CN112941356B - Cu-MoNbTaVW refractory high-entropy alloy bicontinuous structural material and preparation method thereof - Google Patents

Cu-MoNbTaVW refractory high-entropy alloy bicontinuous structural material and preparation method thereof Download PDF

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CN112941356B
CN112941356B CN201911258184.0A CN201911258184A CN112941356B CN 112941356 B CN112941356 B CN 112941356B CN 201911258184 A CN201911258184 A CN 201911258184A CN 112941356 B CN112941356 B CN 112941356B
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monbtavw
entropy alloy
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CN112941356A (en
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邵军超
金海军
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Institute of Metal Research of CAS
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    • 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
    • C22C1/10—Alloys containing non-metals
    • C22C1/1036—Alloys containing non-metals starting from a melt
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D23/00—Casting processes not provided for in groups B22D1/00 - B22D21/00
    • B22D23/04—Casting by dipping
    • 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
    • C22C1/08—Alloys with open or closed pores
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C30/00—Alloys containing less than 50% by weight of each constituent
    • C22C30/02—Alloys containing less than 50% by weight of each constituent containing copper
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C9/00—Alloys based on copper

Abstract

The invention discloses a Cu-MoNbTaVW refractory high-entropy alloy bicontinuous structural material and a preparation method thereof, belonging to the technical field of bicontinuous structural materials and high-entropy alloy preparation. The bicontinuous phases in the Cu-MoNbTaVW refractory high-entropy alloy bicontinuous structural material are a Cu phase and a MoNbTaVW refractory high-entropy alloy phase respectively, and the two phases are continuous in the whole three-dimensional space and penetrate through each other to form a network structure. The preparation method of the bicontinuous structural material comprises the following steps: precursor master alloy AxM1‑xImmersing the alloy into a liquid Cu melt to carry out dealloying corrosion reaction to generate a MoNbTaVW refractory high-entropy alloy porous phase, and then solidifying the refractory high-entropy alloy porous phase and the liquid Cu melt in the porous channel together to obtain the Cu-MoNbTaVW refractory high-entropy alloy bicontinuous structural material. The bicontinuous structural material prepared by the invention has compact structure and good interface combination between phases.

Description

Cu-MoNbTaVW refractory high-entropy alloy bicontinuous structural material and preparation method thereof
Technical Field
The invention relates to the technical field of preparation of bicontinuous structural materials and high-entropy alloys, in particular to a Cu-MoNbTaVW refractory high-entropy alloy bicontinuous structural material and a preparation method thereof.
Background
The bicontinuous structural material is a dual-phase material with a special microstructure, wherein two phases in the material have independent three-dimensional continuous network structures, the two phases are mutually interwoven and penetrate through the whole material, and the phases are mutually separated. The material has a unique two-phase interlocking structure, can fully exert the characteristics of each phase in the using process, is considered to greatly improve the toughness, the wear resistance, the shock absorption capability, the high-temperature performance and the like of the material, and has wide application prospects in the aspects of aerospace, high-strength and high-conductivity, high-energy weapons and the like.
The high-entropy alloy is a novel alloy material, breaks through the design concept that the traditional alloy mainly comprises one or two metal elements, at least comprises five main metal elements, the content of each element is between 5 and 35 percent, and the high-entropy alloy is prepared by methods such as electric arc melting, induction melting, mechanical alloying and the like according to the design proportion of equal atomic ratio or approximate equal atomic ratio. The high entropy effect due to the multiple principal elements can promote the alloy structure to be a simple face-centered cubic structure and a simple body-centered cubic structure. The high-entropy alloy has five major effects, namely a high-entropy effect on thermodynamics, a diffusion retarding effect on kinetics, a severe lattice distortion effect on structure, a 'cocktail' effect on performance and high stability on structure. Among them, refractory high-entropy alloys composed of metals with high melting points, such as W, Mo, Ta, Nb, V, Re, Ti, Zr, and Hf, have attracted considerable attention in recent years because of their excellent high-temperature mechanical properties and high-temperature thermal stability.
At present, research reports on refractory high-entropy alloys mainly focus on the preparation and performance of the high-entropy alloys. Although refractory high-entropy alloys have some outstanding excellent properties, actual service working condition environments often impose requirements on materials with various service properties. Due to the special structural characteristics of the bicontinuous structural material, the structural material can fully exert respective characteristics of two phases in the using process, so that if a network-shaped framework of the refractory high-entropy alloy can be formed in the bicontinuous structural material, the obtained bicontinuous structural material also has the excellent performance of the refractory high-entropy alloy. However, at present, a refractory high-entropy alloy is used as a bicontinuous structural material of one of the composition phases, and particularly, a copper-refractory high-entropy alloy bicontinuous structural material and a related preparation method of the material are not reported.
Disclosure of Invention
The invention aims to provide a Cu-MoNbTaVW refractory high-entropy alloy bicontinuous structural material and a preparation method thereof, wherein the prepared Cu-MoNbTaVW refractory high-entropy alloy bicontinuous structural material consists of two mutually-penetrated Cu phases and a MoNbTaVW refractory high-entropy alloy phase; the bicontinuous structural material prepared by the method has compact structure and good interface combination between phases.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a preparation method of a Cu-MoNbTaVW refractory high-entropy alloy bicontinuous structural material comprises the following steps:
(1) precursor mother for preparing liquid metal melt dealloying corrosion by adopting electric arc melting, induction melting, powder sintering and gas phase or electrochemical deposition processAlloy AxM1-xWherein A is composed of five elements of Mo, Nb, Ta, V and W, M is one or more elements of Ti, Zr, Hf, Ni and Mn, and x is 0.1-0.8;
(2) heating metal Cu to be molten to obtain liquid Cu melt; the heating temperature for melting the metal Cu is lower than that of the precursor master alloy AxM1-xMelting point of (2);
(3) precursor master alloy AxM1-xImmersing the alloy into a metal Cu melt to perform a dealloying corrosion reaction; in the reaction process, M elements capable of being dissolved in metal Cu in the precursor master alloy gradually enter the melt, the rest elements in the master alloy gradually form a MoNbTaVW refractory high-entropy alloy porous hole (the porous hole is formed from the initial interface and gradually generated from outside to inside) at the interface of the precursor and the Cu metal melt, and meanwhile, the Cu metal melt is filled in the porous hole of the MoNbTaVW refractory high-entropy alloy porous hole;
(4) and solidifying the MoNbTaVW refractory high-entropy alloy porous phase and the Cu metal melt in the pore channel thereof together to obtain the Cu-MoNbTaVW refractory high-entropy alloy bicontinuous structural material.
In the step (1), the precursor master alloy AxM1-xIn the A, the proportion of five elements of Mo, Nb, Ta, V and W is the same as the proportion of five elements in the designed MoNbTaVW refractory high-entropy alloy porous phase. .
In the step (3), the reaction temperature in the dealloying corrosion reaction is lower than that of the precursor master alloy AxM1-xIs simultaneously higher than the melting point of Cu, and the time of the dealloying corrosion reaction is between 1 second and 10 hours.
In the step (4), the solidification process may be performed in the liquid Cu melt, or may be performed outside the liquid Cu melt after being taken out of the liquid Cu melt.
In the preparation process of the Cu-MoNbTaVW refractory high-entropy alloy bicontinuous structural material, the structural size of the MoNbTaVW refractory high-entropy alloy phase can be adjusted by regulating and controlling the reaction temperature and the reaction time in the step (3); the higher the reaction temperature is, the larger the structure size of the MoNbTaVW refractory high-entropy alloy phase is; the longer the reaction time, the larger the structural size of the MoNbTaVW refractory high-entropy alloy phase.
In the Cu-MoNbTaVW refractory high-entropy alloy bicontinuous structural material prepared by the method, the content of the MoNbTaVW refractory high-entropy alloy phase can be adjusted by regulating the precursor master alloy AxM1-xThe content of A in the mixture is controlled.
The Cu-MoNbTaVW refractory high-entropy alloy bicontinuous structural material consists of a Cu phase and a MoNbTaVW refractory high-entropy alloy phase. The interface between the phase in the material is well combined with the interface between the phases, all the phases are continuous in three-dimensional space, and have microstructures with independent openings and mutually penetrate to form a bicontinuous phase structure.
The structural size range of a Cu phase and a MoNbTaVW refractory high-entropy alloy phase in the Cu-MoNbTaVW refractory high-entropy alloy bicontinuous structural material is 10 nm-50 mu m.
The invention has the following advantages and beneficial effects:
1. the invention provides a novel Cu-MoNbTaVW refractory high-entropy alloy bicontinuous structural material and a preparation method thereof. The Cu-MoNbTaVW refractory high-entropy alloy bicontinuous structural material with the phase structure size controllably adjusted within the range of 10 nm-50 mu m and the total mole percentage content of the MoNbTaVW refractory high-entropy alloy phase controllably adjusted within the range of 10-80% can be prepared by controlling parameters such as precursor components, heating temperature, heat preservation time and the like.
2. The Cu-MoNbTaVW refractory high-entropy alloy bicontinuous structural material prepared by the method has a compact structure, the interface between the Cu phase and the MoNbTaVW refractory high-entropy alloy phase is well combined, and the two phases are mutually penetrated and interlocked. The bicontinuous structural material not only keeps the high conductivity and heat conductivity and high plasticity of a Cu phase, but also has the excellent high-temperature mechanical and thermal stability of a MoNbTaVW refractory high-entropy alloy phase.
3. The preparation method provided by the invention has the advantages of simple and feasible process, lower equipment requirement, better economic benefit, convenient operation and wide application and popularization.
4. The Cu-MoNbTaVW refractory high-entropy alloy bicontinuous structural material provided by the invention is expected to be applied to the fields of ablation-resistant electrode materials for high-power devices, electronic devices, aerospace, high-energy weapons and the like.
Drawings
FIG. 1 shows a precursor master alloy (MoNbTaVW)40Ti60The scanning electron microscope photograph and the distribution map of the line component and the area component of each element.
FIG. 2 is a scanning electron microscope photograph and a distribution diagram of various element surface components of a Cu-MoNbTaVW refractory high-entropy alloy bicontinuous structural material prepared by dealloying corrosion in example 1.
FIG. 3 is a back-scattered electron photograph obtained from a scanning electron microscope CBS probe of a Cu-MoNbTaVW refractory high-entropy alloy prepared by dealloying corrosion in example 2.
FIG. 4 is a back-scattered electron photograph obtained from a scanning electron microscope CBS probe of the Cu-MoNbTaVW refractory high-entropy alloy prepared by dealloying corrosion in example 3.
FIG. 5 is a back-scattered electron photograph obtained from a scanning electron microscope CBS probe of the Cu-MoNbTaVW refractory high-entropy alloy prepared by dealloying in example 4.
Detailed Description
The invention is described in detail below with reference to the figures and examples.
The invention provides a Cu-MoNbTaVW refractory high-entropy alloy bicontinuous structural material with controllable structural size and component range and a preparation method thereof. Precursor master alloy AxM1-xAnd (wherein A is composed of five elements of Mo, Nb, Ta, V and W, M is one or more of Ti, Zr, Hf, Ni and Mn, and x is 0.1-0.8), immersing the alloy into a metal Cu melt with the temperature lower than the melting point of the precursor master alloy to perform dealloying corrosion to generate a MoNbTaVW refractory high-entropy alloy porous phase, and solidifying the porous phase and the metal Cu melt in the porous channel together to obtain the Cu-MoNbTaVW refractory high-entropy alloy bicontinuous structure material. The present invention will be described in detail below with reference to specific examples.
Example 1:
the Cu-MoNbTaVW refractory high-entropy alloy prepared by the embodiment has a Cu component and a Cu component60(MoNbTaVW)40I.e. MoNbTaVW refractory in bicontinuous structural materialsThe molar percentage of the high-entropy alloy phase is 40%, and the molar percentage of the Cu phase is 60% (the subsequent components are expressed in the same manner).
The specific preparation process flow is as follows:
pure Ti, pure Mo, pure Nb, pure Ta, pure V and pure W (the purity of raw materials is more than 99.5%) are weighed according to the atomic percentage of Ti, Mo, Nb, Ta, V and W being 60:8:8:8:8, mixed and smelted into precursor master alloy (MoNbTaVW) through arc melting in the argon protective atmosphere40Ti60An ingot.
② general (MoNbTaVW)40Ti60The ingot was sealed in a high purity quartz tube filled with argon gas for homogenization heat treatment at 1200 ℃ for 48 hours. .
③ heat-treated by linear cutting (MoNbTaVW)40Ti60The ingot is cut into pieces with the thickness of 2.0mm, and the outer surface of the ingot is polished, cleaned and dried.
Fourthly, precursor master alloy (MoNbTaVW)40Ti60One end of the sheet is punched and then bound by a pure Nb wire, and then is immersed into a liquid pure Cu (purity 99.99%) metal melt at 1150 ℃ under the protection of argon, and is taken out and cooled after heat preservation for 30 minutes.
Fifthly, cutting the reacted sample along the thickness direction, grinding and polishing, and then observing the tissue.
FIG. 1 shows the precursor master alloy (MoNbTaVW) before dealloying in example 140Ti60The scanning electron microscope photograph and the distribution map of the line component and the area component of each element. From the results, it can be seen that the respective elements in the master alloy are uniformly distributed.
FIG. 2 shows the precursor master alloy (MoNbTaVW) in example 140Ti60And keeping the temperature in a liquid Cu metal melt at 1150 ℃ for 30 minutes to obtain a scanning electron microscope photo of the bicontinuous structural material and a composition distribution diagram of each element surface in the bicontinuous structural material. From the results, a clear two-phase structure exists in the material, wherein one phase is a Cu phase (a small amount of residual Ti element exists in the Cu phase), the other phase is a network floccule structure containing five elements of Mo, Nb, Ta, V and W, and the five elements are uniformly distributed in the Cu phase and the network floccule structure. Thus, the final productThe material is a Cu-MoNbTaVW refractory high-entropy alloy bicontinuous structural material which is formed by a Cu phase and a MoNbTaVW refractory high-entropy alloy porous phase, and the structural size of the MoNbTaVW refractory high-entropy alloy porous phase is about 500 nm.
Example 2:
the Cu-MoNbTaVW refractory high-entropy alloy bicontinuous structural material prepared in this example is different from that of example 1 only in that: precursor master alloy composition is changed into (MoNbTaVW)60Ti40。
Fig. 3 is a back scattering electron photograph of the Cu-MoNbTaVW refractory high-entropy alloy bicontinuous structure material prepared in example 2, obtained under a CBS probe of a scanning electron microscope. Comparing with fig. 2, it can be seen that, as the contents of Mo, Nb, Ta, V, and W elements in the precursor master alloy increase, the content of the MoNbTaVW high-entropy alloy porous phase in the obtained Cu-MoNbTaVW refractory high-entropy alloy bicontinuous structural material also increases correspondingly.
Example 3:
the Cu-MoNbTaVW refractory high-entropy alloy bicontinuous structural material prepared in this example is different from that of example 1 only in that: precursor master alloy composition is changed into (MoNbTaVW)20Ti80。
Fig. 4 is a back scattering electron photograph of the Cu-MoNbTaVW refractory high-entropy alloy bicontinuous structure material prepared in example 3, obtained under a CBS probe of a scanning electron microscope. Comparing with fig. 2, it can be seen that, as the contents of Mo, Nb, Ta, V, and W elements in the precursor master alloy are reduced, the content of the MoNbTaVW high-entropy alloy porous phase in the obtained Cu-MoNbTaVW refractory high-entropy alloy bicontinuous structural material is also correspondingly reduced.
Example 4:
the Cu-MoNbTaVW refractory high-entropy alloy bicontinuous structural material prepared in this example is different from that of example 1 only in that: the dealloying corrosion reaction temperature is changed from 1150 ℃ to 1250 ℃.
Fig. 5 is a back scattering electron photograph of the Cu-MoNbTaVW refractory high-entropy alloy bicontinuous structure material prepared in example 4, obtained under a CBS probe of a scanning electron microscope. Comparing with FIG. 2, it can be seen that, with the increase of the dealloying corrosion reaction temperature, the structural size of the MoNbTaVW high-entropy alloy porous pores in the obtained Cu-MoNbTaVW refractory high-entropy alloy bicontinuous structural material is also increased from 500nm to about 3 μm.
Since the embodiments cannot be described in detail, the above description is only a single embodiment of the present invention, and does not limit the present invention in any way. It will be appreciated that those skilled in the art, upon attaining an understanding of the foregoing, may readily produce alterations to, variations of, and equivalents to such embodiments.

Claims (9)

1. A preparation method of a Cu-MoNbTaVW refractory high-entropy alloy bicontinuous structural material is characterized by comprising the following steps of: the bicontinuous structural material is a bicontinuous phase structure consisting of a Cu phase and a MoNbTaVW refractory high-entropy alloy phase, the Cu phase and the MoNbTaVW refractory high-entropy alloy phase both have independent open-cell structures, and the two phases are respectively continuous in a three-dimensional space and mutually penetrate through each other to form a network structure;
the preparation method of the Cu-MoNbTaVW refractory high-entropy alloy bicontinuous structural material comprises the following steps:
(1) preparation of precursor mother alloy AxM1-xWherein A is composed of five elements of Mo, Nb, Ta, V and W; m is one or more of Ti, Zr, Hf, Ni and Mn, and x is 0.1-0.8; the precursor master alloy AxM1-xThe alloy is prepared by adopting electric arc melting, induction melting, powder sintering, gas phase chemical deposition or electrochemical deposition processes;
(2) heating metal Cu to be molten to obtain liquid Cu melt;
(3) dealloying corrosion reaction: immersing the precursor master alloy into a liquid copper melt, and keeping the precursor master alloy at a certain temperature for a period of time to carry out dealloying corrosion reaction to form an open-pore three-dimensional continuous network-shaped MoNbTaVW refractory high-entropy alloy porous hole, and filling the liquid Cu melt into the porous hole of the MoNbTaVW refractory high-entropy alloy porous hole;
(4) solidifying the MoNbTaVW refractory high-entropy alloy porous phase and the liquid Cu melt in the pore channel thereof together, thereby obtaining the Cu-MoNbTaVW refractory high-entropy alloy bicontinuous structural material.
2. The preparation method of the Cu-MoNbTaVW refractory high-entropy alloy bicontinuous structural material of claim 1, characterized by comprising the following steps of: the MoNbTaVW refractory high-entropy alloy phase consists of five elements of Mo, Nb, Ta, V and W, and the molar percentage of each element in the MoNbTaVW refractory high-entropy alloy phase is 5-35%.
3. The preparation method of the Cu-MoNbTaVW refractory high-entropy alloy bicontinuous structural material of claim 1, characterized by comprising the following steps of: in the bicontinuous structural material, the molar percentage content of the MoNbTaVW refractory high-entropy alloy phase is between 10 and 80 percent.
4. The preparation method of the Cu-MoNbTaVW refractory high-entropy alloy bicontinuous structural material of claim 1, characterized by comprising the following steps of: in the bicontinuous structural material, the structural size range of a Cu phase and a MoNbTaVW refractory high-entropy alloy phase is 10 nm-50 mu m.
5. The preparation method of the Cu-MoNbTaVW refractory high-entropy alloy bicontinuous structural material of claim 1, characterized by comprising the following steps of: in the step (1), the precursor master alloy AxM1-xIn the A, the proportion of five elements of Mo, Nb, Ta, V and W is the same as the proportion of five elements in the designed MoNbTaVW refractory high-entropy alloy porous phase.
6. The preparation method of the Cu-MoNbTaVW refractory high-entropy alloy bicontinuous structural material of claim 1, characterized by comprising the following steps of: in the step (3), the reaction temperature in the dealloying corrosion reaction is lower than that of the precursor master alloy AxM1-xIs higher than that of Cu, and the time of dealloying corrosion reaction is between 1 second and 10 hours.
7. The preparation method of the Cu-MoNbTaVW refractory high-entropy alloy bicontinuous structural material of claim 1, characterized by comprising the following steps of: in the step (4), the solidification process can be carried out in the liquid Cu melt, and can also be carried out outside the melt after being taken out of the liquid Cu melt.
8. The preparation method of the Cu-MoNbTaVW refractory high-entropy alloy bicontinuous structural material of claim 1, characterized by comprising the following steps of: in the preparation process of the bicontinuous structural material, the structural size of the MoNbTaVW refractory high-entropy alloy phase can be adjusted by regulating and controlling the reaction temperature and the reaction time in the step (3); the higher the reaction temperature is, the larger the structure size of the MoNbTaVW refractory high-entropy alloy phase is; the longer the reaction time, the larger the structural size of the MoNbTaVW refractory high-entropy alloy phase.
9. The preparation method of the Cu-MoNbTaVW refractory high-entropy alloy bicontinuous structural material of claim 1, characterized by comprising the following steps of: in the prepared Cu-MoNbTaVW refractory high-entropy alloy bicontinuous structural material, the content of the porous phase of the MoNbTaVW refractory high-entropy alloy can be adjusted by regulating the precursor master alloy AxM1-xThe content of A in the mixture is controlled.
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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2007294689A (en) * 2006-04-25 2007-11-08 Toyota Motor Corp Thermoelectric conversion element
CN108603248A (en) * 2016-03-04 2018-09-28 东北泰克诺亚奇股份有限公司 The manufacturing method and carbon composite of carbon composite

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2007294689A (en) * 2006-04-25 2007-11-08 Toyota Motor Corp Thermoelectric conversion element
CN108603248A (en) * 2016-03-04 2018-09-28 东北泰克诺亚奇股份有限公司 The manufacturing method and carbon composite of carbon composite

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