CN115679154B - Ti-W-Ta-Nb intermediate alloy and preparation method thereof - Google Patents
Ti-W-Ta-Nb intermediate alloy and preparation method thereof Download PDFInfo
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- CN115679154B CN115679154B CN202211321876.7A CN202211321876A CN115679154B CN 115679154 B CN115679154 B CN 115679154B CN 202211321876 A CN202211321876 A CN 202211321876A CN 115679154 B CN115679154 B CN 115679154B
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- 239000000956 alloy Substances 0.000 title claims abstract description 88
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 87
- 238000002360 preparation method Methods 0.000 title abstract description 19
- 238000003723 Smelting Methods 0.000 claims abstract description 25
- 239000002994 raw material Substances 0.000 claims abstract description 22
- 238000010894 electron beam technology Methods 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 12
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 39
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 claims description 30
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 30
- 239000000203 mixture Substances 0.000 claims description 18
- 238000002844 melting Methods 0.000 claims description 13
- 230000008018 melting Effects 0.000 claims description 13
- 239000010936 titanium Substances 0.000 claims description 11
- 238000002156 mixing Methods 0.000 claims description 8
- 229910001257 Nb alloy Inorganic materials 0.000 claims description 5
- 229910001362 Ta alloys Inorganic materials 0.000 claims description 5
- 229910001080 W alloy Inorganic materials 0.000 claims description 5
- 239000012535 impurity Substances 0.000 claims description 5
- 230000001681 protective effect Effects 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 238000012216 screening Methods 0.000 claims description 4
- 229910052719 titanium Inorganic materials 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 230000015572 biosynthetic process Effects 0.000 claims description 2
- 238000013461 design Methods 0.000 abstract description 4
- 238000005275 alloying Methods 0.000 description 10
- 229910001069 Ti alloy Inorganic materials 0.000 description 8
- 239000002245 particle Substances 0.000 description 7
- 229910052721 tungsten Inorganic materials 0.000 description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical group [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 6
- 229910000765 intermetallic Inorganic materials 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 4
- 229910052715 tantalum Inorganic materials 0.000 description 4
- 239000010937 tungsten Substances 0.000 description 4
- 229910052786 argon Inorganic materials 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 239000003870 refractory metal Substances 0.000 description 3
- 238000005204 segregation Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 230000008021 deposition Effects 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- 229910000967 As alloy Inorganic materials 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Abstract
The invention relates to a Ti-W-Ta-Nb intermediate alloy and a preparation method thereof, wherein the Ti-W-Ta-Nb intermediate alloy can be synthesized through the processes of target intermediate alloy component design, raw material type selection, raw material proportion content control, electron beam smelting preparation and the like.
Description
Technical Field
The invention relates to the field of alloy raw material preparation, in particular to a Ti-W-Ta-Nb intermediate alloy and a preparation method thereof.
Background
Alloying is one of the main means for microstructure and mechanical property regulation and optimization of high-temperature titanium alloy and intermetallic compounds thereof, and alloy elements with different types and contents can produce multiple influences on oxidation resistance, strength, plasticity, durability, creep and other properties, so that titanium alloy materials and products meeting the application of higher service temperature are obtained. Other alloying elements besides matrix elements Al, ti and the like are usually added into raw materials in a mode of intermediate alloy, and along with the higher service temperature and performance design requirements of high-temperature titanium alloy and intermetallic compounds thereof, some alloying elements such as high-melting-point alloying element W, ta become the choice of key alloying elements, but the design and preparation of the intermediate alloy containing alloying elements such as alloying element W, ta still have great difficulty at present.
Therefore, there is a need to develop a master alloy containing alloying elements such as alloy element W, ta and a preparation method thereof, which can effectively improve the uniformity and stability of alloy components and reduce metallurgical defects such as segregation and inclusion of refractory metal elements.
Disclosure of Invention
The invention aims to overcome the problems in the prior art and provide a Ti-W-Ta-Nb quaternary intermediate alloy and a preparation method thereof.
In order to achieve the above object, the present invention provides the following technical solutions.
A Ti-W-Ta-Nb intermediate alloy comprises the following components in percentage by weight: 10-20% of Nb alloy element, 10-20% of W alloy element, 10-30% of Ta alloy element, less than or equal to 0.5% of impurity alloy element and the balance of Ti.
The melting point of the Ti-W-Ta-Nb intermediate alloy is far lower than that of a metal simple substance, and the Ti-W-Ta-Nb intermediate alloy is used for smelting and preparing the titanium alloy containing tungsten and tantalum and the titanium intermetallic compound, so that the uniformity and stability of alloy components can be effectively improved, and the metallurgical defects of segregation, inclusion and the like of refractory metal elements are reduced. The Ti-W-Ta-Nb intermediate alloy can meet the smelting preparation requirements of tungsten-containing and tantalum-containing titanium alloys and intermetallic compounds thereof in actual scientific research production and engineering application processes.
In some embodiments of the invention, the Nb alloying element content may be 10%, 11%, 12%, 13%, 14%, 15%, 16%, 17%, 18%, 19% or 20%.
In some embodiments of the invention, the content of the W alloy element may be 10%, 11%, 12%, 13%, 14%, 15%, 16%, 17%, 18%, 19% or 20%.
In some embodiments of the invention, the content of Ta alloy elements may be 10%, 11%, 12%, 13%, 14%, 15%, 16%, 17%, 18%, 19%, 20%, 21%, 22%, 23%, 24%, 25%, 26%, 7%, 8%, 29%, or 30%.
In some embodiments of the present invention, the content of the impurity alloying element may be 0, 0.1%, 0.2%, 0.3%, 0.4%, or 0.5%.
In some embodiments of the invention, the Ti-W-Ta-Nb master alloy is in the form of particles and the particle size is 0.2 to 5mm. For example, the particle size may be 0.2mm, 0.5mm, 1mm, 2mm, 3mm, 4mm or 5mm.
The invention also provides a preparation method of the Ti-W-Ta-Nb intermediate alloy, which comprises the following steps:
sponge titanium, ti-Nb intermediate alloy, pure tungsten powder and pure tantalum powder are taken as raw materials and weighed according to the proportion;
mixing the Ti-Nb intermediate alloy, the pure tungsten powder, the pure tantalum powder and part of the titanium sponge to obtain a mixture; placing the rest of the titanium sponge on the bottom layer of a smelting crucible of an electron beam smelting furnace, and then placing the mixture on the upper layer of the crucible; reserving 2-5 pieces of titanium sponge from the weighed titanium sponge, placing the titanium sponge at the top end of the mixture, and preparing for arc striking;
starting the electron beam smelting furnace, rapidly lifting input current to 500-1000A after arc striking is successful, melting the mixture in the smelting crucible under the input current to form a completely melted stable molten pool, and naturally cooling to form an intermediate alloy ingot;
and (3) carrying out fine washing, crushing and screening on the intermediate alloy ingot to obtain the Ti-W-Ta-Nb intermediate alloy.
The invention prepares the required Ti-W-Ta-Nb intermediate alloy through the processes of target intermediate alloy component design, raw material type selection, raw material proportioning content control, electron beam smelting preparation and the like.
It should be noted that 2 to 5 pieces of titanium sponge reserved are a part of the total amount of titanium sponge to be weighed, and cannot be additionally weighed, otherwise, deviation of the components of the prepared master alloy is caused.
In some embodiments of the invention, the titanium sponge is desirably grade 0 titanium sponge, and the particle size may be 2 to 12.7mm, for example 2mm, 3mm, 4mm, 5mm, 6mm, 7mm, 8mm, 9mm, 10mm, 11mm, 12mm or 12.7mm.
In some embodiments of the invention, the Ti-Nb master alloy may be in the form of flakes, wherein the weight percentage of Nb element may be 50% -70% (e.g., 50%, 55%, 60%, 65%, or 70%), with the remainder being Ti.
In some embodiments of the invention, the pure tungsten powder has a purity of 99.99% or more and a particle size of 5 to 20. Mu.m, for example, 5 μm, 6 μm, 7 μm, 8 μm, 9 μm, 10 μm, 11 μm, 12 μm, 13 μm, 14 μm, 15 μm, 16 μm, 17 μm, 18 μm, 19 μm or 20 μm.
In some embodiments of the invention, the pure tantalum powder has a purity of 99.9% or more and a particle size of 5 to 12 μm, such as 5 μm, 6 μm, 7 μm, 8 μm, 9 μm, 10 μm, 11 μm or 12 μm.
In some embodiments of the present invention, the raw materials comprise, in weight percent: 20-50% of titanium sponge, 20-35% of Ti-Nb intermediate alloy, 10-20% of pure tungsten powder and 10-30% of pure tantalum powder.
Alternatively, the titanium sponge may be weighed as a percentage of 20%, 25%, 30%, 35%, 40%, 45% or 50% by weight of the raw material.
Alternatively, the Ti-Nb master alloy may be, for example, 20%, 25%, 30% or 35% in weight percent of the raw materials weighed.
Alternatively, the pure tungsten powder may be weighed in weight percent of the raw material, for example, 10%, 11%, 12%, 13%, 14%, 5%, 16%, 17%, 18%, 19% or 20%.
Alternatively, the pure tantalum powder may be weighed as a percentage of the raw material by weight, for example, 10%, 15%, 20%, 25% or 30%.
In some embodiments of the invention, the preparation of the mix comprises: firstly, uniformly mixing the Ti-Nb intermediate alloy, the tungsten powder and the tantalum powder to ensure that the pure tungsten powder and the pure tantalum powder are uniformly attached to the surface of the Ti-Nb intermediate alloy; and then adding 40% -60% of the titanium sponge and further uniformly mixing to obtain the mixture. The Ti-Nb intermediate alloy used in the invention is in a millimeter level flake shape, tungsten powder and tantalum powder are micron level fine particles, compared with other intermediate alloy raw materials, the tungsten powder and tantalum powder have larger size and shape difference, are not easy to be adsorbed on the surfaces of granular intermediate alloys such as titanium sponge, zirconium sponge and the like, and are directly mixed to generate the phenomenon of mixed deposition of the tungsten powder and the tantalum powder, so that the conditions of splashing, unmelting, non-uniformity and the like of part of tungsten powder and tantalum powder are caused during preparation, and the tungsten powder and the tantalum powder are fully adsorbed on the surfaces of the flake-shaped Ti-Nb intermediate alloy before smelting by utilizing the larger surface characteristics and stronger adsorptivity of the flake-shaped Ti-Nb alloy, thereby reducing the occurrence of mixed deposition phenomenon, avoiding the situations of splashing, unmelting, non-uniformity and the like of part of tungsten powder and tantalum powder, and ensuring that all raw materials are fully melted and have uniform components.
In some embodiments of the invention, after starting the electron beam melting furnace, further comprising: vacuumizing to below 10Pa, filling a protective atmosphere, vacuumizing to below 10Pa, starting a smelting power supply, and performing arc striking. Preferably, the protective atmosphere is argon.
In some embodiments of the invention, the energy input is maintained for no less than 5 minutes after the formation of the stabilized molten pool.
In some embodiments of the invention, prior to performing the fine wash, further comprising: repeating the preparing the intermediate alloy ingot to accumulate the intermediate alloy ingot.
In some embodiments of the present invention, the method for preparing the Ti-W-Ta-Nb master alloy comprises the following steps:
raw material selection and preparation of Ti-W-Ta-Nb intermediate alloy:
the material weighing and proportioning are carried out by taking titanium sponge, ti-Nb intermediate alloy, pure tungsten powder and pure tantalum powder as raw materials, and the raw materials comprise, by weight: 20 to 50 percent of titanium sponge, 20 to 35 percent of Ti-Nb intermediate alloy, 10 to 20 percent of pure tungsten powder and 10 to 30 percent of pure tantalum powder. Wherein the titanium sponge is generally required to be grade 0 titanium sponge, and the granularity is 2-12.7 mm; the Ti-Nb intermediate alloy is flake-shaped, the Nb content is 50-70% by weight, and the balance is Ti; the purity of the pure tungsten powder is more than or equal to 99.99 percent, and the granularity is 5-20 mu m; pure tantalum powder with purity more than or equal to 99.9 percent and granularity of 5-12 mu m;
raw material mixing and arrangement of Ti-W-Ta-Nb master alloy:
firstly, fully and uniformly mixing the Ti-Nb intermediate alloy, the pure tungsten powder and the pure tantalum powder to ensure that the pure tungsten powder and the pure tantalum powder are uniformly attached to the surface of the flaky Ti-Nb intermediate alloy, and then adding 40% -60% of the titanium sponge to further uniformly mix to obtain a mixture; and uniformly placing the rest titanium sponge on the bottom layer of a smelting crucible of the electron beam smelting furnace, placing the mixture on the upper layer of the crucible, and reserving 2-5 titanium sponge preparation arcs at the top end of the crucible.
Electron beam melting preparation of Ti-W-Ta-Nb intermediate alloy:
starting a vacuum electron beam smelting furnace, vacuumizing to below 10Pa, filling protective argon, vacuumizing to below 10Pa, starting a smelting power supply, rapidly increasing input current to 500-1000A after arc striking is successful, melting mixed raw materials in a crucible under the high energy input condition to form a completely melted stable molten pool, stopping after energy input is kept at least 5min, and naturally cooling to form an alloy ingot.
Crushing and preparing Ti-W-Ta-Nb intermediate alloy particles:
repeating the above processes, accumulating intermediate alloy ingots, and carrying out fine washing, crushing and screening procedures to obtain the Ti-W-Ta-Nb intermediate alloy with granularity of 0.2-5 mm.
Compared with the prior art, the invention has the beneficial effects that:
the invention provides a Ti-W-Ta-Nb quaternary intermediate alloy which can be used for smelting and preparing tungsten-containing and tantalum-containing titanium alloys and intermetallic compounds thereof, and can effectively improve the uniformity and stability of alloy components and reduce metallurgical defects such as segregation, inclusion and the like of refractory metal elements. In addition, the Ti-W-Ta-Nb intermediate alloy is added in a mode of Ti-W-Ta-Nb intermediate alloy, and the problems of volatility and burning loss which are the same as those of aluminum alloy elements are avoided.
In addition, the melting point of the Ti-W-Ta-Nb intermediate alloy prepared by the method is about 2000-2500 ℃, is far lower than the melting point 3300-3500 ℃ of a tungsten simple substance and the melting point 2900-3000 ℃ of a tantalum simple substance, and the phenomenon of unstable smelting current caused by overlarge melting point difference can be avoided by adding the Ti-W-Ta-Nb intermediate alloy in the preparation process of the titanium alloy and the intermetallic compound thereof.
Detailed Description
In order to make the contents of the present invention more easily understood, the technical scheme of the present invention will be further described with reference to the specific embodiments, but the present invention is not limited thereto. All techniques implemented based on the above description of the invention are intended to be included within the scope of the invention. Unless otherwise indicated, the starting materials used in the examples were all commercially available. The apparatus or steps of operation not described herein are those routinely determinable by one of ordinary skill in the art.
Example 1: preparation of Ti-W-Ta-Nb intermediate alloy
First, ti-W-Ta-Nb master alloy compositions were designed:
the designed Ti-W-Ta-Nb intermediate alloy is a granular quaternary intermediate alloy, and the alloy comprises the following components in percentage by weight: 15% of Nb alloy element, 10% of W alloy element, 15% of Ta alloy element, less than or equal to 0.5% of impurity alloy element and the balance of Ti.
Then, weighing and proportioning the sponge titanium, the Ti-Nb intermediate alloy, the pure tungsten powder and the pure tantalum powder serving as raw materials, wherein the raw materials comprise the following components in percentage by weight: 50% of titanium sponge, 25% of Ti-Nb intermediate alloy, 10% of pure tungsten powder and 15% of pure tantalum powder. Wherein the titanium sponge is 0-grade titanium sponge, and the granularity is 2-12.7 mm; the Ti-Nb intermediate alloy is flake-shaped, the Nb content is 50-70% by weight, and the balance is Ti; the purity of the pure tungsten powder is more than or equal to 99.99 percent, and the granularity is 5-20 mu m; the purity of the pure tantalum powder is more than or equal to 99.9 percent, and the granularity is 5-12 mu m.
And then fully and uniformly mixing the Ti-Nb intermediate alloy, pure tungsten powder and pure tantalum powder, uniformly attaching the pure tungsten powder and the pure tantalum powder to the surface of the flaky Ti-Nb intermediate alloy, adding 50% of the total amount of the titanium sponge, and further uniformly mixing to obtain a mixture.
2-5 pieces of titanium sponge are reserved from the total titanium sponge, the rest titanium sponge is uniformly placed at the bottom layer of a smelting crucible of a vacuum electron beam smelting furnace, and the mixture is placed at the upper layer of the bottom layer; and placing 2-5 reserved titanium sponge on the top end of the mixture for preliminary arc striking.
Then, starting a vacuum electron beam smelting furnace, vacuumizing to 8Pa, filling protective argon, vacuumizing to 10Pa, starting a smelting power supply, rapidly increasing input current to 800A after arc striking is successful, melting the mixture in the crucible under the high-energy input condition to form a completely melted stable molten pool, stopping after energy input is kept for 5min, and naturally cooling to form an alloy ingot.
Finally, repeating the above processes, accumulating intermediate alloy ingots, and carrying out fine washing, crushing and screening procedures to obtain the Ti-W-Ta-Nb intermediate alloy with granularity of 0.2-5 mm, wherein the verification components comprise 14.3% of Nb alloy element, 10.9% of W alloy element, 14.3% of Ta alloy element, 60.1% of Ti alloy element and less than or equal to 0.2% of impurity alloy element.
The present invention is not limited to the above-mentioned embodiments, and any changes or substitutions that can be easily understood by those skilled in the art within the technical scope of the present invention are intended to be included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (6)
1. The Ti-W-Ta-Nb intermediate alloy is characterized by comprising the following components in percentage by weight: 10% -15% of Nb alloy element, 10% -15% of W alloy element, 10% -30% of Ta alloy element, less than or equal to 0.5% of impurity alloy element and the balance of Ti;
the Ti-W-Ta-Nb intermediate alloy is granular, and the granularity is 0.2-5 mm;
the melting point of the Ti-W-Ta-Nb intermediate alloy is 2000-2500 ℃.
2. The method for producing a Ti-W-Ta-Nb master alloy according to claim 1, comprising the steps of:
sponge titanium, ti-Nb intermediate alloy, pure tungsten powder and pure tantalum powder are taken as raw materials and weighed according to the proportion;
mixing the Ti-Nb intermediate alloy, the pure tungsten powder, the pure tantalum powder and part of the titanium sponge to obtain a mixture; placing the rest of the titanium sponge on the bottom layer of a smelting crucible of an electron beam smelting furnace, and then placing the mixture on the upper layer of the crucible; reserving 2-5 pieces of titanium sponge from the weighed titanium sponge, placing the titanium sponge at the top end of the mixture, and preparing for arc striking;
starting the electron beam smelting furnace, rapidly lifting input current to 500-1000A after arc striking is successful, melting the mixture in the smelting crucible under the input current to form a completely melted stable molten pool, and naturally cooling to form an intermediate alloy ingot;
and (3) carrying out fine washing, crushing and screening on the intermediate alloy ingot to obtain the Ti-W-Ta-Nb intermediate alloy.
3. The method according to claim 2, wherein,
the titanium sponge is 0-grade titanium sponge, and the granularity is 2-12.7 mm;
the Ti-Nb intermediate alloy is lamellar, wherein the weight percentage content of Nb element is 50% -70%, and the balance is Ti;
the purity of the pure tungsten powder is more than or equal to 99.99 percent, and the granularity is 5-20 mu m;
the purity of the pure tantalum powder is more than or equal to 99.9%, and the granularity is 5-12 mu m.
4. A method of manufacturing according to claim 2 or 3, characterized in that after starting the electron beam melting furnace, it further comprises: vacuumizing to below 10Pa, filling a protective atmosphere, vacuumizing to below 10Pa, starting a smelting power supply, and performing arc striking.
5. A production method according to claim 2 or 3, characterized in that after the formation of the stable molten pool, the energy input is maintained for not less than 5 minutes and stopped.
6. A method of preparing according to claim 2 or 3, further comprising, prior to the performing of the fine wash: repeating the preparing the intermediate alloy ingot to accumulate the intermediate alloy ingot.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104762527A (en) * | 2015-04-14 | 2015-07-08 | 咸阳天成钛业有限公司 | Ti-Ta interalloy cast ingot and preparation method thereof |
| CN110408806A (en) * | 2019-08-22 | 2019-11-05 | 承德天大钒业有限责任公司 | A kind of Al-Nb-Ta intermediate alloy and preparation method thereof |
| CN113881871A (en) * | 2021-09-30 | 2022-01-04 | 中国航发北京航空材料研究院 | Ti-W-Nb intermediate alloy and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104762527A (en) * | 2015-04-14 | 2015-07-08 | 咸阳天成钛业有限公司 | Ti-Ta interalloy cast ingot and preparation method thereof |
| CN110408806A (en) * | 2019-08-22 | 2019-11-05 | 承德天大钒业有限责任公司 | A kind of Al-Nb-Ta intermediate alloy and preparation method thereof |
| CN113881871A (en) * | 2021-09-30 | 2022-01-04 | 中国航发北京航空材料研究院 | Ti-W-Nb intermediate alloy and preparation method thereof |
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