CN119332120A - A method for preparing a high-strength and high-plasticity negative enthalpy titanium alloy material - Google Patents
A method for preparing a high-strength and high-plasticity negative enthalpy titanium alloy material Download PDFInfo
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- 239000000956 alloy Substances 0.000 title claims abstract description 100
- 229910001069 Ti alloy Inorganic materials 0.000 title claims abstract description 67
- 238000000034 method Methods 0.000 title claims abstract description 15
- 238000003723 Smelting Methods 0.000 claims abstract description 99
- 239000010936 titanium Substances 0.000 claims abstract description 85
- 239000002994 raw material Substances 0.000 claims abstract description 59
- 229910052751 metal Inorganic materials 0.000 claims abstract description 58
- 239000002184 metal Substances 0.000 claims abstract description 57
- 238000002844 melting Methods 0.000 claims abstract description 45
- 230000008018 melting Effects 0.000 claims abstract description 45
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 37
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 34
- 229910052720 vanadium Inorganic materials 0.000 claims abstract description 26
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 23
- 238000002360 preparation method Methods 0.000 claims abstract description 16
- 239000000463 material Substances 0.000 claims abstract description 14
- 239000010410 layer Substances 0.000 claims abstract description 13
- 230000001681 protective effect Effects 0.000 claims abstract description 9
- 239000002344 surface layer Substances 0.000 claims abstract description 5
- 239000000203 mixture Substances 0.000 claims description 50
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 16
- 239000007789 gas Substances 0.000 claims description 16
- 238000002156 mixing Methods 0.000 claims description 16
- 239000000126 substance Substances 0.000 claims description 13
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 12
- 238000003760 magnetic stirring Methods 0.000 claims description 12
- 239000001301 oxygen Substances 0.000 claims description 12
- 229910052760 oxygen Inorganic materials 0.000 claims description 12
- 229910052786 argon Inorganic materials 0.000 claims description 8
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 229910018125 Al-Si Inorganic materials 0.000 claims description 4
- 229910018507 Al—Ni Inorganic materials 0.000 claims description 4
- 229910018520 Al—Si Inorganic materials 0.000 claims description 4
- 229910018098 Ni-Si Inorganic materials 0.000 claims description 4
- 229910018529 Ni—Si Inorganic materials 0.000 claims description 4
- 229910004349 Ti-Al Inorganic materials 0.000 claims description 4
- 229910004337 Ti-Ni Inorganic materials 0.000 claims description 4
- 229910004339 Ti-Si Inorganic materials 0.000 claims description 4
- 229910004688 Ti-V Inorganic materials 0.000 claims description 4
- 229910004692 Ti—Al Inorganic materials 0.000 claims description 4
- 229910011209 Ti—Ni Inorganic materials 0.000 claims description 4
- 229910010978 Ti—Si Inorganic materials 0.000 claims description 4
- 229910010968 Ti—V Inorganic materials 0.000 claims description 4
- KHYBPSFKEHXSLX-UHFFFAOYSA-N iminotitanium Chemical compound [Ti]=N KHYBPSFKEHXSLX-UHFFFAOYSA-N 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims 3
- 229910052782 aluminium Inorganic materials 0.000 abstract description 6
- 229910052759 nickel Inorganic materials 0.000 abstract description 6
- 238000004140 cleaning Methods 0.000 abstract description 5
- 230000001105 regulatory effect Effects 0.000 abstract description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 33
- 239000002245 particle Substances 0.000 description 12
- 229910000831 Steel Inorganic materials 0.000 description 6
- 239000010959 steel Substances 0.000 description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 5
- 239000012300 argon atmosphere Substances 0.000 description 4
- 238000005266 casting Methods 0.000 description 4
- 238000013461 design Methods 0.000 description 4
- 239000002923 metal particle Substances 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- 238000011161 development Methods 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000011651 chromium Substances 0.000 description 2
- 230000007123 defense Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 239000010955 niobium Substances 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- 229910000975 Carbon steel Inorganic materials 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- 229910000861 Mg alloy Inorganic materials 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000010962 carbon steel Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 230000008094 contradictory effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 229910001562 pearlite Inorganic materials 0.000 description 1
- 239000003870 refractory metal Substances 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
Classifications
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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
- C22C14/00—Alloys based on titanium
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Abstract
本发明提出了一种高强度高塑性的负焓钛合金材料的制备方法，具体包括以下步骤：将Ti、Al、V、Ni和Si各金属原料进行超声清洗，依照质量百分配比进行配料，按熔点从低到高的顺序，依次放入水冷金属坩埚中，熔点最低的金属原料放在底层，熔点最高的金属原料放在表层，并在所述水冷金属坩埚中放置海绵钛；建立真空无氧环境，通入保护气；在无氧环境下引弧熔炼各金属原料，直至充分混溶，即得到所述高强度高塑性的负焓钛合金材料，得到的TiaAlbVcNidSie系列负焓钛合金材料在结构上均含有BCC及HCP结构，且可通过调节元素比例调控合金显微组织结构及力学性能。
The invention provides a preparation method of a high-strength and high-plasticity negative enthalpy titanium alloy material. The method specifically comprises the following steps: ultrasonically cleaning metal raw materials of Ti, Al, V, Ni and Si, preparing the materials according to the mass percentage ratio, and sequentially placing the materials into a water-cooled metal crucible in the order of melting points from low to high, wherein the metal raw material with the lowest melting point is placed on the bottom layer, and the metal raw material with the highest melting point is placed on the surface layer, and sponge titanium is placed in the water-cooled metal crucible; establishing a vacuum oxygen-free environment and introducing a protective gas; and arc-smelting the metal raw materials in the oxygen-free environment until they are fully miscible to obtain the high-strength and high-plasticity negative enthalpy titanium alloy material. The obtained Ti a Al b V c Ni d Si e series negative enthalpy titanium alloy materials all contain BCC and HCP structures in structure, and the alloy microstructure and mechanical properties can be regulated by adjusting the element ratio.
Description
Technical Field
The invention relates to the technical field of metal materials, in particular to a preparation method of a high-strength high-plasticity negative enthalpy titanium alloy material.
Background
Metallic structural materials, including titanium alloys, magnesium alloys, aluminum alloys, steel, and the like, are substrates for advanced national defense weaponry and high precision equipment, and their excellent strength and toughness determine the advancement and safety of these equipment and equipment. However, the strength and toughness of the material are mutually restricted, the toughness is often lost while the strength is improved, and the contradictory relationship of strength-toughness inversion is presented. The development of metallic structural materials with both high strength and high toughness is a constant pursuit for researchers.
The traditional alloy design chemical composition design concept is based on a cocktail type error testing method. Taking iron and steel materials as an example, taking iron (Fe) elements as a base, adding a small amount of alloying elements to regulate microstructure and performance of the iron and steel materials so as to adapt to the requirements of different service environments. For example, chromium (Cr) element can increase hardenability of steel and has a secondary hardening effect, and can improve hardness and wear resistance of carbon steel without embrittling the steel. The nickel (Ni) element can strengthen ferrite and refine pearlite, and has the total effect of improving strength, and the refractory metal elements such as niobium (Nb), tantalum (Ta) and the like play a solid solution strengthening role to improve the strength of steel.
However, with the rapid development of modern technologies and industries, development of materials with higher strength and plasticity is required to meet the more severe service environment. This presents a significant challenge for the design and preparation of the alloy chemistry.
In view of this, there is still a need for further improvement in terms of improving the high strength and high plasticity of negative enthalpy titanium alloy materials.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a preparation method of a high-strength high-plasticity negative enthalpy titanium alloy material, which solves the technical problem that the toughness is often lost while the strength of the material is improved in the prior art.
The technical scheme of the invention is realized as follows:
the invention provides a preparation method of a high-strength high-plasticity negative enthalpy titanium alloy material, which comprises the following steps:
Carrying out ultrasonic cleaning on Ti, al, V, ni and Si metal raw materials, proportioning according to the mass percentage, sequentially placing the materials into a water-cooled metal crucible according to the sequence from low melting point to high melting point, placing the metal raw material with the lowest melting point on the bottom layer, placing the metal raw material with the highest melting point on the surface layer, and placing titanium sponge in one of the water-cooled metal crucibles;
Establishing a vacuum anaerobic environment, and introducing a protective gas;
Smelting all metal raw materials in an anaerobic environment until the metal raw materials are fully mixed and dissolved, and obtaining the high-strength high-plasticity negative enthalpy titanium alloy material;
wherein, the chemical formulas of the high-strength high-plasticity negative enthalpy titanium alloy material are TiaAlbVcNidSie, a, b, c, d and e respectively correspond to the mass percentage of each element, a is 80-90wt%, b is 5-10wt%, c is 2-6wt%, d is 0-5wt% and e is 0-2wt%;
the high-strength high-plasticity negative enthalpy titanium alloy material has a chemical formula of Ti aAlbVcNidSie;
Wherein a, b, c, d and e respectively correspond to the mass percent of each element, a is 80-90wt%, b is 5-10wt%, c is 2-6wt%, d is 0-5wt%, and e is 0-2wt%.
On the basis of the scheme, further preferably, the negative enthalpy titanium alloy material with the chemical formula of Ti aAlbVcNidSie is prepared, wherein the purity of Ti, al, V, ni and Si corresponding to the raw materials is more than or equal to 99.95%.
On the basis of the scheme, the high-strength high-plasticity negative enthalpy titanium alloy material is further preferable, wherein Ti, al, V, ni and Si element have negative mixing enthalpy.
Further preferably, on the basis of this scheme, the mixing enthalpy Δh mix between the Ti, al, V, ni and Si elements is:
ΔHmix(Ti-Al)＝-30kJ/mol,ΔHmix(Ti-V)＝-2kJ/mol,ΔHmix(Ti-Ni)=-35kJ/mol,
ΔHmix(Ti-Si)＝-66kJ/mol,ΔHmix(Al-V)＝-16kJ/mol,ΔHmix(Al-Ni)=-22kJ/mol,
ΔHmix(Al-Si)＝-19kJ/mol,ΔHmix(V-Ni)＝-18kJ/mol,ΔHmix(V-Si)＝-48kJ/mol,ΔHmix
(Ni-Si)=-40kJ/mol。
Further preferably, on the basis of the scheme, the high-strength high-plasticity negative enthalpy titanium alloy material is one of Ti90Al6V4、Ti87.5Al8V4Si0.5、Ti86Al8V4Ni2、Ti85.5Al8V4Ni2Si0.5 and Ti 85Al8V4Ni2Si1.
On the basis of the scheme, it is further preferable that the establishing of the vacuum anaerobic environment and the introducing of the protective gas specifically comprise the following steps:
Closing an arc melting furnace door, opening circulating water and a mechanical pump, vacuumizing, opening a molecular pump to further vacuumize when the vacuum degree is lower than 5Pa, and introducing high-purity argon as shielding gas when the vacuum degree is lower than 5.0X10 -4 Pa.
On the basis of the scheme, further preferably, each metal raw material is subjected to arc striking smelting in an oxygen-free environment, wherein the titanium sponge is subjected to arc striking smelting for 2 times, and residual oxygen is absorbed.
On the basis of the scheme, further preferably, each metal raw material is subjected to arc striking smelting in an oxygen-free environment, wherein the number of times of arc striking smelting is more than 4, each cooled metal raw material in the crucible is turned over after each time of arc striking smelting, then the next time of arc striking smelting is carried out, and the titanium sponge is subjected to 2 times of arc striking smelting before the next time of arc striking smelting alloy, so that residual oxygen is absorbed.
On the basis of the scheme, it is further preferable that the arc striking smelting of other times further comprises magnetic stirring of the metal raw materials besides the first arc striking smelting and the last arc striking smelting.
On the basis of the scheme, it is further preferable that the smelting time of each arc striking smelting is respectively 1.0-2.0min, and the smelting voltage and the smelting current of the arc striking smelting are respectively 10-15V and 300-350A.
The preparation method of the high-strength high-plasticity negative enthalpy titanium alloy material has the following beneficial effects compared with the prior art:
The invention provides a Ti aAlbVcNidSie series negative enthalpy titanium alloy material, which is prepared from titanium, aluminum, vanadium, nickel and silicon elements through a vacuum arc melting furnace, wherein the series negative enthalpy titanium alloy structurally comprises a body-centered cubic structure (BCC, body-centred cubic) and a close-packed hexagonal structure (HCP, hexagonal close packing), the microstructure and the mechanical property of the alloy can be regulated and controlled through element proportion, and compared with a typical two-phase (BCC+HCP) titanium alloy, the BCC is enriched with V element, the HCP is enriched with Ti and Al element, thus the formation of a BCC phase can be promoted through adding Ni element with negative mixing enthalpy with V, and the BCC phase with high volume fraction is obtained.
Drawings
In order to more clearly illustrate the embodiments of the invention or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, it being obvious that the drawings in the following description are only some embodiments of the invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a flow chart of a preparation method of a Ti aAlbVcNidSie negative enthalpy titanium alloy material according to an embodiment of the invention;
FIG. 2 is an X-ray diffraction diagram of a Ti aAlbVcNidSie negative enthalpy titanium alloy material according to an example of the present invention;
Fig. 3 is a tensile stress strain curve of the Ti aAlbVcNidSie negative enthalpy titanium alloy material according to the example of the present invention.
Detailed Description
The following description of the embodiments of the present invention will clearly and fully describe the technical aspects of the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the present invention without making any inventive effort, are intended to fall within the scope of the present invention.
It is to be understood that the terminology used in the description of the embodiments of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of embodiments of the invention. As used in the specification of the embodiments of the invention and the appended claims, the singular forms "a," "an," and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise.
The invention prepares Ti aAlbVcNidSie series negative enthalpy titanium alloy materials by vacuum arc melting furnace through proportioning design composed of titanium (Ti), aluminum (Al), vanadium (V), nickel (Ni) and silicon (Si).
Specifically, the invention discloses a preparation method of a high-strength high-plasticity negative enthalpy titanium alloy material, which comprises the following steps:
Carrying out ultrasonic cleaning on Ti, al, V, ni and Si metal raw materials, proportioning according to the mass percentage, sequentially placing the materials into a water-cooled metal crucible according to the sequence from low melting point to high melting point, placing the metal raw material with the lowest melting point on the bottom layer, placing the metal raw material with the highest melting point on the surface layer, and placing titanium sponge in one of the water-cooled metal crucibles;
Establishing a vacuum anaerobic environment, and introducing a protective gas;
Smelting all metal raw materials in an anaerobic environment until the metal raw materials are fully mixed and dissolved, and obtaining the high-strength high-plasticity negative enthalpy titanium alloy material;
wherein, the chemical formulas of the high-strength high-plasticity negative enthalpy titanium alloy material are TiaAlbVcNidSie, a, b, c, d and e respectively correspond to the mass percentage of each element, a is 80-90wt%, b is 5-10wt%, c is 2-6wt%, d is 0-5wt% and e is 0-2wt%;
the high-strength high-plasticity negative enthalpy titanium alloy material has a chemical formula of Ti aAlbVcNidSie;
Wherein a, b, c, d and e respectively correspond to the mass percent of each element, a is 80-90wt%, b is 5-10wt%, c is 2-6wt%, d is 0-5wt%, and e is 0-2wt%.
Specifically, the purity of Ti, al, V, ni and Si of the corresponding raw materials of Ti aAlbVcNidSie is more than or equal to 99.95%.
Specifically, the high-strength high-plasticity negative enthalpy titanium alloy material has negative mixing enthalpy between Ti, al, V, ni and Si elements.
Specifically, the enthalpy of mixing Δh mix between Ti, al, V, ni and Si elements is:
ΔHmix(Ti-Al)＝-30kJ/mol,ΔHmix(Ti-V)＝-2kJ/mol,ΔHmix(Ti-Ni)=-35kJ/mol,
ΔHmix(Ti-Si)＝-66kJ/mol,ΔHmix(Al-V)＝-16kJ/mol,ΔHmix(Al-Ni)=-22kJ/mol,
ΔHmix(Al-Si)＝-19kJ/mol,ΔHmix(V-Ni)＝-18kJ/mol,ΔHmix(V-Si)＝-48kJ/mol,ΔHmix
(Ni-Si)=-40kJ/mol。
Specifically, the method for establishing the vacuum anaerobic environment and introducing the protective gas specifically comprises the following steps:
Closing an arc melting furnace door, opening circulating water and a mechanical pump, vacuumizing, opening a molecular pump to further vacuumize when the vacuum degree is lower than 5Pa, and introducing high-purity argon as shielding gas when the vacuum degree is lower than 5.0X10 -4 Pa.
Specifically, each metal raw material is subjected to arc striking smelting in an anaerobic environment, wherein the titanium sponge is subjected to arc striking smelting for 2 times, and residual oxygen is absorbed.
Specifically, each metal raw material is subjected to arc striking smelting in an anaerobic environment, wherein the number of times of arc striking smelting is more than 4, each cooled metal raw material in a crucible is turned over after each time of arc striking smelting, then the next arc striking smelting is carried out, and the titanium sponge is subjected to arc striking smelting for 2 times before the next arc striking smelting of alloy, so that residual oxygen is absorbed.
Specifically, in addition to the first arc striking smelting and the last arc striking smelting, the arc striking smelting of other times also comprises the magnetic stirring of the metal raw materials.
Specifically, the smelting time of each arc striking smelting is respectively 1.0-2.0min, and the smelting voltage and the smelting current of the arc striking smelting are respectively 10-15V and 300-350A.
After the optimized arrangement, the prepared negative enthalpy titanium alloy series structurally contains a body-centered cubic structure and a close-packed hexagonal structure, and the Ti aAlbVcNidSie negative enthalpy titanium alloy series material has high strength and high plasticity in mechanical property.
Example 1
A preparation method of a high-strength high-plasticity negative enthalpy titanium alloy material comprises the following steps:
S1, carrying out ultrasonic cleaning on Ti, al, V, ni and Si metal raw materials, mixing according to the mass percentage, sequentially placing the materials into a water-cooled metal crucible from low melting point to high melting point, placing the metal raw material with the lowest melting point at a bottom layer, placing the metal raw material with the highest melting point at a surface layer, and placing titanium sponge in one of the water-cooled metal crucibles;
S2, establishing a vacuum anaerobic environment, and introducing protective gas;
and S3, arc striking and smelting the metal raw materials in an anaerobic environment until the metal raw materials are fully mixed and dissolved, and thus the high-strength high-plasticity negative enthalpy titanium alloy material is obtained.
The chemical formula of the high-strength high-plasticity negative enthalpy titanium alloy material is Ti 85Al8V4Ni2Si1;
wherein a, b, c, d and e respectively correspond to the mass percent of each element, a is 85wt%, b is 8wt%, c is 4wt%, d is 2wt%, and e is 1wt%.
Specifically, the purity of Ti, al, V, ni and Si of the corresponding raw materials of Ti 85Al8V4Ni2Si1 is more than or equal to 99.95.
Specifically, the enthalpy of mixing Δh mix between Ti, al, V, ni and Si elements is:
ΔHmix(Ti-Al)＝-30kJ/mol,ΔHmix(Ti-V)＝-2kJ/mol,ΔHmix(Ti-Ni)=-35kJ/mol,
ΔHmix(Ti-Si)＝-66kJ/mol,ΔHmix(Al-V)＝-16kJ/mol,ΔHmix(Al-Ni)=-22kJ/mol,
ΔHmix(Al-Si)＝-19kJ/mol,ΔHmix(V-Ni)＝-18kJ/mol,ΔHmix(V-Si)＝-48kJ/mol,ΔHmix
(Ni-Si)=-40kJ/mol。
Specifically, the method for establishing the vacuum anaerobic environment and introducing the protective gas specifically comprises the following steps:
Closing an arc melting furnace door, opening circulating water and a mechanical pump, vacuumizing, opening a molecular pump to further vacuumize when the vacuum degree is lower than 5Pa, and introducing high-purity argon as shielding gas when the vacuum degree is lower than 5.0X10 -4 Pa.
Specifically, each metal raw material is subjected to arc striking smelting in an anaerobic environment, wherein the titanium sponge is subjected to arc striking smelting for 2 times, and residual oxygen is absorbed.
Specifically, each metal raw material is subjected to arc striking smelting in an anaerobic environment, wherein the number of times of arc striking smelting is more than 4, after each time of arc striking smelting, the alloy in the crucible is turned over, then the next arc striking smelting is carried out, and 2 times of smelting oxygen inhalation is carried out on the titanium sponge before the next arc striking smelting of the alloy.
Specifically, the smelting time of each arc striking smelting is respectively 1.0-2.0min, and besides the first arc striking smelting and the last arc striking smelting, the arc striking smelting of the metal raw material also comprises the magnetic stirring of the melt, and the smelting voltage and the smelting current of the arc striking smelting are respectively 10-15V and 300-350A.
The mixing enthalpy DeltaH mix(Ti85Al8V4Ni2Si1) = -19.2kJ/mol of Ti 85Al8V4Ni2Si1 prepared in this example, yield strength 1400MPa, breaking strength 1460MPa, and tensile plasticity 2.2%.
Example 2
A preparation method of a high-strength high-plasticity negative enthalpy titanium alloy material comprises the following steps:
s1, respectively placing Ti, V, al, ni and Si high-purity raw material particles in an ultrasonic cleaning instrument, cleaning for two times, then accurately weighing and proportioning the raw material particles according to the component proportion and the mole ratio, sequentially placing the raw material particles in a water-cooled metal crucible from low melting point to high melting point, placing the element with the lowest melting point in a bottom layer and the element with the highest melting point in a top layer, and simultaneously placing titanium sponge in one of the water-cooled metal crucibles;
S2, closing an arc melting furnace door, opening circulating water and a mechanical pump, vacuumizing, opening a molecular pump to further vacuumize when the vacuum degree is lower than 5Pa, and introducing high-purity argon as shielding gas when the vacuum degree is lower than 5.0X10 -4 Pa;
S3, arc striking is carried out under the high-purity argon atmosphere, sponge titanium is smelted for 2 times, residual oxygen in the furnace is absorbed, high-current smelting is firstly adopted, the smelting voltage is 10-15V, the smelting current is 300-350A, all metal particles are melted and uniformly mixed, after alloy buttons are cast and cooled, the alloy buttons are overturned by a manipulator, smelting is carried out in the same mode, magnetic stirring is started in each smelting process after the second time, the alloy buttons are cast and overturned for 180 degrees after each smelting, smelting is carried out for 4 times, so that alloy components are more uniform, the magnetic stirring is closed in the last smelting, the alloy buttons become smooth cast ingots, suction casting is carried out, after the alloy cast ingots are completely cooled, a furnace door is opened, and a sample is taken out, thus the high-strength high-plasticity negative enthalpy titanium alloy material is obtained.
The chemical formula of the high-strength high-plasticity negative enthalpy titanium alloy material is Ti 85.5Al8V4Ni2Si0.5;
Wherein a, b, c, d and e respectively correspond to the mass percent of each element, a is 85.5wt%, b is 8wt%, c is 4wt%, d is 2wt%, and e is 0.5wt%.
Specifically, the purity of the Ti 85.5Al8V4Ni2Si0.5 corresponding to Ti, al, V, ni and Si of the raw materials is more than or equal to 99.95%.
The Ti 85.5Al8V4Ni2Si0.5 alloy material prepared in the embodiment has the mixing enthalpy ΔHmix(Ti85.5Al8V4Ni2Si0.5)＝-17.5kJ/mol,Ti85.5Al8V4Ni2Si0.5, the room temperature tensile yield strength of 1200MPa, the breaking strength of 1300MPa and the uniform elongation of 5.5%.
Example 3
A preparation method of a high-strength high-plasticity negative enthalpy titanium alloy material comprises the following steps:
S1, respectively placing high-purity raw material particles of Ti, V and Al in an ultrasonic cleaning instrument, cleaning for two times, then accurately weighing and proportioning the raw material particles according to the component proportion and the mole ratio, sequentially placing the raw material particles into a water-cooled metal crucible from low melting point to high melting point, placing the element with the lowest melting point in a bottom layer and the element with the highest melting point in a top layer, and simultaneously placing titanium sponge in one of the water-cooled metal crucibles;
S2, closing an arc melting furnace door, opening circulating water and a mechanical pump, vacuumizing, opening a molecular pump to further vacuumize when the vacuum degree is lower than 5Pa, and introducing high-purity argon as shielding gas when the vacuum degree is lower than 5.0X10 -4 Pa;
S3, arc striking is carried out under the high-purity argon atmosphere, sponge titanium is smelted for 2 times, residual oxygen in the furnace is absorbed, high-current smelting is firstly adopted, the smelting voltage is 10-15V, the smelting current is 300-350A, all metal particles are melted and uniformly mixed, after alloy buttons are cast and cooled, the alloy buttons are overturned by a manipulator, smelting is carried out in the same mode, magnetic stirring is started in each smelting process after the second time, the alloy buttons are cast and overturned for 180 degrees after each smelting, smelting is carried out for 4 times, so that alloy components are more uniform, the magnetic stirring is closed in the last smelting, the alloy buttons become smooth cast ingots, suction casting is carried out, after the alloy cast ingots are completely cooled, a furnace door is opened, and a sample is taken out, thus the high-strength high-plasticity negative enthalpy titanium alloy material is obtained.
The chemical formula of the high-strength high-plasticity negative enthalpy titanium alloy material is Ti 90Al6V4;
Wherein a, b, c, d and e respectively correspond to the mass percent of each element, a is 90wt%, b is 6wt%, c is 4wt%, d is 0wt%, and e is 0wt%.
Specifically, the purity of Ti, al and V of the corresponding raw materials of Ti 90Al6V4 is more than or equal to 99.95%.
The Ti 90Al6V4 alloy prepared in this example has a mixing enthalpy value DeltaH mix(Ti90Al6V4)＝-11.1kJ/mol,Ti90Al6V4, a room temperature tensile yield strength of 790MPa, a breaking strength of 900MPa and a uniform elongation of 5.8%.
As shown in fig. 1, ti 90Al6V4 is a typical dual phase (bcc+hcp) titanium alloy in which BCC is rich in V element and HCP is rich in Ti and Al element. Therefore, the formation of the BCC phase can be promoted by adding Ni element with negative mixing enthalpy with V, so that the BCC phase with high volume fraction is obtained, and secondly, the mixing enthalpy of Si element and elements such as Ti, ni, al, V and the like is negative, so that the Si element is uniformly distributed.
Example 4
A preparation method of a high-strength high-plasticity negative enthalpy titanium alloy material comprises the following steps:
s1, respectively placing high-purity raw material particles of Ti, V, al and Si in an ultrasonic cleaning instrument, cleaning for two times, then accurately weighing and proportioning the raw material particles according to the component proportion and the mole ratio, sequentially placing the raw material particles into a water-cooled metal crucible from low melting point to high melting point, placing the element with the lowest melting point in a bottom layer and the element with the highest melting point in a top layer, and simultaneously placing titanium sponge in one of the water-cooled metal crucibles;
S2, closing an arc melting furnace door, opening circulating water and a mechanical pump, vacuumizing, opening a molecular pump to further vacuumize when the vacuum degree is lower than 5Pa, and introducing high-purity argon as shielding gas when the vacuum degree is lower than 5.0X10 -4 Pa;
S3, arc striking is carried out under the high-purity argon atmosphere, sponge titanium is smelted for 2 times, residual oxygen in the furnace is absorbed, high-current smelting is firstly adopted, the smelting voltage is 10-15V, the smelting current is 300-350A, all metal particles are melted and uniformly mixed, after alloy buttons are cast and cooled, the alloy buttons are overturned by a manipulator, smelting is carried out in the same mode, magnetic stirring is started in each smelting process after the second time, the alloy buttons are cast and overturned for 180 degrees after each smelting, smelting is carried out for 4 times, so that alloy components are more uniform, the magnetic stirring is closed in the last smelting, the alloy buttons become smooth cast ingots, suction casting is carried out, after the alloy cast ingots are completely cooled, a furnace door is opened, and a sample is taken out, thus the high-strength high-plasticity negative enthalpy titanium alloy material is obtained.
The chemical formula of the high-strength high-plasticity negative enthalpy titanium alloy material is Ti 87.5Al8V4Si0.5;
Wherein a, b, c, d and e respectively correspond to the mass percent of each element, a is 87.5wt%, b is 8wt%, c is 4wt%, d is 0wt%, and e is 0.5wt%.
Specifically, the purity of Ti, al, V and Si corresponding to the raw materials of Ti 87.5Al8V4Si0.5 is more than or equal to 99.95%.
The Ti 87.5Al8V4Si0.5 alloy material prepared by the embodiment has the mixing enthalpy ΔHmix(Ti87.5Al8V4Si0.5)＝-15.6kJ/mol,Ti87.5Al8V4Si0.5, the room temperature tensile yield strength of 850MPa, the breaking strength of 1000MPa and the uniform elongation of 6.9%.
Example 5
A preparation method of a high-strength high-plasticity negative enthalpy titanium alloy material comprises the following steps:
s1, respectively placing Ti, V, al, ni high-purity raw material particles in an ultrasonic cleaning instrument, cleaning for two times, then accurately weighing and proportioning the raw material particles according to the component proportion and the mole ratio, sequentially placing the raw material particles in a water-cooled metal crucible from low melting point to high melting point, placing the element with the lowest melting point in a bottom layer and the element with the highest melting point in a top layer, and simultaneously placing titanium sponge in one of the water-cooled metal crucibles;
S2, closing an arc melting furnace door, opening circulating water and a mechanical pump, vacuumizing, opening a molecular pump to further vacuumize when the vacuum degree is lower than 5Pa, and introducing high-purity argon as shielding gas when the vacuum degree is lower than 5.0X10 -4 Pa;
S3, arc striking is carried out under the high-purity argon atmosphere, sponge titanium is smelted for 2 times, residual oxygen in the furnace is absorbed, high-current smelting is firstly adopted, the smelting voltage is 10-15V, the smelting current is 300-350A, all metal particles are melted and uniformly mixed, after alloy buttons are cast and cooled, the alloy buttons are overturned by a manipulator, smelting is carried out in the same mode, magnetic stirring is started in each smelting process after the second time, the alloy buttons are cast and overturned for 180 degrees after each smelting, smelting is carried out for 4 times, so that alloy components are more uniform, the magnetic stirring is closed in the last smelting, the alloy buttons become smooth cast ingots, suction casting is carried out, after the alloy cast ingots are completely cooled, a furnace door is opened, and a sample is taken out, thus the high-strength high-plasticity negative enthalpy titanium alloy material is obtained.
The chemical formula of the high-strength high-plasticity negative enthalpy titanium alloy material is Ti 86Al8V4Ni2;
wherein a, b, c, d and e respectively correspond to the mass percent of each element, a is 86wt%, b is 8wt%, c is 4wt%, d is 2wt%, and e is 0wt%.
Specifically, the purity of Ti, al, V and Ni corresponding to raw materials of Ti 86Al8V4Ni2 is more than or equal to 99.95%.
The mixing enthalpy delta H mix(Ti86Al8V4Ni2) = -15.8kJ/mol of the Ti 86Al8V4Ni2 alloy prepared in the example, wherein the tensile yield strength of Ti 86Al8V4Ni2 at room temperature is 1200MPa, the breaking strength is 1310MPa, and the uniform elongation is 4.5%.
Fig. 2 is an X-ray diffraction pattern of the Ti aAlbVcNidSie series negative enthalpy titanium alloy materials prepared in examples 1-5, and it can be seen in fig. 2 that the obtained Ti aAlbVcNidSie negative enthalpy titanium alloy materials all contain a dual-phase structure of bcc+hcp, no other new phases are generated, and meanwhile, as the content of Ni element increases, the volume fraction of BCC phase also increases.
Fig. 3 is a tensile stress-strain curve of the Ti aAlbVcNidSie series negative enthalpy titanium alloy materials prepared in examples 1-5 at room temperature, as shown in fig. 3, with the addition of the negative enthalpy elements Ni and Si, the alloy strength is improved, and meanwhile, the tensile toughness is higher.
In summary, the invention provides a preparation method of a high-strength high-plasticity negative enthalpy titanium alloy material, and the microstructure and mechanical properties of the alloy can be regulated and controlled by adjusting element proportion, so that the negative enthalpy titanium alloy material has great application potential in the important fields of aerospace, marine vessels, national defense, military and the like.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, alternatives, and improvements that fall within the spirit and scope of the invention.
Claims (10)
1. The preparation method of the high-strength high-plasticity negative enthalpy titanium alloy material is characterized by comprising the following steps of:
Carrying out ultrasonic cleaning on Ti, al, V, ni and Si metal raw materials, proportioning according to the mass percentage, sequentially placing the materials into a water-cooled metal crucible according to the sequence from low melting point to high melting point, placing the metal raw material with the lowest melting point on the bottom layer, placing the metal raw material with the highest melting point on the surface layer, and placing titanium sponge in one of the water-cooled metal crucibles;
Establishing a vacuum anaerobic environment, and introducing a protective gas;
Smelting all metal raw materials in an anaerobic environment until the metal raw materials are fully mixed and dissolved, and obtaining the high-strength high-plasticity negative enthalpy titanium alloy material;
Wherein the chemical formulas of the high-strength high-plasticity negative enthalpy titanium alloy material are Ti aAlbVcNidSie, a, b, c, d and e respectively corresponding to the mass percentage of each element, wherein a is 70-90wt%, b is 3-15wt%, c is 1-10wt%, d is 0-10wt% and e is 0-10wt%.
2. The method for preparing a high-strength high-plasticity negative enthalpy titanium alloy material according to claim 1, wherein the negative enthalpy titanium alloy material with the chemical formula of Ti aAlbVcNidSie has the purity of Ti, al, V, ni and Si element of 99.95% or more corresponding raw materials.
3. The method for producing a high-strength high-plasticity negative enthalpy titanium alloy material according to claim 1, wherein the high-strength high-plasticity negative enthalpy titanium alloy material has negative mixing enthalpy between Ti, al, V, ni and Si elements.
4. The method for preparing a high-strength and high-plasticity negative enthalpy titanium alloy material according to claim 3, wherein the mixing enthalpy Δh mix between Ti, al, V, ni and Si elements is:
ΔHmix(Ti-Al)＝-30kJ/mol,ΔHmix(Ti-V)＝-2kJ/mol,ΔHmix(Ti-Ni)=-35kJ/mol,
ΔHmix(Ti-Si)＝-66kJ/mol,ΔHmix(Al-V)＝-16kJ/mol,ΔHmix(Al-Ni)=-22kJ/mol,
ΔHmix(Al-Si)＝-19kJ/mol,ΔHmix(V-Ni)＝-18kJ/mol,ΔHmix(V-Si)＝-48kJ/mol,ΔHmix
(Ni-Si)=-40kJ/mol。
5. the method of producing a high strength, high plasticity negative enthalpy titanium alloy material as claimed in claim 1, wherein the high strength, high plasticity negative enthalpy titanium alloy material is one of Ti90Al6V4、Ti87.5Al8V4Si0.5、Ti86Al8V4Ni2、Ti85.5Al8V4Ni2Si0.5 and Ti 85Al8V4Ni2Si1.
6. The method for preparing the high-strength high-plasticity negative enthalpy titanium alloy material according to claim 1, wherein the method is characterized by establishing a vacuum oxygen-free environment and introducing a protective gas, and specifically comprises the following steps:
Closing an arc melting furnace door, opening circulating water and a mechanical pump, vacuumizing, opening a molecular pump to further vacuumize when the vacuum degree is lower than 5Pa, and introducing high-purity argon as shielding gas when the vacuum degree is lower than 5.0X10 -4 Pa.
7. The method for producing a high-strength high-plasticity negative enthalpy titanium alloy material according to claim 1, characterized in that each metal raw material is arc-melted in an oxygen-free environment, wherein the titanium sponge is arc-melted 2 times to absorb residual oxygen.
8. The method for preparing a high-strength high-plasticity negative enthalpy titanium alloy material according to claim 1, wherein each metal raw material is subjected to arc striking smelting in an oxygen-free environment, the number of times of arc striking smelting is more than 4, each cooled metal raw material in a crucible is turned over after each time of arc striking smelting, next time of arc striking smelting is performed, and 2 times of arc striking smelting are performed on titanium sponge before next time of arc striking smelting alloy to absorb residual oxygen.
9. The method for producing a high-strength high-plasticity negative enthalpy titanium alloy material according to claim 8, wherein the arc striking smelting for other times includes magnetic stirring of the respective metal raw materials in addition to the first arc striking smelting and the last arc striking smelting.
10. The method for preparing a high-strength high-plasticity negative enthalpy titanium alloy material according to claim 9, wherein the smelting time of the arc striking smelting is 1.0-2.0min, and the smelting voltage and the smelting current of the arc striking smelting are 10-15V and 300-350A, respectively.
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