CN101386928A - Method for preparing high-entropy alloy containing immiscible element - Google Patents

Method for preparing high-entropy alloy containing immiscible element Download PDF

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CN101386928A
CN101386928A CNA2008102334779A CN200810233477A CN101386928A CN 101386928 A CN101386928 A CN 101386928A CN A2008102334779 A CNA2008102334779 A CN A2008102334779A CN 200810233477 A CN200810233477 A CN 200810233477A CN 101386928 A CN101386928 A CN 101386928A
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powder
alloy
entropy alloy
immiscible
preparing
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CN101386928B (en
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冯晶
肖冰
陈敬超
于杰
周荣
张利娟
王景
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Kunming University of Science and Technology
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Kunming University of Science and Technology
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Abstract

The invention discloses a preparation method for a novel high-entropy alloy structure material. A plurality kinds of alloy element powder which can not form a miscible system are used as raw materials, thereby solving the solid solution problem of the alloy elements without solid solution region during the high-entropy alloy preparation, that is, mixing the powders in a planetary high-energy ball milling machine and obtaining ultra-fine powder of an immiscible system simultaneously through strong mechanical alloying function. When the alloy powder is pressed into a pressing blank, the heating treatment process condition is controlled to allow the alloy elements to diffuse through a short path and form a uniform multi-principal element mixing body containing no intermetal compound in a blank body, and a single-phase solid solution is obtained. The novel alloy prepared by the method is widely used in engine parts made of a high-temperature and creep resistance material, skins and tails of large thrust weight ratio high-speed aircrafts, corrosion resistant and wear resistant parts, wear-resistant materials such as pipes, gears and bearings and other structural material fields.

Description

A kind of method for preparing high-entropy alloy that contains immiscible element
Technical field
The present invention relates to alloy material preparation science field, particularly relate to the preparation method who contains the immiscible element high-entropy alloy.
Background technology
Known high-entropy alloy present Research: 20 end of the centurys, known conventional alloys is near maturation and state of saturation, the conventional alloys idea has been difficult to the new alloy system of the recreation alloy that breaks in other words in old alloy system, but the high-entropy alloy idea can produce many alloy systems, produces many interesting characteristics.So-called polynary (nanometer) high-entropy alloy is exactly the alloy of multiple element, and wherein each principal element all has high atomic percent, and the someone defines the principal element number of high-entropy alloy more than or equal to 5, but its atomic percent all is no more than 35%.That is to say that high-entropy alloy contains a principal element more than 50% unlike conventional alloys.Known conventional alloys experience makes the people think that a plurality of principal element alloys will produce multiple intermetallic compound by mistake easily, not only is difficult to analysis but also material and becomes fragile, and lacks applicability.Yet by discovering, this experience is not suitable for high-entropy alloy, because metallic element for a long time, high entropy effect can promote the mixing between element on the contrary, form body-centered cubic structure BCC or face-centred cubic structure FCC or non-crystal structure, do not form brittle intermetallic compound and be not inclined to.Known Gibbs one after another is thought, the number p=n+1 of the equilibrium phase that the alloy system of n kind element can produce, the number of phases p that when nonequilibrium freezing, forms〉n+1, but it is in fact really not so, in many pivots high-entropy alloy, the alloy system of n kind element only can form simple body-centered cubic structure BCC or single or limited several items such as face-centred cubic structure FCC or non-crystal structure, and the number of phases that is not the prediction of Gibbs one after another is a lot.The new feature of this alloy makes such alloy have a lot of new character, usually has the magnetic electricity performance of high high-temp stability, solidity to corrosion, high strength, high rigidity, high anti-oxidation character, excellence etc., and alloy compositions can in very large range be adjusted, for metallic substance has been started a new field, become a kind of brand-new material that has development potentiality, related application holds out broad prospects.
The preparation of traditional sosoloid is all according to the dependency rule of equilibrium phase diagram, but can not solid solution between in fact a lot of element, and an aspect is the solid solubility restriction, and other then do not dissolve each other fully.The early-stage Study of this seminar finds, causes that complete immiscible major cause is electronic structure and atomic property between the element, and is not only that known tradition is thought factors such as electronegativity and atomic size.The known element that do not dissolve each other is difficult to form sosoloid, in the preparation of high-entropy alloy, Many researchers has been avoided the interpolation of unmixing element, method is mentioned casting as is well known, spray deposition, rapid solidification methods etc. are main means with rapid solidification method especially, segregation can not take place because only could guarantee the alloying element that reaches the 5-9 kind in the high-entropy alloy in the process of quench solidification, perhaps cause intermetallic compound to form.The main institute of international known high-entropy alloy is the Taiwan, and research is less relatively, perhaps at the early-stage at home.
Summary of the invention
The high-entropy alloy preparation method that this patent is mentioned, can satisfy dissolving each other between the arbitrary element, add the element that alloy only limits to form sosoloid thereby can solve,, can expand the nature and extent of high-entropy alloy greatly for the high-entropy alloy preparation of new special composition provides possibility.The alloy material that the characteristics of this patent are to adopt the mechanical alloying method of high-energy ball milling can be formed arbitrarily in principle, material is by constantly collision in the high-energy ball milling process, cold welding, grind, recrystallize etc. make the continuous refinement of particle can obtain nano-powder material, owing to itself do not dissolve each other between the element that adds, the alloy that forms is actually the miscible complex construction of a kind of standard, and what obtain is non-equilibrium phase or the tissue that does not have on the equilibrium phase diagram.Because high-energy ball milling method can make all even grain refining of high-entropy alloy material structure of many pivots, thereby make high entropy material have new performance and character, this method is applied to the novel non-equilibrium alloy phase that the exploitation of accurate miscible system material can obtain not having on the phasor, thereby researchs and develops out the type material of difference and conventional alloys.
The present invention is that have strong novelty a kind of novel contains difficult miscible high-entropy alloy material preparation method, its objective is and propose a kind of preparation technology who solves unmixing system high-entropy alloy, reach the preparation high function alloys of many pivots (being defined as many pivots alloy of 5 ~ 13 yuan at present), be another alloy world outside the known alloys, because the magnetic electricity performances of its high high-temp stability, solidity to corrosion, high strength, high rigidity, high anti-oxidation character, excellence etc. are frontiers of metallic substance.This patent is a raw material with the multiple alloying element powder that can not form miscible system, solved the alloying element solid solution problem that does not have the solution area in the high-entropy alloy preparation process, its preparation technology's method is reasonable, and the use character and the range of application of novel high-entropy alloy are increased greatly.
The present invention realizes by following scheme.Adopt the pure metal powder; pure non-metal powder is (as silicon; boron etc.) or powdered alloy; the element of shared weight percent and adding requires to adjust according to predetermined alloy material; raw material calculates the stoichiometric ratio of each alloying element by particular requirement; will be through the further refinement in high energy ball mill of the material after the batching; the process argon shield of mechanical alloying; the high-entropy alloy powder of preparation is handled in a vacuum; the mould of under vacuum or protective atmosphere, powder being packed into; adopt the two-way compacting of punching block; and, put into sintering oven and carrying out the sample sintering under argon gas or the reducing atmosphere or under the vacuum condition with the further compression moulding of cold isostatic press.
Described high-entropy alloy is the alloy that contains multiple element, and wherein each principal element all has high atomic percent, and the principal element number is more than or equal to 5, but its atomic percent all is no more than 35%.
Described pure metal powder or alloy powder need be avoided oxidation in operating process, need anneal under hydrogen or other reducing atmosphere before the operation that experimentizes, and guarantee the purity of powder.
It is described that to carry out mechanical alloying in high energy ball mill be that the powder that screening is good is put into planetary high-energy ball mill; abrading-ball and mill jar employing corundum or agate material preparation; milling atmosphere adopts argon shield, rotating speed 800-1200rad/min, 10-60 hour ball milling time.
The two-way compacting of described punching block: 400-600Mpa, cold isostatic compaction: 250-400Mpa.
Described sintering carries out in vacuum oven or feeds protective atmosphere, and sintering temperature: 500-1000 ℃, sintering time 3-8 hour, vacuum sintering required vacuum tightness to be about 10 -6-10 -4Pa, protective atmosphere adopts argon gas or hydrogen.
Described raw material be the granularity of pure metal powder, pure non-metal powder (as silicon, boron etc.) or powdered alloy less than 100 microns, purity requirement〉99%.
Al 31Sn 26Cu 17Ni 10Ti 10Zn 6High-entropy alloy, the composition of this alloy be by weight percentage: 31% aluminium powder, 26% glass putty, 17% copper powder, 10% nickel powder, 10% titanium valve, 6% zinc powder.
Zr 21W 16Cr 14Nb 13Mo 13Fe 10Hf 7Cu 6High-entropy alloy, the composition of this alloy be by weight percentage: 21% zirconium, 16% tungsten powder, 14% chromium powder, 13% niobium powder, 13% molybdenum powder, 10% iron powder, 7% hafnium powder, 6% copper powder.
Pb 21Sn 20Ag 17Nb 16Mg 14Mn 6B 6High-entropy alloy, the composition of this alloy be by weight percentage: the accurate alloy powder of 41% slicker solder, 17% silver powder, 16% niobium powder, 14% magnesium powder, 6% manganese powder, 6% boron powder.
Compare advantage and the positively effect that is had with known technology:
The previous research work of this research team shows, the method for preparing high-entropy alloy of the non-miscible system of processing of present patent application is a kind of high-entropy alloy preparation method at the unmixing alloying element that report is not arranged as yet, its principal feature is to realize dissolving each other between the arbitrary element, add the element that alloy only limits to form sosoloid thereby solved, for the preparation of the high-entropy alloy of new special composition provides possibility, beat the nature and extent of having expanded high-entropy alloy greatly.The alloy material that the characteristics of this patent are to adopt the mechanical alloying method of high-energy ball milling can be formed arbitrarily in principle, material is by constantly collision in the high-energy ball milling process, cold welding, grind, recrystallize etc. make the continuous refinement of particle, can obtain multiple elementary composition high-entropy alloy material, owing to itself do not dissolve each other between the element that adds, the alloy that forms is actually the miscible complex construction of a kind of standard, normally simple face-centered cubic or body-centered cubic, what obtain is non-equilibrium phase or the tissue that does not have on the equilibrium phase diagram.Because high-energy ball milling method can make all even grain refining of high-entropy alloy material structure of many pivots, thereby make high entropy material have high high-temp stability, solidity to corrosion, high strength, high rigidity, high anti-oxidation character, excellent magnetic electricity performance etc., and alloy compositions can in very large range be adjusted, start a wide prospect for metallic substance, become a kind of type material that has development potentiality.
The alloy material that this patent adopts the mechanical alloying method of high-energy ball milling to be formed arbitrarily, material is by constantly collision in the high-energy ball milling process, cold welding, grind, recrystallize etc. make the continuous refinement of particle, can obtain nano bulk material, owing to itself do not dissolve each other between the element that adds, the alloy that forms is actually the miscible complex construction of a kind of standard, what obtain is non-equilibrium phase or the tissue that does not have on the equilibrium phase diagram, its normally simple body-centered cubic or face-centred cubic structure are the novel non-equilibrium alloy phases that does not have on a kind of phasor.
The high-entropy alloy preparation method that this patent is mentioned, can satisfy dissolving each other between the arbitrary element, add the element that alloy only limits to form sosoloid thereby solved,, expanded the nature and extent of high-entropy alloy greatly for the high-entropy alloy preparation of new special composition provides possibility.The method of present patent application is applied to the novel non-equilibrium alloy phase that the exploitation of accurate miscible system material can obtain not having on the phasor, thus the type material of research difference and conventional alloys.
The accurate miscible high-entropy alloy material that this patent is mentioned has been broken through traditional restriction, it is a kind of composition that can in wide range, adjust alloy material, solved the solid solution problem between the unmixing element, thereby obtained the new property of material, it forms Stability Analysis of Structures the alloy of preparation, over-all properties is good, has the magnetic electricity performance of high high-temp stability, solidity to corrosion, high strength, high rigidity, high anti-oxidation character, excellence etc., especially can be applicable to special functional materials and structured material field.The more present known alloy material of its production cost is low, the simple and control easily of entire production process, pollution-free or less contamination, can form production in enormous quantities.The high-entropy alloy material of preparation can adopt metal or non-metallic element arbitrarily according to the demand of character fully, make the research range and the use value of novel alloy material improve greatly, pertinent literature is looked into newly and is shown, the preparation method of the difficult miscible high-entropy alloy of solution mentioned in this article is not at international and domestic open report, related science and technical study field still lack at present, worldwide and find no related application.
Description of drawings
Further specify flesh and blood of the present invention with example below, but content of the present invention is not limited to this.
Fig. 1 is a process flow sheet of the present invention.
Embodiment
Fig. 1 is a process flow sheet of the present invention.Preparation 5-10 kind pure metal or powdered alloy; raw material calculates the stoichiometric ratio of each alloying element by particular requirement; with the material further refinement in high energy ball mill that makes; the process argon shield of mechanical alloying; the high-entropy alloy powder of preparation is handled in vacuum glove box; the suitable mould of under vacuum or protective atmosphere, powder being packed into; adopt the two-way compacting of punching block; and, put into sintering oven and carrying out the sample sintering under argon gas or the reducing atmosphere or under the vacuum condition with the further compression moulding of cold isostatic press.The strict control of sintering process associated process conditions makes alloying constituent even, makes alloying element solid solution or be uniformly dispersed fully, makes the miscible structure of corresponding standard, takes out and promptly gets the high-entropy alloy block materials.
Concrete implementing process and method:
One, material composition, granularity and shared weight percent thereof
1, base-material:
Pure metal powder, pure non-metal powder (as silicon, boron etc.), or powdered alloy; Powder size is less than 100 microns.
Purity requirement:〉99%,
The element of shared weight percent and adding requires to adjust according to predetermined alloy material.
Two, technical qualification
1. pure metal powder or alloy powder need be avoided oxidation in operating process, need anneal under hydrogen or other reducing atmosphere before the operation that experimentizes, and guarantee the purity of powder;
2. in high energy ball mill, carry out mechanical alloying: will screen good powder and put into planetary high-energy ball mill, abrading-ball and mill jar employing corundum or agate material preparation, milling atmosphere adopts argon shield, rotating speed 800-1200rad/min, 10-60 hour ball milling time;
3. operate in glove box: the powder for preparing is inserted particular mold, and the entire treatment process is carried out under vacuum environment, prevents the powder oxidation;
4. biscuit compacting pressure
The two-way compacting of punching block: 400-600MPa;
Cold isostatic compaction: 250-400MPa;
5. sintering temperature: 500-1000 ℃, time 3-8 hour; Carry out in vacuum oven, perhaps feed protective atmosphere, vacuum sintering requires vacuum tightness to be about 10 -6-10 -4Pa; Protective atmosphere adopts argon gas or hydrogen.
Embodiment 1
Al 31Sn 26Cu 17Ni 10Ti 10Zn 6The high-entropy alloy preparation:
31% aluminium (Al) powder (constituent content per-cent mentioned in this article specify all unify to refer to weight percent), 26% glass putty (Sn) by weight percentage, 17% copper powder (Cu), 10% nickel powder (Ni), 10% titanium valve (Ti), 6% zinc powder (Zn), the alloyage powder, wherein aluminium and tin element belong to solid-state immiscible system.Through hydrogen annealing 4 hours in the reducing atmosphere stove, insert in the ball grinder of corundum material, vacuumize, charge into argon gas, under argon shield atmosphere, carry out mechanical alloying.Planetary high-energy ball mill rotating speed 800rad/min, 15 hours ball milling time, the accurate miscible powdered alloy of the ultra-fine high entropy of collecting is taken out in glove box, insert in the preprepared mould, two-way compacting in punching block, compression moulding pressure 350MPa, and further suppress with isostatic cool pressing equipment, compression moulding pressure 300MPa, sample is put into the sintering oven sintering, 650 ℃ of sintering temperatures, sintering time 4 hours, it is even that taking-up obtains grain size distribution, and alloy structure is single body-centered cubic structure mutually.The alloy of preparation has certain ductility and plasticity after testing, and toughness can be carried out to a certain degree extrusion processing and rolling deformation, can be used for the related industries field.
Embodiment 2
Pb 21Sn 20Ag 17Nb 16Mg 14Mn 6B 6The high-entropy alloy preparation:
The accurate alloy powder of 41% lead (Pb) tin (Sn) by weight percentage, 17% silver powder (Ag), 16% niobium powder (Nb), 14% magnesium powder (Mg), 6% manganese powder (Mn), 6% boron powder (B), the alloyage powder, wherein lead and tin and boron belong to solid-state immiscible system each other.Through hydrogen annealing 3 hours in the reducing atmosphere stove, insert in the ball grinder of corundum material, vacuumize, charge into argon gas, under argon shield atmosphere, carry out mechanical alloying.Planetary high-energy ball mill rotating speed 1000rad/min, 25 hours ball milling time, the accurate miscible powdered alloy of the ultra-fine high entropy of collecting is taken out in glove box, insert in the preprepared mould, two-way compacting in punching block, compression moulding pressure 300MPa, and further suppress with isostatic cool pressing equipment, compression moulding pressure 250MPa, sample is put into the sintering oven sintering, 550 ℃ of sintering temperatures, sintering time 5 hours, it is even that taking-up obtains grain size distribution, and alloy structure is single face-centred cubic structure mutually.The alloy of preparation has certain ductility and plasticity after testing, and toughness can be carried out to a certain degree extrusion processing and rolling deformation, and is totally different with known conventional alloys performance, but the fundamental characteristics with known alloys can be used for the related industries field.
Embodiment 3
Zr 21W 16Cr 14Nb 13Mo 13Fe 10Hf 7Cu 6The high-entropy alloy preparation:
21% zirconium (Zr) powder, 16% tungsten powder (W) by weight percentage, 14% chromium powder (Cr), 13% niobium powder (Nb), 13% molybdenum powder (Mo), 10% iron powder (Fe), 7% hafnium powder (Hf), 6% copper powder (Cu), the alloyage powder, wherein copper and chromium element belong to the solid-state difficulty system of dissolving each other.Through hydrogen annealing 8 hours in the reducing atmosphere stove, insert in the ball grinder of corundum material, vacuumize, charge into argon gas, under argon shield atmosphere, carry out mechanical alloying.Planetary high-energy ball mill rotating speed 1200rad/min, 45 hours ball milling time, the accurate miscible powdered alloy of the ultra-fine high entropy of collecting is taken out in glove box, insert in the preprepared mould, two-way compacting in punching block, compression moulding pressure 350MPa, and further suppress with isostatic cool pressing equipment, compression moulding pressure 300MPa, sample is put into the sintering oven sintering, 850 ℃ of sintering temperatures, sintering time 4 hours, it is even that taking-up obtains grain size distribution, and alloy structure is single face-centred cubic structure mutually.The alloy of preparation has higher hardness and wear resistance after testing, can be used for the related industries field.

Claims (10)

1. method for preparing high-entropy alloy that contains immiscible element; it is characterized in that: adopt the pure metal powder; pure non-metal powder or powdered alloy; the element of shared weight percent and adding requires to adjust according to predetermined alloy material; raw material calculates the stoichiometric ratio of each alloying element by particular requirement; will be through the further refinement in high energy ball mill of the material after the batching; the process argon shield of mechanical alloying; the high-entropy alloy powder of preparation is handled in a vacuum; the mould of under vacuum or protective atmosphere, powder being packed into; adopt the two-way compacting of punching block; and, put into sintering oven and carrying out the sample sintering under argon gas or the reducing atmosphere or under the vacuum condition with the further compression moulding of cold isostatic press.
2, preparation according to claim 1 contains the method for preparing high-entropy alloy of immiscible element, it is characterized in that: described high-entropy alloy is the alloy that contains multiple element, wherein each principal element all has high atomic percent, the principal element number is more than or equal to 5, but its atomic percent all is no more than 35%.
3, preparation according to claim 1 contains the method for preparing high-entropy alloy of immiscible element, it is characterized in that: described pure metal powder or alloy powder need be avoided oxidation in operating process, before the operation that experimentizes, need under hydrogen or other reducing atmosphere, anneal, guarantee the purity of powder.
4, preparation according to claim 1 contains the method for preparing high-entropy alloy of immiscible element; it is characterized in that: described to carry out mechanical alloying in high energy ball mill be that the powder that screening is good is put into planetary high-energy ball mill; abrading-ball and mill jar employing corundum or agate material preparation; milling atmosphere adopts argon shield; rotating speed 800-1200rad/min, 10-60 hour ball milling time.
5, preparation according to claim 1 contains the method for preparing high-entropy alloy of immiscible element, it is characterized in that: the two-way compacting of described punching block: 400-600Mpa, cold isostatic compaction: 250-400Mpa.
6, preparation according to claim 1 contains the method for preparing high-entropy alloy of immiscible element; it is characterized in that: described sintering carries out in vacuum oven or feeds protective atmosphere; sintering temperature: 500-1000 ℃, sintering time 3-8 hour, vacuum sintering required vacuum tightness to be about 10 -6-10 -4Pa, protective atmosphere adopts argon gas or hydrogen.
7, preparation according to claim 1 contains the method for preparing high-entropy alloy of immiscible element, it is characterized in that: described raw material be the granularity of pure metal powder, pure non-metal powder or powdered alloy less than 100 microns, purity requirement〉99%.
8, preparation according to claim 1 contains the method for preparing high-entropy alloy of immiscible element, it is characterized in that: Al 31Sn 26Cu 17Ni 10Ti 10Zn 6High-entropy alloy, the composition of this alloy be by weight percentage: 31% aluminium powder, 26% glass putty, 17% copper powder, 10% nickel powder, 10% titanium valve, 6% zinc powder.
9, preparation according to claim 1 contains the method for preparing high-entropy alloy of immiscible element, it is characterized in that: Zr 21W 16Cr 14Nb 13Mo 13Fe 10Hf 7Cu 6High-entropy alloy, the composition of this alloy be by weight percentage: 21% zirconium, 16% tungsten powder, 14% chromium powder, 13% niobium powder, 13% molybdenum powder, 10% iron powder, 7% hafnium powder, 6% copper powder.
10, preparation according to claim 1 contains the method for preparing high-entropy alloy of immiscible element, it is characterized in that: Pb 21Sn 20Ag 17Nb 16Mg 14Mn 6B 6High-entropy alloy, the composition of this alloy be by weight percentage: the accurate alloy powder of 41% slicker solder, 17% silver powder, 16% niobium powder, 14% magnesium powder, 6% manganese powder, 6% boron powder.
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