CN107151755B - A method of preparing the high-entropy alloy of close-packed hexagonal structure - Google Patents
A method of preparing the high-entropy alloy of close-packed hexagonal structure Download PDFInfo
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- CN107151755B CN107151755B CN201710329341.7A CN201710329341A CN107151755B CN 107151755 B CN107151755 B CN 107151755B CN 201710329341 A CN201710329341 A CN 201710329341A CN 107151755 B CN107151755 B CN 107151755B
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- 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
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
- C21D8/005—Modifying the physical properties by deformation combined with, or followed by, heat treatment of ferrous alloys
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C33/00—Making ferrous alloys
- C22C33/04—Making ferrous alloys by melting
- C22C33/06—Making ferrous alloys by melting using master alloys
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
- C22C38/28—Ferrous alloys, e.g. steel alloys containing chromium with titanium or zirconium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
- C22C38/30—Ferrous alloys, e.g. steel alloys containing chromium with cobalt
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
- C22C38/38—Ferrous alloys, e.g. steel alloys containing chromium with more than 1.5% by weight of manganese
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Abstract
The invention discloses a kind of methods for the high-entropy alloy preparing close-packed hexagonal structure, including following preparation process：Using a variety of elemental metals or intermediate alloy as raw material, feed intake according to certain proportioning, the melt raw material in smelting furnace；Melt is molded into mold and obtains ingot casting；The macro-components segregation that homogenizing annealing eliminates ingot casting is carried out to ingot casting；Ingot casting is subjected to compressive deformation in tri- directions x, y and z respectively, obtains the high-entropy alloy with close-packed hexagonal structure.The present invention is by selecting suitable metallic element and matching the alloy constituted, keep the alloy casting state Gibbs free energy and system Gibbs free energy difference when its close-packed hexagonal structure different smaller to have phase transformation ability, pass through the large plastometric set in three directions later, initial structure is set fully mutually to become close-packed hexagonal structure, to obtain the high-entropy alloy with close-packed hexagonal structure.High-entropy alloy mechanical property produced by the present invention is substantially better than the high-entropy alloy of existing close-packed hexagonal structure.
Description
Technical field
The present invention relates to a kind of preparation method of high-entropy alloy, especially a kind of high-entropy alloy with close-packed hexagonal structure
Preparation method.
Background technology
Since TaiWan, China scholar Ye Junwei in 2004 and American scholar Cantor successively propose high-entropy alloy（High-
Entropy Alloys abbreviations HEA）Concept since, high-entropy alloy just causes the interest of vast metal material researcher.It is high
Entropy alloy is a kind of emerging in recent years alloy material, it broken essential element in conventional alloys only have it is a kind of or two kinds
Alloy design concept, but constituted at least five kinds of or more essential elements, and the atom percentage content of each element is 5%
Between ~ 35%.Due to this special composition, high-entropy alloy has the four big effects for being different from other alloys：Height thermodynamically
Entropic effect, sluggish diffusion effect kinetically, the distortion of lattice in structure and cocktail effect.The presence of this four big effect
So that high-entropy alloy shows the property different from other conventional alloys, there are prodigious researching value and development and application
Meaning.Due to application potential diversification, the diversification of industry faced, therefore in the upgrading of conventional alloys industry and high-tech industry
Development in, the space that will also have high-entropy alloy infinitely to play undoubtedly is of great significance to the promotion of conventional metallurgical industry.
Crystal is caused to be easily formed simple cubic solid solution phase, nanometer since alloy constituent element increases the high entropic effect generated
The high performance phases such as grain disperse phase, amorphous phase, and not weld metal zone brittle intermetallic thing.For metal material, face-centered cubic knot
Structure, body-centered cubic structure and close-packed hexagonal structure are most important three types.At present successfully prepared pure face-centered cubic,
The high-entropy alloy of pure body-centered cubic and face-centered cubic mixing body-centered cubic structure, and show unique mechanical property and wide
Application prospect.However the high-entropy alloy about close-packed hexagonal structure is but rarely reported.
Invention content
The purpose of the present invention is quasi- to provide a kind of method for the high-entropy alloy preparing close-packed hexagonal structure.
The thinking of the high-entropy alloy of traditional preparation close-packed hexagonal structure is to select the various simple substance member with close-packed hexagonal
It is then by traditional smelting technology that each simple substance element is fully melt-blended usually as the constituent element of high-entropy alloy, pass through later
Casting forms alloy.This method only successfully prepares the high-entropy alloy of two kinds of close-packed hexagonal structures at present（YGdTbDyLu and
HoDyYGdTb）.
The design and above-mentioned conventional method of the present invention is entirely different, and design of the invention is as follows：It is suitable single to choose some
Matter metallic element first passes through melt casting process and obtains cast alloy, and the crystal structure of the cast alloy is not close-packed hexagonal knot
Structure, however the cast alloy has phase transformation characteristic, specifically the current system gibbs of the cast alloy is free
System Gibbs free energy difference when can be changed into close-packed hexagonal structure with it is different smaller；The cast alloy is subjected to three-dimensional change
Shape specifically carries out compressive deformation respectively in tri- directions x, y and z, to make alloy deform upon induced phase transition from non-
Close-packed hexagonal structure is changed into close-packed hexagonal structure, obtains the high-entropy alloy with close-packed hexagonal structure.
To realize goal of the invention, according to above-mentioned design, the present invention provides a kind of high entropy conjunctions preparing close-packed hexagonal structure
The method of gold, including following preparation process：
（1）Using elemental metals and/or intermediate alloy as raw material, feed intake according to the proportioning of each metallic element, in smelting furnace
Melt raw material；
（2）Melt is molded into mold and obtains ingot casting；
（3）The macro-components segregation that homogenizing annealing eliminates ingot casting is carried out to ingot casting, obtains cast alloy；The as cast condition is closed
Gold utensil has face-centred cubic structure；
（4）Cast alloy is subjected to three-dimensional large plastometric set, i.e., carries out compressive deformation respectively in tri- directions x, y and z, obtains
To the high-entropy alloy with close-packed hexagonal structure.
The present invention by selecting Suitable metal elements and proportioning to constitute alloy, make the Gibbs free energy of the alloy casting state with
System Gibbs free energy difference when the alloy is changed into close-packed hexagonal structure is different smaller to have phase transformation ability,
It carries out compression respectively by tri- directions x, y and z later and generates large plastometric set, make the abundant phase transformation of the initial structure of cast alloy
For close-packed hexagonal structure, to realize goal of the invention.
To make alloy that there is phase transformation ability, the present inventor to be explored by a large amount of theoretical research, is anti-
Multiple big data simplation verification and experimental verification, being determined as the alloy for making to be formed has phase transformation ability, can pass through
Big plasticity compression makes cast alloy through being fully mutually deformed into high-entropy alloy, constitutes the metallic element type and each element of alloy first
Content must meet following condition：1）At room temperature, alloy determined by the metallic element type Yu content of selection, close-packed hexagonal
The Gibbs free energy of structure is higher than the Gibbs free energy of its face-centred cubic structure；2）And the close-packed hexagonal of the preferred alloy
The energy barrier difference of the Gibbs free energy of the corresponding face-centred cubic structure of Gibbs free energy of structure is in 1 ~ 10 eV per former
Son, further preferably 2 ~ 5 eV are per atom；3）The stacking fault energy of the corresponding face-centred cubic structure of the alloy is preferably 1 ~ 50
mJ/m2, further preferably 5 ~ 25 mJ/m2。
In the embodiment for the high-entropy alloy that the present invention prepares the close-packed hexagonal, elemental metals or intermediate alloy in raw material
It is selected, the metallic element of alloy is formed according to above-mentioned determination and the condition of its content carries out.For example, it is preferable to, alloying component
Selected includes five kinds of metallic elements of Fe, Mn, Ti, Co and Cr, and the Cr for Mn, 10at.% that each metal element content is 30at.%,
The Fe of the Ti and 45at.% of Co, 5at.% of 10at.%, it is further preferred that specific raw material is Fe-Mn intermediate alloys, Ti, Co
And the elemental metals of Cr, it feeds intake according to content proportioning.Thus the alloy constituted, the Gibbs free energy of close-packed hexagonal structure
Higher than the every atoms of 2 eV of Gibbs free energy of its face-centred cubic structure, the stacking fault energy of the corresponding face-centred cubic structure of the alloy is
20mJ/m2.For another example preferred, selected alloying component includes tetra- kinds of metallic elements of Fe, Mn, Co and Cr, and each metallic element contains
Amount is the Fe of the Co and 45at.% of Cr, 10at.% of Mn, 10at.% of 35at.%, the alloy thus constituted, close-packed hexagonal knot
For the Gibbs free energy of structure higher than the every atoms of 5 eV of Gibbs free energy of its face-centred cubic structure, the corresponding center of area of the alloy is vertical
The stacking fault energy of square structure is 25mJ/m2。
On the basis of alloy has phase transformation ability, to enable the abundant phase transformation of the initial structure of cast alloy
For close-packed hexagonal structure, the present invention provides the methods using large plastometric set.Conventional stretching or rolling deformation is tradition
Simple tension or compression there are two big deficiencies although also a degree of deformation can be carried out to material：First, tradition
Uniaxial Compression or simple tension mainly apply the stress in a direction to material internal crystal grain, be typically only capable to start 1 ~ 2
Sliding system cannot be such that face-centred cubic 12 sliding systems fully start, achieve the purpose that fully deformed；Second, it is traditional
Uniaxial Compression or simple tension deform the unstability and the fracture that necessarily lead to material in one direction due to continuing, it is difficult to material
Apply aximal deformation value, is also just difficult to that original face-centred cubic structure is made fully mutually to become close-packed hexagonal structure.Therefore, traditional drawing
It stretches or milling method is difficult to realize goal of the invention of the invention.The present invention is particularly pressed using tri- steering wheel streams of x, y and z
Compression deformation realizes large plastometric set, and overcome conventional method two are big insufficient, make the initial of the face-centred cubic structure of cast alloy
Tissue fully can mutually become close-packed hexagonal structure, ultimately form with the high-entropy alloy with close-packed hexagonal structure.
In the method provided by the invention using large plastometric set, it is preferred that for example in three embodiments, in x, y
50% compressive deformation has been carried out respectively with tri- directions z, and making cast alloy fully mutually becomes the high entropy conjunction of close-packed hexagonal structure
Gold；Preferably, in another embodiment, it is 40%, 20% to have carried out deflection respectively in tri- directions x, y and z to cast alloy
With 20% compressive deformation.
Compared with prior art, preparation method provided by the invention has the advantages that：
1）, abandoning tradition thinking of the present invention thinks all usually to constitute target by the simple substance member of close-packed hexagonal structure
The idea of alloy, can select not be close-packed hexagonal structure simple substance element so that alloy system select face it is broader；
2）, the present invention by tri- steering wheel streams of x, y and z carry out compression realize large plastometric set, the process is simply controllable,
It is easy to be generalized to fragile material system；
3), the high-entropy alloy of close-packed hexagonal structure prepared by the present invention includes abundant micro-structure, and mechanical property is apparent
Better than the high-entropy alloy of existing close-packed hexagonal structure, such as yield strength, the 108MPa reported compared with prior art, the present invention
Yield strength be more than 450 MPa.
Description of the drawings
The high-entropy alloy transmission electron microscope center bright field image for the close-packed hexagonal structure that Fig. 1 is obtained by embodiment 1.
The high-entropy alloy transmission electron microscope electron diffraction pattern for the close-packed hexagonal structure that Fig. 2 is obtained by embodiment 1, with solid matter
[01-11] tape spool standard diffraction style of hexagonal structure is completely the same.
The high-entropy alloy high resolution scanning images of transmissive electron microscope for the close-packed hexagonal structure that Fig. 3 is obtained by embodiment 1, and it is close
The atomic arrangement mode for arranging [- 2110] tape spool of hexagonal structure is completely the same.
Specific implementation mode
With specific embodiment, the present invention is described further below.
Embodiment 1
（1）With Fe-Mn intermediate alloys, Ti, Co and Cr elemental metals are raw material, according to the Cr of Mn, 10at.% of 30at.%,
The Fe proportionings of the Ti and 45at.% of Co, 5at.% of 10at.% feed intake, the melt raw material in smelting furnace；
（2）Melt is molded into mold and obtains ingot casting；
（3）The macro-components segregation that ingot casting is eliminated in 1050 degrees Celsius of heat preservations annealing in 12 hours is carried out to ingot casting；Formation has
The cast alloy of face-centred cubic structure；
（4）By the square that above-mentioned ingot casting wire cutting is x=10 mm, y=10 mm, z=10 mm, using forcing press in x, y
Compressive deformation 50% is carried out respectively with tri- directions z, obtains the high-entropy alloy with close-packed hexagonal structure.
Embodiment 2
Difference lies in steps with embodiment 1（1）Middle Mn contents are 35at.% and Ti contents are 0, and other parameters are identical.
Embodiment 3
Difference lies in steps with embodiment 1（4）Middle sample size is the mm of mm, z=10 of mm, y=10 of x=12, forcing press
The compression that deflection is 40%, 20% and 20% is carried out respectively in tri- directions x, y and z, and other parameters are identical.
Using the microstructure of the obtained high-entropy alloy of transmission electron microscope observation the various embodiments described above, and use constituency
Electron diffraction pattern and high-resolution-ration transmission electric-lens technology analysis calibration crystal structure, referring additionally to national standard GB/T228.1-2010
《Metal material stretching test part 1：Room temperature test method》The yield strength of test sample.As Fig. 1 is obtained by embodiment 1
Close-packed hexagonal structure high-entropy alloy transmission electron microscope center bright field image；The close-packed hexagonal structure that Fig. 2 is obtained by embodiment 1
High-entropy alloy transmission electron microscope selective electron diffraction style, show in figure and spread out with [01-11] tape spool standard of Patterns for Close-Packed Hexagonal Crystal
It is completely the same to penetrate style, it was demonstrated that last high-entropy alloy obtained is close-packed hexagonal structure.The solid matter that Fig. 3 is obtained by embodiment 1
The high resolution scanning images of transmissive electron microscope of the high-entropy alloy of hexagonal structure, lattice fringe spacing and angle with close-packed hexagonal knot
Structure coincide, and completely the same with the atomic arrangement mode of [- 2110] tape spool of close-packed hexagonal structure.
Table 1 is the yield strength test result of the high-entropy alloy of close-packed hexagonal structure made from each embodiment.
It can be seen that the sample that embodiment 1 ~ 4 is obtained embodies very high bend compared to bibliography from upper table result
Strength level is taken, there is mechanical property very outstanding.
Claims (5)
1. a kind of method for the high-entropy alloy preparing close-packed hexagonal structure, it is characterised in that include the following steps：
1）It using elemental metals and/or intermediate alloy as raw material, feeds intake, is melted in smelting furnace former according to the proportioning of each metallic element
Material；
2）Melt is molded into mold and obtains ingot casting；
3）The macro-components segregation that homogenizing annealing eliminates ingot casting is carried out to ingot casting, obtains cast alloy；The cast alloy tool
There is face-centred cubic structure；
4）Cast alloy is subjected to three-dimensional large plastometric set, i.e., carries out compressive deformation respectively in tri- directions x, y and z, obtains institute
State the high-entropy alloy of close-packed hexagonal structure;
The raw material includes five kinds of metallic elements of Fe, Mn, Ti, Co and Cr, and according to each metal element content be 30at.% Mn,
The proportioning of the Fe of the Ti and 45at.% of Co, 5at.% of Cr, 10at.% of 10at.% feed intake；Or
The raw material includes tetra- kinds of metallic elements of Fe, Mn, Co and Cr, and according to each metal element content be 35at.% Mn,
The proportioning of the Fe of the Co and 45at.% of Cr, 10at.% of 10at.% feed intake.
2. a kind of method for the high-entropy alloy preparing close-packed hexagonal structure according to claim 1, it is characterised in that：The original
Material is the elemental metals of Fe-Mn intermediate alloys, Ti, Co and Cr.
3. a kind of method for the high-entropy alloy preparing close-packed hexagonal structure according to claim 1, it is characterised in that：Described three
Dimension large plastometric set is to carry out the compressive deformation that deflection is 50% respectively in tri- directions x, y and z.
4. a kind of method for the high-entropy alloy preparing close-packed hexagonal structure according to claim 1, it is characterised in that：Described three
Dimension large plastometric set is to carry out the compressive deformation that deflection is 40%, 20% and 20% respectively in tri- directions x, y and z.
5. special according to a kind of high-entropy alloy of close-packed hexagonal structure made from any one of Claims 1-4 preparation method
Sign is：The yield strength of the high-entropy alloy is higher than 450 MPa.
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| CN108004492A (en) * | 2017-11-17 | 2018-05-08 | 北京理工大学 | A kind of efficient controlled rolling method of modifying of high-entropy alloy |
| CN108959846B (en) * | 2018-07-03 | 2021-09-14 | 南昌立德生物技术有限公司 | Affinity free energy decomposition algorithm for computer-aided pilot medicament optimization design |
| CN111085689B (en) * | 2018-10-23 | 2022-03-04 | 天津大学 | FeCoCrNi series high-entropy alloy selective laser melting in-situ additive manufacturing method and product |
| CN115323240B (en) * | 2022-08-29 | 2023-06-30 | 沈阳工业大学 | High-strength and high-toughness metastable-state biphase FeMnCrCo high-entropy alloy and preparation method thereof |
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| CN104946912A (en) * | 2015-07-14 | 2015-09-30 | 太原理工大学 | Rear earth high-entropy alloy of close-packed hexagonal structure |
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| CN104946912A (en) * | 2015-07-14 | 2015-09-30 | 太原理工大学 | Rear earth high-entropy alloy of close-packed hexagonal structure |
Non-Patent Citations (2)
| Title |
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| A hexagonal close-packed high-entropy alloy:The effect of entropy;Y.J. Zhao et al.;《Materials and Design》;20160201(第96期);第10-15页 * |
| High-entropy Alloys in Hexagonal Close-Packed structure;M.C.GAO et al.;《Metallurgical and materials transactions a》;20160731(第47A期);第3322-3332页 * |
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