CN116287816B - High-uniformity aluminum-tantalum-tungsten-titanium intermediate alloy and preparation method and application thereof - Google Patents
High-uniformity aluminum-tantalum-tungsten-titanium intermediate alloy and preparation method and application thereof Download PDFInfo
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- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 140
- 239000000956 alloy Substances 0.000 title claims abstract description 140
- -1 aluminum-tantalum-tungsten-titanium Chemical compound 0.000 title claims abstract description 49
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 229910001069 Ti alloy Inorganic materials 0.000 claims abstract description 26
- 238000003723 Smelting Methods 0.000 claims abstract description 22
- 238000001914 filtration Methods 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 18
- 238000010791 quenching Methods 0.000 claims abstract description 13
- 230000000171 quenching effect Effects 0.000 claims abstract description 13
- 239000007788 liquid Substances 0.000 claims description 82
- BPUBBGLMJRNUCC-UHFFFAOYSA-N oxygen(2-);tantalum(5+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ta+5].[Ta+5] BPUBBGLMJRNUCC-UHFFFAOYSA-N 0.000 claims description 41
- PBCFLUZVCVVTBY-UHFFFAOYSA-N tantalum pentoxide Inorganic materials O=[Ta](=O)O[Ta](=O)=O PBCFLUZVCVVTBY-UHFFFAOYSA-N 0.000 claims description 41
- 229910052782 aluminium Inorganic materials 0.000 claims description 36
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 36
- 239000002893 slag Substances 0.000 claims description 31
- 239000010936 titanium Substances 0.000 claims description 28
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 27
- 229910052721 tungsten Inorganic materials 0.000 claims description 27
- 239000010937 tungsten Substances 0.000 claims description 27
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 26
- 239000000126 substance Substances 0.000 claims description 26
- 229910052719 titanium Inorganic materials 0.000 claims description 26
- 239000011261 inert gas Substances 0.000 claims description 17
- 238000007670 refining Methods 0.000 claims description 16
- 229910052715 tantalum Inorganic materials 0.000 claims description 16
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 claims description 16
- 238000001816 cooling Methods 0.000 claims description 14
- 238000002844 melting Methods 0.000 claims description 13
- 230000008018 melting Effects 0.000 claims description 13
- 238000009833 condensation Methods 0.000 claims description 11
- 230000005494 condensation Effects 0.000 claims description 11
- 238000009835 boiling Methods 0.000 claims description 9
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 7
- 239000000498 cooling water Substances 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 239000002994 raw material Substances 0.000 abstract description 11
- 239000012535 impurity Substances 0.000 abstract description 8
- 238000005204 segregation Methods 0.000 abstract description 6
- 238000000265 homogenisation Methods 0.000 abstract description 3
- 230000007547 defect Effects 0.000 abstract 1
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 10
- 229910052751 metal Inorganic materials 0.000 description 8
- 239000002184 metal Substances 0.000 description 8
- 239000000203 mixture Substances 0.000 description 8
- 238000007599 discharging Methods 0.000 description 6
- 229910052786 argon Inorganic materials 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 238000004458 analytical method Methods 0.000 description 4
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 4
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 4
- 239000000292 calcium oxide Substances 0.000 description 4
- 230000006698 induction Effects 0.000 description 4
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- JYJXGCDOQVBMQY-UHFFFAOYSA-N aluminum tungsten Chemical compound [Al].[W] JYJXGCDOQVBMQY-UHFFFAOYSA-N 0.000 description 2
- 229910002056 binary alloy Inorganic materials 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- AZCUJQOIQYJWQJ-UHFFFAOYSA-N oxygen(2-) titanium(4+) trihydrate Chemical compound [O-2].[O-2].[Ti+4].O.O.O AZCUJQOIQYJWQJ-UHFFFAOYSA-N 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 241001417490 Sillaginidae Species 0.000 description 1
- 241001062472 Stokellia anisodon Species 0.000 description 1
- 229910001080 W alloy Inorganic materials 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- LNGCCWNRTBPYAG-UHFFFAOYSA-N aluminum tantalum Chemical compound [Al].[Ta] LNGCCWNRTBPYAG-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 description 1
- 229910001634 calcium fluoride Inorganic materials 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 238000007667 floating Methods 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000010079 rubber tapping Methods 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
Classifications
-
- 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
- C22C1/03—Making non-ferrous alloys by melting using master alloys
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D13/00—Centrifugal casting; Casting by using centrifugal force
- B22D13/04—Centrifugal casting; Casting by using centrifugal force of shallow solid or hollow bodies, e.g. wheels or rings, in moulds rotating around their axis of symmetry
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D13/00—Centrifugal casting; Casting by using centrifugal force
- B22D13/10—Accessories for centrifugal casting apparatus, e.g. moulds, linings therefor, means for feeding molten metal, cleansing moulds, removing castings
- B22D13/101—Moulds
- B22D13/105—Cooling for moulds or cores
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D13/00—Centrifugal casting; Casting by using centrifugal force
- B22D13/10—Accessories for centrifugal casting apparatus, e.g. moulds, linings therefor, means for feeding molten metal, cleansing moulds, removing castings
- B22D13/107—Means for feeding molten metal
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D21/00—Casting non-ferrous metals or metallic compounds so far as their metallurgical properties are of importance for the casting procedure; Selection of compositions therefor
- B22D21/002—Castings of light metals
- B22D21/007—Castings of light metals with low melting point, e.g. Al 659 degrees C, Mg 650 degrees C
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D43/00—Mechanical cleaning, e.g. skimming of molten metals
- B22D43/001—Retaining slag during pouring molten metal
- B22D43/004—Retaining slag during pouring molten metal by using filtering means
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B34/00—Obtaining refractory metals
- C22B34/20—Obtaining niobium, tantalum or vanadium
- C22B34/24—Obtaining niobium or tantalum
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B5/00—General methods of reducing to metals
- C22B5/02—Dry methods smelting of sulfides or formation of mattes
- C22B5/04—Dry methods smelting of sulfides or formation of mattes by aluminium, other metals or silicon
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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
- C22C1/026—Alloys based on aluminium
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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
- C22C1/06—Making non-ferrous alloys with the use of special agents for refining or deoxidising
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C21/00—Alloys based on aluminium
- C22C21/003—Alloys based on aluminium containing at least 2.6% of one or more of the elements: tin, lead, antimony, bismuth, cadmium, and titanium
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention relates to the technical field of intermediate alloy, and provides a high-uniformity aluminum-tantalum-tungsten-titanium intermediate alloy, and a preparation method and application thereof. The aluminum-tantalum-tungsten-titanium intermediate alloy with uniform components and low impurity content is prepared by controlling the selection and feeding modes of raw materials and combining the filtering scum and the quenching process, and has high yield and low raw material cost; when the high-uniformity aluminum-tantalum-tungsten-titanium intermediate alloy is used as a raw material for smelting the titanium alloy, the homogenization of the titanium alloy components is facilitated, the metallurgical defects such as the segregation of the titanium alloy components can be effectively prevented, the element burning loss is reduced, and the quality of the titanium alloy is improved.
Description
Technical Field
The invention relates to the technical field of intermediate alloy, in particular to a high-uniformity aluminum-tantalum-tungsten-titanium intermediate alloy and a preparation method and application thereof.
Background
Titanium and its alloy have excellent properties such as high specific strength, corrosion resistance, high temperature resistance and good comprehensive technological properties, are becoming attractive materials in the field of modern industrial grade science and technology, and are widely applied in the fields of aerospace, aviation, petroleum, chemical industry, light industry, metallurgy, machinery, energy sources and the like.
The Ti650 alloy is a near alpha high temperature titanium alloy at 650 ℃, adopts a multi-element solid solution strengthening means, has good heat resistance and room temperature plasticity, can be used in a working environment at 650 ℃ for a long time, and is an ideal light high temperature material for aeroengines. At present, when Ti650 titanium alloy is prepared, aluminum tungsten and aluminum tantalum binary alloy are usually used as raw materials, but the titanium alloy obtained by a method of adding a plurality of binary alloys has poor product performance due to uneven distribution of elements in the titanium alloy, and the existing aluminum tungsten alloy has the problems of unstable quality, uneven alloy and the like due to high melting point and density of metal tungsten.
Therefore, how to solve the problem of uneven distribution of aluminum, tantalum and tungsten elements in titanium alloy is a technical problem to be solved by those skilled in the art.
Disclosure of Invention
In view of the above, the invention provides a high-uniformity aluminum-tantalum-tungsten-titanium intermediate alloy, and a preparation method and application thereof. The intermediate alloy of aluminum, tantalum, tungsten and titanium prepared by the preparation method has uniform components and no segregation, and the elements can be uniformly distributed in the titanium alloy when the intermediate alloy is used for preparing the Ti650 titanium alloy.
In order to achieve the above object, the present invention provides the following technical solutions:
A preparation method of a high-uniformity aluminum-tantalum-tungsten-titanium intermediate alloy comprises the following steps:
Mixing elemental aluminum, elemental tungsten and elemental titanium for smelting, adding tantalum pentoxide and a slag former into the obtained melt, enabling the tantalum pentoxide and the elemental aluminum to undergo exothermic reaction to enable alloy liquid to boil, draining the alloy liquid before boiling is finished, and filtering scum;
Quenching the alloy liquid after filtering the scum to obtain a high-uniformity aluminum-tantalum-tungsten-titanium intermediate alloy; the quenching method comprises the following steps: the alloy liquid after filtering the scum flows into a rotary condensing disc for condensation under the cooling of low-temperature inert gas; the temperature of the low-temperature inert gas is less than or equal to-20 ℃.
Preferably, the shapes of the elemental aluminum, the elemental tungsten and the elemental titanium are blocky; the shapes of the titanium pentoxide and the slag former are powdery; the purity of the simple substance aluminum, the simple substance tungsten, the simple substance titanium, the tantalum pentoxide and the slag former is more than 99.5 weight percent.
Preferably, the mass ratio of the simple substance aluminum to the tantalum pentoxide is (2.676-4.233) 1; the mass ratio of the simple substance tungsten to the tantalum pentoxide is (0.528-0.606): 1; the mass ratio of the simple substance titanium to the tantalum pentoxide is (1.110-1.189): 1; the mass ratio of the tantalum pentoxide to the slag former is 1:0.056-0.063.
Preferably, the smelting comprises sequentially melting and refining, and the power of the melting is 75-85 kW; the refining power is 95-105 kW.
Preferably, the liquid discharge is started for 40-50 seconds after tantalum pentoxide and slag former are added; the time for draining the liquid is 20-25 seconds.
Preferably, a liquid outlet is arranged at the bottom of the smelting device; the liquid outlet is connected with the chute; the upper part of the chute is provided with a plurality of alumina poking sheets; the alloy liquid is discharged from the liquid outlet and enters the chute, and scum is filtered under the action of the alumina plectrum.
Preferably, the material of the condensing disc is titanium alloy; the bottom of the condensing disc is provided with a water-cooling pipeline, and cooling water is continuously introduced into the water-cooling pipeline in the condensing process.
Preferably, the high-uniformity aluminum tantalum tungsten titanium intermediate alloy obtained after condensation on the condensation plate is flake-shaped, and the thickness is less than or equal to 5mm.
The invention also provides the high-uniformity aluminum-tantalum-tungsten-titanium intermediate alloy prepared by the preparation method, which comprises the following components in percentage by mass: 13.00 to 17.00 percent of tantalum, 8.00 to 12.00 percent of tungsten, 18.00 to 22.00 percent of titanium and the balance of aluminum.
The invention also provides application of the high-uniformity aluminum-tantalum-tungsten-titanium intermediate alloy in preparing titanium alloy.
The invention provides a preparation method of a high-uniformity aluminum-tantalum-tungsten-titanium intermediate alloy, which comprises the following steps: mixing elemental aluminum, elemental tungsten and elemental titanium for smelting, adding tantalum pentoxide and a slag former into the obtained melt, enabling the tantalum pentoxide and the elemental aluminum to undergo exothermic reaction to enable alloy liquid to boil, draining the alloy liquid before boiling is finished, and filtering scum; quenching the alloy liquid after filtering the scum to obtain a high-uniformity aluminum-tantalum-tungsten-titanium intermediate alloy; the quenching method comprises the following steps: the alloy liquid after filtering the scum flows into a rotary condensing disc for condensation under the cooling of low-temperature inert gas; the temperature of the low-temperature inert gas is less than or equal to-20 ℃. Tantalum is added together with a slag former in the form of tantalum pentoxide, the tantalum pentoxide reacts with aluminum to generate elemental tantalum which enters the alloy liquid and emits a large amount of heat to enable the alloy liquid to continuously boil, the alloy liquid is convenient to flow out, the uniformity of components in the alloy liquid is improved, and the slag is timely floated by the slag former when reacting; the tantalum simple substance is high in price, and the cost of raw materials can be reduced by adding the tantalum simple substance in the form of oxide; according to the invention, aluminum, tungsten and titanium elements are added in the form of simple substances, so that the generation of aluminum oxide slag is reduced, the phenomena of severe reaction explosion and the like caused by excessive oxides are avoided, the inclusion in the alloy is reduced, and the uniformity of the alloy is improved; in addition, the invention adopts a specific tapping cooling mode, and the alloy liquid is rapidly cooled into a flake shape on the rotary condensing disc by utilizing low-temperature argon, so that component deviation in the up-down direction caused by sinking of high-density metal and floating of low-density metal in the cooling process of the aluminum-tantalum-tungsten-titanium alloy is avoided, meanwhile, the aluminum-tantalum-tungsten-titanium alloy is prevented from being oxidized by oxygen in air in the cooling process, and the purity and uniformity of the aluminum-tantalum-tungsten-titanium intermediate alloy are greatly improved.
In summary, the aluminum-tantalum-tungsten-titanium intermediate alloy with uniform components and low impurity content is prepared by the selection of raw materials and the control of a feeding mode and the combination of filtering scum and a quenching process, and has the advantages of high yield and low raw material cost; when the high-uniformity aluminum-tantalum-tungsten-titanium intermediate alloy is used as a raw material to smelt the titanium alloy, the homogenization of the components of the titanium alloy is facilitated, the component segregation is prevented, the element burning loss is reduced, and the quality of the titanium alloy is improved.
Drawings
FIG. 1 is a schematic diagram of an apparatus for preparing a high-uniformity AlTaW-Ti intermediate alloy according to the present invention; wherein: 1-a smelting furnace, 2-a chute, 3-an alumina poking piece, 4-a condensing disc and 5-an inert gas pipe;
FIG. 2 is a schematic diagram of a sampling method for sampling an AlTaW master alloy according to an embodiment of the present invention.
Detailed Description
The invention provides a preparation method of a high-uniformity aluminum-tantalum-tungsten-titanium intermediate alloy, which comprises the following steps:
Mixing elemental aluminum, elemental tungsten and elemental titanium for smelting, adding tantalum pentoxide and a slag former into the obtained melt, enabling the tantalum pentoxide and the elemental aluminum to undergo exothermic reaction to enable alloy liquid to boil, draining the alloy liquid before boiling is finished, and filtering scum;
Quenching the alloy liquid after filtering the scum to obtain a high-uniformity aluminum-tantalum-tungsten-titanium intermediate alloy; the quenching method comprises the following steps: the alloy liquid after filtering the scum flows into a rotary condensing disc for condensation under the cooling of low-temperature inert gas; the temperature of the low-temperature inert gas is less than or equal to-20 ℃.
The raw materials adopted by the invention are all commercial products unless specified.
The invention mixes and smelts simple substance aluminum, simple substance tungsten and simple substance titanium, then adds tantalum pentoxide and slag former into melt, the tantalum pentoxide and simple substance aluminum produce exothermic reaction to boil alloy liquid, and drains liquid and filters scum before boiling is finished. In the invention, the purity of the simple substance aluminum, the simple substance tungsten, the simple substance titanium, the tantalum pentoxide and the slag former is preferably more than 99.5 weight percent; the shapes of the elemental aluminum, the elemental tungsten and the elemental titanium are preferably blocky; the shapes of the titanium pentoxide and the slag former are preferably powdery; the invention has no special requirement on the specific size of the block and the powder, and the block and the powder are well known to the person skilled in the art; the slag former is preferably one or two of calcium oxide and calcium fluoride; the mass ratio of the elemental aluminum to the tantalum pentoxide is preferably (2.676-4.233) to 1, more preferably (2.9-3.8) to 1, and even more preferably 3.34 to 1; the mass ratio of the elemental tungsten to the tantalum pentoxide is preferably (0.528-0.606): 1, more preferably (0.55-0.59): 1, and even more preferably 0.57:1; the mass ratio of the elemental titanium to the tantalum pentoxide is preferably (1.110-1.189): 1, more preferably (1.12-1.15): 1, and even more preferably 1.14:1; the mass ratio of the tantalum pentoxide to the slag former is preferably 1:0.056-0.063, more preferably 1:0.06.
In the present invention, the melting preferably includes melting and refining performed sequentially, and the melting and refining are preferably performed in an intermediate frequency induction furnace; the melting power is preferably 75-85 kW, more preferably 80kW, and the melting time is not particularly required, so that the metal simple substance is completely melted; the refining power is preferably 95-105 kW, more preferably 100kW; the refining temperature is preferably 1850-1890 ℃, more preferably 1860-1880 ℃; the refining time is preferably 5 to 9min, more preferably 6 to 8min; the invention can control the temperature to make the refining temperature slightly higher than the alloy melting point so as to achieve the refining purpose, and can make the metal melt more fully and more uniformly through refining, and has the effect of purifying and removing impurities.
After refining, adding tantalum pentoxide and a slag former into the refined alloy melt, wherein the tantalum pentoxide and the slag former are preferably added in the form of a mixture; the tantalum pentoxide and the elemental aluminum react in an exothermic manner to generate elemental tantalum, and a large amount of heat emitted simultaneously continuously boils the alloy liquid, so that the alloy liquid can flow out conveniently, the uniformity is improved, and the slag can float upwards in time by the slag former during the reaction. In the specific embodiment of the invention, the temperature for the reaction after adding tantalum pentoxide is 2750-2850 ℃, and the reaction time is 30-45 s.
Before boiling is finished, the invention discharges the alloy liquid and filters scum. In the invention, the time for starting the liquid discharge is preferably 40-50 seconds, more preferably 40-45 seconds after tantalum pentoxide and a slag forming agent are added, and after the time is exceeded, the slag on the upper layer of the alloy liquid starts to solidify, and the slag is not discharged along with the alloy liquid after solidification in the liquid discharge process; the time for the liquid discharge is preferably 20 to 25 seconds, more preferably 20 to 23 seconds, that is, the liquid discharge is stopped 20 to 25 seconds after the liquid discharge is started. In the invention, a liquid outlet is arranged at the bottom of the smelting device, and the smelting device is preferably a smelting furnace; the liquid outlet is connected with the chute; the upper part of the chute is provided with a plurality of aluminum oxide poking sheets, the number of the aluminum oxide poking sheets is preferably 3-7, and the aluminum oxide poking sheets are uniformly arranged on the chute; the alloy liquid is discharged from the liquid outlet and enters the chute, and scum is filtered under the action of the alumina plectrum.
After filtering the scum, the invention carries out quenching on the alloy liquid after filtering the scum to obtain the high-uniformity aluminum-tantalum-tungsten-titanium intermediate alloy; the quenching method comprises the following steps: the alloy liquid after filtering the scum flows into a rotary condensing disc for condensation under the cooling of low-temperature inert gas; the temperature of the low-temperature inert gas is less than or equal to-20 ℃. In the present invention, the inert gas is preferably argon; the temperature of the low-temperature inert gas is preferably-30 ℃ to-20 ℃; the material of the condensing disc is preferably titanium alloy; the bottom of the condensing disc is preferably provided with a water-cooling pipeline, and cooling water is preferably continuously introduced into the water-cooling pipeline in the condensing process; the temperature of the cooling water is preferably 5-25 ℃; in the specific embodiment of the invention, a condensing disc is preferably arranged below the outlet of the chute so as to facilitate alloy liquid to flow onto the condensing disc, and an inert gas pipe is arranged above the outlet of the chute and is used for introducing low-temperature inert gas to the surface of the alloy liquid flowing out of the chute; FIG. 1 is a schematic structural diagram of an apparatus for preparing a high uniformity AlTaW-Ti master alloy according to the present invention, wherein: 1 is a smelting furnace, 2 is a chute, 3 is an alumina poking piece, 4 is a condensing disc, and 5 is an inert gas pipe.
In the quenching process, the condensing disc continuously rotates, alloy liquid continuously flows out from the chute, low-temperature inert gas is continuously introduced into the surface of the flowing alloy liquid, and along with the rotation of the condensing disc, the alloy liquid is solidified into a ring shape on the condensing disc.
In the invention, the rotating speed of the condensing disc is preferably 2-3 r/min; the liquid discharge speed of the alloy liquid is preferably 0.8-1.3 kg/s; the high-uniformity aluminum-tantalum-tungsten-titanium intermediate alloy obtained after condensation on the condensation plate is in a flake shape, in particular an annular flake, and the thickness of the flake is less than or equal to 5mm, preferably 2-4 mm. The invention condenses the alloy liquid into a flake, the flake alloy has no segregation in the vertical direction, no loose material and high yield.
The invention also provides the high-uniformity aluminum tantalum tungsten titanium intermediate alloy prepared by the preparation method, and the aluminum tantalum tungsten titanium intermediate alloy preferably comprises the following components in percentage by mass: 13.00 to 17.00 percent of tantalum, 8.00 to 12.00 percent of tungsten, 18.00 to 22.00 percent of titanium and the balance of aluminum, preferably comprises 14.00 to 16.00 percent of tantalum, 9.00 to 11.00 percent of tungsten, 19.00 to 21.00 percent of titanium and the balance of aluminum, more preferably comprises 15.00 percent of tantalum, 10.00 percent of tungsten, 20.00 percent of titanium and the balance of aluminum.
In the invention, the high-uniformity aluminum-tantalum-tungsten-titanium master alloy also contains unavoidable impurities. In the invention, the impurity content of the aluminum-tantalum-tungsten-titanium intermediate alloy is preferably less than or equal to 0.2 percent in mass fraction. Since the purity of the raw material cannot be 100%, a small amount of unavoidable impurities exist in the aluminum tantalum tungsten titanium master alloy.
The high-uniformity aluminum-tantalum-tungsten-titanium intermediate alloy provided by the invention neutralizes the difference of melting points and density among elements, the density and melting point of the intermediate alloy are more similar to those of titanium alloy, the alloy components are uniform, the impurity content is low, and the high-uniformity aluminum-tantalum-tungsten-titanium intermediate alloy disclosed by the invention is used as a raw material for smelting the titanium alloy, so that the homogenization of the titanium alloy components is facilitated, the component segregation is prevented, the element burning loss is reduced, and the quality of the titanium alloy is improved.
The following description of the embodiments of the present invention will clearly and fully describe the technical solutions 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 invention without making any inventive effort, are intended to be within the scope of the invention.
Because of unavoidable differences in elemental content of different parts of the aluminum tantalum tungsten titanium master alloy, the elemental content of the aluminum tantalum tungsten titanium master alloy in each example is used as the best quality result to represent the alloy composition. The apparatus used in the examples is shown in FIG. 1.
Example 1
(1) 32.04Kg of elemental aluminum, 4.00kg of elemental tungsten and 9.00kg of elemental titanium are mixed and smelted; the smelting device is an intermediate frequency induction furnace, the smelting power is 75kW, the alloy is refined after being completely melted, the refining power is 95kW, and the alloy is refined for 5 minutes at 1850 ℃;
(2) After the metal is completely melted, adding a mixture of 7.57kg of tantalum pentoxide and 0.46kg of calcium oxide into the alloy liquid, and reacting the added tantalum pentoxide with aluminum to generate elemental tantalum which enters the alloy liquid and emits a large amount of heat to boil the alloy liquid;
(3) Discharging alloy liquid after boiling for 40 seconds, and stopping discharging after starting to discharge for 20 seconds;
(4) Filtering slag by using a chute after the alloy liquid flows into the chute;
(5) When the alloy liquid flows into a rotary condensing disc, argon at the temperature of minus 20 ℃ is utilized to cool the alloy into slices, and the high-uniformity aluminum-tantalum-tungsten-titanium intermediate alloy is obtained; the rotating speed of the condensing disc is 2r/min; the liquid discharge speed of the alloy liquid is 0.8kg/s, and the thickness of the obtained aluminum-tantalum-tungsten-titanium intermediate alloy sheet is 2mm.
Through the steps, 46.05kg of aluminum-tantalum-tungsten-titanium intermediate alloy is obtained, and the recovery rate is 92.10%.
Example 2
(1) 26.51Kg of elemental aluminum, 6.00kg of elemental tungsten and 11.00kg of elemental titanium are mixed and smelted; the smelting device is an intermediate frequency induction furnace, the smelting power is 85kW, the alloy is refined after being completely melted, the refining power is 105kW, and the alloy is refined for 9 minutes at 1890 ℃;
(2) After the metal is completely melted, adding a mixture of 9.90kg of tantalum pentoxide and 0.60kg of calcium oxide into the alloy liquid, and reacting the added tantalum pentoxide with aluminum to generate elemental tantalum which enters the alloy liquid and emits a large amount of heat to boil the alloy liquid;
(3) Discharging alloy liquid after boiling for 50 seconds, and stopping discharging after starting to discharge for 25 seconds;
(4) Filtering slag by using a chute after the alloy liquid flows into the chute;
(5) When the alloy liquid flows into a rotary condensing disc, argon at the temperature of minus 25 ℃ is utilized to cool the alloy into slices, and the high-uniformity aluminum-tantalum-tungsten-titanium intermediate alloy is obtained; the rotating speed of the condensing disc is 2.5r/min; the liquid discharge speed of the alloy liquid is 1.0kg/s, and the thickness of the obtained aluminum-tantalum-tungsten-titanium intermediate alloy sheet is 3.5mm.
Through the steps, 46.53kg of aluminum-tantalum-tungsten-titanium intermediate alloy is obtained, and the recovery rate is 93.06%.
Example 3
(1) 29.28Kg of elemental aluminum, 5.00kg of tungsten and 10.00kg of titanium are mixed for smelting; the smelting device is an intermediate frequency induction furnace, the smelting power is 80kW, the alloy is refined after being completely melted, the refining power is 100kW, and the alloy is refined for 7 minutes at 1870 ℃;
(2) After the metal is completely melted, adding a mixture of 8.74kg of tantalum pentoxide and 0.53kg of calcium oxide into the alloy liquid, and reacting the added tantalum pentoxide with aluminum to generate elemental tantalum which enters the alloy liquid and emits a large amount of heat to boil the alloy liquid;
(3) Discharging the alloy liquid after boiling for 45 seconds, and stopping discharging after starting to discharge for 23 seconds;
(4) Filtering slag by using a chute after the alloy liquid flows into the chute;
(5) When the alloy liquid flows into a rotary condensing disc, argon at the temperature of minus 25 ℃ is utilized to cool the alloy into slices, and the high-uniformity aluminum-tantalum-tungsten-titanium intermediate alloy is obtained; the rotating speed of the condensing disc is 3r/min; the liquid discharge speed of the alloy liquid is 1.2kg/s, and the thickness of the obtained aluminum-tantalum-tungsten-titanium intermediate alloy sheet is 5mm.
Through the steps, 46.30kg of aluminum-tantalum-tungsten-titanium intermediate alloy is obtained, and the recovery rate is 92.60%.
Performance detection
The aluminum tantalum tungsten titanium intermediate alloys prepared in examples 1 to3 were sampled in the manner shown in fig. 2, and each point was taken from four directions of the condensing plate, two circles of alloy were flowed out in each example of the present invention (the first circle of alloy was collected after the condensing plate was solidified into a circle, and the next circle of alloy was cooled on the condensing plate), 8 points were taken in each example in total, and the analysis results for each point were shown in tables 1 to 3.
TABLE 1 example 1 analysis of chemical composition of AlTaWTiintermediate alloy ingot
TABLE 2 example 2 analysis results of chemical composition of AlTaWTiintermediate alloy ingot
TABLE 3 example 3 analysis of chemical composition of AlTaWTiW intermediate alloy ingot
As can be seen from tables 1 to 3, the aluminum-tantalum-tungsten-titanium intermediate alloys prepared in examples 1 to 3 of the invention have high purity, uniform and stable components, smaller segregation and lower impurity content, and can better meet the production requirements of titanium alloys.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (9)
1. The preparation method of the high-uniformity aluminum-tantalum-tungsten-titanium intermediate alloy is characterized by comprising the following steps of:
Mixing elemental aluminum, elemental tungsten and elemental titanium for smelting, adding tantalum pentoxide and a slag former into the obtained melt, enabling the tantalum pentoxide and the elemental aluminum to undergo exothermic reaction to enable alloy liquid to boil, draining the alloy liquid before boiling is finished, and filtering scum;
Quenching the alloy liquid after filtering the scum to obtain a high-uniformity aluminum-tantalum-tungsten-titanium intermediate alloy; the quenching method comprises the following steps: the alloy liquid after filtering the scum flows into a rotary condensing disc for condensation under the cooling of low-temperature inert gas; the temperature of the low-temperature inert gas is less than or equal to-20 ℃; the condensing disc is made of titanium alloy; the bottom of the condensing disc is provided with a water-cooling pipeline, and cooling water is continuously introduced into the water-cooling pipeline in the condensing process;
the high-uniformity aluminum-tantalum-tungsten-titanium intermediate alloy comprises the following components in percentage by mass: 13.00-17.00% of tantalum, 8.00-12.00% of tungsten, 18.00-22.00% of titanium and the balance of aluminum.
2. The method according to claim 1, wherein the elemental aluminum, elemental tungsten, and elemental titanium are in the shape of a block; the tantalum pentoxide and the slag former are in powder shapes; the purity of the simple substance aluminum, the simple substance tungsten, the simple substance titanium, the tantalum pentoxide and the slag former is more than 99.5 weight percent.
3. The preparation method according to claim 1, wherein the mass ratio of the elemental aluminum to tantalum pentoxide is (2.676-4.233): 1; the mass ratio of the simple substance tungsten to the tantalum pentoxide is (0.528-0.606): 1; the mass ratio of the simple substance titanium to the tantalum pentoxide is (1.110-1.189): 1; the mass ratio of the tantalum pentoxide to the slag former is 1:0.056-0.063.
4. The preparation method according to claim 1, wherein the smelting comprises sequentially melting and refining, and the power of the melting is 75-85 kw; the refining power is 95-105 kW.
5. The method according to claim 1, wherein the liquid discharge is started for 40 to 50 seconds after adding tantalum pentoxide and a slag former; the liquid draining time is 20-25 seconds.
6. The production method according to claim 1 or 4, wherein a drain port is provided at the bottom of the smelting apparatus; the liquid outlet is connected with the chute; the upper part of the chute is provided with a plurality of alumina poking sheets; the alloy liquid is discharged from the liquid outlet and enters the chute, and scum is filtered under the action of the alumina plectrum.
7. The preparation method according to claim 1, wherein the high-uniformity aluminum-tantalum-tungsten-titanium master alloy obtained after condensation on the condensation plate is flake-shaped and has a thickness of 5mm or less.
8. The high-uniformity aluminum-tantalum-tungsten-titanium intermediate alloy prepared by the preparation method of any one of claims 1-7 is characterized by comprising the following components in percentage by mass: 13.00-17.00% of tantalum, 8.00-12.00% of tungsten, 18.00-22.00% of titanium and the balance of aluminum.
9. The use of the high uniformity aluminum tantalum tungsten titanium master alloy of claim 8 in the preparation of titanium alloys.
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