CN114000029A - High-strength high-toughness high-entropy alloy and preparation method thereof - Google Patents
High-strength high-toughness high-entropy alloy and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of high-entropy alloys, and relates to a high-entropy alloy with high strength and high toughness and a preparation method thereof. The high-entropy alloy is NbTiMoVXSi alloy, and X is Hf or Zr; when the atomic percentage of Si element is more than 0 and less than or equal to 6 percent, the high-entropy alloy is NbTiMoVXSi hexahydric high-entropy alloy; when the atomic percentage of Si element is more than 6 and less than or equal to 20 percent, the high-entropy alloy is NbTiMoVX quinary high-entropy alloy, and Nb and Si react in situ to generate Nb5Si3A high melting point reinforcing phase; the inventionThe alloy forms a multi-component high-entropy solid solution matrix phase with good toughness and strength through additive manufacturing, and Nb which is thermodynamically stable at high temperature is generated5Si3The intermetallic compound enhances the phase, thus the performance advantage of the material can be fully exerted, and the good matching of the high-temperature strength and the room-temperature toughness is realized.
Description
Technical Field
The invention belongs to the technical field of high-entropy alloys, and relates to a high-entropy alloy with high strength and high toughness and a preparation method thereof.
Background
With the continuous improvement of the turbine front temperature and the thrust-weight ratio of the advanced aeroengine, higher requirements are put on the working temperature of hot end parts such as turbine blades and the like, and the traditional materials and most ultrahigh-temperature structural materials cannot meet the design requirements. The development of a new generation of ultra-high temperature structural material with higher temperature bearing capacity is imminent, and is a key task in the development of advanced aeroengines.
The Nb-Si-based refractory alloy has excellent comprehensive properties such as extremely high melting point, low density, good high-temperature strength and the like, is one of hot spots in the research field of the existing ultra-high temperature structural material, has high temperature bearing capacity (1200-1400 ℃) and is a potential future ultra-high temperature structural material for a high-performance gas turbine engine. However, the room temperature fracture toughness of the Nb — Si based alloy is slightly insufficient for excellent high temperature strength. In most of the better research results reported at present, the room temperature fracture toughness of the multi-element Nb-Si-based alloy is 15-20 MPa-m1/2Left and right. Therefore, the good matching of the room-temperature fracture toughness and the high-temperature strength of the Nb-Si-based alloy is extremely difficult to realize, which is a main obstacle for restricting the trend of engineering application of Nb-Si-based ultrahigh-temperature structural materials.
High entropy alloys are a class of disordered alloys discovered in recent years based on the search for bulk amorphous alloys. The most typical structure is a multi-component super solid solution, the solid solution strengthening effect is extremely strong, and the crystal lattice distortion exists. The unique crystal structure enables the high-entropy alloy to have some excellent performances which cannot be compared with the traditional alloy, such as high strength, high hardness, high room temperature toughness, high wear resistance, high corrosion resistance, high resistance to heat, excellent high temperature resistance and the like. In particular, the fracture toughness of the high-entropy alloy is obviously superior to that of other alloys.
Disclosure of Invention
The purpose of the invention is: the high-entropy alloy with high strength and high toughness is prepared by designing a novel high-entropy alloy with Nb, Ti, Mo, V and Hf (Zr) as main components, adding an alloying element Si, reasonably designing alloy components by comprehensively considering factors such as element melting points, atomic radii and mixed enthalpy among elements, and preparing by adopting a laser additive manufacturing technology.
In order to solve the technical problem, the technical scheme of the invention is as follows:
on the one hand, the high-strength high-toughness high-entropy alloy is provided, the high-entropy alloy is NbTiMoVXSi alloy, and X is Hf or Zr;
when the atomic percentage of Si element is more than 0 and less than or equal to 6 percent, the high-entropy alloy is NbTiMoVXSi hexahydric high-entropy alloy;
in the high-entropy alloy, the atomic percent of Nb element is 24.5-31%, the atomic percent of Ti element is 17.5-23%, the atomic percent of Mo element is 17-24.5%, the atomic percent of V element is 15-19%, and the atomic percent of X element is 6.5-9%;
when the atomic percentage of Si element is more than 6 and less than or equal to 20 percent, the high-entropy alloy is NbTiMoVX quinary high-entropy alloy, and Nb and Si react in situ to generate Nb5Si3A high melting point reinforcing phase;
in the high-entropy alloy, the atomic percent of Nb element is 18-28.5%, the atomic percent of Ti element is 13.5-20%, the atomic percent of Mo element is 13.5-21.5%, the atomic percent of V element is 8.5-22%, and the atomic percent of X element is 8.5-18%.
In the designed alloy, except for Si element, the enthalpy of mixing among other elements is very small, and chemical reaction is not easy to occur, so that a multi-component super solid solution phase is formed; meanwhile, elements with too high melting points such as Ta and W are not added into the alloy, so that the risk of segregation of alloy components is reduced. Wherein, Ti, V and Zr can be dissolved with Nb infinitely and can play a toughening role in the alloy; mo and Hf elements have larger lattice distortion and solid solution strengthening effect, can obviously refine alloy structure and improve high-temperature strength, hardness and plasticity.
The addition of the Si element has two functions: when the content of the Si element is less than 0-6%, designing and generating a NbTiMoVHf (Zr) Si six-element high-entropy solid solution alloy;when the content of Si element is 6-20%, the NbTiMoVHf (Zr) five-element high-entropy solid solution matrix is designed and obtained, and Nb is precipitated on the solid solution matrix5Si3A high melting point reinforcing phase. When the content of the Si element is 6-20%, the purpose is to react the Si element with part of the Nb element to generate Nb5Si3An intermetallic compound. By reasonably controlling the element content and the alloy solidification condition, the reaction between Si and other elements can be effectively avoided, and Nb in the multi-element Nb-Si-based alloy5Si3Intermetallic compounds tend to be the most readily formed high melting reinforcing phases.
On the other hand, the preparation method of the high-strength high-toughness high-entropy alloy is provided, and pure Nb, pure Ti, pure Mo, pure V, pure Si, pure Hf or pure Zr powder is used as raw materials for laser material increase manufacturing;
when the atomic percentage of Si element is more than 0 and less than or equal to 6 percent, uniformly mixing all the powders and preparing the powder by adopting a single-channel mode;
when the atomic percentage of Si is more than 6 and less than or equal to 20 percent, uniformly mixing pure Si and a part of pure Nb powder according to the mass ratio of 2: 11-2: 13, uniformly mixing the other part of pure Nb, pure Ti, pure Mo, pure V and pure X powder, and preparing by adopting a dual-channel mode.
Mixing pure Si and a portion of pure Nb powder in a mass ratio of 2:11 can make the atomic ratio of Si to Nb exactly 3:5, which is advantageous for direct Nb formation5Si3The intermetallic compound, if any surplus pure Nb powder, can directly enter the high-entropy alloy matrix. By adopting a double-channel coaxial powder feeding mode and adopting one channel to specially convey Nb + Si mixed powder, the Si element can preferentially react with the Nb element to avoid the reaction between other metal elements, which are beneficial to Nb on the high-entropy solid solution matrix5Si3And (5) generating a phase.
The single-channel preparation process parameters are as follows:
the laser power is 2100W-3200W, the scanning speed is 550 mm/min-900 mm/min, the spot diameter is 2.0 mm-2.5 mm, the protective gas flow is 10L/min-30L/min, the powder feeding amount is 1350 rpm-2550 rpm, and the powder carrier flow is 7L/min-9L/min.
The double-channel preparation process parameters are as follows:
the laser power is 1800W-2700W, the scanning speed is 400 mm/min-750 mm/min, the diameter of a light spot is 1.0 mm-2.0 mm, the protective gas flow is 10L/min-30L/min, the powder feeding amount is 1200 rpm-2000 rpm, and the powder carrier flow is 6L/min-8L/min.
The invention has the beneficial effects that:
the invention designs alloy and forms a multi-component high-entropy solid solution matrix phase with good toughness and strength through additive manufacturing, and generates Nb with stable thermodynamics at high temperature5Si3The intermetallic compound enhances the phase, thus the performance advantage of the material can be fully exerted, and the good matching of the high-temperature strength and the room-temperature toughness is realized.
According to the different addition amount of Si element, the formation of NbTiMoVHf (Zr) Si six-element high-entropy solid solution phase is promoted (Si element atomic percent is more than 0 and less than or equal to 6 percent), or the precipitation of Nb on NbTiMoVHf (Zr) five-element high-entropy solid solution matrix is promoted5Si3The intermetallic compound is used as a reinforcing phase (Si is more than 6 and less than or equal to 20 percent in atomic percentage), thereby obtaining the ultra-high temperature structural material with good room temperature toughness and high temperature strength.
The addition of the Si element has two functions: when the content of the Si element is less than 6 at.%, the NbTiMoVHf (Zr) Si six-element high-entropy solid solution alloy is designed and generated; when the content of the Si element is 6-20 at.%, designing to obtain a NbTiMoVHf (Zr) five-element high-entropy solid solution matrix, and precipitating Nb on the solid solution matrix5Si3A high melting point reinforcing phase.
The high-entropy alloy prepared by adopting the laser additive manufacturing technology has the following advantages: 1) the extremely fast cooling solidification speed can effectively inhibit the atomic diffusion and the formation of complex phases, is beneficial to the generation of multi-element solid solution and fine grains, and can eliminate the composition segregation and the uneven structure; 2) the technical problem that shell is required to be high-temperature resistant due to smelting and casting of refractory metal elements can be avoided, and pollution of electrodes, crucibles and the like to high-activity alloy melt is avoided; 3) the high-entropy alloy can be prepared by carrying out in-situ reaction on pure metal powder; 4) the method is convenient for preparing the complex-shaped member.
Detailed Description
In the following description, well-known structures and techniques are not shown to avoid unnecessarily obscuring the present invention.
Example 1:
(1) the designed high-entropy alloy comprises the following elements in atomic percentage: nb: 28.5%, Ti: 15.5%, Mo: 20%, V: 9%, Hf: 15%, Si: 12 percent.
(2) Respectively and uniformly mixing Nb + Ti + Mo + V + Hf powder and Nb + Si powder according to designed components, respectively placing the Nb + Ti + Mo + V + Hf mixed powder and the Nb + Si mixed powder in two synchronous powder feeders of laser additive manufacturing equipment, adopting Ti-6Al-4V alloy as a substrate material for laser additive manufacturing, and pre-depositing an Nb + Si layer with the thickness of about 0.5mm on the substrate material to reduce the influence of interface stress and the substrate material on deposited alloy; and adjusting laser additive manufacturing parameters according to specific chemical components of the alloy to be prepared, so that Nb + Ti + Mo + V + Hf powder and Nb + Si powder react in situ on the substrate to form the bulk high-entropy alloy. The preparation parameters are as follows: the laser power is 2000W, the scanning speed is 450mm/min, the diameter of a light spot is 1.5mm, the flow of protective gas is 20L/min, the powder feeding amount is 1400rpm, and the flow of a powder carrier is 6L/min.
Example 2:
(1) the designed high-entropy alloy comprises the following elements in atomic percentage: nb: 26.5%, Ti: 22%, Mo: 22.5%, V: 16.5%, Hf: 7%, Si: 5.5 percent.
(2) According to the designed components, six element powders of Nb + Ti + Mo + V + Hf + Si are uniformly mixed and loaded into a single-channel powder feeder of laser additive manufacturing equipment. The Ti-6Al-4V alloy is used as a substrate material for laser additive manufacturing to prepare the high-entropy alloy. The preparation parameters are as follows: the laser power is 2800W, the scanning speed is 750mm/min, the diameter of a light spot is 2.0mm, the flow rate of protective gas is 20L/min, the powder feeding amount is 1700rpm, and the flow rate of a powder carrier is 7L/min.
Example 3:
different from the embodiment 1, the designed high-entropy alloy comprises the following elements in atomic percentage: nb: 18%, Ti: 18%, Mo: 18%, V: 18%, Hf: 18%, Si: 10 percent. The laser power is 2100W, the scanning speed is 500mm/min, the diameter of a light spot is 1.0mm, the flow of protective gas is 30L/min, the powder feeding amount is 1200rpm, and the flow of a powder carrier is 8L/min.
Example 4:
different from the embodiment 1, the designed high-entropy alloy comprises the following elements in atomic percentage: nb: 23%, Ti: 17%, Mo: 21%, V: 16%, Zr: 13%, Si: 10 percent. The laser power is 2400W, the scanning speed is 550mm/min, the diameter of a light spot is 2.0mm, the flow of protective gas is 15L/min, the powder feeding amount is 1600rpm, and the flow of a powder carrier is 6L/min.
Example 5:
different from the embodiment 2, the designed high-entropy alloy comprises the following elements in atomic percentage: nb: 29%, Ti: 23%, Mo: 19%, V: 15%, Zr: 9%, Si: 5 percent. Laser power 3000W, scanning speed 900mm/min, spot diameter 2.5mm, protective gas flow 30L/min, powder feeding capacity 2200rpm, and powder carrier flow 9L/min.
Example 6:
different from the embodiment 1, the designed high-entropy alloy comprises the following elements in atomic percentage: nb: 24.5%, Ti: 16%, Mo: 16%, V: 22%, Zr: 11.5%, Si: 10 percent. The laser power is 2500W, the scanning speed is 700mm/min, the diameter of a light spot is 2.0mm, the flow of protective gas is 10L/min, the powder feeding amount is 1200rpm, and the flow of a powder carrier is 6L/min.
The mechanical properties of the samples prepared in the 6 examples were tested, and the test results are shown in table 1:
TABLE 1
As can be seen from the data in Table 1, the high-entropy alloy designed and prepared by the technical scheme of the invention has better strength, plasticity and toughness, and particularly the NbTiMoVHf (Zr) quinary high-entropy solid solution matrix + Nb5Si3The material of the high-melting-point reinforcing phase has excellent high-temperature strength and room-temperature toughness.
Claims (8)
1. A high-strength high-toughness high-entropy alloy is characterized in that: the high-entropy alloy is NbTiMoVXSi alloy, and X is Hf or Zr;
when the atomic percentage of Si element is more than 0 and less than or equal to 6 percent, the high-entropy alloy is NbTiMoVXSi hexahydric high-entropy alloy;
in the high-entropy alloy, the atomic percent of Nb element is 24.5-31%, the atomic percent of Ti element is 17.5-23%, the atomic percent of Mo element is 17-24.5%, the atomic percent of V element is 15-19%, and the atomic percent of X element is 6.5-9%;
when the atomic percentage of Si element is more than 6 and less than or equal to 20 percent, the high-entropy alloy is NbTiMoVX quinary high-entropy alloy, and Nb and Si react in situ to generate Nb5Si3A high melting point reinforcing phase;
in the high-entropy alloy, the atomic percent of Nb element is 18-28.5%, the atomic percent of Ti element is 13.5-20%, the atomic percent of Mo element is 13.5-21.5%, the atomic percent of V element is 8.5-22%, and the atomic percent of X element is 8.5-18%.
2. The high strength, high toughness and high entropy alloy of claim 1, wherein: x is Hf, and the atomic percentages of the elements of the high-entropy alloy are as follows: nb: 26.5%, Ti: 22%, Mo: 22.5%, V: 16.5%, Hf: 7%, Si: 5.5 percent.
3. The high strength, high toughness and high entropy alloy of claim 1, wherein: x is Hf, and the atomic percentages of the elements of the high-entropy alloy are as follows: nb: 28.5%, Ti: 15.5%, Mo: 20%, V: 9%, Hf: 15%, Si: 12 percent.
4. The high strength, high toughness and high entropy alloy of claim 1, wherein: x is Zr, and the atomic percentages of the elements of the high-entropy alloy are as follows: nb: 29%, Ti: 23%, Mo: 19%, V: 15%, Zr: 9%, Si: 5 percent.
5. The high strength, high toughness and high entropy alloy of claim 1, wherein: x is Zr, and the atomic percentages of the elements of the high-entropy alloy are as follows: nb: 23%, Ti: 17%, Mo: 21%, V: 16%, Zr: 13%, Si: 10 percent.
6. A method of preparing a high strength, high toughness and high entropy alloy according to claim 1, wherein: pure Nb, pure Ti, pure Mo, pure V, pure Si and pure Hf or pure Zr powder are used as raw materials to carry out laser additive manufacturing;
when the atomic percentage of Si element is more than 0 and less than or equal to 6 percent, uniformly mixing all the powders and preparing the powder by adopting a single-channel mode;
when the atomic percentage of Si is more than 6 and less than or equal to 20 percent, uniformly mixing pure Si and a part of pure Nb powder according to the mass ratio of 2: 11-2: 13, uniformly mixing the other part of pure Nb, pure Ti, pure Mo, pure V and pure X powder, and preparing by adopting a dual-channel mode.
7. The method of claim 6, wherein: preparing technological parameters in a single-channel mode:
the laser power is 2100W-3200W, the scanning speed is 550 mm/min-900 mm/min, the spot diameter is 2.0 mm-2.5 mm, the protective gas flow is 10L/min-30L/min, the powder feeding amount is 1350 rpm-2550 rpm, and the powder carrier flow is 7L/min-9L/min.
8. The method of claim 6, wherein: the preparation process parameters in a double-channel mode are as follows:
the laser power is 1800W-2700W, the scanning speed is 400 mm/min-750 mm/min, the diameter of a light spot is 1.0 mm-2.0 mm, the protective gas flow is 10L/min-30L/min, the powder feeding amount is 1200 rpm-2000 rpm, and the powder carrier flow is 6L/min-8L/min.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| KR20200004566A (en) * | 2018-07-04 | 2020-01-14 | 국방과학연구소 | High-entropy based composite and its manufacturing method |
| CN110923539A (en) * | 2019-12-17 | 2020-03-27 | 南方科技大学 | High-entropy alloy, preparation method thereof and compression performance testing method |
| CN111893364A (en) * | 2020-08-06 | 2020-11-06 | 中南大学 | Multi-element doped reinforced toughened high-entropy alloy and preparation method thereof |
| CN113215468A (en) * | 2021-05-06 | 2021-08-06 | 西北工业大学 | Two-phase high-entropy high-temperature alloy and additive manufacturing method thereof |
| CN113234986A (en) * | 2021-06-03 | 2021-08-10 | 哈尔滨工程大学 | Low-activation refractory medium-entropy alloy and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20200004566A (en) * | 2018-07-04 | 2020-01-14 | 국방과학연구소 | High-entropy based composite and its manufacturing method |
| CN110923539A (en) * | 2019-12-17 | 2020-03-27 | 南方科技大学 | High-entropy alloy, preparation method thereof and compression performance testing method |
| CN111893364A (en) * | 2020-08-06 | 2020-11-06 | 中南大学 | Multi-element doped reinforced toughened high-entropy alloy and preparation method thereof |
| CN113215468A (en) * | 2021-05-06 | 2021-08-06 | 西北工业大学 | Two-phase high-entropy high-temperature alloy and additive manufacturing method thereof |
| CN113234986A (en) * | 2021-06-03 | 2021-08-10 | 哈尔滨工程大学 | Low-activation refractory medium-entropy alloy and preparation method thereof |
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