CN113549779A - Low-density plastic refractory multi-principal-element alloy and preparation method thereof - Google Patents
Low-density plastic refractory multi-principal-element alloy and preparation method thereof Download PDFInfo
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Abstract
The invention relates to low-density plastic refractory NbxTiyAlzV10(TaHfMoW)90‑(x+y+z)A multi-principal-element alloy and a preparation method thereof belong to the field of metal materials. The method prepares Ti/Al/V master alloy balls and Nb/Ta/Hf/Mo/W master alloy balls by smelting, and prepares master alloy ingots by mixed smelting; and melting the master alloy ingot by electric arc melting and heating, and casting the master alloy ingot into an alloy bar by a copper mold casting method to obtain the multi-principal-element alloy. According to the invention, the intrinsic plasticity and deformability of the alloy are obtained by adding the Nb element, and the solubility of the solid solution strengthening element is improved; the addition of Ti/Al elements obviously reduces the density of the alloy, improves the oxidation resistance of the alloy, and effectively improves the high-temperature strength of the alloy by the generated nano-scale B2 precipitated phase; the addition of Mo element makes the alloy highThe warm strength is obviously increased. The multi-principal-element alloy has excellent specific strength between 25 ℃ and 1000 ℃, short preparation process and low cost, and has high application value in the field of aerospace high-temperature structural materials.
Description
Technical Field
The invention relates to low-density plastic refractory NbxTiyAlzV10(TaHfMoW)90-(x+y+z)A multi-principal-element alloy and a preparation method thereof belong to the field of metal materials.
Background
The Body Centered Cubic (BCC) refractory multi-principal-element alloy has excellent strength and high-temperature stability, and has great potential application value in the field of aerospace high-temperature structural materials. The high density and brittleness inherent in conventional refractory alloys severely limit the applications of refractory alloys. Therefore, the characteristics of wide component design space and structural performance of the high-entropy alloy are utilized to develop the low-density plastic refractory multi-principal-element alloy, and the method has important significance for expanding the field of high-temperature structural materials. The low-density plastic refractory multi-principal-element alloy is developed through a component design and preparation process, and meanwhile, the nano-scale B2 phase is utilized for strengthening, so that the room temperature strength and the high temperature strength of the alloy are improved, and the alloy has important significance for the application of the alloy in the aerospace field.
The refractory multi-principal-element alloy developed by the prior art has a single-phase BCC solid solution or a B2 (matrix) + BCC (precipitated phase) dual-phase structure, and although the alloy has excellent high-temperature performance, the problems of density, plasticity and high-temperature strength matching cannot be solved due to the high density and ductile-brittle transition temperature, and the application requirements of structural materials cannot be met.
Disclosure of Invention
The main purpose of the invention is to provide a low-density plastic refractory NbxTiyAlzV10(TaHfMoW)90-(x+y+z)Multi-principal element alloy and preparation method thereofThe technical problem to be solved is to make the alloy material have lower density, excellent high-temperature strength and intrinsic room temperature plasticity, thereby being more practical.
The invention aims to solve the technical problem and adopts the following technical scheme to realize the preparation method of the low-density plastic refractory multi-principal-element alloy, which comprises the following steps:
(1) preparing Ti/Al/V master alloy balls: weighing according to a preset component ratio, placing a titanium raw material, an aluminum raw material and a vanadium raw material into a crucible, and preparing a Ti/Al/V intermediate alloy ball with a smooth surface by adopting electric arc melting;
(2) preparing an Nb/Ta/Hf/Mo/W master alloy ball: weighing niobium raw materials, tantalum raw materials, hafnium raw materials, molybdenum raw materials and tungsten raw materials according to preset component proportions, placing the niobium raw materials, the tantalum raw materials, the hafnium raw materials, the molybdenum raw materials and the tungsten raw materials in a crucible, and preparing Nb/Ta/Hf/Mo/W intermediate alloy balls by adopting electric arc melting;
(3) preparing a master alloy ingot: mixing and smelting the Ti/Al/V master alloy ball obtained in the step (1) and the Nb/Ta/Hf/Mo/W master alloy ball obtained in the step (2), and repeatedly carrying out arc smelting until the components are uniform to obtain a master alloy ingot;
(4) preparing an alloy bar: melting the master alloy ingot obtained in the step (4) by electric arc melting and heating, and casting the master alloy ingot into low-density plastic refractory Nb by a copper mold casting methodxTiyAlzV10(TaHfMoW)90-(x+y+z)A multi-principal element alloy bar;
among them, low density plastic refractory NbxTiyAlzV10(TaHfMoW)90-(x+y+z)The multi-principal element alloy is an as-cast dendritic structure, and the atomic ratio of Nb, Ti, Al, V and (TaHfMoW) is x: y: z: 10: 90- (x + y + z), wherein: x is more than or equal to 35 and less than or equal to 45, y is more than or equal to 25 and less than or equal to 30, z is more than or equal to 10 and less than or equal to 15, and the Ta/Hf/Mo/W is not equal in proportion.
The preparation method of the low-density plastic refractory multi-principal-element alloy adopts vacuum arc melting in the steps (1) to (3), and a vacuum chamber is pre-pumped to the vacuum degree of 10-4～10-3Pa, filling high-purity argon into the vacuum gauge to show that the argon is 2 multiplied by 104～4×104Pa, arc melting is carried out, and the melting current is 300-600A.
The low densityThe preparation method of the plasticity refractory multi-principal-element alloy comprises the following steps of (4) adopting vacuum arc melting, and pre-pumping a vacuum chamber to a vacuum degree of 10-4～10-3Pa, filling high-purity argon into the vacuum gauge to show that the vacuum gauge is 3 multiplied by 104～5×104And Pa, carrying out arc melting on the master alloy ingot, wherein the melting current is 500-600A.
The preparation method of the low-density plastic refractory multi-principal-element alloy comprises the following steps of (4): and heating and melting the master alloy ingot to the temperature of the alloy melt, and pouring the alloy melt into a copper mold with a corresponding size to obtain the alloy bar.
According to the preparation method of the low-density plastic refractory multi-principal-element alloy, the temperature of an alloy melt is 200-400 ℃ above the melting point of the alloy.
Low-density plastic refractory NbxTiyAlzV10(TaHfMoW)90-(x+y+z)The multi-principal element alloy is an as-cast dendritic structure, and the atomic ratio of Nb, Ti, Al, V and (TaHfMoW) is x: y: z: 10: 90- (x + y + z), wherein: x is more than or equal to 35 and less than or equal to 45, y is more than or equal to 25 and less than or equal to 30, z is more than or equal to 10 and less than or equal to 15, and the Ta/Hf/Mo/W is not equal in proportion.
The low-density plastic refractory NbxTiyAlzV10(TaHfMoW)90-(x+y+z)The density of the multi-principal element alloy is not less than 7.2 and not more than 7.9g/cm3(ii) a The room temperature compressive yield strength is 950-1100 MPa, and the corresponding room temperature maximum compressive plasticity>50 percent; the compressive yield strength is 560-680 MPa at 800 ℃, and the maximum compressive plasticity at room temperature is correspondingly>50 percent; the compressive yield strength is 430-580 MPa at 900 ℃, and the maximum compressive plasticity at room temperature is correspondingly>50 percent; the compression yield strength is 230-400 MPa at 1000 ℃, and the maximum compression plasticity at the corresponding room temperature>50％。
The low-density plastic refractory NbxTiyAlzV10(TaHfMoW)90-(x+y+z)A multi-element alloy (TaHfMoW) comprising at least: ta and Hf as well as Mo and W as alloying elements.
The design idea of the invention is as follows:
the method of the invention prepares the product by smeltingTiy/Alz/V10Master alloy ball and method of making Nbx/(TaHfMoW)90-(x+y+z)An intermediate alloy ball; mixing TiyAlzV10Master alloy ball and Nbx/(TaHfMoW)90-(x+y+z)Mixing and smelting the intermediate alloy balls to prepare master alloy ingots; heating and melting the master alloy ingot by electric arc melting, casting into alloy bar by a copper mold casting method, and obtaining the low-density plastic refractory NbxTiyAlzV10(TaHfMoW)90-(x+y+z)A multi-principal element alloy. According to the invention, the intrinsic plasticity and deformability of the alloy are obtained by adding the Nb element, and the solubility of the solid solution strengthening element is improved; the addition of Ti/Al elements obviously reduces the density of the alloy, improves the oxidation resistance of the alloy, and effectively improves the high-temperature strength of the alloy by the generated nanoscale B2 precipitated phase; the addition of Mo element obviously increases the high-temperature strength of the alloy.
In addition, the addition of V element further reduces the alloy density and plays a role in solid solution strengthening; the addition of Ta element is used for improving the plasticity and the solid solution strengthening effect; the addition of Hf element has the functions of improving plasticity and strengthening a certain grain boundary; the addition of W element has the function of high-temperature solid solution strengthening; the elements have high melting points at the same time, and can obviously improve the integral melting point of the alloy, thereby improving the high-temperature softening resistance of the alloy.
By means of the technical scheme, the low-density plastic refractory Nb disclosed by the inventionxTiyAlzV10(TaHfMoW)90-(x+y+z)The multi-principal-element alloy and the preparation method thereof at least have the following advantages:
1. according to the invention, through the addition of Ti/Al elements, a rapid solidification process is utilized to modulate the precipitation of a nano-scale B2 phase, meanwhile, the Ti/Al/V elements are utilized to reduce the material density, the Al element improves the alloy oxidation resistance, the room temperature and high temperature strength of the alloy is improved through second phase strengthening, the alloy plasticity is maintained, and the alloy application value is improved.
2. The multi-principal-element alloy has excellent specific strength between 25 ℃ and 1000 ℃, has low alloying cost, short preparation flow and simple process, and has higher application value in the field of aerospace high-temperature structural materials.
The above description is only an overview of the technical solution of the present invention, and in order to clearly understand the technical means of the present invention and to implement the technical solution according to the content of the description, the following detailed description is made with the preferred embodiment of the present invention and the accompanying drawings (NbTiAl-1 represents Nb)40Ti25Al15V10Ta5Hf3W2(ii) a NbTiAl-2 stands for Nb40Ti25Al10V10Ta5Hf5Mo5)。
Drawings
FIG. 1 is an as-cast XRD pattern of NbTiAl-1 and NbTiAl-2 alloys.
FIG. 2 is an as-cast SEM image of an alloy of NbTiAl-1 and NbTiAl-2.
FIG. 3 is a TEM dark field image of B2 precipitated phase in the as-cast state of NbTiAl-1 alloy.
FIG. 4 is a graph of room temperature compressive true stress versus true strain for NbTiAl-1 and NbTiAl-2 alloys.
FIG. 5 is a graph of compressive true stress versus true strain at 800 ℃ for an alloy of NbTiAl-1 and NbTiAl-2.
FIG. 6 is a graph of compressive true stress versus true strain at 900 deg.C for an alloy of NbTiAl-1 and NbTiAl-2.
FIG. 7 is a 1000 ℃ compressive true stress-true strain plot for an alloy of NbTiAl-1 and NbTiAl-2.
FIG. 8 is a graph showing the statistical comparison of compressive yield strength of NbTiAl-1 and NbTiAl-2 alloys at 800 deg.C, 900 deg.C, and 1000 deg.C.
Detailed Description
To further illustrate the technical means and effects of the present invention adopted to achieve the predetermined objects, the following description is made in conjunction with the accompanying drawings and preferred embodiments of the low-density plastic refractory Nb according to the present inventionxTiyAlzV10(TaHfMoW)90-(x+y+z)The detailed description of the embodiments, structures, characteristics and effects of the multi-principal-element alloy and the preparation method thereof are as follows. In the following description, the various "one embodiment" or "an embodiment" refers toNeed not be the same embodiment. Furthermore, the particular features, structures, or characteristics may be combined in any suitable manner in one or more embodiments.
The invention provides a low-density plastic refractory NbxTiyAlzV10(TaHfMoW)90-(x+y+z)The preparation method of the multi-principal-element alloy comprises the following steps:
(1) preparing Ti/Al/V master alloy balls: weighing according to a preset component ratio, placing a titanium raw material, an aluminum raw material and a vanadium raw material into a crucible, adopting vacuum arc melting, and pre-pumping a vacuum chamber to 10 DEG C-4～10-3Pa, then filling high-purity argon (volume purity 99.999%) until the vacuum table shows 2X 104～4×104Pa. The alloy smelting current is 300-400A, each smelting time lasts for 2-5 minutes, the alloy is turned and smelted again after each smelting, the smelting is repeated for at least 3 times until the alloy components are uniform, and Ti/Al/V intermediate alloy balls with smooth surfaces are obtained, wherein the granularity of the Ti/Al/V intermediate alloy balls is 2-4 cm;
(2) preparing an Nb/Ta/Hf/Mo/W master alloy ball: weighing according to a preset component ratio, placing a niobium raw material, a tantalum raw material, a hafnium raw material, a molybdenum raw material and a tungsten raw material into a crucible, adopting vacuum arc melting, and pre-pumping a vacuum chamber to 10 DEG C-4～10-3Pa, then filling high-purity argon (volume purity 99.999%) until the vacuum table shows 2X 104～4×104Pa. The alloy smelting current is 400-600A, each smelting time lasts for 4-6 minutes, the alloy is turned over and smelted again after each smelting, and the smelting is repeated at least 5 times until the alloy components are uniform, so that Nb/Ta/Hf/Mo/W intermediate alloy balls are obtained, and the granularity of the Nb/Ta/Hf/Mo/W intermediate alloy balls is 3-5 cm;
(3) preparing a master alloy ingot: mixing and smelting the Ti/Al/V intermediate alloy ball and the Nb/Ta/Hf/Mo/W intermediate alloy ball, adopting vacuum arc smelting, pre-pumping a vacuum chamber to 10 DEG-4～10-3Pa, then filling high-purity argon (volume purity 99.999%) until the vacuum table shows 2X 104～4×104Pa. The alloy smelting current is 400-600A, each smelting time is 4-6 minutes, the alloy is turned over after each smelting and is smelted again, and the smelting is repeated until the components are uniform, so that a master alloy ingot is obtained;
(4) preparing an alloy bar: putting the master alloy ingot into a water-cooled copper crucible, and pumping the vacuum chamber to 10 DEG-4～10-3Pa, then filling high-purity argon (the volume purity is 99.999 percent) until the vacuum table shows that the argon is 3 multiplied by 104～5×104Pa. Heating and melting a master alloy ingot by arc melting, wherein the alloy melting current is 500-600A, heating the master alloy ingot to an alloy molten state, the alloy melt temperature is 200-400 ℃ above the alloy melting point, and then quickly pouring the alloy melt into a copper mold with a corresponding size by using a copper mold casting method to obtain an alloy bar with the size of phi 8mm multiplied by 40 mm;
among them, low density plastic refractory NbxTiyAlzV10(TaHfMoW)90-(x+y+z)The multi-principal-element alloy is an as-cast dendritic structure, and the atomic ratio of Nb, Ti, Al and V is x: y: z: 10, wherein x is more than or equal to 35 and less than or equal to 45, y is more than or equal to 25 and less than or equal to 30, z is more than or equal to 10 and less than or equal to 15, (TaHfMoW) is 90- (x + y + z), and Ta/Hf/Mo/W is not in equal proportion. The density of the multi-principal-element alloy is 7.2-7.9 g/cm3(ii) a The room temperature compressive yield strength is 950-1100 MPa, and the corresponding room temperature maximum compressive plasticity>50 percent; the compressive yield strength is 560-680 MPa at 800 ℃, and the maximum compressive plasticity at room temperature is correspondingly>50 percent; the compressive yield strength is 430-580 MPa at 900 ℃, and the maximum compressive plasticity at room temperature is correspondingly>50 percent; the compression yield strength is 230-400 MPa at 1000 ℃, and the maximum compression plasticity at the corresponding room temperature>50％。
The present invention will be explained in further detail below by way of examples and figures.
Example 1
This example provides a method for preparing NbTiAl-1 multi-principal element alloy, weighing 48.68g of raw materials Nb, 15.68g of Ti, 5.30g of Al, 6.68g of V, 11.85g of Ta, 7.01g of Hf and 4.83g of W according to a predetermined composition ratio, wherein all the raw materials have industrial purity; the method comprises the following specific steps:
(1) preparing Ti/Al/V master alloy balls: 15.68g of titanium, 5.30g of aluminum and 6.68g of vanadium are placed in a crucible, vacuum arc melting is adopted, and a vacuum chamber is pre-pumped to 10 DEG-4Pa, then filling high-purity argon (volume purity 99.999%) until the vacuum table shows 4X 104Pa. Alloy meltingThe current is 350A, the alloy is smelted for 3 minutes each time, the alloy is turned over and smelted again after each smelting, the smelting is repeated for 5 times until the alloy components are uniform, and Ti/Al/V intermediate alloy balls with smooth surfaces are obtained after the alloy balls are cooled in a crucible, wherein the granularity of the Ti/Al/V intermediate alloy balls is 2-4 cm;
(2) preparing an Nb/Ta/Hf/W master alloy ball: 48.68g niobium, 11.85g tantalum, 7.01g hafnium and 4.83g tungsten wire are placed in a crucible and melted by vacuum arc, and the vacuum chamber is pre-pumped to 10-4Pa, then filling high-purity argon (volume purity 99.999%) until the vacuum table shows 4X 104Pa. The alloy smelting current is 550A, each smelting is carried out for 5 minutes, the alloy is turned over and smelted again after each smelting, the smelting is repeated for 5 times until the alloy components are uniform, and Nb/Ta/Hf/W intermediate alloy balls with the granularity of 3-5 cm are obtained after cooling in a crucible;
(3) preparing a master alloy ingot: and mixing and smelting the Nb/Ta/Hf/W master alloy ball and the Ti/Al/V master alloy ball. Vacuum arc melting is adopted, and a vacuum chamber is pre-pumped to 10-4Pa, then filling high-purity argon (volume purity 99.999%) until the vacuum table shows 4X 104Pa. Then arc melting is carried out, the alloy melting current is 550A, the alloy is melted for 5 minutes each time, the alloy is turned over and melted again after each melting, the melting is carried out repeatedly until the components are uniform, and a master alloy ingot is obtained after the alloy is cooled in a crucible;
(4) preparing an alloy bar: placing the master alloy ingot in a water-cooled copper crucible, pumping the vacuum chamber to 3 × 10-4Pa, then filling high-purity argon (the volume purity is 99.999 percent) until the vacuum table shows that the argon is 4 multiplied by 104Pa. And (2) melting the master alloy ingot by electric arc melting and heating, wherein the alloy melting current is 600A, heating for 2 minutes until the alloy is molten, the temperature of the alloy melt is 200 ℃ above the alloy melting point, and then quickly pouring the alloy melt into a copper mold with a corresponding size to obtain an alloy bar with the size of phi 8mm multiplied by 40 mm.
The alloy bar of the embodiment is NbTiAl-1 multi-principal-element alloy and is prepared by the method. Low-density plastic refractory NbTiAl-1 (Nb)40Ti25Al15V10Ta5Hf3W2) In the multi-principal-element alloy, the addition amount of each element is calculated by atomic ratio,40 percent of Nb, 25 percent of Ti, 15 percent of Al, 10 percent of V, 5 percent of Ta, 3 percent of Hf and 2 percent of W. Nb40Ti25Al15V10Ta5Hf3W2Has a density of 7.29g/cm3(ii) a The room temperature compressive yield strength is 1024MPa, and the corresponding room temperature maximum compressive plasticity>50% (60% in this example); the compressive yield strength is 611MPa at 800 ℃, and the maximum compression plasticity at room temperature is correspondingly>50% (51% in this example); compressive yield strength of 437MPa at 900 ℃ and corresponding maximum compression plasticity at room temperature>50% (51% in this example); the compressive yield strength is 237MPa at 1000 ℃, and the maximum compression plasticity at room temperature is correspondingly>50% (51% in this example).
Example 2
The embodiment provides a preparation method of NbTiAl-2 multi-principal-element alloy, which comprises the steps of weighing 46.63g of raw materials Nb, 15.02g of Ti, 3.39g of Al, 6.39g of V, 11.35g of Ta, 11.20g of Hf and 6.02g of Mo according to preset component proportions, wherein all the raw materials have industrial-grade purity; the method comprises the following specific steps:
(1) preparing Ti/Al/V master alloy balls: 15.02g of titanium, 3.39g of aluminum and 6.39g of vanadium were placed in a crucible and melted by vacuum arc melting, the vacuum chamber being pre-evacuated to 10 deg.f-3Pa, then filling high-purity argon (volume purity 99.999%) until the vacuum table shows 4X 104Pa. The alloy smelting current is 350A, each smelting is carried out for 3 minutes, the alloy is turned over and smelted again after each smelting, the smelting is repeated for 6 times until the alloy components are uniform, and Ti/Al/V intermediate alloy balls with smooth surfaces are obtained after the alloy is cooled in a crucible, wherein the granularity of the Ti/Al/V intermediate alloy balls is 2-4 cm;
(2) preparing an Nb/Ta/Hf/Mo master alloy ball: 46.63g niobium, 11.35g tantalum, 11.20g hafnium and 6.02g molybdenum are placed in a crucible and melted by vacuum arc melting, the vacuum chamber is pre-evacuated to 10 deg.C-4Pa, then filling high-purity argon (volume purity 99.999%) until the vacuum table shows 4X 104Pa. The alloy smelting current is 550A, each smelting is carried out for 5 minutes, the alloy is turned over and smelted again after each smelting, the smelting is repeated for 6 times until the alloy components are uniform, and Nb/Ta/Hf/Mo intermediate alloy balls with the granularity of 3-5 cm are obtained after cooling in a crucible;
(3) preparation ofMother alloy ingot: and mixing and smelting the Nb/Ta/Hf/Mo intermediate alloy ball and the Ti/Al/V intermediate alloy ball. Vacuum arc melting is adopted, and a vacuum chamber is pre-pumped to 10-4Pa, then filling high-purity argon (volume purity 99.999%) until the vacuum table shows 4X 104Pa. Then arc melting is carried out, the alloy melting current is 550A, the alloy is melted for 5 minutes each time, the alloy is turned over and melted again after each melting, the melting is carried out repeatedly until the components are uniform, and a master alloy ingot is obtained after the alloy is cooled in a crucible;
(4) preparing an alloy bar: placing the master alloy ingot in a water-cooled copper crucible, pumping the vacuum chamber to 3 × 10-4Pa, then filling high-purity argon (the volume purity is 99.999 percent) until the vacuum table shows that the argon is 4 multiplied by 104Pa. Heating and melting a master alloy ingot by arc melting, wherein the alloy melting current is 600A, heating for 2 minutes until the alloy is molten, the temperature of the alloy melt is 200 ℃ above the alloy melting point, and then quickly pouring the alloy melt into a copper mold with corresponding size to obtain an alloy bar with the size of phi 8mm multiplied by 40 mm;
the alloy bar of the embodiment is NbTiAl-2 multi-principal-element alloy and is prepared by the method. Low-density plastic refractory NbTiAl-2 (Nb)40Ti25Al10V10Ta5Hf5Mo5) In the multi-principal-element alloy, the addition amounts of all the elements are 40 percent of Nb, 25 percent of Ti, 10 percent of Al, 10 percent of V, 5 percent of Ta, 5 percent of Hf and 5 percent of Mo in terms of atomic ratio. Nb40Ti25Al10V10Ta5Hf5Mo5Has a density of 7.57g/cm3(ii) a The room-temperature compressive yield strength is 995MPa, and the corresponding room-temperature maximum compressive plasticity>50% (60% in this example); the compressive yield strength is 583MPa at 800 ℃, and the maximum compression plasticity at room temperature is correspondingly>50% (51% in this example); the compressive yield strength at 900 ℃ is 504MPa, and the maximum compression plasticity at room temperature is correspondingly>50% (51% in this example); the compressive yield strength is 360MPa at 1000 ℃, and the maximum compressive plasticity at room temperature is correspondingly>50% (51% in this example).
As shown in FIG. 1, the phase compositions of the as-cast samples of examples 1-2, NbTiAl-1 alloy and NbTiAl-2 alloy, resulted in a single phase-centered cubic structure on XRD.
As shown in FIG. 2, both the NbTiAl-1 alloy and the NbTiAl-2 alloy have cast dendrite structures and similar grain sizes. And (3) performing centerless grinding on the cast sample with the size of phi 8mm multiplied by 40mm by adopting a centerless grinding method to obtain a rod-shaped sample with the size of phi 6mm multiplied by 40mm, and then cutting a cylinder with the length of 8mm from the cast bar by adopting a CNC scribing method to obtain a cylinder compression sample with the standard size of phi 6mm multiplied by 8 mm.
The room-temperature compression test was carried out using an Instron model 5582 Universal Material testing machine, and the compression rates of the NbTiAl-1 alloy and the NbTiAl-2 alloy were the same and were 1X 10-3s-1The room temperature compression curve of the alloy is shown in figure 4, the yield strength (sigma 0.2) of the NbTiAl-1 alloy material is 1024MPa, and the NbTiAl-1 alloy material shows certain work hardening capacity and total true strain deformation after yielding>60 percent. The yield strength (sigma 0.2) of the NbTiAl-2 alloy material is 995MPa, and the NbTiAl-2 alloy material also shows certain work hardening capacity and total true strain deformation after yielding>60％。
As shown in FIG. 5, the compressive yield strengths of the NbTiAl-1 alloy and the NbTiAl-2 alloy at 800 ℃ are 611MPa and 583MPa, respectively, and both have certain work hardening capacity in the initial stage of deformation, but the deformation is changed from work hardening to work softening with the increase of the deformation amount, and the total true strain deformation amount is more than 60%.
As shown in FIG. 6, the compressive yield strengths of NbTiAl-1 alloy and NbTiAl-2 alloy at 900 deg.C were 437MPa and 504MPa, respectively, both of which exhibited a continuous work softening phenomenon after yielding.
As shown in FIG. 7, the compressive yield strengths of the NbTiAl-1 alloy and the NbTiAl-2 alloy at 1000 ℃ are 237MPa and 360MPa respectively, and the NbTiAl-1 alloy and the NbTiAl-2 alloy also show a continuous processing softening phenomenon after yielding, and the softening phenomenon is more obvious than that at 900 ℃. The NbTiAl-1 alloy and the NbTiAl-2 alloy both keep good compression plasticity at the temperature, and the true strain deformation is more than 60 percent.
As shown in FIG. 8, the compressive yield strength of the NbTiAl-1 alloy and the NbTiAl-2 alloy at various temperatures is summarized, and although the yield strength of the NbTiAl-2 alloy at room temperature and 800 ℃ is lower than that of the NbTiAl-1 alloy, the high-temperature softening resistance of the NbTiAl-2 alloy is better than that of the NbTiAl-1 alloy along with the temperature rise, and the high-temperature solid solution strengthening effect of the Mo element is embodied.
As shown in FIG. 3, the TEM dark field image of the NbTiAl-1 alloy shows that the NbTiAl-1 alloy has a large amount of nanoscale B2 precipitated phase. Thus, the excellent room temperature and high temperature yield strength of the alloy is due in part to the nanoscale B2 precipitate phase driven by the Al/Ti element, which acts as a significant second phase strengthening. And the nanometer B2 precipitated phase driven by the Al/Ti element has high temperature stability and high temperature strength, so that the high temperature strength of the alloy can be effectively improved. However, since the NbTiAl-1 alloy and the NbTiAl-2 alloy contain a small amount of Al element, most of them are dissolved in the matrix and only a trace amount of B2 precipitated phase is formed, and thus a diffraction peak of B2 phase cannot be recognized by XRD.
The embodiment result shows that Ti/Al/V elements are introduced into the Nb matrix, so that the density of the refractory alloy is remarkably reduced while the intrinsic plasticity of the alloy is maintained, and the oxidation resistance of the refractory alloy is effectively improved by adding the Al elements. Simultaneously, Nb with excellent mechanical property is prepared by a certain process meansxTiyAlzV10(TaHfMoW)90-(x+y+z)A multi-principal element alloy. According to the invention, by alloying of Al element and utilizing Al/Ti drive of incomplete amplitude modulation decomposition induced by a rapid solidification process, the alloy precipitation behavior is modulated, so that the strength of the alloy is obviously improved by the precipitation strengthening effect of the nanoscale second phase, and meanwhile, the intrinsic plasticity of the alloy is maintained. And the high-temperature strength of the alloy is improved, the density is reduced, and the refractory multi-principal-element alloy with high specific strength is developed.
In addition, the low-density plastic refractory Nb of the inventionxTiyAlzV10(TaHfMoW)90-(x+y+z)The density distribution of the multi-principal-element alloy is that rho is more than or equal to 7.2 and less than or equal to 7.9g/cm3Far lower than the traditional Ni and Co base high temperature alloy; the room temperature compressive yield strength is 950-1100 MPa, and the corresponding room temperature maximum compressive plasticity>50 percent; the compressive yield strength is 560-680 MPa at 800 ℃, and the maximum compressive plasticity at room temperature is correspondingly>50 percent; the compressive yield strength is 430-580 MPa at 900 ℃, and the maximum compressive plasticity at room temperature is correspondingly>50 percent; compressive yield at 1000 deg.CThe strength is 230-400 MPa, and the maximum compression plasticity at the corresponding room temperature>50 percent. The series of alloys have excellent specific strength characteristics in a wide temperature range, and realize the optimized matching of low density, intrinsic plasticity and high temperature strength of refractory alloys.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, and any simple modification, equivalent change and modification made to the above embodiment according to the technical spirit of the present invention are still within the scope of the technical solution of the present invention.
Claims (8)
1. The preparation method of the low-density plastic refractory multi-principal-element alloy is characterized by comprising the following steps of:
(1) preparing Ti/Al/V master alloy balls: weighing according to a preset component ratio, placing a titanium raw material, an aluminum raw material and a vanadium raw material into a crucible, and preparing a Ti/Al/V intermediate alloy ball with a smooth surface by adopting electric arc melting;
(2) preparing an Nb/Ta/Hf/Mo/W master alloy ball: weighing niobium raw materials, tantalum raw materials, hafnium raw materials, molybdenum raw materials and tungsten raw materials according to preset component proportions, placing the niobium raw materials, the tantalum raw materials, the hafnium raw materials, the molybdenum raw materials and the tungsten raw materials in a crucible, and preparing Nb/Ta/Hf/Mo/W intermediate alloy balls by adopting electric arc melting;
(3) preparing a master alloy ingot: mixing and smelting the Ti/Al/V master alloy ball obtained in the step (1) and the Nb/Ta/Hf/Mo/W master alloy ball obtained in the step (2), and repeatedly carrying out arc smelting until the components are uniform to obtain a master alloy ingot;
(4) preparing an alloy bar: melting the master alloy ingot obtained in the step (4) by electric arc melting and heating, and casting the master alloy ingot into low-density plastic refractory Nb by a copper mold casting methodxTiyAlzV10(TaHfMoW)90-(x+y+z)A multi-principal element alloy bar;
among them, low density plastic refractory NbxTiyAlzV10(TaHfMoW)90-(x+y+z)The multi-principal element alloy is an as-cast dendritic structure, and the atomic ratio of Nb, Ti, Al, V and (TaHfMoW) is x: y: z: 10: 90- (x + y + z), wherein: x is more than or equal to 35 and less than or equal to 45, y is more than or equal to 25 and less than or equal to 30, z is more than or equal to 10 and less than or equal to 15, and the Ta/Hf/Mo/W is not equal in proportion.
2. The method of claim 1, wherein the vacuum arc melting is used in steps (1) - (3), and the vacuum chamber is pre-evacuated to a vacuum level of 10-4～10-3Pa, filling high-purity argon into the vacuum gauge to show that the argon is 2 multiplied by 104～4×104Pa, arc melting is carried out, and the melting current is 300-600A.
3. The method of claim 1, wherein the vacuum arc melting is used in step (4) to pre-pump the vacuum chamber to a vacuum level of 10-4～10-3Pa, filling high-purity argon into the vacuum gauge to show that the vacuum gauge is 3 multiplied by 104～5×104And Pa, carrying out arc melting on the master alloy ingot, wherein the melting current is 500-600A.
4. The method of making a low density plastic refractory multi-component alloy as claimed in claim 1 wherein in step (4) the casting comprises: and heating and melting the master alloy ingot to the temperature of the alloy melt, and pouring the alloy melt into a copper mold with a corresponding size to obtain the alloy bar.
5. The method for preparing the low-density plastic refractory multi-principal-element alloy according to claim 4, wherein the temperature of the alloy melt is 200-400 ℃ above the melting point of the alloy.
6. A low density plastic refractory multi-principal element alloy, characterized in that the low density plastic refractory Nb prepared by any one of claims 1 to 5xTiyAlzV10(TaHfMoW)90-(x+y+z)A multi-principal element alloy; the multi-principal-element alloy is an as-cast dendritic structure, and the atomic ratio of Nb, Ti, Al, V and (TaHfMoW) is x: y: z: 10: 90- (x + y + z), wherein: x is more than or equal to 35 and less than or equal to 45, y is more than or equal to 25 and less than or equal to 30, z is more than or equal to 10 and less than or equal to 15, and the Ta/Hf/Mo/W is not equal in proportion.
7. Low density plastic refractory multi-body according to claim 6The multi-principal-element alloy is characterized in that the density of the multi-principal-element alloy is 7.2-7.9 g/cm3(ii) a The room temperature compressive yield strength is 950-1100 MPa, and the corresponding room temperature maximum compressive plasticity>50 percent; the compressive yield strength is 560-680 MPa at 800 ℃, and the maximum compressive plasticity at room temperature is correspondingly>50 percent; the compressive yield strength is 430-580 MPa at 900 ℃, and the maximum compressive plasticity at room temperature is correspondingly>50 percent; the compression yield strength is 230-400 MPa at 1000 ℃, and the maximum compression plasticity at the corresponding room temperature>50％。
8. A low density plastic refractory multi-element alloy according to claim 6, wherein the multi-element alloy (TaHfMoW) comprises at least: ta and Hf as well as Mo and W as alloying elements.
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