CN116984613A - Preparation method of approximately-formed tantalum-tungsten alloy special-shaped piece - Google Patents
Preparation method of approximately-formed tantalum-tungsten alloy special-shaped piece Download PDFInfo
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- CN116984613A CN116984613A CN202310974664.7A CN202310974664A CN116984613A CN 116984613 A CN116984613 A CN 116984613A CN 202310974664 A CN202310974664 A CN 202310974664A CN 116984613 A CN116984613 A CN 116984613A
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- 229910001080 W alloy Inorganic materials 0.000 title claims abstract description 118
- XGZGDYQRJKMWNM-UHFFFAOYSA-N tantalum tungsten Chemical compound [Ta][W][Ta] XGZGDYQRJKMWNM-UHFFFAOYSA-N 0.000 title claims abstract description 116
- 238000002360 preparation method Methods 0.000 title abstract description 16
- 239000000843 powder Substances 0.000 claims abstract description 67
- 229910052758 niobium Inorganic materials 0.000 claims abstract description 40
- 239000010955 niobium Substances 0.000 claims abstract description 40
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims abstract description 40
- 238000001513 hot isostatic pressing Methods 0.000 claims abstract description 17
- 238000010438 heat treatment Methods 0.000 claims abstract description 15
- 238000000889 atomisation Methods 0.000 claims abstract description 10
- 238000003754 machining Methods 0.000 claims abstract description 10
- 238000007789 sealing Methods 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims description 26
- 238000010894 electron beam technology Methods 0.000 claims description 10
- 238000003466 welding Methods 0.000 claims description 10
- 238000011068 loading method Methods 0.000 claims description 8
- 238000004519 manufacturing process Methods 0.000 claims description 7
- 229910052760 oxygen Inorganic materials 0.000 claims description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 6
- 238000002844 melting Methods 0.000 claims description 6
- 230000008018 melting Effects 0.000 claims description 6
- 239000001301 oxygen Substances 0.000 claims description 6
- 238000000465 moulding Methods 0.000 claims description 5
- 238000005429 filling process Methods 0.000 claims description 4
- 239000010935 stainless steel Substances 0.000 claims description 4
- 229910001220 stainless steel Inorganic materials 0.000 claims description 4
- 229910052721 tungsten Inorganic materials 0.000 claims description 3
- 239000000155 melt Substances 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- 229910052715 tantalum Inorganic materials 0.000 claims description 2
- 239000012535 impurity Substances 0.000 abstract description 8
- 239000000463 material Substances 0.000 abstract description 6
- 239000000126 substance Substances 0.000 abstract description 4
- 238000005056 compaction Methods 0.000 abstract description 3
- 230000007797 corrosion Effects 0.000 abstract description 3
- 238000005260 corrosion Methods 0.000 abstract description 3
- 238000005516 engineering process Methods 0.000 abstract description 3
- 238000005242 forging Methods 0.000 description 9
- 238000011049 filling Methods 0.000 description 6
- 230000003287 optical effect Effects 0.000 description 6
- 238000004321 preservation Methods 0.000 description 5
- 238000010146 3D printing Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 238000007514 turning Methods 0.000 description 4
- 230000007547 defect Effects 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000003723 Smelting Methods 0.000 description 2
- 239000011362 coarse particle Substances 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000006356 dehydrogenation reaction Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 239000010419 fine particle Substances 0.000 description 2
- 238000005984 hydrogenation reaction Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000004663 powder metallurgy Methods 0.000 description 2
- 238000007639 printing Methods 0.000 description 2
- 238000003672 processing method Methods 0.000 description 2
- 239000003870 refractory metal Substances 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 229910001069 Ti alloy Inorganic materials 0.000 description 1
- 229910001093 Zr alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
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- 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
- B22F5/00—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
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- 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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/06—Metallic powder characterised by the shape of the particles
- B22F1/065—Spherical particles
-
- 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
- B22F3/02—Compacting only
- B22F3/093—Compacting only using vibrations or friction
-
- 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
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
- B22F3/15—Hot isostatic pressing
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- 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
- B22F3/24—After-treatment of workpieces or articles
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- 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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/14—Making metallic powder or suspensions thereof using physical processes using electric discharge
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
- C22C27/02—Alloys based on vanadium, niobium, or tantalum
-
- 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
- B22F3/24—After-treatment of workpieces or articles
- B22F2003/248—Thermal after-treatment
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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
- Y02P10/00—Technologies related to metal processing
- Y02P10/25—Process efficiency
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Abstract
The invention discloses a preparation method of an approximately formed tantalum-tungsten alloy special-shaped piece, which comprises the following steps: 1. preparing tantalum-tungsten alloy spherical powder by adopting a plasma rotary electrode atomization method; 2. designing and preparing a niobium mold; 3. putting the tantalum-tungsten alloy spherical powder into a niobium mold for vibration, and sealing the preform; 4. performing hot isostatic pressing on the prefabricated part to obtain a pressed body of the approximately-formed tantalum-tungsten alloy special-shaped piece; 5. and removing the niobium mould, carrying out finish machining and then carrying out vacuum heat treatment to obtain the approximately formed tantalum-tungsten alloy special-shaped piece. The tantalum-tungsten alloy spherical powder prepared by the plasma rotary electrode atomization method is filled into a designed sheath for compaction, and is combined with hot isostatic pressing and high-temperature vacuum heat treatment to form the large thin-wall approximately-formed tantalum-tungsten alloy shell, so that the tantalum-tungsten alloy spherical powder has low impurity content and good mechanical property, and can be used as a functional structural material with high temperature resistance, high pressure resistance, corrosion resistance and the like to be applied to the fields of chemical industry, aerospace, atomic energy industry and high temperature technology.
Description
Technical Field
The invention belongs to the technical field of refractory metal preparation, and particularly relates to a preparation method of an approximately formed tantalum-tungsten alloy special-shaped piece.
Background
The tantalum-tungsten alloy has excellent performances of high temperature resistance, high pressure resistance, corrosion resistance and the like, and can be widely applied to the fields of chemical industry, aerospace, atomic energy industry and high temperature technology as a functional structural material. The large thin-wall tantalum-tungsten alloy shell is a key rare metal part in the atomic energy industry, is small in dosage, generally only needs 1-2 parts, has high requirements on the overall mechanical properties of the workpiece, and cannot be provided with welding seams. If the traditional forging process is adopted, a large-sized high-temperature forging die is required to be designed and processed, and a large-sized tantalum-tungsten alloy cast ingot is adopted, so that the raw material demand is large, and the mass of the large-sized thin-wall tantalum-tungsten alloy shell only accounts for less than 5% of the mass proportion of the cast ingot to be forged. Because the tantalum-tungsten alloy material has high-temperature strength, difficult forging, easy deformation of a die, easy forging failure, severe oxidation during high-temperature heating and forging of a workpiece, need to process and remove a surface pollution layer, large reserved cutting removal amount, generally more than 10mm on one side, extremely low yield and high comprehensive cost. If the powder is prepared by adopting a 3D printing process, at least the powder amount filling the whole space of the powder bed is needed to be prepared, and the total feeding amount is more than one time than that of a forging method. Under the condition that only one or two products are usually needed, the amount of residual powder is large, the consumption of rare metal powder is small, the probability of secondary utilization is low, and the single production and feeding amount is overlarge and the cost is overlarge. In addition, the 3D printing product is difficult to avoid printing defects, the tantalum-tungsten alloy printing grains are thicker, and the mechanical comprehensive performance of the workpiece is poor.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method for approximately forming a tantalum-tungsten alloy special-shaped piece aiming at the defects in the prior art. The method is characterized in that the tantalum-tungsten alloy spherical powder prepared by the plasma rotary electrode atomization method is filled into a designed sheath for compaction, hot isostatic pressing and high-temperature vacuum heat treatment are combined to form the large-sized thin-wall approximately-formed tantalum-tungsten alloy shell, the preparation method is simple, raw materials are saved, the impurity content in the product is low, the mechanical property is good, and the problems that the material waste of the traditional forging processing is serious, the powder amount required by the 3D printing process is large, and the equipment size is limited are solved.
In order to solve the technical problems, the invention adopts the following technical scheme: a method for preparing a shaped piece of an approximately shaped tantalum-tungsten alloy, the method comprising the steps of:
firstly, preparing tantalum-tungsten alloy cast ingots into tantalum-tungsten alloy spherical powder by adopting a plasma rotary electrode atomization method;
secondly, designing the structure and the size of a niobium mold according to the structural size of a target product tantalum-tungsten alloy special-shaped piece and reserving machining allowance, and then adopting a niobium plate to prepare the niobium mold for approximate molding of the tantalum-tungsten alloy special-shaped piece through electron beam welding in a vacuum furnace;
step three, loading the tantalum-tungsten alloy spherical powder prepared in the step one into the niobium mold prepared in the step two for vibration, so that the tantalum-tungsten alloy spherical powder is fully distributed in the inner cavity of the niobium mold, and then sealing the inner cavity by vacuum electron beam welding to obtain a prefabricated member;
step four, performing hot isostatic pressing on the prefabricated member obtained in the step three to prepare a compact approximately-formed tantalum-tungsten alloy special-shaped member pressed body;
removing the niobium mold on the approximately formed tantalum-tungsten alloy special-shaped piece pressed body in the fourth step through a machining method, finely machining to the size of a finished product, and then performing vacuum heat treatment to obtain the approximately formed tantalum-tungsten alloy special-shaped piece; the approximately formed tantalum-tungsten alloy special-shaped piece is a large thin-wall shell, the diameter is 150-500 mm, the height is 120-500 mm, and the wall thickness is 5-40 mm.
The preparation method of the approximately formed tantalum-tungsten alloy special-shaped piece is characterized in that the tantalum-tungsten alloy cast ingot in the first step comprises the following components in percentage by mass: 88 to 89 percent of Ta and 11 to 12 percent of W.
The preparation method of the approximately molded tantalum-tungsten alloy special-shaped piece is characterized in that the process of preparing the tantalum-tungsten alloy cast ingot into the tantalum-tungsten alloy spherical powder by adopting the plasma rotary electrode atomization method in the first step is as follows: placing the tantalum-tungsten alloy ingot into a vacuum degree of less than 5.0X10 -2 Melting into a melt under the action of a plasma arc in a vacuum furnace of Pa, and rotationally atomizing into fine tantalum-tungsten alloy spherical powder under the action of centrifugal force at a high speed of 12000 r/min-18000 r/min.
The preparation method of the approximately molded tantalum-tungsten alloy special-shaped piece is characterized in that the oxygen content of the tantalum-tungsten alloy spherical powder in the first step is 30 ppm-80 ppm, and the granularity is 25 μm-153 μm.
The preparation method of the approximately molded tantalum-tungsten alloy special-shaped piece is characterized in that a stainless steel sieve is adopted to sieve the tantalum-tungsten alloy spherical powder prepared in the first step to obtain two tantalum-tungsten alloy spherical powders with the granularity of 80-150 mu m and less than 50 mu m respectively, in the powder filling process in the third step, firstly, the tantalum-tungsten alloy spherical powder with the granularity of 80-150 mu m is filled in a niobium mold, then, the tantalum-tungsten alloy spherical powder with the granularity of less than 50 mu m is filled, and in the powder filling process, the niobium mold is vibrated. According to the invention, the tantalum-tungsten alloy spherical powder with coarse particles and fine particles is filled, so that fine particles can fill gaps of the coarse particles, and the filling density is improved.
The preparation method of the approximately molded tantalum-tungsten alloy special-shaped piece is characterized in that the hot isostatic pressing temperature in the fourth step is 1500-1800 ℃, the pressure is 150-180 MPa, and the heat preservation and pressure maintaining time is 4-5 h. The melting point of the niobium mould sheath adopted by the invention is as high as 2468 ℃, the high temperature can be born, meanwhile, the tantalum-tungsten alloy is refractory metal, and the required hot pressing temperature is high, so the invention adopts the temperature higher than that of the traditional hot isostatic pressing, and is favorable for the compact and approximate molding of the tantalum-tungsten alloy special-shaped part pressed body.
The preparation method of the approximately formed tantalum-tungsten alloy special-shaped piece is characterized by adopting lathe processing to remove the niobium mold in the fifth step.
The preparation method of the approximately molded tantalum-tungsten alloy special-shaped piece is characterized in that the temperature of the vacuum heat treatment in the fifth step is 2000-2200 ℃, the heat preservation time is 2h, and the vacuum degree is less than 5.0x10 -2 Pa. The mechanical properties of the approximately formed tantalum-tungsten alloy special-shaped piece can be optimized by controlling the temperature, the heat preservation time and the vacuum degree of the vacuum heat treatment.
The preparation method of the approximately molded tantalum-tungsten alloy special-shaped piece is characterized in that the room-temperature tensile strength of the approximately molded tantalum-tungsten alloy special-shaped piece in the fifth step is 600 MPa-620 MPa, the yield strength is 480 MPa-500 MPa, and the elongation is 25% -30%. Compared with the existing tantalum-tungsten alloy prepared by adopting powder metallurgy sintering or powder metallurgy hot isostatic pressing, the elongation of the tantalum-tungsten alloy is lower than 3%, the similar-formed tantalum-tungsten alloy special-shaped piece prepared by the method has the advantages that the strength is improved, the plasticity is greatly improved, and the forming of the large thin-wall tantalum-tungsten alloy special-shaped piece is ensured.
Compared with the prior art, the invention has the following advantages:
1. the invention adopts a plasma rotary electrode atomization method to prepare tantalum-tungsten alloy spherical powder, and the large-sized thin-wall tantalum-tungsten alloy shell is obtained through the design and manufacture of a niobium sheath, powder filling compaction, vacuum sealing welding, hot isostatic pressing, mechanical finish machining and high-temperature vacuum heat treatment.
2. The tantalum-tungsten alloy has high melting point, high activity and easy reaction with O, N, C and other impurity elements to introduce the impurity elements, the traditional hydrogenation and dehydrogenation powder preparation is easy to be influenced by hydrogen impurities, and the hydrogenated powder needs to be crushed under a machine and is easy to be polluted, so the powder prepared by hydrogenation and dehydrogenation has high impurity content, and the oxygen content of different powder particle sizes is generally 0.05-0.15 wt%. The invention takes tantalum-tungsten alloy cast ingot as raw material, adopts a plasma rotary electrode atomization method to prepare tantalum-tungsten alloy spherical powder under high vacuum condition, and the tungsten content in the prepared powder is uniform, powder is prepared under high vacuum, and the powder is spherical powder, and has small specific surface area, smooth surface, low impurity and oxygen content of less than 0.01 wt%.
3. The tantalum-tungsten alloy spherical powder has good fluidity, high filling density and small deformation after hot isostatic pressing, and the forming precision of the tantalum-tungsten alloy special-shaped piece is effectively improved, so that the design allowance and the processing allowance are reduced, and the yield is further improved.
4. The tantalum-tungsten alloy prepared by 3D printing is easy to generate defects, has thicker crystal grains and poorer mechanical property, and the invention adopts hot isostatic pressing to act on the tantalum-tungsten alloy spherical powder for a long time under high temperature and high pressure, so that the tantalum-tungsten alloy spherical powder is fully densified, and a tantalum-tungsten alloy special-shaped piece with excellent comprehensive mechanical property can be obtained through high-temperature vacuum heat treatment, and the tantalum-tungsten alloy special-shaped piece has good strength and fine metallographic structure crystal grains.
5. The niobium sheath adopted by the invention can bear the high temperature of over 1700 ℃, is obviously higher than the highest use temperature of common sheath materials of steel, titanium alloy and zirconium alloy, and the higher hot isostatic pressing temperature can enable the materials to be better densified to form metallurgical bonding, so that the mechanical property of the tantalum-tungsten alloy special-shaped piece is improved.
6. The approximately formed tantalum-tungsten alloy special-shaped piece prepared by the method has low impurity content and good mechanical property, and can be widely applied to the fields of chemical industry, aerospace, atomic energy industry and high temperature technology as a functional structural material with high temperature resistance, high pressure resistance, corrosion resistance and the like.
The technical scheme of the invention is further described in detail through the drawings and the embodiments.
Drawings
FIG. 1 is a morphology diagram of TaW12 tantalum tungsten alloy spherical powder prepared in example 1 of the invention.
Fig. 2 is a schematic diagram of an approximately shaped TaW12 tantalum tungsten alloy part prepared in example 1 of the present invention.
FIG. 3 is a morphology diagram of TaW11 tantalum tungsten alloy spherical powder prepared in example 2 of the present invention.
Fig. 4 is a schematic diagram of an approximately shaped TaW11 tantalum tungsten alloy part according to example 2 of the present invention.
Detailed Description
Example 1
The embodiment comprises the following steps:
firstly, placing a TaW12 cast ingot prepared by smelting into a high-temperature box-type resistance furnace, heating and preserving heat at 1300 ℃ for 1h, and then forging to obtain a TaW12 bar with the diameter phi of 60mm multiplied by L; turning the TaW12 bar, namely turning the threads M45×50mm, wherein the rest is the optical bar with the diameter phi 50mm, so as to ensure that the threads are matched with the threads of the plasma rotating electrode device, and obtaining the TaW12 optical bar;
placing TaW12 optical rod under vacuum degree of less than 5.0X10 -2 Melting into a molten liquid under the action of a plasma arc in a vacuum furnace of Pa, and performing high-speed rotary atomization at 12000 r/min-18000 r/min under the action of centrifugal force to obtain fine TaW12 spherical powder, wherein the oxygen content of the tungsten alloy spherical powder is 30 ppm-80 ppm as shown in figure 1, and a stainless steel screen is adopted to screen the TaW12 spherical powder to obtain two TaW12 spherical powders with the granularity of 80-150 mu m and below 50 mu m respectively;
step two, designing the structure and the size of a niobium mold according to the structural size of a target product tantalum-tungsten alloy special-shaped piece and reserving machining allowance, and then adopting a niobium plate with the thickness of 2mm to process and weld by an electron beam in a vacuum furnace to prepare the niobium mold for approximate molding of the tantalum-tungsten alloy special-shaped piece;
step three, firstly loading TaW12 spherical powder with the granularity of 80-150 mu m into a niobium die, then loading TaW12 spherical powder with the granularity of less than 50 mu m, vibrating the niobium die in the powder loading process to ensure that the TaW12 spherical powder is fully distributed in the inner cavity of the niobium die so as to ensure that the filling theoretical density is close to the tap density, and then adopting a vacuum electron beam welding machine to carry out vacuum electron beam welding sealing on the niobium die, wherein the vacuum degree is less than 5 multiplied by 10 -2 Pa, obtaining a prefabricated member;
step four, performing hot isostatic pressing on the prefabricated member obtained in the step three, and cooling to room temperature along with a furnace to obtain a compact approximately-formed tantalum-tungsten alloy special-shaped member compact; the hot isostatic pressing temperature is 1800 ℃, the pressure is 180MPa, and the heat preservation and pressure maintaining time is 5 hours;
removing the niobium mould on the pressed body of the approximately formed tantalum-tungsten alloy special-shaped piece in the fourth step by a lathe processing method, finely processing the pressed body to the size of a finished product, and then performing vacuum heat treatment at the temperature of 2200 ℃ for 2 hours, wherein the vacuum degree is less than 5.0x10 -2 Pa, an approximately shaped tantalum tungsten alloy profile with a diameter of 220mm, a height of 185mm and a wall thickness of 7mm was obtained, as shown in FIG. 2.
Mechanical property detection is carried out on the approximately-formed tantalum-tungsten alloy special-shaped piece prepared in the embodiment, and the result shows that: the room temperature tensile strength is 609MPa, the yield strength is 488MPa, and the elongation is 30%.
Example 2
The embodiment comprises the following steps:
firstly, placing a TaW11 cast ingot prepared by smelting into a high-temperature box-type resistance furnace, heating and preserving heat at 1300 ℃ for 1h, and then forging to obtain a TaW11 bar with the diameter phi of 60mm multiplied by L; turning the TaW11 bar, namely turning the threads M45×50mm, wherein the rest is the optical bar with the diameter phi of 50mm, so as to ensure that the threads are matched with the threads of the plasma rotating electrode device, and obtaining the TaW11 optical bar;
placing TaW11 optical rod under vacuum degree of less than 5.0X10 -2 Melting into a molten liquid under the action of a plasma arc in a vacuum furnace of Pa, and performing high-speed rotary atomization at 12000 r/min-18000 r/min under the action of centrifugal force to obtain fine TaW11 spherical powder, wherein the oxygen content of the tungsten alloy spherical powder is 30 ppm-80 ppm, and a stainless steel screen is adopted to screen the TaW11 spherical powder to obtain two TaW11 spherical powders with the granularity of 80-150 mu m and below 50 mu m respectively;
step two, designing the structure and the size of a niobium mold according to the structural size of a target product tantalum-tungsten alloy special-shaped piece and reserving machining allowance, and then adopting a niobium plate with the thickness of 2mm to process and weld by an electron beam in a vacuum furnace to prepare the niobium mold for approximate molding of the tantalum-tungsten alloy special-shaped piece;
step three, firstly loading TaW11 spherical powder with the granularity of 80-150 mu m into a niobium die, then loading TaW11 spherical powder with the granularity of less than 50 mu m, vibrating the niobium die in the powder loading process to ensure that the TaW11 spherical powder is fully distributed in the inner cavity of the niobium die so as to ensure that the filling theoretical density is close to the tap density, and then adopting a vacuum electron beam welding machine to carry out vacuum electron beam welding sealing on the niobium die, wherein the vacuum degree is less than 5 multiplied by 10 -2 Pa, obtaining a prefabricated member;
step four, performing hot isostatic pressing on the prefabricated member obtained in the step three, and cooling to room temperature along with a furnace to obtain a compact approximately-formed tantalum-tungsten alloy special-shaped member compact; the hot isostatic pressing temperature is 1700 ℃, the pressure is 150MPa, and the heat preservation and pressure maintaining time is 4 hours;
removing the niobium mould on the pressed body of the approximately formed tantalum-tungsten alloy special-shaped piece in the fourth step by a lathe processing method, finely processing the pressed body to the size of a finished product, and then performing vacuum heat treatment at the temperature of 2000 ℃ for 2 hours, wherein the vacuum degree is less than 5.0x10 -2 Pa, an approximately shaped tantalum tungsten alloy profile with a short diameter of 150mm, a long diameter of 186mm, a height of 210mm and a wall thickness of 13mm was obtained, as shown in FIG. 4.
Mechanical property detection is carried out on the approximately-formed tantalum-tungsten alloy special-shaped piece prepared in the embodiment, and the result shows that: the room temperature tensile strength is 607MPa, the yield strength is 494MPa, and the elongation is 25%.
The above description is only of the preferred embodiments of the present invention, and is not intended to limit the present invention. Any simple modification, variation and equivalent variation of the above embodiments according to the technical substance of the invention still fall within the scope of the technical solution of the invention.
Claims (9)
1. A method for preparing a shaped piece of an approximately shaped tantalum-tungsten alloy, the method comprising the steps of:
firstly, preparing tantalum-tungsten alloy cast ingots into tantalum-tungsten alloy spherical powder by adopting a plasma rotary electrode atomization method;
secondly, designing the structure and the size of a niobium mold according to the structural size of a target product tantalum-tungsten alloy special-shaped piece and reserving machining allowance, and then adopting a niobium plate to prepare the niobium mold for approximate molding of the tantalum-tungsten alloy special-shaped piece through electron beam welding in a vacuum furnace;
step three, loading the tantalum-tungsten alloy spherical powder prepared in the step one into the niobium mold prepared in the step two for vibration, so that the tantalum-tungsten alloy spherical powder is fully distributed in the inner cavity of the niobium mold, and then sealing the inner cavity by vacuum electron beam welding to obtain a prefabricated member;
step four, performing hot isostatic pressing on the prefabricated member obtained in the step three to prepare a compact approximately-formed tantalum-tungsten alloy special-shaped member pressed body;
removing the niobium mold on the approximately formed tantalum-tungsten alloy special-shaped piece pressed body in the fourth step through a machining method, finely machining to the size of a finished product, and then performing vacuum heat treatment to obtain the approximately formed tantalum-tungsten alloy special-shaped piece; the approximately formed tantalum-tungsten alloy special-shaped piece is a large thin-wall shell, the diameter is 150-500 mm, the height is 120-500 mm, and the wall thickness is 5-40 mm.
2. The method for preparing a shaped tantalum-tungsten alloy part according to claim 1, wherein the tantalum-tungsten alloy ingot in the first step comprises the following components in percentage by mass: 88 to 89 percent of Ta and 11 to 12 percent of W.
3. The method for preparing a shaped tantalum-tungsten alloy part according to claim 1, wherein the step one comprises the steps of: placing the tantalum-tungsten alloy ingot into a vacuum degree of less than 5.0X10 -2 Melting into a melt under the action of a plasma arc in a vacuum furnace of Pa, and rotationally atomizing into fine tantalum-tungsten alloy spherical powder under the action of centrifugal force at a high speed of 12000 r/min-18000 r/min.
4. The method of producing a shaped tantalum-tungsten alloy product according to claim 1, wherein said spherical tantalum-tungsten alloy powder in said step one has an oxygen content of 30ppm to 80ppm and a particle size of 25 μm to 153. Mu.m.
5. The method for manufacturing a shaped tantalum-tungsten alloy part according to claim 1, wherein the tantalum-tungsten alloy spherical powder manufactured in the first step is sieved by a stainless steel sieve to obtain two kinds of tantalum-tungsten alloy spherical powder with the granularity of 80-150 μm and below 50 μm, respectively, the tantalum-tungsten alloy spherical powder with the granularity of 80-150 μm is firstly filled into a niobium mold in the powder filling process in the third step, the tantalum-tungsten alloy spherical powder with the granularity of below 50 μm is filled in, and the niobium mold is vibrated in the powder filling process.
6. The method for manufacturing a shaped tantalum-tungsten alloy part according to claim 1, wherein the hot isostatic pressing temperature in the fourth step is 1700-1800 ℃, the pressure is 150-180 MPa, and the holding time is 4-5 h.
7. The method for producing a shaped article of approximately formed tantalum-tungsten alloy according to claim 1, wherein in step five, the niobium mold is removed by lathe work.
8. The method for manufacturing a shaped tantalum-tungsten alloy product according to claim 1, wherein the vacuum heat treatment in the fifth step is performed at 2000-2200 ℃ for 2h with a vacuum degree of less than 5.0x10 -2 Pa。
9. The method for manufacturing a shaped tantalum-tungsten alloy part according to claim 1, wherein the room temperature tensile strength of the shaped tantalum-tungsten alloy part is 600-620 MPa, the yield strength is 480-500 MPa, and the elongation is 25-30%.
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