WO2017209419A1 - Alliage à entropie élevée - Google Patents

Alliage à entropie élevée Download PDF

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Publication number
WO2017209419A1
WO2017209419A1 PCT/KR2017/005179 KR2017005179W WO2017209419A1 WO 2017209419 A1 WO2017209419 A1 WO 2017209419A1 KR 2017005179 W KR2017005179 W KR 2017005179W WO 2017209419 A1 WO2017209419 A1 WO 2017209419A1
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high entropy
entropy alloy
alloy
solid solution
content
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PCT/KR2017/005179
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English (en)
Korean (ko)
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나영상
임가람
이광석
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한국기계연구원
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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
    • C22C1/02—Making non-ferrous alloys by melting
    • C22C1/03—Making non-ferrous alloys by melting using master alloys
    • 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
    • C22C1/02—Making non-ferrous alloys by melting
    • 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
    • C22C1/02—Making non-ferrous alloys by melting
    • C22C1/026—Alloys based on aluminium
    • 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
    • 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
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B7/00—Heating by electric discharge
    • H05B7/18—Heating by arc discharge

Definitions

  • the present invention relates to a high entropy alloy.
  • the high entropy alloy which is recently attracting attention, is an alloy system in which several metal elements are composed of similar fractions, and all added elements serve as main elements, and high mixing is caused by similar atomic fractions in the alloy. Entropy is induced to form a solid solution of simple structure stable at high temperature instead of intermetallic or intermediate compound.
  • the solid solution has a complex internal stress due to the large radius difference between the members, which causes severe lattice deformation.
  • a plurality of alloying elements all act as solute atoms, they have very slow diffusion rates, thereby maintaining mechanical properties at high temperatures.
  • high-entropy alloys which are easily produced from intermetallic compounds in general multicomponent alloys
  • high-entropy alloys exhibit high strength through solid solution strengthening by forming a solid solution due to high mixed entropy. Indicates.
  • the present invention seeks to provide a novel high entropy alloy.
  • a high entropy alloy includes a body-centered cubic crystal structure, the body-centered cubic crystal structure is Al element; Ti element; And at least one element selected from Cr, Mo, V, Hf, Zr, and Nb as main elements, wherein the difference in content between the main elements is 10 at% or less, and the content of irregular solid solution of the high entropy alloy is 50 It provides a high entropy alloy that is at least%.
  • the high entropy alloy according to one embodiment of the present invention has superior hardness as compared to conventional alloys.
  • the article manufactured using the same may have excellent durability.
  • the high entropy alloy according to another embodiment of the present invention has excellent thermal stability, deformation due to heat can be minimized and excellent high temperature mechanical strength can be obtained.
  • Figure 1 shows the XRD analysis of the high entropy alloy according to Example 1, Example 4 and Example 7.
  • Figure 2 shows the XRD analysis of the high entropy alloy according to Example 2, Example 5 and Example 6.
  • Example 3 is an image of the microstructure analysis of the molten AlMoTiV quaternary high entropy alloy according to Example 6 and then through a transmission electron microscope (TEM).
  • FIG. 4 is an image obtained by melting a five-element high entropy alloy of AlCrMoTiV according to Example 7 and analyzing the microstructure through a transmission electron microscope (TEM).
  • TEM transmission electron microscope
  • One embodiment of the present invention is a high entropy alloy
  • the high entropy alloy includes a body centered cubic crystal structure
  • the body centered cubic crystal structure is an Al element; Ti element; And one or more elements selected from Cr, Mo, V, Hf, Zr, and Nb as main elements,
  • the content difference between the main elements is less than 10 at%
  • the content of the irregular solid solution of the high entropy alloy provides a high entropy alloy of 50% or more.
  • the high entropy alloy according to the present invention may be characterized by a mixed entropy of 1 R or more.
  • the mixed entropy when the high entropy alloy is a ternary alloy composed of three main elements, the mixed entropy may be 1 R or more.
  • the mixed entropy when the high entropy alloy is a quaternary alloy composed of four main elements, the mixed entropy may be 1.3 R or more.
  • the high entropy alloy is a five-membered alloy composed of five main elements, the mixed entropy may be 1.6 R or more.
  • traditional alloys have very low mixed entropy values, for example, the mixed entropy of traditional alloys Ti-6Al-4V is only 0.48 R.
  • the high entropy alloy according to the present invention has a content difference of less than or equal to 10 at%, specifically 5 at% It is characterized by the following. As such, the high-entropy alloys having the same content of the main elements have different physical properties from those of the conventional alloys.
  • the content of each main element may be 15 at% or more and 35 at% or less with respect to the high entropy alloy.
  • the high entropy alloy according to the present invention comprises a body centered cubic crystal structure.
  • the high entropy alloy may be made of a body-centered cubic crystal structure.
  • the main element may form the body-centered cubic crystal structure.
  • the high entropy alloy includes at least 50% of an irregular solid solution, and specifically, the content of the irregular solid solution in the high entropy alloy may be greater than 50%.
  • the body centered cubic crystal constituting the high entropy alloy may exist in the form of a regular solid solution and an irregular solid solution, and the irregular solid solution may form a single phase solid solution.
  • the higher the content of the irregular solid solution the better the properties as a high entropy alloy, according to the high entropy alloy according to the present invention, since the content of the irregular solid solution is 50% or more can be better implemented the properties of the high entropy alloy Can be.
  • the body-centered cubic crystal structure of the high entropy alloy according to the present invention can form a single-phase solid solution according to the combination of the main elements, even if it is not electrified employment between the main elements.
  • the content of the irregular solid solution of the high entropy alloy according to the present invention may be 70% or more or 80% or more.
  • the content of the irregular solid solution of the high entropy alloy may be 90% or more or 95% or more, and more specifically, the content of the irregular solid solution of the high entropy alloy may be 100%.
  • the content of the irregular solid solution is measured by X-ray diffraction (XRD) analysis.
  • XRD X-ray diffraction
  • the peaks of the regular solid solution and the irregular solid solution appear, and the sum of the peak values minus the peak value of the regular solid solution may be the content of the irregular solid solution.
  • the content of the irregular solid solution of the high entropy alloy may be 50% or more or 80% or more, and more specifically, the content of the irregular solid solution of the high entropy alloy is 90 Or at least 95% or at least 100%.
  • the content of the irregular solid solution may be measured through microstructure analysis through a transmission electron microscope (TEM).
  • TEM transmission electron microscope
  • the regular solid solution can be observed in a brighter shape than the irregular solid solution in the image through the transmission electron microscope.
  • the content of the regular solid solution When the content of the regular solid solution is very small in the image through the transmission electron microscope, it can be observed brightly in a shape such as a solid line or a scratch, and when the content of the regular solid solution is gradually increased, the bright solid is observed in a larger area such as a plate or a circle. Can be.
  • the regular solid solution when analyzing the microstructure of the surface of the high entropy alloy with a transmission electron microscope, the regular solid solution may be observed brightly in a shape such as a solid line or a scratch.
  • the content of the irregular solid solution can be measured through the ratio of the area excluding the area of the regular solid solution in the image sampled through the transmission electron microscope.
  • the content of the irregular solid solution of the high entropy alloy may be 50% or more or 80% or more, and more specifically, the content of the irregular solid solution of the high entropy alloy is 90% or more. Or 95% or more.
  • the high entropy alloy according to the present invention has a high content of stabilized irregular solid solution crystals, it may have an excellent high entropy effect.
  • the high entropy alloy according to the present invention has a high content of irregular solid solution crystals, lattice distortion may be maximized to have high hardness.
  • the high entropy alloy according to the present invention has a high content of irregular solid solution crystals, it is difficult to diffuse internal atoms, thereby providing excellent stability at high temperatures.
  • the body-centered cubic crystal structure is Al element; Ti element; And two or three elements selected from Cr, Mo, V, Hf, Zr, and Nb as main elements.
  • the body-centered cubic crystal structure essentially includes Al and Ti as main elements, and two or three elements selected from the group consisting of Cr, Mo, V, Hf, Zr, and Nb as main elements. It may include.
  • the high entropy alloy is Al, Ti and Cr; Al, Ti, and Mo; Or a ternary alloy having Al, Ti and V as main elements.
  • the high entropy alloy is Al, Ti, Cr and Mo; Al, Ti, Cr and V; Al, Ti, Mo and V; Al, Ti, Hf and Zr; Al, Ti, Hf and Nb; Al, Ti, Zr and Nb; Al, Ti, Mo and Nb; Al, Ti, Mo and V; Or a quaternary alloy having Al, Ti, Nb and V as main elements.
  • the high entropy alloy is Al, Ti, Cr, Mo and V; Al, Ti, Hf, Nb and Zr; Or a five-membered alloy having Al, Ti, Mo, Nb and V as main elements.
  • the three-, four- and five-membered high entropy alloys are based on the number of main elements forming the body-centered cubic crystal structure.
  • the high entropy alloy may include a non-metallic element as a sub-element.
  • the secondary element may be an impurity inevitably included in the manufacturing process of the high entropy alloy.
  • the sub-element may be artificially included in the high entropy alloy to improve the properties of the high entropy alloy.
  • the secondary element may exist as an invasive element in the lattice of the body centered cubic crystal structure of the high entropy alloy. Specifically, the secondary element does not exist as a substitutional element that affects the body centered cubic crystal structure of the high entropy alloy.
  • the nonmetallic element may include one or more selected from the group consisting of H, B, C, N, O, P, and S. Specifically, the nonmetallic element may include one or more selected from the group consisting of C, O, N, and B. Specifically, the nonmetallic elements included to improve the properties of the high entropy alloy may be C, O, N or B.
  • the minor element may be less than 5 at% based on the total high entropy alloy.
  • the sub-element may be 0.01 at% or more and less than 5 at% with respect to the entire high entropy alloy. More specifically, the sub-element may be 0.01 at% or more and 3 at% or less, or 0.01 at% or more and 1 at% or less with respect to the entire high entropy alloy.
  • the content of the secondary element When the content of the secondary element is in the above range, it may be included as impurities to the extent that does not affect the crystal structure of the high entropy alloy. In addition, when the content of the secondary element is in the above range, it is possible to improve the physical properties of the high entropy alloy without inhibiting the basic physical properties of the high entropy alloy.
  • the content difference between the main elements may be 5 at% or less. Specifically, the content difference between the main elements may be 2 at% or less. More specifically, the atomic content between one of the main elements and the other of the main elements may be 1: 1.
  • the high entropy alloy has almost no difference in atomic content of main elements, or has the same atomic content (at%) and forms a crystal structure, thereby showing stable physical properties and high hardness.
  • the high entropy alloy includes main elements of Al, Ti, Cr, and Mo; It is composed of Al, Ti, Cr, Mo and V, the single solid solution content of the high entropy alloy may be 100%.
  • the high entropy alloy is composed of main elements Al, Ti, and Cr; Or Al, Ti, and Mo; Al, Ti, Cr and V; It is composed of Al, Ti, Mo and V, the single-phase solid solution content of the high entropy alloy may be 95% or more.
  • Al of 99.99% purity, Cr of 99.99% purity, and Ti of 99.99% purity were prepared in the same molar number, and then melted and cooled by vacuum plasma arc melting to prepare a button-shaped master alloy 60 g.
  • the egg was divided into four, placed in an alumina crucible, melted through vacuum induction melting at a temperature of 1700 ° C., and poured into a mold to prepare a ternary high entropy alloy of AlCrTi.
  • Al of 99.99% purity, V of 99.99% purity, and Ti of 99.99% purity were prepared in the same mole number, and then melted and cooled by vacuum plasma arc melting to prepare a button-shaped master alloy 60 g.
  • the egg was divided into four, placed in an alumina crucible, melted through vacuum induction melting at a temperature of 1700 ° C., and poured into a mold to prepare a ternary high entropy alloy of AlVTi.
  • Al of 99.99% purity, Cr of 99.99% purity, Mo of 99.99% purity, and Ti of 99.99% purity were prepared in the same number of moles, and then melted and cooled by vacuum plasma arc melting. g was prepared. The egg was divided into four, placed in an alumina crucible, melted through vacuum induction melting at a temperature of 1700 ° C., and poured into a mold to prepare a quaternary high entropy alloy of AlCrMoTi.
  • Al of 99.99% purity, Cr of 99.99% purity, Ti of 99.99% purity and V of 99.99% purity were prepared in the same number of moles, and then melted and cooled by vacuum plasma arc melting. g was prepared.
  • the eggs were divided into four, placed in an alumina crucible, melted by vacuum induction melting at a temperature of 1700 ° C., and poured into a mold to prepare a quaternary high entropy alloy of AlCrTiV.
  • Al of 99.99% purity, Mo of 99.99% purity, Ti of 99.99% purity, and V of 99.99% purity were prepared in the same number of moles, and then melted and cooled by vacuum plasma arc melting. g was prepared.
  • the egg was divided into four, placed in an alumina crucible, melted through a vacuum induction melting method at a temperature of 1700 ° C., and poured into a mold to prepare a quaternary high entropy alloy of AlMoTiV.
  • Al of 99.99% purity, Cr of 99.99% purity, Mo of 99.99% purity, Ti of 99.99% purity and V of 99.99% purity were prepared in the same molar number, and then melted and cooled by vacuum plasma arc melting.
  • 60 g of a button-shaped master alloy was prepared. The egg was divided into four, placed in an alumina crucible, melted through vacuum induction melting at a temperature of 1700 ° C., and poured into a mold to prepare a 5-membered high entropy alloy of AlCrMoTiV.
  • Figure 1 shows the XRD analysis of the high entropy alloy according to Example 1, Example 4 and Example 7. According to FIG. 1, it can be confirmed that the ternary high entropy alloy of AlCrTi according to Example 1 has very little regular solid solution and most of them are irregular solid solution. In addition, the quaternary high entropy alloy of AlCrMoTi according to Example 4 and the ternary high entropy alloy of AlCrMoTiV according to Example 7 can be confirmed that only irregular solid solutions are detected without regular solid solutions.
  • the x-axis denotes an angle between X-rays incident on the specimen and X-rays reflected from the specimen during XRD analysis.
  • the peaks are observed at specific locations to determine the crystal structure of the specimen.
  • Figure 2 shows the XRD analysis of the high entropy alloy according to Example 2, Example 5 and Example 6.
  • the ternary high entropy alloy of AlMoTi according to Example 2 the quaternary high entropy alloy of AlCrTiV according to Example 5 and the quaternary alloy of AlMoTiV according to Example 6 detect very little regular solid solution, It can be seen that most of them are irregular solid solutions.
  • FIG. 3 is an image of the microstructure analysis of the molten AlMoTiV quaternary high entropy alloy according to Example 6 and then through a transmission electron microscope (TEM). According to FIG. 3, it can be seen that the ternary high entropy alloy of AlMoTiV has only a small portion of a regular solid solution represented by a bright solid line in the form of a scratch, indicated by an arrow, and most of it is made of an irregular solid solution.
  • FIG. 4 is an image obtained by melting a five-element high entropy alloy of AlCrMoTiV according to Example 7 and analyzing the microstructure through a transmission electron microscope (TEM). According to FIG. 4, it can be seen that the ternary high entropy alloy of AlCrMoTiV has only a small portion of the rule solid solution represented by a bright solid line in the form of a scratch, which is indicated by an arrow, and is mostly composed of an irregular solid solution.
  • TEM transmission electron microscope
  • Vickers hardness was measured. Specifically, the Vickers hardness was measured by indenting the high entropy alloy according to Examples 1 to 7 using a diamond indenter having a 0.5 kg load and measuring the diagonal of the recess. The results obtained by measuring the Vickers hardness of 5 parts for each high entropy alloy and obtaining the average value are shown in Table 1 below.
  • Figure 5 is a graph showing the Vickers hardness of the high entropy alloy according to Examples 1 to 7. Specifically, Figure 5 is a graph of the data for Table 1.

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Abstract

La présente invention concerne un nouvel alliage à entropie élevée et, plus précisément, un alliage à entropie élevée comprenant une structure cristalline cubique centrée, la structure cristalline cubique centrée comprenant, comme éléments principaux, Al, Ti, et un ou plusieurs éléments choisis parmi Cr, Mo, V, Hf, Zr et Nb, une différence de quantité parmi les éléments principaux étant inférieure ou égale à 10 % atomique et la quantité d'une solution solide irrégulière de l'alliage à entropie élevée étant de 50 % ou plus.
PCT/KR2017/005179 2016-06-01 2017-05-18 Alliage à entropie élevée WO2017209419A1 (fr)

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CN110548869B (zh) * 2018-06-04 2022-03-04 中南大学 一种含氮高熵合金复合材料及其制备方法
CN110257682A (zh) * 2019-07-05 2019-09-20 昆明理工大学 一种高熵合金材料及其涂层的制备方法
CN112725677A (zh) * 2019-10-15 2021-04-30 有研资源环境技术研究院(北京)有限公司 高强度高韧性TiZrHfNbSc难熔高熵合金及其制备方法
CN111088490A (zh) * 2020-01-11 2020-05-01 贵州大学 一种高硬度高耐磨性的高熵合金涂层及其制备方法
CN111088490B (zh) * 2020-01-11 2022-05-17 贵州大学 一种高硬度高耐磨性的高熵合金涂层及其制备方法
CN111235457A (zh) * 2020-03-24 2020-06-05 贵州航天新力铸锻有限责任公司 一种超高强轻质Al-Ti-V中熵合金
CN111206175A (zh) * 2020-03-24 2020-05-29 贵州航天新力铸锻有限责任公司 一种超高强轻质Al-Ti-V中熵合金高纯高均质的制备方法
CN111676408A (zh) * 2020-05-25 2020-09-18 北京理工大学 一种钨-含能高熵合金复合材料及其制备方法
CN112921267A (zh) * 2020-06-08 2021-06-08 自贡市量子金属制造有限公司 球阀圆头表面TiVZrCrAl高熵合金涂层及其制备方法
CN112030053A (zh) * 2020-09-02 2020-12-04 中国航发北京航空材料研究院 一种高温环境应用的轻质多主元合金
CN112680647A (zh) * 2020-11-30 2021-04-20 攀钢集团钒钛资源股份有限公司 钒钼铬铁铝合金的生产方法
CN113151725A (zh) * 2020-12-02 2021-07-23 西北工业大学 一种增强难熔高熵合金耐磨性的方法
CN113621958A (zh) * 2021-07-20 2021-11-09 燕山大学 一种铜表面激光熔覆高熵合金涂层的方法
CN113996780A (zh) * 2021-11-02 2022-02-01 南京国重新金属材料研究院有限公司 一种含超低原子比元素的高熵合金粉末的混合方法
CN113996780B (zh) * 2021-11-02 2023-08-22 南京国重新金属材料研究院有限公司 一种含超低原子比元素的高熵合金粉末的混合方法
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CN114672715A (zh) * 2022-03-04 2022-06-28 太原理工大学 高温高熵合金表面碳化物/金刚石颗粒涂层的制备方法
CN114672715B (zh) * 2022-03-04 2022-11-25 太原理工大学 高温高熵合金表面碳化物/金刚石颗粒涂层的制备方法

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