CN111187962B - High thermal stability AlxFeCrV multi-principal-element solid solution alloy, preparation and application - Google Patents
High thermal stability AlxFeCrV multi-principal-element solid solution alloy, preparation and application Download PDFInfo
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Abstract
The invention relates to the technical field of metal materials and preparation, and provides Al with high thermal stabilityxFeCrV multi-principal element solid solution alloy, preparation and application. The atomic percent expression of the alloy is AlxFeCrV, where x is the molar ratio, 0<x is less than or equal to 1; the alloy is prepared by a vacuum melting method, which comprises the following steps: removing surface oxide skin of metal raw materials Fe, Cr, V and Al; accurately weighing the metal raw materials Fe, Cr, V and Al according to a set proportion, and preparing the target alloy in a water-cooled copper crucible by using a non-consumable vacuum arc melting furnace or a vacuum magnetic suspension melting furnace. The alloy has controllable lattice distortion, high phase structure stability, irradiation resistance, high strength, high hardness, high thermal stability and low diffusivity, has wide application prospect in the field of high-temperature materials, is an ideal alloy component of a tritium-resistant coating material for a fusion reactor, and has a certain application prospect in the field of fusion reactor materials.
Description
Technical Field
The invention relates to the technical field of metal materials and preparation, in particular to Al with high thermal stabilityxFeCrV multi-principal element solid solution alloy, preparation and application.
Background
The design of the traditional alloy generally takes one or two elements as main alloy components, and since 2004, professor Yeh in taiwan proposes the concept of multi-principal element high-entropy alloy, and the design concept of novel alloy characterized by high concentration of the multi-principal element is involved in both basic research and engineering application fields. In recent years, the research of multi-principal-element solid solution alloys is no longer limited to 5 or more principal elements, and ternary or quaternary multi-principal-element solid solution alloys or intermediate entropy alloys gradually enter the research category of researchers.
Research results show that the multi-principal-element solid solution alloy has the mechanical properties of high strength and high hardness due to the fact that the multi-principal-element solid solution alloy has larger lattice distortion. Meanwhile, recent studies [ t. -n.yang, c.lu, g.velisa, k.jin, p.xiu, y.zhang, h.bei, l.wang, scriptamaterial 158(2019)57-61 ] indicate that a high lattice distortion rate of the multi-host solid solution alloy significantly suppresses the movement of irradiation defects.
The development and design of the multi-principal-element solid solution alloy material with stable phase structure and controllable lattice distortion have important significance for researching the dependence relationship of lattice distortion on mechanical properties and irradiation resistance.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide Al with high thermal stabilityxFeCrV multi-principal element solid solution alloy, preparation and application.
The principle of the invention is illustrated as follows:
1. the inventor finds in the research that: non-equal atomic ratio alloys, such as Fe-10Cr-10V, Fe-10Cr-15V (wt.%) have a sigma phase inside the grains, while equal atomic ratio FeCrV alloys have a single phase BCC structure with no sigma phase generation; as shown in fig. 6.
2. The Al element is an alloy element of a stable phase of a body-centered cubic structure (BCC) in the multi-principal-element alloy and has the characteristic of stabilizing the BCC structure of the multi-principal-element alloy;
3. the numerical value of the mixing entropy of the atomic alloy such as FeCrV is larger than that of the non-equal atomic alloy, so that the effect of the mixing entropy can overcome the effect of the mixing enthalpy among elements, the formation of a sigma phase is inhibited to a certain extent, and the formation of a single-phase solid solution alloy phase can be promoted.
The invention adopts the following technical scheme:
al with high thermal stabilityxFeCrV multi-principal element solid solution alloy, wherein the atomic percent expression of the alloy is AlxFeCrV, where x is the molar ratio, 0<x≤1。
Further, x is any one of 0.1, 0.3, 0.5, 0.7 and 1.0.
Furthermore, the purity of the metal raw materials Fe, Cr, V and Al used for smelting the alloy is not lower than 99.9 wt.%.
The invention also provides the Al with high thermal stabilityxThe preparation method of the FeCrV multi-principal-element solid solution alloy comprises the following steps:
s1, removing surface scale from metallic raw materials Fe, Cr, V and Al used for smelting alloy;
s2, accurately weighing the metal raw materials Fe, Cr, V and Al according to a set proportion, and preparing the target alloy in a water-cooled copper crucible by using a non-consumable vacuum arc melting furnace or a vacuum magnetic suspension melting furnace.
Further, in step S2, an Al metal raw material and an Fe metal raw material are taken and melted into an intermediate alloy a # according to the mass ratio of 1:1, and simultaneously, the remaining other metal raw materials are melted into an intermediate alloy B #, and finally, the intermediate alloys a # and B # are melted into a target alloy.
Further, the preparation method of the intermediate alloy A # comprises the following steps: al metal raw materials and Fe metal raw materials are put at the bottom of a crucible according to the mass ratio of 1:1, and Fe is put on the Al; after the raw materials are placed, a mechanical pump and a molecular pump are started in sequence for vacuumizing, and when the vacuum degree reaches 5 multiplied by 10-3After Pa, the chamber is filled with argon to a certain pressure (e.g. 0.5 atm), and then evacuated again to 5X 10-3Pa, filling argon into the furnace chamber to a certain pressure (for example, 0.5 atmospheric pressure), striking an arc, and further adjusting the current in a stepped manner until the alloy is melted to prepare an intermediate alloy A # consisting of Al and Fe;
the preparation method of the intermediate alloy B # comprises the following steps: placing the rest other metal raw materials of Fe, Cr and V into a crucible cavity according to the sequence of the melting point; starting the mechanical pump and the molecular pump in sequence to carry out vacuum pumping, and when the vacuum degree reaches 5 multiplied by 10-3After Pa, the chamber is filled with argon to a certain pressure (e.g. 0.5 atm), and then evacuated again to 5X 10-3Pa, filling argon into the furnace chamber to a certain pressure (for example, 0.5 atmospheric pressure), striking an arc, further regulating the current in a stepped manner until the alloy is melted, and performing turnover smelting for 4 times or more to prepare an intermediate alloy B # consisting of the remaining three elements of Fe, Cr and V;
the preparation method of the target alloy comprises the following steps: placing the intermediate alloy A # at the bottom of the crucible, placing the intermediate alloy B # on the crucible, starting a mechanical pump and a molecular pump in sequence to carry out vacuum pumping, and when the vacuum degree reaches 5 multiplied by 10-3After Pa, the chamber was filled with argon to 0.5 atm, and then evacuated again to 5X 10-3Pa, filling argon into the furnace chamber to 0.5 atmosphere,and (3) arc striking, further adjusting current in a step mode until the alloy is melted, carrying out turnover smelting for 4 times or more, after the target alloy is fully and uniformly smelted, carrying out suction casting on the target alloy into a water-cooled copper mold by using vacuum suction casting equipment, and obtaining the low-activation multi-principal element solid solution alloy material.
Further, in step S1, the oxidized scale on the surface of the metal material is mechanically removed, and preferably, the metal material is placed in absolute ethanol for ultrasonic oscillation to remove the impurities remaining on the surface.
Further, in step S2, the target alloy is turned over and melted 4 times or more.
The invention also provides a high-thermal-stability coating, and the coating material adopts the high-thermal-stability AlxFeCrV multi-principal element solid solution alloy.
The coating with high thermal stability can be applied to tritium-resistant coating materials or thermal diffusion barrier layers for fusion reactors.
The invention has the beneficial effects that: the method realizes the regulation and control of the lattice distortion of the alloy system under the condition of not changing the single-phase BCC structure of the alloy system by changing the content of the Al element; lattice distortion is expressed in atomic radius difference and lattice mismatch strain; the atomic radius difference δ increases from 2.65% to 5.84% with the change in the content of Al element. The lattice mismatching strain of the AlFeCrV is increased by 1.1 percent compared with that of the FeCrV reference alloy; the alloy has high phase structure thermal stability, and in the field of engineering application, the alloy system has a gradually-changed Al component, and if the alloy is used as a coating material, the alloy system can relieve the problem of thermal matching between a substrate and the coating material, is an ideal alloy component of a thermal diffusion barrier layer and a tritium-resistant coating material for a fusion reactor, and has wide application prospects in the fields of fusion reactor materials and high-temperature materials.
Drawings
FIG. 1 illustrates Al of an embodiment of the present inventionxRelationship diagram of FeCrV multi-principal element alloy omega and delta.
FIG. 2 illustrates AlxXRD pattern of FeCrV system (x is molar ratio, x ═ 0.1, 0.3, 0.5, 0.7 and 1.0).
FIG. 3 illustrates AlxOf FeCrV systems (x is the molar ratio, x is 0.1, 0.5 and 1.0)BSE-SEM and EDX line scan maps; wherein (a), (b): x is 0.1; (c) and (d): x is 0.5; (e) and (f): x is 1.0.
FIG. 4 illustrates XRD patterns of AlFeCrV multi-principal element solid solution alloy before and after heat treatment at 1000 ℃ for 3 days, and shows that the alloy system has high phase structure thermal stability.
FIG. 5 illustrates respective engineering stress-strain curves of FeCrV and AlFeCrV multi-principal element solid solution alloys under the conditions of room temperature and 800 ℃, and shows that an Al alloy system has high phase structure thermal stability.
FIG. 6 illustrates a microstructure comparison of an equal atomic ratio FeCrV alloy and a non-equal atomic ratio FeCrV alloy, showing that the equal atomic ratio FeCrV alloy has a single phase structure.
Detailed Description
Specific embodiments of the present invention will be described in detail below with reference to the accompanying drawings. It should be noted that technical features or combinations of technical features described in the following embodiments should not be considered as being isolated, and they may be combined with each other to achieve better technical effects. In the drawings of the embodiments described below, the same reference numerals appearing in the respective drawings denote the same features or components, and may be applied to different embodiments.
Example 1
High thermal stability Al of the present examplexFeCrV multi-principal element solid solution alloy, wherein the atomic percent expression of the alloy is AlxFeCrV, where x is the molar ratio, 0<x is less than or equal to 1. Preferably, x is any one of 0.1, 0.3, 0.5, 0.7 and 1.0.
Example 2
This example is Al of high thermal stabilityxA preparation method of FeCrV multi-principal element solid solution alloy.
In the embodiment, Fe, Cr, V and Al are equal atomic ratios, and in order to reflect the influence of Al addition on the phase structure stability of the entropy alloy in FeCrV, the invention also designs and prepares the FeCrV entropy alloy as a reference alloy under the same preparation condition.
Preparing raw materials: the purity of the metal raw materials Fe, Cr, V and Al is more than or equal to 99.9 wt.%; removing surface oxide skin of metal raw materials Fe, Cr, V and Al by using grinding wheels, sand paper and other methods, accurately weighing according to a set molar ratio, washing the metal raw materials in alcohol by using ultrasonic oscillation, and naturally airing the metal raw materials for subsequent alloy smelting.
The target alloy has a mass of 50g, and the mass ratios of all the components in the AlFeCrV are respectively Fe15.0301g, Cr13.9937g, V13.7099g and Al7.2665g. The mass of each raw material was accurately weighed using an electronic balance with an accuracy of 0.0001g (within an error of. + -. 0.0002 g). Weighed Al and an equal mass of Fe, 7.2665g, were placed in the bottom of the crucible, and the Fe was placed on the Al in turn in the non-consumable vacuum arc furnace crucible. After the raw materials are placed, a mechanical pump and a molecular pump are started in sequence for vacuumizing, and when the vacuum degree reaches 5 multiplied by 10-3After Pa, the furnace chamber is filled with high-purity argon to half atmospheric pressure, and then the furnace chamber is vacuumized again to 5 multiplied by 10-3Pa, filling argon into the furnace chamber to half atmospheric pressure, striking an arc, and further regulating current in a stepped manner until the alloy is melted to prepare the FeAl intermediate alloy A # with equal mass ratio;
and mixing the rest of Fe7.7636g, Cr13.9937g and V13.7099g. Placing the materials in a non-consumable vacuum arc furnace crucible according to the melting point. After the raw materials are placed, a mechanical pump and a molecular pump are started in sequence for vacuumizing, and when the vacuum degree reaches 5 multiplied by 10-3After Pa, the furnace chamber is filled with high-purity argon to half atmospheric pressure, and then the furnace chamber is vacuumized again to 5 multiplied by 10-3Pa, filling argon into the furnace chamber to half atmospheric pressure, striking an arc, further regulating the current in a stepped manner until the alloy is melted, cooling and turning over after the gold is melted, and repeatedly melting for more than 4 times to prepare the intermediate alloy B # consisting of Fe, Cr and V.
Placing the intermediate alloy A # at the bottom of the crucible, placing the intermediate alloy B # on the crucible, starting a mechanical pump and a molecular pump in sequence to carry out vacuum pumping, and when the vacuum degree reaches 5 multiplied by 10-3After Pa, the chamber was filled with argon to half atmospheric pressure and then evacuated again to 5X 10-3Pa, filling argon into the furnace chamber to half atmospheric pressure, striking an arc, further regulating current in a step mode until the alloy is melted, turning over and smelting for more than 4 times, after the target alloy is fully and uniformly smelted, suction casting the target alloy into a water-cooling copper mold by using vacuum suction casting equipment to obtain a series of alloyThe low-activation multi-principal-element solid solution alloy material with the Al element content has the atomic radius difference delta and omega values of the alloy system existing in the forming area of the solid solution alloy, as shown in figure 1. Further, the results of XRD pattern (see FIG. 2) and BSE-SEM and EDX scanning pattern (see FIG. 3) show that Al isxThe FeCrV system alloy system keeps the characteristics of a single-phase BCC solid solution structure, and a structure with uniformly distributed elements.
It should be noted that the elements of the alloy of the present embodiment are equal in atomic ratio, which is only used for illustrating the present invention and is not used for limiting the present invention, and the scope of protection of the present invention is subject to the claims.
Example 3
This example is a high thermal stability coating, and the coating material used is the high thermal stability Al of example 1xFeCrV multi-principal element solid solution alloy, or Al with high thermal stability prepared by the preparation method in example 2xFeCrV multi-principal element solid solution alloy.
The Al prepared by the alloy design component and the smelting method of the inventionxThe FeCrV multi-principal element solid solution alloy has controllable lattice distortion, the atomic radius difference delta is increased from 2.65% to 5.84%, and the lattice mismatching strain AlFeCrV is increased by 3.25% compared with alpha-Fe, and meanwhile, the alloy also has high phase structure stability, and still keeps a single-phase BCC structure under the conditions of 1000 ℃ and 3 days of heat treatment, as shown in figure 4. Wherein the compressive yield strength of the AlFeCrV alloy at 800 ℃ is about 1GPa, and the fracture strain is more than 10 percent, as shown in FIG. 5. High lattice distortion, high entropy of mixing induced AlxThe FeCrV multi-principal element solid solution alloy has the characteristics of high strength, high hardness, high thermal stability and low diffusivity, has wide application prospect in the field of high-temperature materials, is also an ideal alloy component of a tritium-resistant coating material for a fusion reactor, and has certain application prospect in the field of fusion reactor materials.
While several embodiments of the present invention have been presented herein, it will be appreciated by those skilled in the art that changes may be made to the embodiments herein without departing from the spirit of the invention. The above examples are merely illustrative and should not be taken as limiting the scope of the invention.
Claims (7)
1. Al with high thermal stabilityxThe FeCrV multi-principal element solid solution alloy is characterized in that the atomic percent expression of the alloy is AlxFeCrV, wherein x is a molar ratio, and the value of x is any one of 0.1, 0.5 and 0.7;
the preparation method of the alloy comprises the following steps:
s1, removing surface scale from metallic raw materials Fe, Cr, V and Al used for smelting alloy;
s2, accurately weighing the metal raw materials Fe, Cr, V and Al according to a set proportion, and preparing a target alloy in a water-cooled copper crucible by using a non-consumable vacuum arc melting furnace or a vacuum magnetic suspension melting furnace;
in step S2, Al metal raw materials and Fe metal raw materials are taken to be smelted into intermediate alloy A # according to the mass ratio of 1:1, meanwhile, the rest other metal raw materials are smelted into intermediate alloy B #, and finally, the intermediate alloys A # and B # are smelted into target alloy;
the preparation method of the intermediate alloy A # comprises the following steps: al metal raw materials and Fe metal raw materials are put at the bottom of a crucible according to the mass ratio of 1:1, and Fe is put on the Al; after the raw materials are placed, a mechanical pump and a molecular pump are started in sequence for vacuumizing, and when the vacuum degree reaches not more than 5 multiplied by 10-3After Pa, filling argon into the furnace chamber to a certain pressure, and then vacuumizing again to not more than 5 multiplied by 10-3Pa, filling argon into the furnace chamber to a certain pressure, striking an arc, and further regulating the current in a stepped manner until the alloy is melted to prepare an intermediate alloy A # consisting of Al and Fe;
the preparation method of the intermediate alloy B # comprises the following steps: putting the rest of other metal raw materials Fe, Cr and V into a crucible cavity; starting the mechanical pump and the molecular pump in sequence to carry out vacuum pumping, and when the vacuum degree reaches not more than 5 multiplied by 10-3After Pa, filling argon into the furnace chamber to a certain pressure, and then vacuumizing again to not more than 5 multiplied by 10-3Pa, filling argon into the furnace chamber to a certain pressure, striking an arc, further regulating the current in a step manner until the alloy is melted, and performing turnover smelting for 4 times or more to prepare an intermediate alloy B # consisting of the residual Fe, Cr and V elements;
target alloyThe preparation method comprises the following steps: placing the intermediate alloy A # at the bottom of the crucible, placing the intermediate alloy B # on the crucible, starting a mechanical pump and a molecular pump in sequence to carry out vacuum pumping, and when the vacuum degree reaches not more than 5 multiplied by 10-3After Pa, filling argon into the furnace chamber to a certain pressure, and then vacuumizing again to not more than 5 multiplied by 10-3And Pa, filling argon into the furnace chamber to a certain pressure, striking an arc, further regulating the current in a step mode until the alloy is molten, turning and smelting for 4 times or more, and after the target alloy is fully and uniformly smelted, suction casting the target alloy into a water-cooling copper mold by using vacuum suction casting equipment to obtain the low-activation multi-principal-element solid solution alloy material.
2. Al of claim 1 having high thermal stabilityxFeCrV multi-principal element solid solution alloy is characterized in that the purity of metal raw materials Fe, Cr, V and Al used for smelting the alloy is not lower than 99.9 wt.%.
3. Al of high thermal stability according to any of claims 1-2xThe preparation method of the FeCrV multi-principal-element solid solution alloy is characterized by comprising the following steps of:
s1, removing surface scale from metallic raw materials Fe, Cr, V and Al used for smelting alloy;
s2, accurately weighing the metal raw materials Fe, Cr, V and Al according to a set proportion, and preparing a target alloy in a water-cooled copper crucible by using a non-consumable vacuum arc melting furnace or a vacuum magnetic suspension melting furnace;
in step S2, Al metal raw materials and Fe metal raw materials are taken to be smelted into intermediate alloy A # according to the mass ratio of 1:1, meanwhile, the rest other metal raw materials are smelted into intermediate alloy B #, and finally, the intermediate alloys A # and B # are smelted into target alloy;
the preparation method of the intermediate alloy A # comprises the following steps: al metal raw materials and Fe metal raw materials are put at the bottom of a crucible according to the mass ratio of 1:1, and Fe is put on the Al; after the raw materials are placed, a mechanical pump and a molecular pump are started in sequence for vacuumizing, and when the vacuum degree reaches not more than 5 multiplied by 10-3After Pa, filling argon into the furnace chamber to a certain pressure, and then vacuumizing again to not more than 5 multiplied by 10-3PaThen filling argon into the furnace chamber to a certain pressure, striking an arc, and further regulating the current in a stepped manner until the alloy is melted to prepare an intermediate alloy A # consisting of Al and Fe;
the preparation method of the intermediate alloy B # comprises the following steps: putting the rest of other metal raw materials Fe, Cr and V into a crucible cavity; starting the mechanical pump and the molecular pump in sequence to carry out vacuum pumping, and when the vacuum degree reaches not more than 5 multiplied by 10-3After Pa, filling argon into the furnace chamber to a certain pressure, and then vacuumizing again to not more than 5 multiplied by 10-3Pa, filling argon into the furnace chamber to a certain pressure, striking an arc, further regulating the current in a step manner until the alloy is melted, and performing turnover smelting for 4 times or more to prepare an intermediate alloy B # consisting of the residual Fe, Cr and V elements;
the preparation method of the target alloy comprises the following steps: placing the intermediate alloy A # at the bottom of the crucible, placing the intermediate alloy B # on the crucible, starting a mechanical pump and a molecular pump in sequence to carry out vacuum pumping, and when the vacuum degree reaches not more than 5 multiplied by 10-3After Pa, filling argon into the furnace chamber to a certain pressure, and then vacuumizing again to not more than 5 multiplied by 10-3And Pa, filling argon into the furnace chamber to a certain pressure, striking an arc, further regulating the current in a step mode until the alloy is molten, turning and smelting for 4 times or more, and after the target alloy is fully and uniformly smelted, suction casting the target alloy into a water-cooling copper mold by using vacuum suction casting equipment to obtain the low-activation multi-principal-element solid solution alloy material.
4. Al of claim 3 having high thermal stabilityxThe preparation method of the FeCrV multi-principal-element solid solution alloy is characterized in that in step S1, oxide skin on the surface of a metal raw material is mechanically removed, and then the metal raw material is placed in absolute ethyl alcohol for ultrasonic oscillation to remove impurities remained on the surface.
5. Al of claim 3 having high thermal stabilityxThe preparation method of the FeCrV multi-principal-element solid solution alloy is characterized in that in the step S2, the target alloy is turned over and smelted for 4 times or more.
6. A coating having high thermal stability, the coating material being as claimed in any one of claims 1 to 2High thermal stability Al as defined inxFeCrV multi-principal element solid solution alloy.
7. The coating with high thermal stability as claimed in claim 6, which is applied to tritium resistant coating materials or thermal diffusion barrier layers for fusion reactors.
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| US20020159914A1 (en) * | 2000-11-07 | 2002-10-31 | Jien-Wei Yeh | High-entropy multielement alloys |
| CN109338200A (en) * | 2018-11-07 | 2019-02-15 | 北京科技大学 | A kind of high temperature high-damping high-entropy alloy and preparation method thereof |
| CN110306094A (en) * | 2018-03-20 | 2019-10-08 | 斯沃奇集团研究和开发有限公司 | High-entropy alloy for external module |
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| US20020159914A1 (en) * | 2000-11-07 | 2002-10-31 | Jien-Wei Yeh | High-entropy multielement alloys |
| CN110306094A (en) * | 2018-03-20 | 2019-10-08 | 斯沃奇集团研究和开发有限公司 | High-entropy alloy for external module |
| CN109338200A (en) * | 2018-11-07 | 2019-02-15 | 北京科技大学 | A kind of high temperature high-damping high-entropy alloy and preparation method thereof |
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