in China were pleased with the thinking-fixed form of the traditional alloy design, and the design idea of the high-entropy alloy was firstly proposed. The high entropy alloy is defined as: the number n of the constituent elements is more than or equal to 5, each element has equal molar ratio or nearly equal molar ratio, and the atomic percentage content of all elements is not more than 35 percent. None of the high entropy alloys has an element content exceeding 50% and therefore no so-called alloy matrix. The high-entropy alloy has a large number of elements and high content of each alloy element, so that the mixing entropy of the alloy is large, and the alloy elements tend to be disorderly arranged to form a simple Body Centered Cubic (BCC) or Face Centered Cubic (FCC) phase. The high distortion of the lattice structure of the high-entropy alloy and the 'cocktail effect' of the properties of each element enable the novel alloy material to have excellent comprehensive properties such as high hardness, high strength, high temperature creep resistance, high temperature oxidation resistance, corrosion resistance, high resistivity, good electromagnetic property and the like, and the application prospect is very wide.
Over the past decade, high-entropy alloy materials are widely researched by scholars at home and abroad, and have made important progress in various fields such as preparation methods, thermodynamics, kinetics, phase formation rules, tissue stability, mechanical properties, magnetic properties, electric heating properties and the like. In 2013, Libang professor introduces a matrix into the high-entropy alloy, puts forward the concept of the basic high-entropy alloy for the first time, successfully develops a series of basic high-entropy alloy materials with novel nanometer structures and excellent mechanical properties, and opens up a new field of high-entropy alloy design. Therefore, the research and development of the basic high-entropy alloy with excellent microstructure and mechanical property has very important significance and wide application prospect.
However, in the conventional alloy design process, when the content of the added alloying elements is high, a large brittle intermetallic compound phase is easily formed, and the performance of the alloy is deteriorated. Therefore, the conventional alloying method has limitations;
in the design process of the existing high-entropy alloy, the definition and the design principle limit the design space of the alloy, and the existing high-entropy alloy has high hardness and high strength, but the plasticity is poor, and the limit strain epsilonp(%) is less than 30%. Meanwhile, according to the design idea of the traditional high-entropy alloy, the performance of the alloy is difficult to be greatly optimized, because the component adjusting range of the traditional high-entropy alloy is usually small. Therefore, in order to obtain a novel alloy material with excellent comprehensive mechanical properties, the content of the high-entropy alloy needs to be broken through urgently, and a new design principle and a new method are developed.
Disclosure of Invention
The invention aims to solve the problems of poor mechanical property of the existing high-entropy alloy, and poor phase and plasticity of a large brittle intermetallic compound contained in the high-entropy alloy, and provides a basic high-entropy alloy and a preparation method thereof.
The basal high-entropy alloy is prepared from 50-90% of alloy matrix and 10-50% of alloying elements by mass percent; the alloy matrix is one or two of Fe, Al, Cr, Ni, Co, Cu, Ti, Mn, Mo, Zr, Hf, Nb and Sn; the alloying elements are two or more of Fe, Al, Cr, Ni, Co, Cu, Ti, Mn, Mo, Zr, Hf, Nb and Sn; when the alloy matrix is composed of two elements, the molar ratio of the two elements is b, and the value range of b is more than or equal to 0.5 and less than or equal to 2; the molar ratio of any two elements in the alloying elements is a, and a satisfies the following conditions: a is more than or equal to 0.8 and less than or equal to 1.25.
A preparation method of a basal high-entropy alloy is completed according to the following steps:
firstly, preparing raw materials:
weighing 50-90% of alloy matrix and 10-50% of alloying elements according to the mass percentage to obtain the raw material of the base high-entropy alloy;
the alloy matrix in the first step is one or two of Fe, Al, Cr, Ni, Co, Cu, Ti, Mn, Mo, Zr, Hf, Nb and Sn;
the alloying elements in the first step are two or more of Fe, Al, Cr, Ni, Co, Cu, Ti, Mn, Mo, Zr, Hf, Nb and Sn;
when the alloy matrix in the step one is two elements, the molar ratio of the two elements is b, and the value range of b is more than or equal to 0.5 and less than or equal to 2;
the molar ratio of any two elements in the alloying elements in the step one is a, and the value range of a is more than or equal to 0.8 and less than or equal to 1.25.
And secondly, smelting the raw materials of the base high-entropy alloy weighed in the step one by adopting an arc smelting method or an induction smelting method to obtain the base high-entropy alloy.
The invention has the advantages that:
the difference between the basic high-entropy alloy and the method for preparing the basic high-entropy alloy in the invention and the prior art is that: the content of each element in the traditional high-entropy alloy is 5-35%, and the content of any element is less than 50%, namely, no matrix exists in the traditional high-entropy alloy; the mass fraction of the alloy matrix in the basic high-entropy alloy is more than 50%, namely the matrix exists, so the basic high-entropy alloy is called;
secondly, the difference between the alloy in the basic high-entropy alloy and the traditional high-entropy alloy is as follows: the element types and the element contents are relatively more, so the entropy of the high-entropy alloy with the base is larger than that of the traditional high-entropy alloy, and the high-entropy alloy is a novel high-entropy alloy;
thirdly, the alloy in the high-entropy alloy with the base breaks through the design limitation of the traditional high-entropy alloy, and greatly expands the content and component design range of the high-entropy alloy; according to the invention, proper elements are selected as an alloy matrix, and the types and contents of alloying elements are optimized, so that a basic high-entropy alloy material with excellent microstructure and excellent comprehensive mechanical properties can be prepared, and the application prospect is very wide;
fourthly, the yield strength of the basal high-entropy alloy prepared by the invention is 1000MPa to 2000MPa, the breaking strength is 2000MPa to 4000MPa, and the ultimate strain epsilonp(%) is 20% -70%;
compared with the traditional high-entropy alloy with equal or nearly equal molar ratio, the base high-entropy alloy prepared by the invention has more excellent microstructure and comprehensive mechanical property, for example, a large amount of nano-structure microstructure with nano precipitated phases dispersed in a matrix can be obtained, so that the high-strength and high-plasticity excellent comprehensive mechanical property is obtained.
The invention can obtain the high-entropy alloy with the base.
Drawings
FIG. 1 shows Fe prepared in example one55(AlCrNi)45XRD pattern of iron-based high entropy alloy;
FIG. 2 shows Fe prepared in example one55(AlCrNi)45SEM microscopic structure picture of the iron-based high-entropy alloy;
FIG. 3 shows Fe prepared in example one55(AlCrNi)45Pressing of iron-based high-entropy alloysA compressive stress-strain curve;
FIG. 4 is (FeCr) prepared in example two80(AlNi)20XRD (X-ray diffraction) pattern of the iron-chromium double-base high-entropy alloy;
FIG. 5 is (FeCr) prepared in example two80(AlNi)20SEM microscopic structure picture of iron-chromium double-base high-entropy alloy;
FIG. 6 is (FeCr) prepared in example two80(AlNi)20Compressive stress-strain curve of Fe-Cr double-base high-entropy alloy.
Detailed Description
The first embodiment is as follows: the embodiment is that the basal high-entropy alloy is prepared by 50-90% of alloy basal body and 10-50% of alloying element according to mass percentage; the alloy matrix is one or two of Fe, Al, Cr, Ni, Co, Cu, Ti, Mn, Mo, Zr, Hf, Nb and Sn; the alloying elements are two or more of Fe, Al, Cr, Ni, Co, Cu, Ti, Mn, Mo, Zr, Hf, Nb and Sn; when the alloy matrix is composed of two elements, the molar ratio of the two elements is b, and the value range of b is more than or equal to 0.5 and less than or equal to 2; the molar ratio of any two elements in the alloying elements is a, and a satisfies the following conditions: a is more than or equal to 0.8 and less than or equal to 1.25.
The second embodiment is as follows: the preparation method of the basal high-entropy alloy is completed according to the following steps:
firstly, preparing raw materials:
weighing 50-90% of alloy matrix and 10-50% of alloying elements according to the mass percentage to obtain the raw material of the base high-entropy alloy;
the alloy matrix in the first step is one or two of Fe, Al, Cr, Ni, Co, Cu, Ti, Mn, Mo, Zr, Hf, Nb and Sn;
the alloying elements in the first step are two or more of Fe, Al, Cr, Ni, Co, Cu, Ti, Mn, Mo, Zr, Hf, Nb and Sn;
when the alloy matrix in the step one is two elements, the molar ratio of the two elements is b, and the value range of b is more than or equal to 0.5 and less than or equal to 2;
the molar ratio of any two elements in the alloying elements in the step one is a, and the value range of a is more than or equal to 0.8 and less than or equal to 1.25.
And secondly, smelting the raw materials of the base high-entropy alloy weighed in the step one by adopting an arc smelting method or an induction smelting method to obtain the base high-entropy alloy.
The advantages of this embodiment:
the difference between the basic high-entropy alloy and the method for preparing the basic high-entropy alloy in the embodiment and the prior art is that: the content of each element in the traditional high-entropy alloy is 5-35%, and the content of any element is less than 50%, namely, no matrix exists in the traditional high-entropy alloy; the mass fraction of the alloy matrix in the basic high-entropy alloy in the embodiment is more than 50%, namely the matrix exists, so the basic high-entropy alloy is called as the basic high-entropy alloy;
secondly, the difference between the alloy in the basic high-entropy alloy of the embodiment and the traditional high-entropy alloy is as follows: the element types and the element contents are relatively more, so that the entropy of the high-entropy alloy with the base in the embodiment is larger than that of the traditional high-entropy alloy, and the high-entropy alloy is a novel high-entropy alloy;
thirdly, the alloy in the high-entropy alloy with the base breaks through the design limitation of the traditional high-entropy alloy, and the content and the component design range of the high-entropy alloy are greatly expanded; according to the embodiment, proper elements are selected as the alloy matrix, and the types and the contents of alloying elements are optimized, so that the base high-entropy alloy material with excellent microstructure and excellent comprehensive mechanical properties can be prepared, and the application prospect is very wide;
fourthly, the yield strength of the basal high-entropy alloy prepared by the embodiment is 1000MPa to 2000MPa, the breaking strength is 2000MPa to 4000MPa, and the ultimate strain epsilonp(%) is 20% -70%;
compared with the traditional high-entropy alloy with equal or nearly equal molar ratio, the base high-entropy alloy prepared by the embodiment has more excellent microstructure and comprehensive mechanical property, for example, a large amount of nano-structure microstructure with nano precipitated phases dispersed in a matrix can be obtained, so that the high-strength and high-plasticity excellent comprehensive mechanical property is obtained.
This embodiment can obtain a high-entropy alloy having a base.
The third concrete implementation mode: the present embodiment is different from the second embodiment in that: the arc melting method in the second step is completed according to the following steps:
①, sequentially adding the raw materials of the basic high-entropy alloy weighed in the step one into a copper mold crucible in a non-consumable vacuum arc melting furnace according to the sequence of the melting points of the materials from low to high;
②, vacuumizing the non-consumable vacuum arc melting furnace until the vacuum degree of the non-consumable vacuum arc melting furnace is lower than 1.0 multiplied by 10-3Introducing argon into the non-consumable vacuum arc melting furnace until the pressure in the non-consumable vacuum arc melting furnace is 0.05 MPa;
③, repeating the step ② 3 times to 5 times;
④, repeatedly smelting the raw material of the basic high-entropy alloy for 5 to 6 times under the condition that the smelting current is 250 to 400A, wherein the smelting time is 2 to 5min each time, and cooling along with the furnace to obtain the basic high-entropy alloy.
The fourth concrete implementation mode: the present embodiment differs from the second to third embodiments in that: the molar ratio of any two elements in the alloying elements in the first step is a, and a is 1. The other steps are the same as those in the second to third embodiments.
The fifth concrete implementation mode: the second to fourth embodiments are different from the first to fourth embodiments in that: when the alloy matrix in the first step is two elements, the molar ratio between the two elements is b, and b is 1. The other steps are the same as those in the second to fourth embodiments.
The sixth specific implementation mode: the second to fifth embodiments are different from the first to fifth embodiments in that: in the first step, 55% of alloy matrix and 45% of alloying elements are weighed according to the mass percentage to obtain the raw material of the base high-entropy alloy. The other steps are the same as those in the second to fifth embodiments.
The seventh embodiment: the present embodiment differs from one of the second to sixth embodiments in that: in the first step, 80% of alloy matrix and 20% of alloying elements are weighed according to the mass percentage to obtain the raw material of the base high-entropy alloy. The other steps are the same as those in the second to sixth embodiments.
The specific implementation mode is eight: the second embodiment differs from the first embodiment in that: the alloy matrix in the step one is Fe. The other steps are the same as those in the second to seventh embodiments.
The specific implementation method nine: the second to eighth differences from the first embodiment are as follows: the alloying elements in the step one are Al, Cr and Ni. The other steps are the same as those in the second to eighth embodiments.
The detailed implementation mode is ten: the present embodiment differs from the second to ninth embodiments in that: the induction melting method in the second step is completed according to the following steps:
①, sequentially adding the raw materials of the base high-entropy alloy weighed in the step one into a ceramic crucible in an induction melting furnace according to the sequence of the melting points of the materials from low to high;
②, vacuumizing the induction melting furnace until the vacuum degree of the induction melting furnace is lower than 2.0 multiplied by 10-3Introducing argon into the induction smelting furnace until the pressure in the induction smelting furnace reaches 0.05 MPa;
③, repeating the step ② 3 times to 5 times;
④, smelting the raw material of the basic high-entropy alloy for 5-10 min under the argon atmosphere and the smelting current of 50-70A, and cooling along with the furnace to obtain the basic high-entropy alloy.
The following examples were used to demonstrate the beneficial effects of the present invention:
the first embodiment is as follows: the preparation method of the basal high-entropy alloy is completed according to the following steps:
firstly, preparing raw materials:
weighing 55% of alloy matrix and 45% of alloying elements according to mass percent to obtain a raw material of the high-entropy alloy with the matrix;
the alloy matrix in the first step is Fe;
the alloying elements in the first step are Al, Cr and Ni; the molar ratio of any two elements in the alloying elements is a, and a is 1;
secondly, adding the raw materials of the base high-entropy alloy weighed in the step one into a copper mold crucible in a non-consumable vacuum arc melting furnace in sequence according to the sequence of the melting points of the materials from low to high;
thirdly, vacuumizing the non-consumable vacuum arc melting furnace until the vacuum degree of the non-consumable vacuum arc melting furnace is lower than 1.0 multiplied by 10-3Introducing argon into the non-consumable vacuum arc melting furnace until the pressure in the non-consumable vacuum arc melting furnace is 0.05 MPa;
fourthly, repeating the third step for 3 times;
fifthly, repeatedly smelting the raw material of the base high-entropy alloy for 5 times under the condition that the smelting current is 250A, wherein the smelting time is 2min each time, and cooling along with the furnace to obtain Fe55(AlCrNi)45An iron-based high entropy alloy.
Fe prepared in example one55(AlCrNi)45Grinding and polishing the iron-based high-entropy alloy, and then performing phase analysis by using a Japanese physical optical D/max-rB type X-ray diffractometer; as shown in fig. 1;
FIG. 1 shows Fe prepared in example one55(AlCrNi)45XRD pattern of iron-based high entropy alloy;
as can be seen from FIG. 1, Fe prepared in example one55(AlCrNi)45The iron-based high-entropy alloy has a simple crystal structure, and the result of microstructure analysis shows that the iron-based high-entropy alloy consists of an alpha-Fe matrix phase and a (Ni, Fe) Al phase with a B2 structure, and the lattice constants of the alpha-Fe matrix phase and the (Ni, Fe) Al phase are very close to each other, so that diffraction peaks are overlapped.
FIG. 2 shows Fe prepared in example one55(AlCrNi)45SEM microscopic structure picture of the iron-based high-entropy alloy;
as can be seen from FIG. 2, Fe prepared in example one55(AlCrNi)45The iron-based high-entropy alloy has a large amount of nano precipitated phases with the size of about 200-300 nm.
From the embodiment onePrepared Fe55(AlCrNi)45Cutting iron-based high-entropy alloyAfter the surface of the cylindrical compression sample is polished, the compression performance is measured by using an INSTRON-5569 mechanical testing machine under the room temperature condition, and the loading speed of a pressure head is 1mm/min, as shown in figure 3;
FIG. 3 shows Fe prepared in example one55(AlCrNi)45The compressive stress-strain curve of the iron-based high-entropy alloy;
from FIG. 3, Fe prepared in example one55(AlCrNi)45The compression yield strength of the iron-based high-entropy alloy exceeds 1000MPa, the compression deformation exceeds 60 percent, and the iron-based high-entropy alloy is not broken, so that the iron-based high-entropy alloy has excellent comprehensive mechanical properties.
Example one preparation of Fe55(AlCrNi)45The yield strength of the iron-based high-entropy alloy is 1028MPa, the breaking strength is more than 3000MPa, and the ultimate strain epsilonp(%) is greater than 60%.
Example two: a preparation method of a basal high-entropy alloy is completed according to the following steps:
firstly, preparing raw materials:
weighing 80% of alloy matrix and 20% of alloying elements according to the mass percentage to obtain a raw material of the high-entropy alloy with the matrix;
the alloy matrix in the first step is Fe and Cr; the molar ratio of Fe to Cr in the alloy matrix is b, and b is 1;
the alloying elements in the first step are Al and Ni; the molar ratio of Al to Ni in the alloying elements is a, and a is 1;
secondly, adding the raw materials of the base high-entropy alloy weighed in the step one into a ceramic crucible in an induction melting furnace in sequence from low melting point to high melting point;
thirdly, vacuumizing the induction melting furnace until the vacuum degree of the induction melting furnace is lower than 2.0 multiplied by 10-3Introducing argon into the induction smelting furnace until the pressure in the induction smelting furnace reaches 0.05 MPa;
fourthly, repeating the step three for 5 times;
fifthly, smelting the raw material of the base high-entropy alloy for 10min under the argon atmosphere and the smelting current of 60A, and cooling along with the furnace to obtain (FeCr)80(AlNi)20Fe-Cr double-base high-entropy alloy.
Prepared from example two (FeCr)80(AlNi)20Cutting a sample from the Fe-Cr double-base high-entropy alloy, grinding and polishing the sample, and performing phase analysis by using a Japanese physical optical D/max-rB type X-ray diffractometer as shown in figure 4;
FIG. 4 is (FeCr) prepared in example two80(AlNi)20XRD (X-ray diffraction) pattern of the iron-chromium double-base high-entropy alloy;
as can be seen from FIG. 4, the (FeCr) prepared in example two80(AlNi)20The iron-chromium double-base high-entropy alloy has a simple crystal structure, and is composed of an alpha-Fe solid solution phase and a (Ni, Fe) Al phase with a B2 structure as shown by combining microstructure analysis.
FIG. 5 is (FeCr) prepared in example two80(AlNi)20SEM microscopic structure picture of iron-chromium double-base high-entropy alloy;
as can be seen from FIG. 5, the (FeCr) prepared in example two80(AlNi)20The Fe-Cr double-base high-entropy alloy has a large amount of nano precipitated phases, and the size of the nano phase is about 100-200 nm.
Prepared from example two (FeCr)80(AlNi)20Cutting out of Fe-Cr double-base high-entropy alloy
Figure BDA0001664221860000071
After the surface of the cylindrical compression sample is polished, the compression performance is measured by using an INSTRON-5569 mechanical testing machine under the room temperature condition, and the loading speed of a pressure head is 1mm/min, as shown in figure 6;
FIG. 6 is (FeCr) prepared in example two80(AlNi)20Compressive stress-strain curve of Fe-Cr double-base high-entropy alloy.
As can be seen from FIG. 6, example two produced (FeCr)80(AlNi)20The Fe-Cr double-base high-entropy alloy has high yield strength and breaking strength and good plasticity, so that the Fe-Cr double-base high-entropy alloy has excellent propertiesComprehensive mechanical property.
EXAMPLE two prepared (FeCr)80(AlNi)20The yield strength of the iron-chromium double-base high-entropy alloy is 1261MPa, the breaking strength is 2772MPa, and the ultimate strain epsilonp(%) was 47%.

Claims (2)

1. A preparation method of a basal high-entropy alloy is characterized by comprising the following steps:
firstly, preparing raw materials:
weighing 55% of alloy matrix and 45% of alloying elements according to mass percent to obtain a raw material of the high-entropy alloy with the matrix;
the alloy matrix in the first step is Fe;
the alloying elements in the first step are Al, Cr and Ni; the molar ratio of any two elements in the alloying elements is a, and a is 1;
secondly, adding the raw materials of the base high-entropy alloy weighed in the step one into a copper mold crucible in a non-consumable vacuum arc melting furnace in sequence according to the sequence of the melting points of the materials from low to high;
thirdly, vacuumizing the non-consumable vacuum arc melting furnace until the vacuum degree of the non-consumable vacuum arc melting furnace is lower than 1.0 multiplied by 10-3Introducing argon into the non-consumable vacuum arc melting furnace until the pressure in the non-consumable vacuum arc melting furnace is 0.05 MPa;
fourthly, repeating the third step for 3 times;
fifthly, repeatedly smelting the raw material of the base high-entropy alloy for 5 times under the condition that the smelting current is 250A, wherein the smelting time is 2min each time, and cooling along with the furnace to obtain Fe55(AlCrNi)45An iron-based high entropy alloy.
2. A preparation method of a basal high-entropy alloy is characterized by comprising the following steps:
firstly, preparing raw materials:
weighing 80% of alloy matrix and 20% of alloying elements according to the mass percentage to obtain a raw material of the high-entropy alloy with the matrix;
the alloy matrix in the first step is Fe and Cr; the molar ratio of Fe to Cr in the alloy matrix is b, and b is 1;
the alloying elements in the first step are Al and Ni; the molar ratio of Al to Ni in the alloying elements is a, and a is 1;
secondly, adding the raw materials of the base high-entropy alloy weighed in the step one into a ceramic crucible in an induction melting furnace in sequence from low melting point to high melting point;
thirdly, vacuumizing the induction melting furnace until the vacuum degree of the induction melting furnace is lower than 2.0 multiplied by 10-3Introducing argon into the induction smelting furnace until the pressure in the induction smelting furnace reaches 0.05 MPa;
fourthly, repeating the step three for 5 times;
fifthly, smelting the raw material of the base high-entropy alloy for 10min under the argon atmosphere and the smelting current of 60A, and cooling along with the furnace to obtain (FeCr)80(AlNi)20Fe-Cr double-base high-entropy alloy.
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