CN115896579B - Ti-V-C refractory high-entropy alloy and preparation method thereof - Google Patents
Ti-V-C refractory high-entropy alloy and preparation method thereof Download PDFInfo
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- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 101
- 239000000956 alloy Substances 0.000 title claims abstract description 101
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 21
- 229910052720 vanadium Inorganic materials 0.000 claims abstract description 18
- 239000000203 mixture Substances 0.000 claims abstract description 11
- 229910052715 tantalum Inorganic materials 0.000 claims abstract description 7
- 239000010936 titanium Substances 0.000 claims description 47
- 238000003723 Smelting Methods 0.000 claims description 36
- 239000002994 raw material Substances 0.000 claims description 26
- 229910052751 metal Inorganic materials 0.000 claims description 9
- 239000002184 metal Substances 0.000 claims description 8
- 229910052719 titanium Inorganic materials 0.000 claims description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 238000002844 melting Methods 0.000 claims description 4
- 230000008018 melting Effects 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 3
- 239000012535 impurity Substances 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 238000005498 polishing Methods 0.000 claims description 3
- 230000007306 turnover Effects 0.000 claims description 3
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 3
- 238000010586 diagram Methods 0.000 description 16
- 238000002441 X-ray diffraction Methods 0.000 description 10
- 238000001938 differential scanning calorimetry curve Methods 0.000 description 10
- 229910000905 alloy phase Inorganic materials 0.000 description 8
- 238000010521 absorption reaction Methods 0.000 description 5
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000011161 development Methods 0.000 description 2
- 150000001247 metal acetylides Chemical class 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000007792 addition Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 229910001325 element alloy Inorganic materials 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910000753 refractory alloy Inorganic materials 0.000 description 1
- 239000003870 refractory metal Substances 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 1
Abstract
The invention discloses a Ti-V-C refractory high-entropy alloy and a preparation method thereof, wherein the composition element is W, ta, ti, V, C, and the component is W x Ta y Ti 34 V 35 C 1 Wherein x+y=30, x=5 to 25, and x and y are atomic percentages of W and Ta, respectively. The refractory high-entropy alloy has high strength, high hardness and good plasticity.
Description
Technical Field
The invention belongs to the technical field of metal materials and preparation thereof, and particularly relates to a Ti-V-C refractory high-entropy alloy and a preparation method thereof.
Background
With the development of society and the progress of technology, the application field of metal materials is gradually expanding, however, the conventional alloy system cannot meet the demands of fields such as nuclear industry, aerospace, energy and the like. To meet the increasing demands of life and production, researchers have developed many new alloys, one of which is a high entropy alloy. The concept of the high-entropy alloy, also called multi-principal element alloy, is first proposed by taiwan scholars She Junwei in 2004, and the composition of the high-entropy alloy comprises four or more alloy elements, and the proportion of each alloy element is 5% -35%. Once the high-entropy alloy is proposed, the high-entropy alloy has attracted research interests of a plurality of scholars by virtue of the excellent properties of high strength, high plasticity, strong corrosion resistance, irradiation resistance and the like. In recent years, many high-entropy alloys having good properties have been studied. The initial high-entropy alloy is mainly studied around equimolar ratio, and as the research is advanced, the students gradually put the eyes on the non-equimolar ratio high-entropy alloy, and the design method for improving the comprehensive mechanical property of the alloy by adding microelements is also developed.
The WNbMoTa refractory high-entropy alloy is the most mature high-entropy alloy studied so far, has high strength and high hardness, and particularly has excellent mechanical properties such as higher strength at high temperature, but has poor plasticity at normal temperature, so that engineering application is greatly limited, and the development of the high-entropy alloy with good strength and plasticity is very important.
Disclosure of Invention
Based on the problems existing in the prior art, the invention provides a Ti-V-C refractory high-entropy alloy and a preparation method thereof, and aims to enable the obtained high-entropy alloy to have higher strength and better plasticity by adjusting the proportion of each element.
In order to achieve the above purpose, the invention adopts the following technical scheme:
a Ti-V-C refractory high-entropy alloy is characterized in that: the high-entropy alloy has a composition element of W, ta, ti, V, C and a composition of W x Ta y Ti 34 V 35 C 1 Wherein x+y=30, x=5 to 25, and x and y are atomic percentages of W and Ta, respectively.
The preparation method of the Ti-V-C refractory high-entropy alloy comprises the following steps:
step 1, taking W, ta, ti and V blocky metal raw materials, removing an oxide layer and impurities on the metal surface by using a mechanical polishing method, then placing the raw materials in ethanol for ultrasonic cleaning, and drying the cleaned raw materials; taking WC powder (WC atomic percentage is 1:1) as a C raw material;
weighing the raw materials according to the proportion;
step 2, placing the prepared raw materials into two crucibles of vacuum non-consumable arc melting equipment, wherein one crucible is used for placing W and Ta raw materials, and the other crucible is used for placing Ti, V and WC raw materials;
the apparatus was evacuated to 8X 10 -4 Under Pa, argon is filled as shielding gas, and the pressure of the smelting chamber reaches-0.05 MPa;
step 3, after arc striking, adjusting the smelting current to be 180A-190A, smelting a titanium ingot to absorb residual oxygen, then adjusting the smelting current to be 220A-290A, smelting the alloy in the two crucibles for 3-4 times respectively, and after each smelting, using a turning spoon to turn over the alloy, wherein the single smelting time is not less than 5 minutes; then transferring the alloy ingots in the two crucibles into the same crucible for complete smelting, wherein the smelting times reach 10-12 times, and each smeltingAfter the smelting is finished, the alloy is turned over by using a turning spoon, and the single smelting time is not less than 10 minutes, so that the uniform alloy is ensured to be prepared; after smelting is finished, the component W is obtained x Ta y Ti 34 V 35 C 1 Refractory high entropy alloy of (a).
Preferably, in step 1, the purity of both the W, ta, ti, V bulk metal feedstock and the WC powder feedstock is not less than 99.99%.
Preferably, in step 1, the weighing is accurate to + -0.001 g.
Preferably, in step 3, the striking current is 20-25A.
The beneficial effects of the invention are as follows:
1. the Ti-V-C high-entropy alloy is composed of W, ta, ti, V refractory metal elements and nonmetallic elements C, and has high strength, high hardness and good plasticity.
2. DSC data show that the high-entropy alloy has no obvious phase change at the temperature below 1400 ℃ and has good thermal stability.
3. The high-entropy alloy provided by the invention uses high-melting-point tungsten and tantalum and low-density titanium and vanadium, so that the alloy melting point is improved, and meanwhile, the alloy density is reduced, and the high-entropy alloy has a good application prospect in the fields of aerospace, nuclear energy and the like.
Drawings
FIG. 1 shows W obtained in example 1 of the present invention 5 Ta 25 Ti 34 V 35 C 1 XRD pattern of the alloy.
FIG. 2 is a diagram of W obtained in example 1 of the present invention 5 Ta 25 Ti 34 V 35 C 1 Room temperature compressive stress-strain diagram of the alloy.
FIG. 3 is a diagram of W obtained in example 1 of the present invention 5 Ta 25 Ti 34 V 35 C 1 DSC curve of the alloy.
FIG. 4 is a diagram of W obtained in example 2 of the present invention 10 Ta 20 Ti 34 V 35 C 1 XRD pattern of the alloy.
FIG. 5 is a diagram of W obtained in example 2 of the present invention 10 Ta 20 Ti 34 V 35 C 1 Room temperature compressive stress-strain diagram of the alloy.
FIG. 6 is a diagram of W obtained in example 2 of the present invention 10 Ta 20 Ti 34 V 35 C 1 DSC curve of the alloy.
FIG. 7 is a diagram of W obtained in example 3 of the present invention 15 Ta 15 Ti 34 V 35 C 1 Alloy XRD pattern.
FIG. 8 is a diagram of W obtained in example 3 of the present invention 15 Ta 15 Ti 34 V 35 C 1 Room temperature compressive stress-strain diagram of the alloy.
FIG. 9 is a diagram of W obtained in example 3 of the present invention 15 Ta 15 Ti 34 V 35 C 1 DSC curve of the alloy.
FIG. 10 is a diagram of W obtained in example 4 of the present invention 20 Ta 10 Ti 34 V 35 C 1 Alloy XRD pattern.
FIG. 11 is a diagram of W obtained in example 4 of the present invention 20 Ta 10 Ti 34 V 35 C 1 Room temperature compressive stress-strain diagram of the alloy.
FIG. 12 is a graph showing W obtained in example 4 of the present invention 20 Ta 10 Ti 34 V 35 C 1 DSC curve of the alloy.
FIG. 13 is a view of W obtained in example 5 of the present invention 25 Ta 5 Ti 34 V 35 C 1 XRD pattern of the alloy.
FIG. 14 is a view of W obtained in example 5 of the present invention 25 Ta 5 Ti 34 V 35 C 1 Room temperature compressive stress-strain diagram of the alloy.
FIG. 15 is a view of W obtained in example 5 of the present invention 25 Ta 5 Ti 34 V 35 C 1 DSC curve of the alloy.
FIG. 16 is a graph of hardness of Ti-V-C based refractory alloy alloys according to various embodiments of the invention.
Detailed Description
In order that the above objects, features and advantages of the invention will be readily understood, a more particular description of the invention will be rendered by reference to the appended drawings. The following is merely illustrative and explanatory of the principles of the invention, as it would be apparent to those skilled in this art that various modifications or additions may be made to the specific embodiments described or in a similar manner without departing from the principles of the invention or beyond the scope of the claims.
The Ti-V-C refractory high-entropy alloys prepared in the following examples were all obtained as follows:
step 1, taking W, ta, ti and V blocky metal raw materials, removing an oxide layer and impurities on the metal surface by using a mechanical polishing method, then placing the raw materials in ethanol for ultrasonic cleaning, and drying the cleaned raw materials; taking WC powder (WC atomic percentage is 1:1) as a C raw material;
weighing the raw materials according to the proportion;
step 2, placing the prepared raw materials into two crucibles of vacuum non-consumable arc melting equipment, wherein one crucible is used for placing W and Ta raw materials, and the other crucible is used for placing Ti, V and WC raw materials;
the apparatus was evacuated to 8X 10 -4 Under Pa, argon is filled as shielding gas, and the pressure of the smelting chamber reaches-0.05 MPa;
step 3, after arc striking, adjusting the smelting current to be 180A-190A, smelting a titanium ingot to absorb residual oxygen, then adjusting the smelting current to be 220A-290A, smelting the alloy in the two crucibles for 3-4 times respectively, and after each smelting, using a turning spoon to turn over the alloy, wherein the single smelting time is not less than 5 minutes; transferring alloy ingots in the two crucibles into the same crucible for complete smelting, wherein the smelting times reach 10-12 times, and after each smelting is finished, turning over the alloy by using a turning spoon for not less than 10 minutes in a single smelting time so as to ensure that uniform alloy is prepared;
after smelting is finished, the component W is obtained x Ta y Ti 34 V 35 C 1 Refractory high entropy alloy of (a).
Example 1
The Ti-V-C refractory high-entropy alloy of the embodiment has the composition W 5 Ta 25 Ti 34 V 35 C 1 I.e. W, ta, ti, V, C atomic percent is 5at.%, 25at.%, 34at.%, 35at.%, 1at.%, respectively.
FIG. 1 shows W obtained in this example 5 Ta 25 Ti 34 V 35 C 1 XRD patterns of the alloy indicate that the alloy phase is a single BCC phase.
FIG. 2 shows W obtained in the present example 5 Ta 25 Ti 34 V 35 C 1 The Vickers hardness of the alloy at room temperature is 421.7HV, the yield strength is 1231.5MPa, and the plastic deformation is more than 50%, which shows that the alloy has higher strength, hardness and good plasticity.
FIG. 3 shows W obtained in the present example 5 Ta 25 Ti 34 V 35 C 1 The DSC curve of the alloy shows that the alloy phase has good heat stability in the temperature range as tested without obvious absorption/heat release peaks in the temperature range of 25-1400 ℃.
Example 2
The Ti-V-C refractory high-entropy alloy of the embodiment has the composition W 10 Ta 20 Ti 34 V 35 C 1 I.e. the atomic percentages of W, ta, ti, V, C are 10at.%, 20at.%, 34at.%, 35at.%, 1at.%, respectively.
FIG. 4 shows W obtained in the present example 10 Ta 20 Ti 34 V 35 C 1 XRD patterns of the alloy indicate that the alloy is a single BCC phase.
FIG. 5 shows W obtained in the present example 10 Ta 20 Ti 34 V 35 C 1 The Vickers hardness of the alloy at room temperature is 441.2HV, the yield strength is 1259.8MPa, and the plastic deformation is more than 50%, which shows that the alloy has higher strength, hardness and good plasticity. The yield strength and hardness of the resulting alloy are improved as compared to example 1.
FIG. 6 shows W obtained in the present example 10 Ta 20 Ti 34 V 35 C 1 The DSC curve of the alloy shows that the alloy phase has good heat stability in the temperature range as tested without obvious absorption/heat release peaks in the temperature range of 25-1400 ℃.
Example 3
The Ti-V-C refractory high-entropy alloy of the embodiment has the composition W 15 Ta 15 Ti 34 V 35 C 1 I.e. the atomic percentages of W, ta, ti, V, C are 15at.%, 34at.%, 35at.%, 1at.%, respectively.
FIG. 7 shows W obtained in the present example 15 Ta 15 Ti 34 V 35 C 1 XRD patterns of the alloys indicate that the alloys contain a single BCC phase and a small amount of carbides.
FIG. 8 is a diagram of W obtained in the present embodiment 15 Ta 15 Ti 34 V 35 C 1 The room temperature compression stress-strain curve graph of the alloy shows that the alloy has higher strength, hardness and good plasticity at the same time, as tested, the Vickers hardness of the alloy at room temperature is 528.2HV, the yield strength is 1542.6MPa, the compressive strength is 2246.8MPa and the plastic deformation is 20.6%. The yield strength and hardness of the resulting alloy were improved, but the plastic properties were significantly reduced, as compared to example 1.
FIG. 9 shows W obtained in the present example 15 Ta 15 Ti 34 V 35 C 1 The DSC curve of the alloy shows that the alloy phase has good heat stability in the temperature range as tested without obvious absorption/heat release peaks in the temperature range of 25-1400 ℃.
Example 4
The Ti-V-C refractory high-entropy alloy of the embodiment has the composition W 20 Ta 10 Ti 34 V 35 C 1 I.e. the atomic percentages of W, ta, ti, V, C are 20at.%, 10at.%, 34at.%, 35at.%, 1at.%, respectively.
FIG. 10 shows W obtained in the present example 20 Ta 10 Ti 34 V 35 C 1 The XRD pattern of the alloy,indicating that the alloy phase contains a single BCC phase and a small amount of carbides.
FIG. 11 shows W obtained in the present example 20 Ta 10 Ti 34 V 35 C 1 The Vickers hardness of the alloy at room temperature is 526.8HV, the yield strength is 1473.2MPa, the compressive strength is 2168.2MPa, and the plastic deformation is 23.7%, which shows that the alloy has higher strength and good plasticity. The yield strength and hardness of the resulting alloy were improved, but the plasticity was significantly reduced, as compared to example 1, but the yield strength and hardness of the resulting alloy were slightly reduced and the plasticity was slightly increased, as compared to example 3.
FIG. 12 shows W obtained in the present example 20 Ta 10 Ti 34 V 35 C 1 The DSC curve of the alloy shows that the alloy phase has good heat stability in the temperature range as tested without obvious absorption/heat release peaks in the temperature range of 25-1400 ℃.
Example 5
The Ti-V-C refractory high-entropy alloy of the embodiment has the composition W 25 Ta 5 Ti 34 V 35 C 1 I.e. the atomic percentages of W, ta, ti, V, C are 25at.%, 5at.%, 34at.%, 35at.%, 1at.%, respectively.
FIG. 13 shows W obtained in the present example 25 Ta 5 Ti 34 V 35 C 1 XRD patterns of the alloy indicate that the alloy phase is a single BCC phase.
FIG. 14 shows W obtained in the present example 25 Ta 5 Ti 34 V 35 C 1 The Vickers hardness of the alloy at room temperature is 523.9HV, the yield strength is 1388.3MPa, the compressive strength is 2238.4MPa and the plastic deformation is 28.8%, which shows that the alloy has higher strength and good plasticity. The yield strength and hardness of the resulting alloy were improved, but the plasticity was significantly reduced, as compared to example 1, but the yield strength and hardness of the resulting alloy were slightly reduced and the plasticity was slightly increased, as compared to example 3.
FIG. 15 shows W obtained in the present example 25 Ta 5 Ti 34 V 35 C 1 The DSC curve of the alloy shows that the alloy phase has good heat stability in the temperature range as tested without obvious absorption/heat release peaks in the temperature range of 25-1400 ℃.
The foregoing is illustrative only and is not intended to limit the present invention, and any modifications, equivalents, improvements and modifications falling within the spirit and principles of the invention are intended to be included within the scope of the present invention.
Claims (4)
1. A preparation method of a Ti-V-C refractory high-entropy alloy is characterized in that the high-entropy alloy has a composition element of W, ta, ti, V, C and a composition of W x Ta y Ti 34 V 35 C 1 Wherein x+y=30, x=5 to 25, x and y are atomic percentages of W and Ta, respectively, the preparation method comprises the following steps:
step 1, taking W, ta, ti and V blocky metal raw materials, removing an oxide layer and impurities on the metal surface by using a mechanical polishing method, then placing the raw materials in ethanol for ultrasonic cleaning, and drying the cleaned raw materials; taking WC powder as a raw material C;
weighing the raw materials according to the proportion;
step 2, placing the prepared raw materials into two crucibles of vacuum non-consumable arc melting equipment, wherein one crucible is used for placing W and Ta raw materials, and the other crucible is used for placing Ti, V and WC raw materials;
the apparatus was evacuated to 8X 10 -4 Under Pa, argon is filled as shielding gas, and the pressure of the smelting chamber reaches-0.05 MPa;
step 3, after arc striking, adjusting the smelting current to be 180A-190A, smelting a titanium ingot to absorb residual oxygen, then adjusting the smelting current to be 220A-290A, smelting the alloy in the two crucibles for 3-4 times respectively, and after each smelting, using a turning spoon to turn over the alloy, wherein the single smelting time is not less than 5 minutes; transferring alloy ingots in the two crucibles into the same crucible for complete smelting, wherein the smelting times reach 10-12 times, and after each smelting is finished, turning over the alloy by using a turning spoon for not less than 10 minutes in a single smelting time so as to ensure that uniform alloy is prepared;
after smelting is finished, the component W is obtained x Ta y Ti 34 V 35 C 1 Refractory high entropy alloy of (a).
2. The method of manufacturing according to claim 1, characterized in that: in step 1, the purity of the W, ta, ti, V bulk metal raw material and the WC powder raw material is not lower than 99.99%.
3. The method of manufacturing according to claim 1, characterized in that: in step 1, the weighing was accurate to.+ -. 0.001g.
4. The method of manufacturing according to claim 1, characterized in that: in the step 3, the striking current is 20-25A.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109023004A (en) * | 2018-09-03 | 2018-12-18 | 合肥工业大学 | A kind of single-phase infusibility high-entropy alloy and preparation method thereof towards plasma tungstenic |
| CN109182877A (en) * | 2018-11-07 | 2019-01-11 | 北京科技大学 | (NbMoTaW)100-xMxIt is infusibility high-entropy alloy and preparation method thereof |
| KR20190113353A (en) * | 2018-03-28 | 2019-10-08 | 국민대학교산학협력단 | Quaternary high entropy alloy composition, Quaternary high entropy alloy using the same and Manufacturing method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20190113353A (en) * | 2018-03-28 | 2019-10-08 | 국민대학교산학협력단 | Quaternary high entropy alloy composition, Quaternary high entropy alloy using the same and Manufacturing method thereof |
| CN109023004A (en) * | 2018-09-03 | 2018-12-18 | 合肥工业大学 | A kind of single-phase infusibility high-entropy alloy and preparation method thereof towards plasma tungstenic |
| CN109182877A (en) * | 2018-11-07 | 2019-01-11 | 北京科技大学 | (NbMoTaW)100-xMxIt is infusibility high-entropy alloy and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 含钨难熔高熵合金的制备、结构与性能;黄文军等;物理学报;第70卷(第10期);106201-1~106201-13 * |
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