CN115896501B - Preparation method and application of titanium-aluminum alloy - Google Patents
Preparation method and application of titanium-aluminum alloy Download PDFInfo
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- CN115896501B CN115896501B CN202211717796.3A CN202211717796A CN115896501B CN 115896501 B CN115896501 B CN 115896501B CN 202211717796 A CN202211717796 A CN 202211717796A CN 115896501 B CN115896501 B CN 115896501B
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- UQZIWOQVLUASCR-UHFFFAOYSA-N alumane;titanium Chemical compound [AlH3].[Ti] UQZIWOQVLUASCR-UHFFFAOYSA-N 0.000 title claims abstract description 88
- 229910000838 Al alloy Inorganic materials 0.000 title claims abstract description 80
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 238000003723 Smelting Methods 0.000 claims abstract description 110
- 238000002844 melting Methods 0.000 claims abstract description 53
- 230000008018 melting Effects 0.000 claims abstract description 53
- 238000000034 method Methods 0.000 claims abstract description 40
- 239000000725 suspension Substances 0.000 claims abstract description 28
- 239000002994 raw material Substances 0.000 claims abstract description 16
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 32
- 229910052782 aluminium Inorganic materials 0.000 claims description 32
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 32
- 238000005266 casting Methods 0.000 claims description 22
- 239000010936 titanium Substances 0.000 claims description 20
- 229910052719 titanium Inorganic materials 0.000 claims description 20
- 238000003825 pressing Methods 0.000 claims description 17
- 239000000463 material Substances 0.000 claims description 10
- 238000005303 weighing Methods 0.000 claims description 5
- 230000000087 stabilizing effect Effects 0.000 claims description 4
- 238000005204 segregation Methods 0.000 abstract description 6
- 238000012545 processing Methods 0.000 abstract description 5
- 230000000052 comparative effect Effects 0.000 description 18
- 238000003466 welding Methods 0.000 description 14
- 230000007547 defect Effects 0.000 description 13
- 238000001816 cooling Methods 0.000 description 11
- 229910045601 alloy Inorganic materials 0.000 description 9
- 239000000956 alloy Substances 0.000 description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- 229910002804 graphite Inorganic materials 0.000 description 6
- 239000010439 graphite Substances 0.000 description 6
- 229910021330 Ti3Al Inorganic materials 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 4
- 229910052802 copper Inorganic materials 0.000 description 4
- 239000010949 copper Substances 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 238000007599 discharging Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 229910001069 Ti alloy Inorganic materials 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 238000010587 phase diagram Methods 0.000 description 3
- 210000003625 skull Anatomy 0.000 description 3
- 238000010561 standard procedure Methods 0.000 description 3
- 239000013077 target material Substances 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000005275 alloying Methods 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 239000011888 foil Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000007872 degassing Methods 0.000 description 1
- 210000001787 dendrite Anatomy 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000004299 exfoliation Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 229910000765 intermetallic Inorganic materials 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000010309 melting process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 238000005477 sputtering target Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000001771 vacuum deposition Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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Abstract
The application discloses a preparation method of a titanium-aluminum alloy and the application of the titanium-aluminum alloy. The method comprises the following steps: a first vacuum consumable arc melting step: fixing an electrode prepared from a titanium aluminum raw material in a vacuum consumable arc furnace for preliminary smelting to form a first blank; vacuum suspension smelting step: vacuum suspension smelting is carried out on the first blank to form a second blank; a second vacuum consumable arc melting step: and fixing the second blank serving as an electrode in a vacuum consumable arc furnace to perform vacuum consumable arc melting again to form the titanium-aluminum alloy. The preparation method of the application can obtain the titanium-aluminum alloy with high density, no air holes and segregation, no cracks, good processing performance and uniform structure.
Description
Technical Field
The application belongs to the technical field of metallurgical preparation, and particularly relates to a preparation method of a titanium-aluminum alloy, the titanium-aluminum alloy and application.
Background
The titanium-aluminum alloy can be used for alloy sputtering target materials for vacuum coating. The preparation of the titanium-aluminum alloy target material is difficult, and according to the phase diagram of the titanium-aluminum alloy, various intermetallic compounds can be formed between titanium and aluminum, so that the titanium-aluminum alloy has processing brittleness. Meanwhile, in the alloying process, the heat release expansion is easy to generate bubbles, shrinkage cavities and looseness, so that the porosity of the alloy is high, and the requirement of the density of the target cannot be met.
Meanwhile, as the density and the melting point of two elements of titanium and aluminum are very large, the preparation of the titanium-aluminum alloy with uniform components is very difficult, the titanium-aluminum alloy target prepared by the prior art has uneven components and excessive cost, and the titanium-aluminum alloy target has a large number of defects of shrinkage cavity, looseness and the like, so that the use and the development of the titanium-aluminum alloy target are seriously restricted.
Disclosure of Invention
Aiming at the defects and shortcomings of the prior art, the application aims to provide a preparation method of a titanium-aluminum alloy, the titanium-aluminum alloy and application. The preparation method of the application can obtain the titanium-aluminum alloy with high density, no air holes and segregation, no cracks, good processing performance and uniform structure.
In order to achieve the above purpose, the present application adopts the following technical scheme:
the first aspect of the application provides a preparation method of a titanium-aluminum alloy, which comprises the following steps:
a first vacuum consumable arc melting step: fixing an electrode prepared from a titanium aluminum raw material in a vacuum consumable arc furnace for preliminary smelting to form a first blank;
vacuum suspension smelting step: vacuum suspension smelting is carried out on the first blank to form a second blank;
a second vacuum consumable arc melting step: and fixing the second blank serving as an electrode in a vacuum consumable arc furnace to perform vacuum consumable arc melting again to form the titanium-aluminum alloy.
The first-step smelting of the application adopts the vacuum consumable arc melting to play a role of preliminary alloying, if the titanium aluminum raw material is directly smelted in the vacuum suspension smelting furnace, the aluminum is seriously evaporated, so the raw material is firstly smelted in the vacuum consumable arc furnace, and the aluminum evaporation and inaccurate proportioning caused by large melting point difference of titanium and aluminum in the second-step process can be avoided. However, the first blank obtained in the step still has a large amount of macrosegregation, and then the second step smelting is vacuum suspension smelting to ensure the adequate mixing of titanium and aluminum so as to eliminate the macrosegregation caused by the first step smelting, but the second blank obtained in the step has the defects of large amount of shrinkage cavities, looseness and cracks. In order to reduce the defects caused by the second step, the application adopts the third-step smelting, namely the vacuum consumable arc smelting is adopted again, and the method can feed, control crystal grains and reduce casting defects.
The application does not limit the smelting times of the first vacuum consumable arc smelting step, the vacuum suspension smelting step and the second vacuum consumable arc smelting step, and the smelting times of one or more steps can be increased according to the needs. Preferably, the titanium-aluminum alloy with high density, no air holes and segregation, no cracks, good processability and uniform structure can be obtained by only one first vacuum consumable arc melting step, one vacuum suspension melting step and one second vacuum consumable arc melting step.
In some embodiments, in the first vacuum consumable arc melting step, the preliminary melting conditions include: the vacuum degree of the vacuum consumable arc furnace is less than or equal to 0.1Pa, the arc stabilizing voltage is 25-35V, the arc stabilizing current is 2500-4000A, the vacuum degree in the furnace is continuously kept less than or equal to 0.1Pa after smelting is finished, and the furnace is cooled to below 300 ℃ along with the furnace and is discharged; preferably, the arcing voltage is 20-30V, the arcing current is 2000-3000A, preferably, the smelting temperature is 1750-1850 ℃, and the smelting time is 20-40 minutes.
In some embodiments, in the first vacuum consumable arc melting step, the molten pool height reaches 300mm, the high melting temperature brings about a high molten pool height, and raw materials such as titanium sponge and aluminum blocks are melted as much as possible, so that macrosegregation is reduced.
In some embodiments, in the vacuum suspension smelting step, the smelting temperature is 1800-2200 ℃, the smelting time is 25-60 minutes, the vacuum degree is less than or equal to 0.1Pa, and the power is 80-120 kilowatts. Preferably, the vacuum suspension smelting is cold crucible vacuum induction semi-suspension smelting.
In the vacuum suspension smelting step, the whole alloy is uniformly melted by reasonably controlling smelting process parameters, and titanium and aluminum are fully mixed to eliminate segregation.
In some embodiments, the vacuum suspension smelting step further comprises casting after smelting, wherein the casting temperature is 2000-2500 ℃, the casting speed is 8-12 kg/s, and the cast ingot is cooled to below 300 ℃ along with the furnace and is discharged.
In some embodiments, in the second vacuum consumable arc melting step, the vacuum degree is less than or equal to 0.1Pa, the arcing voltage is 20-40V, the arcing current is 2000-3000A, the arcing voltage is 35-45V, the arcing current is 2500-4000A, the melting temperature is 1550-1650 ℃, and the melting time is 1-4 h. And after smelting, continuously maintaining the vacuum degree to be 0.1-10 Pa, and cooling along with the furnace.
In the second vacuum consumable arc melting step, the melting temperature is controlled at 1550-1650 ℃, shrinkage cavity, porosity and the like existing in the second blank can be fed at a proper melting temperature, cracks are healed, a higher melting pool is not formed, and coarse grains and other casting defects are avoided. The high temperature of the molten pool indicates that the height of the molten pool is high, and although feeding can be completed, casting defects such as shrinkage cavity, looseness and the like can be formed when the molten pool is cooled, and meanwhile, coarse equiaxed crystals are formed at the center part, so that the mechanical property is poor.
In the invention, the primary consumable smelting is controlled to have higher smelting temperature, so that the sponge titanium and small aluminum blocks are better melted, macrosegregation is reduced as much as possible, and the secondary consumable smelting is performed, because the raw materials are completely titanium-aluminum alloy after suspension smelting, the smelting temperature is lower than that of the primary consumable smelting, and the excessive smelting temperature can cause the excessive height of a molten pool, difficult feeding during solidification, and a large number of casting defects such as shrinkage cavity, looseness and the like are formed.
In some embodiments, in the second vacuum consumable arc melting step, the height of the molten pool reaches 50mm, so that feeding can be finished, meanwhile, the height of the molten pool is not high, all defects are concentrated in a lower molten pool, and the material utilization rate is improved.
In some embodiments, the electrode in the first vacuum consumable arc melting step is prepared according to the following steps:
The preparation method comprises the following steps of respectively weighing raw materials titanium and aluminum according to the proportion of titanium and aluminum in the titanium-aluminum alloy, wherein the titanium-aluminum alloy comprises the following components in percentage by atom: al: 30-50%, ti: 50-70%;
And a material baking step, namely baking the titanium and aluminum which are subjected to the material preparation, wherein the baking conditions are as follows: the baking temperature is 140-200 ℃, the baking time is 4-6h, and the vacuum degree is 500-5000Pa.
An electrode pressing step of pressing the baked raw materials into an electrode;
In the preparation process of the electrode, the raw material titanium is preferably 0-grade titanium sponge and the raw material aluminum is preferably aluminum blocks with purity higher than 99.9%; the baking treatment helps to sufficiently remove moisture. The electrode pressing may be performed by a conventional electrode pressing method, such as a four-column electrode pressing machine, in which aluminum is placed in the middle of the titanium raw material. The electrode obtained after pressing is preferably dried before smelting, and if the specification of a single electrode is smaller, a plurality of electrodes can be welded together in a welding mode and then vacuum consumable smelting is carried out.
The second aspect of the application provides a titanium-aluminum alloy prepared by the method of any one of the above.
The third aspect of the application provides an application of the titanium-aluminum alloy, wherein the titanium-aluminum alloy is used as a target after being processed.
Compared with the prior art, the application has the beneficial effects that:
(1) According to the application, through the synergistic effect of each smelting step, the titanium-aluminum alloy obtained by smelting has high density, no air holes and segregation and no cracks.
(2) The titanium-aluminum alloy prepared by the method does not generate brittle phase Ti3Al and is convenient to process.
(3) The mechanical property of the titanium-aluminum alloy prepared by the method is superior to that of the titanium-aluminum alloy prepared by the traditional process, the resistivity is equal to that of the titanium-aluminum alloy prepared by the traditional process, the thermal conductivity is slightly higher than that of the titanium-aluminum alloy prepared by the traditional process, and the comprehensive performance is good.
(4) The titanium-aluminum alloy prepared by the method has a layered microstructure at all angles, and is different from a brittle dendritic structure of the titanium-aluminum alloy prepared by the traditional process, and the layered structure has better mechanical property.
(5) The titanium-aluminum alloy prepared by the method has good comprehensive performance and can be used for titanium-aluminum alloy targets.
Drawings
FIG. 1 is a macroscopic photograph of a titanium-aluminum alloy prepared in example 1 of the present application;
FIG. 2 is a macroscopic photograph of the titanium-aluminum alloy prepared in comparative example 1;
FIG. 3 is a microstructure of a titanium-aluminum alloy prepared in example 1 of the present application;
FIG. 4 is a microstructure of the titanium-aluminum alloy prepared in comparative example 1;
FIG. 5 is a microstructure of a titanium-aluminum alloy prepared in example 1 of the present application;
FIG. 6 is a microstructure of the titanium-aluminum alloy prepared in comparative example 1;
FIG. 7 is an XRD diffraction pattern of the titanium aluminum alloy prepared in example 1 and the titanium aluminum alloy prepared in comparative example 1.
Detailed Description
Embodiments of the present application will be described in detail below with reference to examples, but it will be understood by those skilled in the art that the following examples are only for illustrating the present application and should not be construed as limiting the scope of the present application. The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The drugs or instruments used were conventional products available commercially without the manufacturer's attention.
The method adopts the first vacuum consumable arc melting and the subsequent vacuum suspension melting and the second vacuum consumable arc melting to prepare the titanium-aluminum alloy, and the preparation method comprises the steps of batching, material drying, electrode pressing, electrode welding, the first vacuum consumable arc melting, the vacuum suspension melting and the second vacuum consumable arc melting. The method comprises the following steps:
1. And (3) proportioning:
According to the design requirement of the components of the titanium-aluminum alloy, respectively weighing 0-level sponge titanium and aluminum blocks with purity higher than 99.9%, wherein the aluminum-titanium alloy comprises the following components in percentage by atom: al: 30-50%, ti: 50-70%;
2. And (3) material drying:
And baking the prepared grade 0 titanium sponge and aluminum block in a vacuum baking oven to remove water. Baking at 140-200deg.C for 4-6h under vacuum of 500-5000Pa, and cooling with furnace after baking.
3. Electrode pressing:
And (3) pressing the baked raw materials to obtain the electrode. And placing the baked raw materials of titanium sponge and metal aluminum into a grinding tool of a special electrode pressing machine, and pressing into the electrode.
4. Electrode welding:
And welding the plurality of electrodes to obtain the welded electrodes.
5. A first vacuum consumable arc melting step:
and carrying out vacuum consumable arc melting on the welded electrode to obtain a first blank.
Specifically, a vacuum consumable electrode arc furnace is used for smelting, during the smelting process, the vacuum degree is kept to be less than or equal to 0.1Pa (such as 0.08Pa, 0.05Pa, 0.01Pa, 0.005Pa and the like), the arcing voltage is 20-30V (such as 21V, 23V, 25V or 28V), the arcing current is 2000-3000A (such as 2100A, 2300A, 2500A, 2700A and 2900A), the arcing voltage is 25-35V (such as 26V, 28V, 32V and 34V), the arcing current is 2500-4000A (such as 2600A, 3000A, 3200A, 3500A and 3800A), the vacuum degree is kept to be less than or equal to 0.1Pa (such as 0.08Pa, 0.05Pa, 0.01Pa and 0.005Pa and the like) after the smelting is finished, the furnace is cooled to be lower than 300 ℃ (such as 280 ℃, 250 ℃, 230 ℃ and 200 ℃) and the smelting temperature is 1750-1850 ℃ (such as 1760 ℃, 1790 ℃ and 1830 ℃) for 20 min (such as 32min, 38min and 38 min).
6. Vacuum suspension smelting:
And carrying out vacuum suspension smelting on the first blank after vacuum consumable arc smelting to obtain a second blank. Specifically, the vacuum suspension smelting equipment is used for smelting, the smelting temperature is 1800-2200 ℃ (such as 1850 ℃, 1890 ℃, 2050 ℃, 2100 ℃ 2150 ℃), the smelting time is 25-60 minutes (such as 30min, 35min, 40min, 45min and 50 min), the vacuum degree is less than or equal to 0.1Pa (such as 0.08Pa, 0.05Pa, 0.01Pa, 0.005Pa and the like), and the power is 80-120 kilowatts (such as 85KW, 95KW, 100KW, 110KW and 115 KW).
Casting is carried out after smelting is finished, the casting temperature is 2000-2500 ℃ (such as 2100 ℃, 2200 ℃, 2300 ℃ and 2400 ℃), the casting speed is 8-12 kg/s, and the cast ingot is cooled to below 300 ℃ along with the furnace and is discharged.
In the vacuum suspension smelting step, the whole alloy is uniformly melted, and titanium and aluminum are fully mixed to eliminate segregation.
7. A second vacuum consumable arc melting step:
And (3) carrying out second vacuum consumable arc melting on the second blank to obtain the titanium-aluminum alloy. Specifically, a vacuum consumable electrode arc furnace is adopted for smelting, in the smelting process, the vacuum degree is less than or equal to 0.1Pa (such as 0.08Pa, 0.05Pa, 0.01Pa, 0.005Pa and the like), the arcing voltage is 20-40V (such as 22V, 25V, 30V and 35V), the arcing current is 2000-3000A (such as 2100A, 2300A, 2500A, 2700A and 2900A), the arcing voltage is 35-45V (such as 38V, 40V, 42V and 44V), the arcing current is 2500-4000A (such as 38V, 2800A, 3000A, 3200A, 3500A and 3800A), the smelting temperature is 1550-1650 ℃ (such as 1580 ℃, 1600 ℃, 1640 ℃) and the smelting time is 1-4 h (such as 1.5h, 2.5h and 3.5 h). And after smelting, continuously maintaining the vacuum degree at 0.1-10 Pa (such as 0.5Pa, 1Pa, 2Pa, 3Pa, 4Pa, 5Pa, 7Pa and 9 Pa), and cooling along with the furnace.
The melted titanium-aluminum alloy can be processed into a titanium-aluminum target material with a certain size according to the requirement.
The following examples further illustrate the present application in detail, but the scope of the present application is not limited to the following examples.
Example 1
The preparation method comprises the following steps:
(1) And (3) batching: respectively weighing 0-level sponge titanium and aluminum blocks with purity higher than 99.9%, wherein the aluminum-titanium alloy comprises the following components in percentage by atom: al:50%, ti:50%.
(2) And (3) baking: putting the weighed grade 0 titanium sponge and aluminum block into a vacuum baking oven (the vacuum degree is 5000 Pa), preserving heat for 5 hours at 140 ℃, cooling to 35 ℃ along with the oven, and taking out.
(3) Pressing an electrode: aluminum blocks (30 mm in size, 30mm in size and 30mm in size) are wrapped with aluminum foil, titanium sponge is divided into two parts, a part of 0-grade titanium sponge is placed into a die of an electrode pressing machine, the wrapped aluminum blocks are placed into the die, and the rest of 0-grade titanium sponge is placed into the die.
(4) Welding electrodes: and welding the pressed electrodes together in an end-to-end mode by adopting argon tungsten-arc welding, wherein the welding material is pure titanium welding wires, and the electrode size is D150x500mm.
(5) A first vacuum consumable arc melting step: smelting by adopting a vacuum consumable electrode arc furnace, and preparing a water-cooled copper crucible with the diameter of D180 mm. In the smelting process, the vacuum degree is kept to be less than or equal to 0.1Pa, the arcing voltage is 24V, the arcing current is 2500A, the arcing voltage is 28V, and the arcing current is 3500A: and after the smelting is finished, continuously keeping the vacuum degree to be less than or equal to 0.1Pa, cooling to 300 ℃ along with a furnace, discharging, smelting at 1800 ℃ for 30min, and obtaining a first blank after smelting, wherein the depth of a molten pool is 200 mm.
(6) Vacuum suspension smelting: smelting the first blank by adopting vacuum suspension smelting equipment, wherein the smelting temperature is 2000 ℃, the smelting time is 1h, the vacuum degree is less than or equal to 0.1Pa, the power is 100KW in the smelting process, casting is carried out after the smelting is finished, the casting temperature is 2300 ℃, the casting speed is 10kg/s, and the cast ingot is cooled to 200 ℃ along with a furnace and is discharged from the furnace, so that a second blank is obtained.
(7) Second vacuum consumable arc melting: the second billet was melted by means of a vacuum consumable electrode arc furnace, equipped with a water-cooled copper crucible with a diameter D150 mm. In the smelting process, the vacuum degree is kept to be less than or equal to 0.1Pa, the arcing voltage is 30V, the arcing current is 2500A, the arcing voltage is 40V, the arcing current is 3500A, the vacuum degree is kept to be 5Pa after smelting is finished, the smelting temperature is 1600 ℃ along with furnace cooling, the depth of a molten pool is 50mm, and the smelting time is 2h.
Example 2
The preparation method comprises the following steps:
(1) And (3) batching: respectively weighing 0-level sponge titanium and aluminum blocks with purity higher than 99.9%, wherein the aluminum-titanium alloy comprises the following components in percentage by atom: al:40%, ti:60%.
(2) And (3) baking: putting the weighed grade 0 titanium sponge and aluminum block into a vacuum baking oven (the vacuum degree is 5000 Pa), preserving heat for 5 hours at 140 ℃, cooling to 35 ℃ along with the oven, and taking out.
(3) Pressing an electrode: aluminum blocks (30 mm in size, 30mm in size and 30mm in size) are wrapped with aluminum foil, titanium sponge is divided into two parts, a part of 0-grade titanium sponge is placed into a die of an electrode pressing machine, the wrapped aluminum blocks are placed into the die, and the rest of 0-grade titanium sponge is placed into the die.
(4) Welding electrodes: and welding the pressed electrodes together in an end-to-end mode by adopting argon tungsten-arc welding, wherein the welding material is pure titanium welding wires, and the electrode size is D150x500mm.
(5) A first vacuum consumable arc melting step: smelting by adopting a vacuum consumable electrode arc furnace, and preparing a water-cooled copper crucible with the diameter of D180 mm. In the smelting process, the vacuum degree is kept to be less than or equal to 0.1Pa, the arcing voltage is 30V, the arcing current is 2000A, the arcing voltage is 35V, and the arcing current is 2500A: and after the smelting is finished, continuously keeping the vacuum degree to be less than or equal to 0.1Pa, cooling to 300 ℃ along with a furnace, discharging, smelting at 1800 ℃ for 40min, and obtaining a first blank after smelting, wherein the depth of a molten pool is 300 mm.
(6) Vacuum suspension smelting: smelting the first blank by adopting vacuum suspension smelting equipment, wherein the smelting temperature is 1850 ℃, the smelting time is 50min, the vacuum degree is less than or equal to 0.1Pa, the power is 120KW in the smelting process, casting is carried out after the smelting is finished, the casting temperature is 2400 ℃, the casting speed is 10kg/s, and the cast ingot is cooled to 300 ℃ along with a furnace and is discharged from the furnace, so that a second blank is obtained.
(7) Second vacuum consumable arc melting: the second billet was melted by means of a vacuum consumable electrode arc furnace, equipped with a water-cooled copper crucible with a diameter D150 mm. In the smelting process, the vacuum degree is kept to be less than or equal to 0.1Pa, the arcing voltage is 40V, the arcing current is 2000A, the arcing voltage is 45V, the arcing current is 2500A, the vacuum degree is kept to be 9Pa after smelting is finished, the smelting temperature is 1600 ℃ along with furnace cooling, the depth of a molten pool is 50mm, and the smelting time is 3h.
The titanium-aluminum alloy obtained in example 2 has no defects such as shrinkage cavity, loosening and peeling, and has an equiaxed microstructure and a layered microstructure. XRD analysis shows diffraction peaks of the brittle-free phase Ti3 Al.
Comparative example 1
The preparation method comprises the following steps:
steps (1) to (5) are the same as in example 1;
(6) Vacuum consumable skull smelting: smelting by adopting a vacuum consumable electrode skull furnace, and casting by adopting a high-purity graphite die; firstly, degassing a graphite mold in a vacuum oven, wherein the heating temperature is 550 ℃, and the baking time is 10 hours; placing the baked graphite mold in a vacuum shell condensing furnace, and fixing the graphite mold by using iron wires to align a pouring gate to the center of the graphite mold; then keeping the vacuum degree of the vacuum skull furnace at 0.08Pa, smelting the ingot blank obtained in the step (5) by using 20000A current as an electrode, stopping power supply after the smelting voltage is controlled at 35V for 5 minutes, and starting an automatic pouring system for casting (alloy liquid obtained by smelting flows into a graphite mold through a pouring gate); after casting, keeping the vacuum degree in the furnace at 0.07Pa, cooling to room temperature along with the furnace, and discharging the furnace to obtain corresponding alloy cast ingots;
(7) Secondary vacuum consumable arc melting: performing secondary vacuum consumable arc melting by taking the alloy cast ingot obtained in the step (6) as an electrode, wherein the vacuum degree is kept to be less than or equal to 0.1Pa, the arcing voltage is 30V, the arcing current is 1500A, the arcing voltage is 35V, and the arcing current is 2000A in the melting process: and after the smelting is finished, continuously keeping the vacuum degree to be less than or equal to 0.1Pa, cooling to 300 ℃ along with the furnace, discharging, smelting at 1700 ℃ for 40min, and keeping the height of a molten pool to be 200mm.
Analytical detection
(1) Macroscopic defect analysis
FIG. 1 is a macroscopic photograph of a titanium-aluminum alloy prepared in example 1 of the present application, and it can be seen that the titanium-aluminum alloy prepared by the method of the present application has no defects such as shrinkage cavity, porosity and exfoliation.
In contrast, with reference to fig. 2, when a macroscopic photograph of the titanium-aluminum alloy prepared by the method of comparative example 1 is taken, it can be seen that defects such as shrinkage cavity, porosity, and flaking exist on the test piece.
(2) Microstructure of microstructure
FIG. 3 is a golden phase diagram of the titanium-aluminum alloy prepared in example 1, wherein the microstructure of the titanium-aluminum alloy prepared by the method of the application is equiaxed crystal, each grain branch is firmly lapped, no weak surface exists, and the overall mechanical property is excellent.
Fig. 4 is a golden phase diagram of the titanium-aluminum alloy prepared in comparative example 1, wherein the microstructure of the titanium-aluminum alloy prepared in the comparative example is columnar crystal, and the mechanical properties are directional, so that the disadvantages exist.
FIG. 5 is a photograph showing the microstructure of the titanium-aluminum alloy prepared in example 1, wherein the microstructure of the titanium-aluminum alloy prepared by the method of the present application is a layered structure. The mechanical property is better, and the subsequent processing is not easy to crack.
Fig. 6 is a photograph of a microstructure of the titanium-aluminum alloy prepared in comparative example 1, the microstructure of the titanium-aluminum alloy prepared by the method of comparative example 1 is a dendrite structure, and belongs to a brittle microstructure, and subsequent processing is easy to crack.
(3) XRD analysis
FIG. 7 shows XRD detection results of the titanium aluminum alloy prepared in example 1 and the titanium aluminum alloy prepared in comparative example 1, wherein the titanium aluminum alloy prepared by the method of the application has no diffraction peak of the brittle phase Ti3Al phase, namely the alloy has no diffraction peak of the brittle phase Ti3Al phase, and the titanium aluminum alloy prepared in comparative example 1 has diffraction peak of the brittle phase Ti3Al phase, which indicates that the alloy has the Ti3Al phase and is not easy to process.
(4) Analysis of mechanical Properties
The mechanical properties of the titanium-aluminum alloys prepared in example 1 and comparative example 1 were measured according to the GB/T2298-2002 standard method, and the measurement results are shown in Table 1. It can be seen that the mechanical properties of the titanium-aluminum alloy prepared by the method of the application are better than those of comparative example 1.
TABLE 1
(5) Analysis of conductivity
The titanium-aluminum alloys prepared in example 1 and comparative example 1 were subjected to conductivity test according to GB/T1410-2006 standard method, and the test results are shown in Table 2. It can be seen that the conductivity of the titanium-aluminum alloy prepared by the method of the present application is superior to that of comparative example 1.
TABLE 2
(6) Thermal conductivity of materials
The heat conduction performance of the titanium-aluminum alloys prepared in example 1 and comparative example 1 was measured according to the GB/T3561-2008 standard method, and the measurement results are shown in Table 3. It can be seen that the heat conductivity of the titanium-aluminum alloy prepared by the method of the present application is superior to that of comparative example 1. Each sample was tested 3 times at different sites.
TABLE 3 Table 3
According to the test results, the titanium-aluminum alloy prepared by the method has good comprehensive performance, is easy to process, and can be used for preparing titanium-aluminum alloy targets.
Claims (6)
1. The preparation method of the titanium-aluminum alloy is characterized by comprising the following steps of:
a first vacuum consumable arc melting step: fixing an electrode prepared from a titanium aluminum raw material in a vacuum consumable arc furnace for preliminary smelting to form a first blank;
In the first vacuum consumable arc melting step, the preliminary melting conditions include: the vacuum degree of the vacuum consumable arc furnace is less than or equal to 0.1Pa, the arc stabilizing voltage is 25-35V, the arc stabilizing current is 2500-4000A, the smelting temperature is 1750-1850 ℃, the smelting time is 20-40 minutes, the vacuum degree in the furnace is continuously kept less than or equal to 0.1Pa after the smelting is finished, and the furnace is cooled to below 300 ℃ along with the furnace and is discharged;
vacuum suspension smelting step: vacuum suspension smelting is carried out on the first blank to form a second blank;
In the vacuum suspension smelting step, the smelting temperature is 1800-2200 ℃, the smelting time is 25-60 minutes, the vacuum degree is less than or equal to 0.1Pa, and the power is 80-120 kilowatts;
a second vacuum consumable arc melting step: fixing the second blank serving as an electrode in a vacuum consumable arc furnace for vacuum consumable arc melting again to form a titanium-aluminum alloy;
In the second vacuum consumable arc melting step, the vacuum degree is less than or equal to 0.1 Pa, the arcing voltage is 20-40V, the arcing current is 2000-3000A, the arcing voltage is 35-45V, the arcing current is 2500-4000A, the melting temperature is 1550-1650 ℃, the melting time is 1-4 hours, the vacuum degree is continuously maintained to be 0.1-10 Pa after the melting is finished, and the furnace is cooled;
the titanium-aluminum alloy comprises the following components in percentage by atom: al: 30-50%, ti: 50-70%.
2. The method of claim 1, wherein in the first vacuum consumable arc melting step, the preliminary melting conditions further comprise: the arcing voltage is 20-30V, and the arcing current is 2000-3000A.
3. The method according to claim 1, wherein the vacuum suspension smelting step further comprises casting after smelting at a casting temperature of 2000-2500 ℃ and a casting speed of 8-12 kg/s, and the ingot is cooled to 300 ℃ or lower with the furnace and discharged.
4. The method of claim 1, wherein the electrode in the first vacuum consumable arc melting step is prepared by:
a batching step, namely respectively weighing raw materials titanium and aluminum according to the proportion of titanium and aluminum in the titanium-aluminum alloy;
And a material baking step, namely baking the titanium and aluminum which are subjected to the material preparation, wherein the baking conditions are as follows: baking at 140-200deg.C for 4-6 hr with vacuum degree of 500-5000Pa;
and an electrode pressing step, namely pressing the baked raw materials into an electrode.
5. A titanium-aluminum alloy prepared by the preparation method of any one of claims 1 to 4.
6. The use of the titanium-aluminum alloy of claim 5 as a target.
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