CN116287826A - Production method of aluminum-tungsten alloy - Google Patents
Production method of aluminum-tungsten alloy Download PDFInfo
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- CN116287826A CN116287826A CN202310301622.7A CN202310301622A CN116287826A CN 116287826 A CN116287826 A CN 116287826A CN 202310301622 A CN202310301622 A CN 202310301622A CN 116287826 A CN116287826 A CN 116287826A
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- 229910001080 W alloy Inorganic materials 0.000 title claims abstract description 124
- JYJXGCDOQVBMQY-UHFFFAOYSA-N aluminum tungsten Chemical compound [Al].[W] JYJXGCDOQVBMQY-UHFFFAOYSA-N 0.000 title claims abstract description 124
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 20
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 52
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 41
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 38
- 239000010937 tungsten Substances 0.000 claims abstract description 37
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 23
- 238000005245 sintering Methods 0.000 claims abstract description 22
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910052802 copper Inorganic materials 0.000 claims abstract description 16
- 239000010949 copper Substances 0.000 claims abstract description 16
- 230000008569 process Effects 0.000 claims abstract description 16
- 238000003723 Smelting Methods 0.000 claims abstract description 15
- 238000005266 casting Methods 0.000 claims abstract description 14
- 235000010627 Phaseolus vulgaris Nutrition 0.000 claims abstract description 11
- 244000046052 Phaseolus vulgaris Species 0.000 claims abstract description 11
- 238000002156 mixing Methods 0.000 claims abstract description 11
- 235000021251 pulses Nutrition 0.000 claims abstract description 10
- 238000003466 welding Methods 0.000 claims abstract description 8
- 238000007599 discharging Methods 0.000 claims abstract description 7
- 230000003068 static effect Effects 0.000 claims abstract description 6
- 229910045601 alloy Inorganic materials 0.000 claims description 52
- 239000000956 alloy Substances 0.000 claims description 52
- 238000001816 cooling Methods 0.000 claims description 21
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 14
- 238000002490 spark plasma sintering Methods 0.000 claims description 9
- 229910052786 argon Inorganic materials 0.000 claims description 7
- 229910052593 corundum Inorganic materials 0.000 claims description 7
- 239000010431 corundum Substances 0.000 claims description 7
- 239000007789 gas Substances 0.000 claims description 7
- 238000003825 pressing Methods 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 5
- 239000011261 inert gas Substances 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 239000000498 cooling water Substances 0.000 claims description 3
- 238000005520 cutting process Methods 0.000 claims description 3
- 238000009740 moulding (composite fabrication) Methods 0.000 claims description 3
- 238000009489 vacuum treatment Methods 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims 2
- 229910052751 metal Inorganic materials 0.000 abstract description 20
- 239000002184 metal Substances 0.000 abstract description 20
- 238000005204 segregation Methods 0.000 abstract description 13
- 229910001069 Ti alloy Inorganic materials 0.000 abstract description 4
- 238000002844 melting Methods 0.000 abstract description 4
- 230000008018 melting Effects 0.000 abstract description 4
- 230000007547 defect Effects 0.000 abstract description 2
- 238000005272 metallurgy Methods 0.000 abstract description 2
- 239000013078 crystal Substances 0.000 description 12
- 229910000765 intermetallic Inorganic materials 0.000 description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- 239000012535 impurity Substances 0.000 description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 238000005275 alloying Methods 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 230000005484 gravity Effects 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000000654 additive Substances 0.000 description 2
- 238000007133 aluminothermic reaction Methods 0.000 description 2
- 238000000498 ball milling Methods 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 238000005551 mechanical alloying Methods 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000005056 compaction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 238000003886 thermite process Methods 0.000 description 1
- 229910001930 tungsten oxide Inorganic materials 0.000 description 1
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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
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/0408—Light metal alloys
- C22C1/0416—Aluminium-based alloys
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D7/00—Casting ingots, e.g. from ferrous metals
- B22D7/005—Casting ingots, e.g. from ferrous metals from non-ferrous metals
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
- B22F2003/1051—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding by electric discharge
-
- 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
- Y02P10/00—Technologies related to metal processing
- Y02P10/25—Process efficiency
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- Metallurgy (AREA)
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- Optics & Photonics (AREA)
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Abstract
The invention relates to the technical field of metallurgy, in particular to a production method of aluminum-tungsten alloy. The aluminum tungsten alloy provided by the invention comprises the following components: 40-68wt%, al: the balance of less than or equal to 0.03wt% of O, less than or equal to 0.04wt% of C, less than or equal to 0.05wt% of N and less than 0.1wt% of Si. The process comprises the following steps: (1) Mixing superfine tungsten powder and superfine aluminum powder according to a certain proportion, loading into a strip-shaped die, pressurizing, pulse discharging and static pressure sintering to obtain the strip-shaped aluminum-tungsten alloy. (2) Welding aluminum-tungsten alloy strips into a frame, and putting the frame into a water-cooled copper crucible. (3) Smelting a metal tungsten block and aluminum beans in an intermediate frequency furnace according to the content ratio of aluminum and tungsten in the aluminum-tungsten alloy strip, and casting the molten metal tungsten block and the aluminum beans into a water-cooled copper crucible provided with an aluminum-tungsten alloy frame to obtain aluminum-tungsten alloy ingots with uniform components. The invention solves the defects of serious segregation and low yield of cast ingots caused by large difference of metal melting points and densities of aluminum-tungsten alloys for titanium alloys, and prepares the aluminum-tungsten alloy with high yield and high uniformity.
Description
Technical Field
The invention relates to the technical field of metallurgy, in particular to a production method of aluminum-tungsten alloy.
Background
Among metals, tungsten has the highest melting point, high-temperature strength and creep resistance, and good heat conduction, electric conduction and electron emission properties, and has a large specific gravity, and is widely used for manufacturing hard alloy and titanium alloy additives. The aluminum-tungsten alloy is used as an excellent titanium alloy additive, has the advantages of light weight, good ductility and oxidation resistance of aluminum, and also has the high temperature resistance of tungsten; after aluminum and tungsten alloying, the aluminum-tungsten alloy has the advantages of high microhardness, good stability, high temperature resistance, low density and high wear resistance. The aluminum-tungsten alloy can be applied to golf clubs, medical equipment, automobile hubs, engine pistons, space engines and the like.
The main preparation method of the current aluminum-tungsten alloy comprises the following steps: mechanical alloying (ball milling) synthesizes aluminum-tungsten alloy powder, but the mechanical alloying is influenced by ball milling strength, ball mixing proportion, environment, atmosphere, time and temperature, has great influence on impurity alloy of alloy, such as iron (iron ball), oxygen, nitrogen and the like, and aluminum-tungsten alloy impurity element iron is produced by the American reading alloy company: 0.6wt%, oxygen: 0.2wt%, nitrogen: the high impurity content of 0.06wt% limits the application of the aluminum-tungsten alloy in the high-end field. Thermite process: tungsten oxide is processed,The aluminum source and the slag former are mixed according to a certain proportion, and are ignited by magnesium strips to generate aluminothermic reduction reaction to obtain an aluminum-tungsten alloy ingot, but because the density difference of the aluminum and tungsten is larger (aluminum: 2.7 g/cm) 3 Tungsten: 19.35g/cm 3 ) The aluminothermic reaction alloy ingot has serious segregation up and down, the yield is 35-60%, the control is not easy, and the loss is serious. Smelting method: the metal tungsten and the aluminum block are mixed according to a proportion and are smelted in a smelting furnace to directly prepare the aluminum-tungsten alloy, but the single tungsten has high melting point, the smelting process is slow (6-8 h), excessive aluminum is added, and the problems of content segregation, upper and lower layering and the like can also occur in the cooling process of an ingot mould after pouring. Therefore, there is currently no process for preparing high quality aluminum tungsten alloys. Spark plasma sintering is described in patent CN114559040a, where pure W, pure Cr and pure Al powders are ball milled and then spark plasma sintering is performed, but this method requires higher purity for the powdery raw material, and high uniformity requires that the raw material is ultrafine powder, which limits the use of the product due to cost problems in the industrialization process.
Disclosure of Invention
In view of this, the present disclosure provides a method for producing an aluminum-tungsten alloy.
The invention uses superfine tungsten powder and aluminum powder to mix uniformly according to proportion, then sinters into aluminum tungsten alloy strips in a discharge plasma sintering furnace, further welds the aluminum tungsten alloy strips into aluminum tungsten alloy frames, and uses the metal frames to be placed in a water-cooled copper crucible for casting in an intermediate frequency furnace, and then casts molten metal tungsten and aluminum beans into the water-cooled copper crucible containing the aluminum tungsten alloy frames, and uses the metal frames as seed crystals, thereby improving the growth of alloy solution along the direction of intermetallic compounds in the cooling process, reducing segregation caused by density difference, greatly improving the yield and the yield of aluminum tungsten alloy while ensuring high purity and low impurity of the aluminum tungsten alloy, solving the industrial problem and providing a possibility for popularization of the aluminum tungsten alloy with low cost and high quality.
In order to achieve the above object, the present invention provides the following technical solutions:
the production method of the aluminum-tungsten alloy comprises the following steps:
(1) Preparing an aluminum-tungsten alloy strip: fully mixing tungsten powder and aluminum powder according to a proportion, adding the mixture into a strip corundum mould, placing the mould into a discharge plasma sintering furnace, vacuumizing, pressurizing and compacting the mixture, adding pulse current, performing static pressure sintering and forming, and cooling to room temperature to obtain an aluminum-tungsten alloy strip;
(2) Preparing an aluminum-tungsten alloy frame: cutting the aluminum-tungsten alloy strip, welding the aluminum-tungsten alloy strip into an aluminum-tungsten alloy frame under the protection of tungsten electrode inert gas under the protection of argon, and placing the top of the aluminum-tungsten alloy frame into a casting water-cooled copper crucible of an intermediate frequency furnace for standby;
(3) Preparing an aluminum-tungsten alloy ingot: and (3) mixing materials according to the aluminum and tungsten contents in the aluminum-tungsten alloy strips, loading tungsten blocks and aluminum beans into an intermediate frequency furnace, smelting, casting into a water-cooled copper crucible with an aluminum-tungsten alloy frame, and cooling to obtain the high-uniformity aluminum-tungsten alloy.
In the aluminum tungsten alloy of the present invention, W:40-68wt% of Al in the aluminum-tungsten alloy 4 W、Al 5 In the step (2), aluminum-tungsten alloy frames with different contents are customized according to the requirements of preparing aluminum-tungsten alloy with different contents and the thickness of the alloy frames is reasonably adjusted according to the change of the overall density of the alloy due to the change of the tungsten content. In high content aluminum tungsten alloy, al is used as 4 W is mainly due to Al 4 W Jibuss function is higher than Al 5 W is thermodynamically more stable than Al 5 W is poor and is easily decomposed into Al 5 W and W macroscopically represent severe segregation of the alloy. Similarly, when W is less than 40wt%, the main phase is Al 12 W, also has a stability greater than Al 5 W. Therefore, if the aluminum-tungsten alloy with the tungsten content of 40-60wt% is to be stably produced, a large amount of intermetallic compounds with the required production grade are required to be provided as seed crystals in the cooling process of the alloy solution, a metal frame is used as seed crystals, the intermetallic compound seed crystals can be provided for the alloy, aluminum and tungsten in the alloy solution are grown along the crystal face direction of the intermetallic compound in the metal frame, and the metal frame is used as an aluminum-tungsten alloy growth matrix, so that the high-purity aluminum-tungsten alloy frame is prepared by an SPS sintering method. Meanwhile, the addition of the alloy frame can improve the cooling speed of the alloy after casting to a certain extentDegree, segregation is reduced.
In addition, the alloy frame is mixed according to the metal proportion of the alloy frame, smelted in a medium frequency furnace, cast into a water-cooled copper crucible with the alloy frame, cast into the copper crucible after high-power solution clearing, cooled by low-temperature condensate water of-10 to 5 ℃, and the like, thereby playing the roles of fast solidification, reducing the overlong solution time of the alloy, decomposing intermetallic compounds and generating macroscopic phenomena of segregation.
Optionally, the mass ratio of the tungsten powder to the aluminum powder is (0.82-2.1): 1, the granularity of the aluminum powder is less than or equal to 3 mu m, and the granularity of the tungsten powder is less than or equal to 1.5 mu m.
Further, the length, width and height specifications of the strip corundum mould are 30cm (0.4 cm-0.8 cm), and after the mixed alloy powder is filled, the pressing pressure is 10-25MPa; and the vacuum treatment is carried out in the discharge plasma sintering furnace, and the vacuum degree is less than 10Pa.
Further, in the discharging process, the pulse current is 600-900A, the pulse discharging time is 45ms, the discharging is performed once at intervals of 1.5s, and the duration is 60-120s;
and the temperature-raising program of the spark plasma sintering furnace is room temperature- (1000-1500 ℃), the temperature-raising speed is 150-220 ℃/min, the heat-preserving time is 5-20min, the pressing pressure in the heat-preserving process is 35-45MPa, and the cooling speed is 250-300 ℃/min after the pressure is withdrawn.
Optionally, in the step (2), the shielding gas used for welding the aluminum-tungsten alloy frame is argon, and the purity is more than or equal to 99%; and the specification of the aluminum-tungsten alloy frame top alloy strip is 30cm 0.8cm.
Further, the square side length a in the horizontal direction of the aluminum-tungsten alloy frame is as follows: 20-30cm, and the vertical height is c:5-15cm, the side length b of the square bottom surface of the small cuboid is 2.5-10cm, and the height is 2.5-15cm;
and the diameter of the intermediate frequency furnace casting water-cooled copper crucible is 26-45cm.
Optionally, in the step (3), the weight ratio of the intermediate frequency furnace material-mixing tungsten block to the aluminum beans is (0.82-2.1): 1; and the vacuum degree is less than 20Pa before smelting in the intermediate frequency furnace, and the smelting power is 140-170kW.
Further, the water inlet temperature of the cooling water of the intermediate frequency furnace is-10-5 ℃, and the weight of the prepared aluminum-tungsten alloy ingot is 50-90kg.
Compared with the prior art, the invention discloses a production method of aluminum-tungsten alloy, which has the following excellent effects:
the invention solves the defects of serious segregation and low yield of cast ingots caused by large difference of metal melting points and densities of aluminum-tungsten alloys for titanium alloys, and prepares the aluminum-tungsten alloy with high yield and high uniformity.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are required to be used in the embodiments or the description of the prior art will be briefly described below, and it is obvious that the drawings in the following description are only embodiments of the present invention, and that other drawings can be obtained according to the provided drawings without inventive effort for a person skilled in the art.
Fig. 1 is a structural view of an aluminum tungsten alloy frame.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but 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.
The invention provides a production method of aluminum-tungsten alloy, which comprises the following steps:
(1) Preparing an aluminum-tungsten alloy strip: fully mixing tungsten powder and aluminum powder according to a proportion, adding the mixture into a strip corundum mould, placing the mould into a discharge plasma sintering furnace, vacuumizing, pressurizing and compacting the mixture, adding pulse current, performing static pressure sintering and forming, and cooling to room temperature to obtain an aluminum-tungsten alloy strip;
(2) Preparing an aluminum-tungsten alloy frame: cutting the aluminum-tungsten alloy strip, welding the aluminum-tungsten alloy strip into an aluminum-tungsten alloy frame under the protection of tungsten electrode inert gas under the protection of argon, and placing the top of the aluminum-tungsten alloy frame into a casting water-cooled copper crucible of an intermediate frequency furnace for standby;
(3) Preparing an aluminum-tungsten alloy ingot: and (3) mixing materials according to the aluminum and tungsten contents in the aluminum-tungsten alloy strips, loading tungsten blocks and aluminum beans into an intermediate frequency furnace, smelting, casting into a water-cooled copper crucible with an aluminum-tungsten alloy frame, and cooling to obtain the high-uniformity aluminum-tungsten alloy.
According to the invention, the W is obtained after spark plasma sintering by controlling the proportion of tungsten powder to aluminum powder: 40-68wt% of aluminum-tungsten alloy strips, and controlling the granularity of tungsten powder and aluminum powder to ensure that the tungsten powder and the aluminum powder are fully and uniformly mixed so as to ensure the uniformity of the aluminum-tungsten alloy strips; the specification of the aluminum-tungsten alloy strip is controlled to be 30cm (0.4 cm-0.8 cm) and 0.4cm-0.8cm, so that seed crystals of the aluminum-tungsten alloy with different contents are sufficient in the pouring process; the pressing pressure is controlled to be 10-25MPa, after preliminary compaction, a vacuum pump is started to vacuumize the discharge plasma sintering furnace to be below 10Pa, so that the aluminum-tungsten alloy strip is ensured not to introduce gas impurities in the sintering process.
The discharge plasma sintering furnace has the pulse current range of 600-900A at certain discharge time and interval for 60-120s, ensures alloying of aluminum-tungsten alloys with different contents and does not generate segregation; the temperature-raising program of the spark plasma sintering furnace is room temperature- (1000-1500 ℃), the temperature-raising rate is 150-220 ℃/min, the heat-preserving time is 5-20min, the alloy of aluminum tungsten (40-68 wt%) is guaranteed to be fully melted and alloyed, the pressing pressure in the heat-preserving process is 35-45MPa, after the pressure is withdrawn, the cooling rate is 250-300 ℃/min, and the rapid cooling ensures that a large amount of crystal seeds (Al) exist in the aluminum alloy strip 4 W、Al 5 W), providing seed crystal for the aluminum-tungsten alloy melt in the casting process.
According to the invention, the aluminum-tungsten alloy strip is cut, and the tungsten electrode inert gas with the purity of more than 99% is welded into the aluminum-tungsten alloy frame under the protection of argon gas, so that gas impurities are prevented from being introduced into the aluminum-tungsten alloy frame in the welding process, the metal strip at the upper part of the alloy frame is 30cm 0.8cm, the upper part of the alloy frame is prevented from being melted in the casting process of alloy melt, and seed crystals cannot be provided for the alloy melt; alloy rack a:20-30cm, and the vertical height is c:5-15cm, the square side length b of the bottom surface of the small cuboid is 2.5-10cm, the height d is 2.5-15cm, and Al is added along with the increase of tungsten content in the aluminum-tungsten alloy 4 The proportion of W is increased, the segregation degree of tungsten in the alloy is increased, the height of the metal frame needs to be reduced, and the weight of the metal frame is increased to liftHigh seed specific gravity and reduced segregation.
In the aluminum tungsten alloy of the invention, W:40-68wt% of aluminum-tungsten alloy main phase Al 4 W、Al 5 W is two intermetallic compounds, and the thickness of the alloy frame is reasonably adjusted according to the requirements of preparing tungsten alloy aluminum tungsten alloys with different contents. In the aluminum-tungsten alloy with high tungsten content, the main phase is Al 4 W due to Al 4 W Jibuss function is higher than Al 5 W, stability is higher than Al 5 W is poor and is easily decomposed into Al 5 W and W macroscopically represent severe segregation of the alloy. Similarly, when W is less than 40wt%, the main phase is Al 12 W, also has a stability greater than Al 5 W. Therefore, if the aluminum-tungsten alloy with the tungsten content of 40-60wt% is to be stably produced, a large amount of intermetallic compounds with the required production grade are required to be provided as seed crystals in the cooling process of alloy solution, the alloying degree of the metal frame is high by adopting an SPS sintering method, the seed crystals caused by rapid cooling are more, the crystallinity is low, and the seed crystals are easier to be provided for the alloy melt after casting.
The metal frame is used as an aluminum-tungsten alloy growth matrix, so that the SPS sintering method is used for preparing the high-purity aluminum-tungsten alloy frame. Meanwhile, the addition of the alloy frame can improve the cooling speed of the alloy after casting to a certain extent and reduce segregation.
Preparing an aluminum-tungsten alloy ingot: 1 is filled into an intermediate frequency furnace according to the weight ratio of tungsten blocks and aluminum beans in the aluminum-tungsten alloy strip of (0.82-2.1), the content of aluminum-tungsten alloy is ensured to be consistent with that of an aluminum-tungsten alloy metal frame, the vacuum degree of the intermediate frequency furnace is controlled to be less than 20Pa, the purity of the alloy is ensured, the smelting power is controlled to be 140-170kW, the alloy is ensured to be normally melted, the alloy is cast into a water-cooled copper crucible provided with the aluminum-tungsten alloy frame after smelting, and the aluminum-tungsten alloy with high uniformity is obtained after cooling.
The technical solutions of the present invention will be clearly and completely described in the following in connection with the embodiments of the present invention. It will be apparent that the described embodiments are only some, but not all, embodiments of the invention. 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.
Example 1
The production method of the aluminum-tungsten alloy specifically comprises the following steps:
mixing 36.5kg tungsten powder and 33.6kg aluminum powder (granularity: 0.1-1.5 μm) uniformly in a mixer, adding a corundum mould, starting a Roots pump, vacuumizing a discharge plasma sintering furnace, applying pressure to the materials in the corundum mould to 15Mpa when the vacuum degree is 8Pa, compacting the mixed materials, maintaining the pressure, applying pulse current, setting the current to 800A and the discharge interval to 1.5s s, continuing the temperature-raising procedure of the discharge plasma sintering furnace to room temperature to 1200 ℃, setting the temperature-raising rate to 180 ℃/min, setting the heat-preserving time to 15min, setting the static pressure sintering pressure to 40Mpa, setting the cooling rate to 300 ℃/min, and cooling to room temperature to obtain the aluminum-tungsten alloy strips.
And (3) taking 99.5% of argon as shielding gas, and welding the alloy strips into a 30cm, b 6cm, c 10cm, d 2.5cm, wherein the height and width of the top alloy strip are 0.8cm, and the height and width of the rest metal strips are 0.5cm.
41.4kg of tungsten blocks and 38.5kg of aluminum beans are put into an intermediate frequency furnace, a Roots pump is opened to vacuum the alloy to be dissolved and clear under 15Pa and 150kW, the alloy is cast into a water-cooled copper crucible with an aluminum-tungsten alloy frame, the water inlet temperature is 0-3 ℃, and 81.4kg of alloy ingots are obtained after cooling.
The alloy ingot is sampled and detected at the same point, at the middle and at the lower part, and the data are shown in the following table 1:
TABLE 1 aluminum tungsten alloy data summary table
The observation table 1 shows that the tungsten content in the alloy is extremely poor and is only 0.41 weight percent, the oxygen content is lower than 0.03 weight percent, and compared with the conventional aluminum tungsten alloy prepared by the aluminothermic reaction, the uniformity and the purity are greatly improved.
Example 2
Compared with the embodiment 1, only the tungsten powder and the aluminum powder are required to be changed into 36.5kg of tungsten powder and 19.6kg of aluminum powder.
Changing the discharge current into 700A in a discharge plasma sintering furnace, wherein the discharge interval is 1.5s, the continuous discharge time is 80s, the sintering process is room temperature to 1250 ℃, the heat preservation time is 10min, and the static pressure sintering pressure is 40Mpa;
the alloy strips are welded into a 30cm, b 5cm, c 10cm and d 2.5cm, the height and width of all the alloy strips are 0.8cm, and the alloy strips are transferred to a copper crucible with the diameter of an intermediate frequency furnace.
The intermediate frequency furnace is provided with 43kg of tungsten blocks, 23.5kg of aluminum beans, the smelting power is 165kW, the cooling water inlet temperature is-8 to-4 ℃, and 72.9kg of alloy ingots are obtained after smelting.
Gold ingot co-site up, middle and down sampling detection, data as in table 2 below:
TABLE 2 aluminum tungsten alloy data summary table
The observation of Table 2 shows that the alloy with high tungsten specific gravity has extremely poor tungsten content of only 0.32wt%, and the uniformity and purity of the alloy are at the same level with those of the alloy with low tungsten content, thus proving the superiority of the invention.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (8)
1. The production method of the aluminum-tungsten alloy is characterized by comprising the following steps of:
(1) Preparing an aluminum-tungsten alloy strip: fully mixing tungsten powder and aluminum powder according to a proportion, adding the mixture into a strip corundum mould, placing the mould into a discharge plasma sintering furnace, vacuumizing, pressurizing and compacting the mixture, adding pulse current, performing static pressure sintering and forming, and cooling to room temperature to obtain an aluminum-tungsten alloy strip;
(2) Preparing an aluminum-tungsten alloy frame: cutting the aluminum-tungsten alloy strip, welding the aluminum-tungsten alloy strip into an aluminum-tungsten alloy frame under the protection of tungsten electrode inert gas under the protection of argon, and placing the top of the aluminum-tungsten alloy frame into a casting water-cooled copper crucible of an intermediate frequency furnace for standby;
(3) Preparing an aluminum-tungsten alloy ingot: and (3) mixing materials according to the aluminum and tungsten contents in the aluminum-tungsten alloy strips, loading tungsten blocks and aluminum beans into an intermediate frequency furnace, smelting, casting into a water-cooled copper crucible with an aluminum-tungsten alloy frame, and cooling to obtain the high-uniformity aluminum-tungsten alloy.
2. The method of producing an aluminum-tungsten alloy according to claim 1, wherein the mass ratio of the tungsten powder to the aluminum powder is (0.82-2.1): 1, the particle size of the aluminum powder is not more than 3 μm, and the particle size of the tungsten powder is not more than 1.5 μm.
3. The method for producing aluminum-tungsten alloy according to claim 1 or 2, wherein the length, width and height specifications of the strip-shaped corundum mold are 30cm (0.4 cm-0.8 cm), and the pressing pressure is 10-25MPa after the mixed alloy powder is filled; and the vacuum treatment is carried out in the discharge plasma sintering furnace, and the vacuum degree is less than 10Pa.
4. The method for producing aluminum-tungsten alloy according to claim 3, wherein in the discharging process, the pulse current is 600-900A, the pulse discharging time is 45ms, the discharging is performed once at intervals of 1.5s, and the duration is 60-120s;
and the temperature-raising program of the spark plasma sintering furnace is room temperature- (1000-1500 ℃), the temperature-raising speed is 150-220 ℃/min, the heat-preserving time is 5-20min, the pressing pressure in the heat-preserving process is 35-45MPa, and the cooling speed is 250-300 ℃/min after the pressure is withdrawn.
5. The method for producing aluminum-tungsten alloy according to claim 1, wherein in the step (2), the shielding gas for welding the aluminum-tungsten alloy frame is argon gas, and the purity is more than or equal to 99%; and the specification of the aluminum-tungsten alloy frame top alloy strip is 30cm 0.8cm.
6. The method for producing aluminum-tungsten alloy according to claim 5, wherein the aluminum-tungsten alloy frame has a square side length a in the horizontal direction: 20-30cm, and the vertical height is c:5-15cm, the side length b of the square bottom surface of the small cuboid is 2.5-10cm, and the height d is 2.5-15cm.
7. The method for producing aluminum-tungsten alloy according to claim 1, wherein in the step (3), the weight ratio of the intermediate frequency furnace material-mixing tungsten block to the aluminum bean is (0.82-2.1): 1; and the vacuum degree is less than 20Pa before smelting in the intermediate frequency furnace, and the smelting power is 140-170kW.
8. The method for producing aluminum-tungsten alloy according to claim 1 or 7, wherein the water inlet temperature of the cooling water of the intermediate frequency furnace is-10-5 ℃, and the weight of the prepared aluminum-tungsten alloy ingot is 50-90kg.
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