CN117107138A - Method for improving toughness of refractory high-entropy alloy by doping rare earth Ce - Google Patents
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- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 32
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 27
- 238000000034 method Methods 0.000 title claims abstract description 26
- 239000002994 raw material Substances 0.000 claims abstract description 19
- 238000003723 Smelting Methods 0.000 claims abstract description 16
- 229910052720 vanadium Inorganic materials 0.000 claims abstract description 10
- 239000012856 weighed raw material Substances 0.000 claims abstract description 6
- 229910052751 metal Inorganic materials 0.000 claims abstract description 5
- 229910052758 niobium Inorganic materials 0.000 claims abstract description 5
- 239000002184 metal Substances 0.000 claims abstract description 4
- 238000005303 weighing Methods 0.000 claims abstract description 4
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- 238000002844 melting Methods 0.000 claims description 6
- 230000008018 melting Effects 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 5
- 229910052684 Cerium Inorganic materials 0.000 claims description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 3
- 229910052802 copper Inorganic materials 0.000 claims description 3
- 239000010949 copper Substances 0.000 claims description 3
- 239000011888 foil Substances 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 3
- 239000012535 impurity Substances 0.000 claims description 3
- 238000003760 magnetic stirring Methods 0.000 claims description 3
- 239000013049 sediment Substances 0.000 claims description 3
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 2
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- 238000007670 refining Methods 0.000 description 3
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- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000003870 refractory metal Substances 0.000 description 2
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- 229910000838 Al alloy Inorganic materials 0.000 description 1
- 229910000861 Mg alloy Inorganic materials 0.000 description 1
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- 229910000831 Steel Inorganic materials 0.000 description 1
- 229910007727 Zr V Inorganic materials 0.000 description 1
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- 230000002411 adverse Effects 0.000 description 1
- 229910000905 alloy phase Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
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- 229910052759 nickel Inorganic materials 0.000 description 1
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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
- 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
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C16/00—Alloys based on zirconium
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Abstract
The invention discloses a method for improving the toughness of refractory high-entropy alloy by doping rare earth Ce, which comprises the following steps: s1, proportioning, namely weighing Nb, ti, zr, V pure metal raw materials and Ce pure rare earth raw materials according to the component proportion; the content of Ce is 0 to 0.01at percent according to the atomic percentage; s2, smelting, namely putting the weighed raw materials into a smelting furnace for smelting to obtain refractory high-entropy alloy ingots with uniform components. The method for improving the toughness of the refractory high-entropy alloy by doping the rare earth Ce has the advantages that the rare earth Ce has obvious grain refinement effect, and a second phase favorable for plastic deformation is separated out at the grain boundary, so that the problem of Nb can be solved 0.5 TiZrV 0.5 The refractory high-entropy alloy has poor room-temperature plasticity, and realizes good matching of room-temperature tensile yield strength and plasticity.
Description
Technical Field
The invention relates to the technical field of alloys, in particular to a method for improving the toughness of refractory high-entropy alloy by doping rare earth Ce.
Background
The refractory high-entropy alloy (RHEA) is composed of 4 or more refractory metal elements (V, cr, ti, mo, nb, ta, W, zr, hf, etc.) of sub-groups IV to VI in equimolar or non-equimolar ratios. To achieve a more comprehensive performance, many non-refractory metals such as (Al, si, co and Ni) are also added to refractory high-entropy alloy systems. However, most refractory high-entropy alloy systems have the defects of high density, poor room-temperature plasticity, high-temperature oxidation resistance and the like, and the practical application of the refractory high-entropy alloy systems in the high-temperature field is severely limited. Therefore, the realization of the light weight of the refractory high-entropy alloy, the improvement of the deformability at room temperature, the improvement of the high-temperature oxidation resistance and the effective reduction of the cost are the basic research directions for realizing the wide application of the refractory high-entropy alloy.
The Nb-Ti-Zr-V refractory high-entropy alloy composed of low-density elements can effectively reduce the density of the alloy, has high melting point and higher high-temperature yield strength, and is expected to become an ideal candidate material of a novel structural material or a high-temperature thermal protection system. It has been reported that the room temperature plasticity of refractory high-entropy alloys can be improved by lowering the valence electron concentration VEC (< 4.4). Nb with VEC of 4.33 0.5 TiZrV 0.5 Refractory high-entropy alloys have a lower density (6.1 g/cm) 3 ) And better room temperature plasticity (. Epsilon. About.4.44%).
In addition, the method for improving room temperature plasticity by Ce microalloying is successfully applied to Mg alloy, fe-Mn-C steel, al alloy and Co-Al-W high-temperature alloy, and the research on the application of Ce in high-entropy alloy is very lack.
Thus, rare earth element Ce is adopted for Nb 0.5 TiZrV 0.5 The technical problem to be solved is that the refractory high-entropy alloy is microalloyed, and the room-temperature plasticity of the refractory high-entropy alloy is improved in a mode of refining grains, precipitating second phases at grain boundaries and the like.
Disclosure of Invention
The invention aims to provide a method for improving the toughness of refractory high-entropy alloy by doping rare earth Ce, which improves Nb by refining grains and changing the type of grain boundary precipitated phase 0.5 TiZrV 0.5 Room temperature tensile plasticity of refractory high-entropy alloys and achieving a good match of room temperature tensile yield strength and plasticity.
In order to achieve the above purpose, the invention provides a method for improving the toughness of refractory high-entropy alloy by doping rare earth Ce, which comprises the following steps:
s1, proportioning, namely weighing Nb, ti, zr, V pure metal raw materials and Ce pure rare earth raw materials according to the component proportion; the content of Ce is 0 to 0.01at percent according to the atomic percentage;
s2, smelting, namely putting the weighed raw materials into a smelting furnace for smelting to obtain refractory high-entropy alloy ingots with uniform components.
Preferably, the Nb, ti, zr, V, ce in the step S1 has an atomic percentage of (Nb) 0.5 TiZrV 0.5 ) 99.995 Ce 0.005 。
Preferably, before the raw materials are weighed in the step S1, the raw materials in block and sheet form are mechanically polished and put into acetone or absolute ethyl alcohol for ultrasonic cleaning, so that oxide films and other sediment impurities are removed.
Preferably, in the step S2, the weighed raw materials Ce, ti, V, zr, nb are sequentially put into Nb foil in order of melting point from low to high, and are coated together and placed at the bottom of the copper crucible.
Preferably, in the step S2, vacuum is pumped to 4-5×10 during smelting -3 Pa, and charging high purity argon gas to 1.0X10 5 Pa is protected, the raw materials are repeatedly smelted for 5 to 6 times under the protection of argon, and magnetic stirring is started in the smelting process.
Therefore, the method for improving the toughness of the refractory high-entropy alloy by doping rare earth Ce has the following technical effects:
(1) Nb containing 0.005at.% rare earth element Ce 0.5 TiZrV 0.5 The refractory high-entropy alloy has an average grain size of 248.6 mu m and the same component Nb without doping rare earth elements 0.5 TiZrV 0.5 The average grain size of refractory high-entropy alloy is 338.3 mu m, and the rare earth element Ce is doped in Nb 0.5 TiZrV 0.5 The average grain size can be significantly reduced in refractory high entropy alloys;
(2)(Nb 0.5 TiZrV 0.5 ) 99.995 Ce 0.005 the V-Ce-enriched Zr-depleted ribbon with BCC crystal structure is separated out at the grain boundary in the refractory high-entropy alloy, which is more beneficial to the dislocation to pass through the grain boundary deformation and promote the formation of the ductile pit fracture, thereby improving Nb 0.5 TiZrV 0.5 Room temperature stretch plasticity of refractory high entropy alloys.
The technical scheme of the invention is further described in detail through the drawings and the embodiments.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below. It will be apparent to those of ordinary skill in the art that the drawings in the following description are exemplary only and that other implementations can be obtained from the extensions of the drawings provided without inventive effort.
FIG. 1 is an XRD pattern of a sample of one to three casting states of a method for improving the toughness of a refractory high-entropy alloy by doping rare earth Ce;
FIG. 2 is a metallographic microstructure (OM) of one to three as-cast samples of a method for improving the toughness of refractory high-entropy alloys by doping rare earth Ce according to the present invention;
FIG. 3 is an EBSD orientation imaging diagram (IPF) of a method embodiment of the invention for improving the toughness of refractory high-entropy alloy by doping rare earth Ce;
FIG. 4 is a graph showing grain boundary microstructure characteristics (TEM) and element distribution (TEM-EDS) of a second to third as-cast sample of a method for improving toughness of refractory high-entropy alloy by doping rare earth Ce according to the present invention;
FIG. 5 is a Scanning Electron Microscope (SEM) of a tensile sample fracture of a one-to-three cast sample of an embodiment of a method for doping rare earth Ce to improve the toughness of refractory high-entropy alloys according to the present invention.
Detailed Description
The technical scheme of the invention is further described below through the attached drawings and the embodiments.
Unless defined otherwise, technical or scientific terms used herein should be given the ordinary meaning as understood by one of ordinary skill in the art to which this invention belongs.
Example 1
A method for improving the toughness of refractory high-entropy alloy by doping rare earth Ce comprises the following steps:
s1, mixing materials according to the atomic percentage (Nb) 0.5 TiZrV 0.5 ) 100 Ce 0 Taking Nb with purity of 99.99%, ti with purity of 99.995%, zr with purity of 99.95%, V pure metal raw material with purity of 99.95%, and pureA Ce pure rare earth raw material with the degree of 99.99 percent.
Before weighing, mechanically polishing the block-shaped and sheet-shaped raw materials, putting the raw materials into acetone for ultrasonic cleaning, removing oxide films and other sediment impurities, and ensuring the accuracy of sample preparation.
S2, smelting, namely sequentially putting the weighed raw materials into Nb foil according to the sequence (Ce, ti, V, zr, nb) from low melting point to high melting point, coating the raw materials together, and placing the raw materials at the bottom of a copper crucible. Vacuum was applied to 4X 10 during melting of the sample -3 Pa, and charging high-purity Ar gas to 1.0X10 5 Pa is protected. Repeatedly smelting raw materials under the protection of argon for 5 times, starting magnetic stirring in the smelting process to ensure uniform components and reduce segregation, and finally obtaining (Nb) with the mass of about 200g and uniform components 0.5 TiZrV 0.5 ) 100 Ce 0 Refractory high entropy alloys.
S3, preparing a sample, namely cutting the smelted cast ingot according to the die size of the tensile testing equipment to obtain a tensile sample.
Example two
The method for improving the toughness of refractory high-entropy alloy by doping rare earth Ce comprises the following specific steps as in the first embodiment: the atomic percentage content ratio is (Nb) 0.5 TiZrV 0.5 ) 99.995 Ce 0.005 。
Example III
The method for improving the toughness of refractory high-entropy alloy by doping rare earth Ce comprises the following specific steps as in the first embodiment: the atomic percentage content ratio is (Nb) 0.5 TiZrV 0.5 ) 99.99 Ce 0.01 。
Effect example
Room temperature tensile mechanical property test was performed on the tensile samples obtained in examples one to three
Room temperature tensile mechanical property test was performed on a 10kN MTS universal tester with a tensile strain rate of 10 -3 s -1 . The test specimens were polished on 200#, 400#, 600#, 800# and 1000# sandpaper to remove linear cutting traces on the surfaces of the samples before use, and after the test specimens were subjected to the plastic deformation stage, the stress-strain curves were subjected to the following stepsThe test can be stopped when the maximum stress begins to decrease. To ensure the repeatability of the data, 3 experiments were repeated for each alloy composition.
After the test sample is subjected to room temperature tensile property test, the test results of yield strength, tensile strength, elongation and the like are shown in table 1.
Table 1 room temperature tensile properties of three refractory high entropy alloys
Effect example two
(1) As-cast (Nb) obtained in examples one to three was obtained by using a D/MAX-2500 multifunctional X-ray diffraction apparatus (XRD) of Japanese national company 0.5 TiZrV 0.5 ) 100 Ce 0 、(Nb 0.5 TiZrV 0.5 ) 99.995 Ce 0.005 Sum (Nb) 0.5 TiZrV 0.5 ) 99.99 Ce 0.01 The mass was subjected to phase composition analysis.
Three samples were polished flat for measurement using a sand paper with a particle size of 2000. XRD test adopts Cu K alpha target, lambda= 0.15405nm, working voltage is 40kV, current is 200mA, scanning speed is 5 DEG/min, and scanning range is 20-90 deg. Calibration analysis is carried out on diffraction peaks after the completion of the test by Jade 6 software.
The XRD patterns of the as-cast samples obtained in examples one to three are shown in FIG. 1, and examples 1, 2 and 3 in FIG. 1 correspond to examples one, two and three, respectively. It can be derived (Nb) 0.5 TiZrV 0.5 ) 100 Ce 0 、(Nb 0.5 TiZrV 0.5 ) 99.995 Ce 0.005 Sum (Nb) 0.5 TiZrV 0.5 ) 99.99 Ce 0.01 All three as-cast refractory high-entropy alloys consist of single-phase BCC solid solutions, which shows that the doping of trace Ce elements does not cause Nb 0.5 TiZrV 0.5 And (3) refractory high-entropy alloy phase structure change.
(2) As-cast (Nb) obtained in examples one to three 0.5 TiZrV 0.5 ) 100 Ce 0 、(Nb 0.5 TiZrV 0.5 ) 99.995 Ce 0.005 Sum (Nb) 0.5 TiZrV 0.5 ) 99.99 Ce 0.01 Sequentially polishing three refractory high-entropy alloy ingots by using frosted paper with granularity of 400-3000, and then using SiO 2 And (5) mechanically polishing the polishing solution. The dendrite morphology of the three as-cast samples was characterized using a Leica LEICADM4000 metallographic microscope, germany. The surface of an as-cast sample of three refractory high-entropy alloys is scanned by a back scattering probe (EBSD, electron Backscattered Diffraction) arranged on an Apreo S LoVac field emission scanning electron microscope to obtain grain size information, and the acceleration voltage of the collected back scattering electrons is 20kV, and the scanning step length is 1-3 mu m.
The metallographic microstructure diagrams of the as-cast samples obtained in examples one to three are shown in fig. 2, in which (a) 1 in fig. 2 corresponds to the as-cast sample in example one, in which (b) 2 in fig. 2 corresponds to the as-cast sample in example two, and in which (c) 3 in fig. 2 corresponds to the as-cast sample in example three. It can be seen in the figure that (Nb 0.5 TiZrV 0.5 ) 100 Ce 0 、(Nb 0.5 TiZrV 0.5 ) 99.995 Ce 0.005 Sum (Nb) 0.5 TiZrV 0.5 ) 99.99 Ce 0.01 All three as-cast refractory high-entropy alloys have obvious dendrite structures.
EBSD orientation imaging diagrams (IPFs) of the as-cast samples obtained in examples one to three are shown in fig. 3. Fig. 3 (a) 1 and (a ') 1 correspond to the as-cast samples in the first embodiment, fig. 3 (b) 1 and (b ') 1 correspond to the as-cast samples in the second embodiment, and fig. 3 (c) 1 and (c ') 1 correspond to the as-cast samples in the third embodiment.
From the graph, (Nb) 0.5 TiZrV 0.5 ) 99.995 Ce 0.005 The as-cast sample had a minimum average grain size of 248.6 μm; (Nb) 0.5 TiZrV 0.5 ) 100 Ce 0 The as-cast sample had a maximum average grain size of 338.3 μm. The doping of a proper amount of Ce element can play a role in obviously refining grains.
With the smallest grain size (Nb) 0.5 TiZrV 0.5 ) 99.995 Ce 0.005 The room temperature stretching elongation of the as-cast sample is highest and can reach 6.95+/-0.47%;meanwhile, the yield strength can still keep 960.14 +/-33.89 MPa, and (Nb) 0.5 TiZrV 0.5 ) 100 Ce 0 The yield strengths 987.77.+ -. 26.17MPa are not very different (as shown in Table 1).
Therefore, 0.005at.% of Ce element doping can effectively achieve a good match of room temperature tensile yield strength and plasticity.
(3) Examples two and three (Nb) were performed using GL-696 ion attenuation apparatus 0.5 TiZrV 0.5 ) 99.995 Ce 0.005 Sum (Nb) 0.5 TiZrV 0.5 ) 99.99 Ce 0.01 And thinning the as-cast samples of the two refractory high-entropy alloys so as to observe the microcosmic appearance, grain boundary structure and element distribution of a precipitated phase at a grain boundary near a thinning position. The observation was carried out by using a JEM-2100F transmission electron microscope (TEM, transmission Electron Microscope), the operating voltage was 200KV and the filament current was 20mA.
The grain boundary microstructure characteristics (TEM) and the element distribution (TEM-EDS) of the as-cast samples of the second and third examples are shown in FIG. 4.
In fig. 4 (a), the morphology of the two crystal boundaries (GB) is shown, in fig. 4 (b), which is a partial enlarged view of the block b in (a), and in fig. 4 (c), which is the element distribution curve of the straight line AB in (b).
It can be concluded that there are V-Ce-rich Zr-lean band-like precipitates with BCC crystal structure at the grain boundaries of example two. Is more favorable for dislocation to pass through the grain boundary deformation and promote the formation of ductile pit fracture, thereby improving (Nb) 0.5 TiZrV 0.5 ) 99.995 Ce 0.005 Room temperature stretch plasticity of refractory high entropy alloys (as shown in table 1).
Fig. 4 (d) shows the three-boundary (GB) morphology of the example, fig. 4 (e) shows a partial enlarged view of a block e in (d), and fig. 4 (f) shows an element distribution curve of a straight line CD in (e).
It can be seen that there is an omega phase precipitation rich in V-Ce, lean in Ti and having HCP crystal structure at the grain boundary of example three. Brittle omega phase can hinder dislocation movement, adversely effecting plastic deformation, causing (Nb) 0.5 TiZrV 0.5 ) 99.99 Ce 0.01 Room temperature stretch plasticity of refractory high-entropy alloys is significantly reduced (as shown in table 1).
(4) The room temperature tensile fracture morphology of the three refractory high-entropy alloys was characterized by Apreo S LoVac field emission scanning electron microscopy (SEM, scanning Electron Microscope).
Scanning Electron Microscope (SEM) images of the fracture of the tensile sample obtained in examples one to three are shown in fig. 5.
(Nb 0.5 TiZrV 0.5 ) 100 Ce 0 、(Nb 0.5 TiZrV 0.5 ) 99.995 Ce 0.005 Sum (Nb) 0.5 TiZrV 0.5 ) 99.99 Ce 0.01 The fracture morphology of the three refractory high-entropy alloys all had mixed fracture characteristics, including ductile and brittle fracture modes, with boxes 1 and 2 in fig. 5 (a), 5 (b), and 5 (c) being ductile and brittle fracture characteristics, respectively. (Nb) 0.5 TiZrV 0.5 ) 99.995 Ce 0.005 The ductile fracture characteristics with the highest proportion (61.7%) indicate the best room temperature plasticity, as shown in table 1.
Therefore, the method for improving the toughness of the refractory high-entropy alloy by doping rare earth Ce can solve the problem of poor room-temperature plasticity of the conventional refractory high-entropy alloy, and realize good matching of room-temperature tensile yield strength and plasticity.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention and not for limiting it, and although the present invention has been described in detail with reference to the preferred embodiments, it will be understood by those skilled in the art that: the technical scheme of the invention can be modified or replaced by the same, and the modified technical scheme cannot deviate from the spirit and scope of the technical scheme of the invention.
Claims (6)
1. The method for improving the toughness of the refractory high-entropy alloy by doping rare earth Ce is characterized by comprising the following steps of:
s1, proportioning, namely weighing Nb, ti, zr, V pure metal raw materials and Ce pure rare earth raw materials according to the component proportion; the content of Ce is 0 to 0.01at percent according to the atomic percentage;
s2, smelting, namely putting the weighed raw materials into a smelting furnace for smelting to obtain refractory high-entropy alloy ingots with uniform components.
2. The method for improving the toughness of refractory high-entropy alloy by doping rare earth Ce according to claim 1, which is characterized in that: the atomic percentage content ratio of Nb, ti, zr, V, ce in the step S1 is (Nb) 0.5 TiZrV 0.5 ) 99.995 Ce 0.005 。
3. The method for improving the toughness of refractory high-entropy alloy by doping rare earth Ce according to claim 1, which is characterized in that: before raw materials are weighed in the step S1, the raw materials in the form of blocks and sheets are mechanically polished, and are put into acetone or absolute ethyl alcohol for ultrasonic cleaning, so that oxide films and other sediment impurities are removed.
4. The method for improving the toughness of refractory high-entropy alloy by doping rare earth Ce according to claim 1, which is characterized in that: in the step S2, the weighed raw materials Ce, ti, V, zr, nb are sequentially put into Nb foil according to the order of the melting point from low to high, and are coated together and placed at the bottom of the copper crucible.
5. The method for improving the toughness of refractory high-entropy alloy by doping rare earth Ce according to claim 1, which is characterized in that: in the step S2, vacuum is pumped to 4 to 5 multiplied by 10 during smelting -3 Pa, and charging high purity argon gas to 1.0X10 5 Pa is protected, the raw materials are repeatedly smelted for 5 to 6 times under the protection of argon, and magnetic stirring is started in the smelting process.
6. Rare earth element Ce in Nb 0.5 TiZrV 0.5 Use in refractory high entropy alloys.
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| CN118406998A (en) * | 2024-04-25 | 2024-07-30 | 中国农业机械化科学研究院集团有限公司 | Rare earth doped high-entropy alloy coating and preparation method thereof |
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| CN118406998A (en) * | 2024-04-25 | 2024-07-30 | 中国农业机械化科学研究院集团有限公司 | Rare earth doped high-entropy alloy coating and preparation method thereof |
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