CN113981390A - Preparation method of high-purity low-oxygen tantalum target material - Google Patents
Preparation method of high-purity low-oxygen tantalum target material Download PDFInfo
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- CN113981390A CN113981390A CN202111272080.2A CN202111272080A CN113981390A CN 113981390 A CN113981390 A CN 113981390A CN 202111272080 A CN202111272080 A CN 202111272080A CN 113981390 A CN113981390 A CN 113981390A
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- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 title claims abstract description 223
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 150
- 239000001301 oxygen Substances 0.000 title claims abstract description 149
- 229910052715 tantalum Inorganic materials 0.000 title claims abstract description 130
- 239000013077 target material Substances 0.000 title claims abstract description 62
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 79
- 238000011282 treatment Methods 0.000 claims abstract description 59
- 238000000034 method Methods 0.000 claims abstract description 52
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims abstract description 32
- 230000009467 reduction Effects 0.000 claims abstract description 31
- 238000001513 hot isostatic pressing Methods 0.000 claims abstract description 26
- 238000007872 degassing Methods 0.000 claims abstract description 25
- 238000009694 cold isostatic pressing Methods 0.000 claims abstract description 22
- 238000001035 drying Methods 0.000 claims abstract description 22
- 238000012216 screening Methods 0.000 claims abstract description 15
- 238000006356 dehydrogenation reaction Methods 0.000 claims abstract description 14
- 239000002253 acid Substances 0.000 claims abstract description 13
- 239000001257 hydrogen Substances 0.000 claims abstract description 12
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 12
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000005406 washing Methods 0.000 claims description 47
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 23
- 229910001220 stainless steel Inorganic materials 0.000 claims description 18
- 239000010935 stainless steel Substances 0.000 claims description 18
- 238000003754 machining Methods 0.000 claims description 16
- 238000005984 hydrogenation reaction Methods 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 11
- 238000011049 filling Methods 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- 238000007789 sealing Methods 0.000 claims description 8
- 238000001291 vacuum drying Methods 0.000 claims description 8
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 7
- 230000007935 neutral effect Effects 0.000 claims description 7
- 229910017604 nitric acid Inorganic materials 0.000 claims description 7
- 238000003466 welding Methods 0.000 claims description 7
- 239000011812 mixed powder Substances 0.000 claims description 5
- 238000005096 rolling process Methods 0.000 claims description 5
- 238000010902 jet-milling Methods 0.000 claims description 3
- 238000004321 preservation Methods 0.000 claims 1
- 230000008569 process Effects 0.000 abstract description 23
- 239000012535 impurity Substances 0.000 abstract description 11
- 239000007789 gas Substances 0.000 abstract description 8
- 239000000395 magnesium oxide Substances 0.000 abstract description 8
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 abstract description 8
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 abstract description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 abstract description 4
- 238000005554 pickling Methods 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 11
- 238000005245 sintering Methods 0.000 description 11
- 239000000843 powder Substances 0.000 description 7
- 238000004544 sputter deposition Methods 0.000 description 7
- 239000007787 solid Substances 0.000 description 5
- 150000002500 ions Chemical class 0.000 description 4
- 238000004663 powder metallurgy Methods 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 238000005240 physical vapour deposition Methods 0.000 description 3
- 238000005477 sputtering target Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000010409 thin film Substances 0.000 description 3
- 238000003723 Smelting Methods 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 125000004429 atom Chemical group 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000010884 ion-beam technique Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 230000001133 acceleration Effects 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010891 electric arc Methods 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000010892 electric spark Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 238000000462 isostatic pressing Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000001451 molecular beam epitaxy Methods 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000007738 vacuum evaporation Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
- C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
-
- 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
- B22F3/04—Compacting only by applying fluid pressure, e.g. by cold isostatic pressing [CIP]
-
- 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
-
- 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
- B22F9/023—Hydrogen absorption
-
- 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
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
-
- 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
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/044—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by jet milling
-
- 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
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/045—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by other means than ball or jet milling
- B22F2009/047—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by other means than ball or jet milling by rolling
-
- 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
- B22F2201/00—Treatment under specific atmosphere
- B22F2201/20—Use of vacuum
Abstract
The invention relates to a preparation method of a high-purity low-oxygen tantalum target material, which comprises the steps of firstly adopting a hydrogenation-dehydrogenation process for a high-purity tantalum source, reducing various oxide or chloride impurities in the high-purity tantalum source by using hydrogen to ensure that the high-purity tantalum source becomes brittle, crushing and dehydrogenating to prepare high-purity tantalum powder, wherein in the crushing and screening processes, the oxygen content in the high-purity tantalum powder is increased, then adopting oxygen reduction treatment of magnesium powder to convert oxygen into magnesium oxide, and then removing redundant magnesium powder and magnesium oxide by using acid pickling and drying to obtain the high-purity low-oxygen tantalum powder; and then, carrying out cold isostatic pressing on the high-purity low-oxygen tantalum powder to obtain a tightly combined cold-pressed blank, further removing impurity gas through degassing treatment and improving the density, and finally, preparing the high-purity low-oxygen tantalum target material with the density reaching the standard by means of hot isostatic pressing, wherein the oxygen content in the tantalum target material is controlled to be less than or equal to 400ppm, preferably less than or equal to 300ppm, and meanwhile, the yield of the target material is improved.
Description
Technical Field
The invention relates to the technical field of target preparation, in particular to a preparation method of a high-purity low-oxygen tantalum target.
Background
Physical Vapor Deposition (PVD) refers to a process of evaporating a material source by using a low-voltage and large-current arc discharge technique under a vacuum condition, ionizing both evaporated substances and gas by using gas discharge, and then depositing the evaporated substances and reaction products thereof on a workpiece by an acceleration action of an electric field to form a film with a special function. The PVD technology is the core technology of various industries such as semiconductor chip manufacturing industry, solar energy industry, LCD manufacturing industry and the like, and the main methods comprise vacuum evaporation, arc plasma plating, ion coating, molecular beam epitaxy, sputtering coating and the like.
Sputtering is one of the main techniques for preparing thin film materials, and is characterized in that ions generated by an ion source are accelerated and gathered in vacuum to form ion beam flow with high speed energy, the ion beam flows bombard the surface of a solid, kinetic energy exchange is carried out between the ions and atoms on the surface of the solid, the atoms on the surface of the solid leave the solid and are deposited on the surface of a substrate, and the bombarded solid is a raw material for preparing a thin film deposited by a sputtering method and is generally called as a sputtering target material. Sputtering targets are generally obtained by powder metallurgy sintering molding processes because the sputtering targets prepared by the processes have unique chemical compositions and mechanical and physical properties that cannot be obtained by conventional fusion casting methods.
In the field of microelectronics, tantalum target materials are commonly used for preparing common target materials of thin film electrodes, interconnection lines and barrier layers of semiconductor devices, and the requirements on the purity and the gas content of the target materials are very high in the using process. At present, a tantalum ingot is mainly prepared by a traditional smelting method in a sputtering tantalum target, and then plastic deformation and annealing are carried out for multiple times, so that a tantalum target blank with uniform grain size and internal texture is obtained, but the sputtering performance of the target is seriously influenced by 'inherent texture belt' in the tantalum target. Meanwhile, the process is complex, long in flow and low in yield, and the cost of the tantalum target material is high. The tantalum target material prepared by the powder metallurgy method has the advantages of small grain size, uniform structure, simple process and the like, so that the sputtering coating is more uniform and compact, and the machining difficulty is greatly reduced. However, in the process of preparing tantalum powder, C, O and other metal impurities can be brought in due to ball milling and crushing, meanwhile, the sintering temperature of the tantalum target is far lower than the smelting temperature, and gas in the tantalum powder cannot be discharged, so that the oxygen content of the tantalum target obtained by powder metallurgy is high, and the sputtering performance is influenced; in addition, the tantalum powder has low apparent density and low yield when directly sintered. Therefore, the method for reducing the oxygen content in the tantalum target and improving the yield of the tantalum target is of great significance.
CN105177513A discloses a method for preparing a high-performance tantalum target material by using a powder metallurgy method, which comprises the following steps: (1) loading tantalum powder to be sintered into a die; (2) placing the die into an electric spark sintering furnace to perform discharge plasma sintering on the powder; (3) after sintering, cooling to a temperature not higher than 160 ℃, discharging, and demolding; (4) and machining the obtained tantalum target blank into the required size. The preparation method adopts a discharge plasma sintering process with high energy consumption, increases the preparation cost, does not strictly control the oxygen content of the raw material tantalum powder, requires O in the tantalum powder to be less than or equal to 2500ppm, and cannot prepare the high-purity low-oxygen tantalum target material.
CN102367568A discloses a preparation method of a high-purity tantalum target, which comprises the following steps: uniformly mixing tantalum powder; filling the mixed tantalum powder into a die; cold press molding; and (4) vacuum hot-pressing sintering. The preparation method does not mention the control of oxygen content, and the high-purity low-oxygen tantalum target material cannot be prepared.
CN104480439A discloses a preparation process of a tantalum target, which comprises the following steps: A) carrying out isostatic pressing on tantalum powder to obtain a tantalum blank; B) sintering the tantalum blank, rolling the tantalum blank obtained by sintering, and carrying out heat treatment on the tantalum blank obtained by rolling to obtain the tantalum target material. The preparation method does not mention the control of oxygen content, and the high-purity low-oxygen tantalum target material cannot be prepared.
CN103147050A discloses a production method of a high-purity tantalum target, which comprises the steps of (1) placing a tantalum block with the size of 5-10 mm multiplied by 5-10 mm in a hydrogenation furnace for hydrogen absorption; (2) crushing the tantalum after hydrogen absorption into powder of 200 meshes, placing the powder in a steel sheath, heating and exhausting according to a certain speed and stage, then placing the steel sheath in a hot isostatic pressing machine for sintering, wherein the sintering temperature is 1100-1500 ℃, the atmosphere pressure is 50-200 MPa, finally machining and cutting the powder into a specified shape. According to the method, the obtained powder is directly subjected to degassing treatment, the oxygen content is still high, the powder is low in loose density and easy to escape, subsequent hot isostatic pressing is influenced, and the deformation amount of the sintered target material is large and the yield is low.
In summary, there is a need to develop a method for preparing a high-purity low-oxygen tantalum target, which can reduce the oxygen content and increase the yield of the target while ensuring the purity of the target.
Disclosure of Invention
In order to solve the technical problems, the invention provides a preparation method of a high-purity low-oxygen tantalum target material, which comprises the steps of sequentially carrying out hydrogenation, crushing, screening, dehydrogenation, oxygen reduction treatment by adding magnesium powder, washing and drying on a high-purity tantalum source to obtain high-purity low-oxygen tantalum powder, sequentially carrying out cold isostatic pressing, degassing treatment, hot isostatic pressing and machining on the high-purity low-oxygen tantalum powder to obtain the high-purity low-oxygen tantalum target material, effectively reducing oxygen content under the condition of ensuring the purity of the target material, controlling the oxygen content in the tantalum target material to be less than or equal to 400ppm, preferably less than or equal to 300ppm, and simultaneously improving the yield of the target material.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a preparation method of a high-purity low-oxygen tantalum target material, which comprises the following steps:
(1) placing a high-purity tantalum source with the purity of more than or equal to 99.99% in a vacuum environment, filling hydrogen and heating to obtain a hydrogenated high-purity tantalum source;
(2) sequentially crushing, screening and dehydrogenating the hydrogenated high-purity tantalum source in the step (1) to obtain dehydrogenated high-purity tantalum powder;
(3) mixing magnesium powder with the dehydrogenated high-purity tantalum powder in the step (2), and sequentially performing oxygen reduction treatment, washing and drying to obtain high-purity low-oxygen tantalum powder;
(4) and (4) sequentially carrying out cold isostatic pressing, degassing treatment, hot isostatic pressing and machining on the high-purity low-oxygen tantalum powder in the step (3) to obtain the high-purity low-oxygen tantalum target material.
According to the preparation method, a hydrogenation-dehydrogenation process is firstly adopted for the high-purity tantalum source, various oxide or chloride impurities in the high-purity tantalum source are reduced by using hydrogen, so that the high-purity tantalum source becomes brittle, then the high-purity tantalum source is crushed and dehydrogenated to prepare high-purity tantalum powder, however, in the crushing and screening processes, the oxygen content in the high-purity tantalum powder is increased, then the oxygen is converted into magnesium oxide by adopting oxygen reduction treatment of magnesium powder, and then the redundant magnesium powder and the magnesium oxide can be removed by acid washing and drying, so that the high-purity low-oxygen tantalum powder is obtained; and then, carrying out cold isostatic pressing on the high-purity low-oxygen tantalum powder to obtain a tightly combined cold-pressed blank, further removing impurity gas through degassing treatment and improving the density, and finally, preparing the high-purity low-oxygen tantalum target material with the density reaching the standard by means of hot isostatic pressing, wherein the oxygen content in the tantalum target material is controlled to be less than or equal to 400ppm, preferably less than or equal to 300ppm, and meanwhile, the yield of the target material is improved.
Wherein the purity of the high purity tantalum source in step (1) is 99.99% or more, such as 99.99%, 99.991%, 99.992%, 99.995%, 99.997% or 99.999%, but not limited to the recited values, and other values not recited in the range of the recited values are also applicable.
The following technical solutions are preferred technical solutions of the present invention, but not limited to the technical solutions provided by the present invention, and technical objects and advantageous effects of the present invention can be better achieved and achieved by the following technical solutions.
As a preferable technical scheme of the invention, the high-purity tantalum source in the step (1) comprises tantalum ingots.
Preferably, in step (1), the high-purity tantalum source is placed in a hydrogenation furnace and vacuumized, so that the vacuum environment can be obtained.
Preferably, the heating temperature in step (1) is 600 to 700 ℃, for example 600 ℃, 620 ℃, 640 ℃, 660 ℃, 680 ℃ or 700 ℃, but is not limited to the recited values, and other values not recited in the range of the values are also applicable.
As a preferable technical scheme of the invention, the crushing in the step (2) comprises rolling and jet milling which are sequentially carried out, and the rolling and the jet milling are respectively carried out by adopting a double-roller machine and a jet mill.
Preferably, the twin-roll mill and the air flow mill are both provided with an inner liner.
Preferably, the lining is made of tantalum with purity of more than or equal to 99.99%.
It is worth saying that, in the crushing and screening process, the inner lining of the equipment contacted with the high-purity tantalum source adopts tantalum with the purity of more than or equal to 99.99 percent, thereby effectively reducing the introduction of impurity elements, reducing the introduction of oxygen and reducing the oxygen content.
Preferably, after sieving in step (2), hydrogenated high purity tantalum powder with a particle size of 180 to 325 mesh is obtained, such as 180 mesh, 200 mesh, 230 mesh, 250 mesh, 270 mesh, 300 mesh or 325 mesh, but not limited to the recited values, and other values not recited in the range of the values are also applicable.
Preferably, the dehydrogenation treatment of step (2) is carried out in a hydrogenation furnace.
Preferably, the dehydrogenation treatment in step (2) is carried out at a temperature of 750 to 850 ℃, for example 750 ℃, 770 ℃, 780 ℃, 800 ℃, 820 ℃ or 850 ℃, but not limited to the recited values, and other values not recited in the range of the values are also applicable.
In a preferred embodiment of the present invention, in the step (3), the magnesium powder accounts for 0.8 to 1.5 wt%, for example, 0.8 wt%, 0.9 wt%, 1.0 wt%, 1.1 wt%, 1.2 wt%, 1.3 wt%, 1.4 wt%, or 1.5 wt% of the dehydrogenated high purity tantalum powder in the step (2), but the present invention is not limited to the above-mentioned values, and other values not listed in the above-mentioned range are also applicable.
As a preferred embodiment of the present invention, the temperature of the oxygen reduction treatment in the step (3) is 780 to 860 ℃, for example 780 ℃, 800 ℃, 810 ℃, 830 ℃, 850 ℃ or 860 ℃, but is not limited to the values listed, and other values not listed in the numerical range are also applicable.
Preferably, the temperature of the oxygen reduction treatment in step (3) is 3 to 5 hours, such as 3 hours, 3.5 hours, 4 hours, 4.5 hours or 5 hours, but not limited to the recited values, and other values not recited in the range of the values are also applicable.
As a preferable technical scheme of the invention, the washing in the step (3) comprises acid washing and water washing which are sequentially carried out.
Preferably, the acid washing is performed with nitric acid at a concentration of 10 to 15 wt.%, for example 10 wt.%, 11 wt.%, 12 wt.%, 13 wt.%, 14 wt.% or 15 wt.%, but not limited to the recited values, and other values not recited within this range of values are equally applicable.
Preferably, the water washing is performed with deionized water.
Preferably, the end point of the water washing is that the washing liquid is neutral.
Preferably, the drying in step (3) is vacuum drying, and is performed in a vacuum drying oven.
Preferably, the drying temperature in step (3) is 55 to 65 ℃, for example 55 ℃, 56 ℃, 58 ℃, 60 ℃, 62 ℃ or 65 ℃, but not limited to the recited values, and other values not recited in the range of the values are also applicable.
Preferably, the drying time in step (3) is 11-13 h, such as 11h, 11.5h, 12h, 12.5h or 13h, but not limited to the recited values, and other values not recited in the range of the values are also applicable.
As a preferable technical scheme of the invention, the cold isostatic pressing in the step (4) is carried out by adopting rubber sleeve sealing.
Preferably, the cold isostatic pressing in step (4) has a pressure of 160 to 190MPa, such as 160MPa, 170MPa, 180MPa or 190MPa, but not limited to the recited values, and other values not recited in the range of values are also applicable.
Preferably, the cold isostatic pressing in step (4) is performed for 20-30 min, such as 20min, 22min, 24min, 26min, 28min or 30min, but not limited to the recited values, and other values not recited in the range of values are also applicable.
As a preferable technical scheme of the invention, the degassing treatment in the step (4) is carried out by adopting a stainless steel sheath seal.
Preferably, the temperature of the degassing treatment in step (4) is 400 to 600 ℃, for example, 400 ℃, 450 ℃, 500 ℃, 550 ℃ or 600 ℃, but is not limited to the recited values, and other values not recited in the range of the values are also applicable.
Preferably, the degassing treatment in step (4) is carried out for 6-9 h, such as 6h, 7h, 8h or 9h, but not limited to the recited values, and other values not recited in the range of the values are also applicable.
Preferably, the vacuum degree of the degassing treatment in the step (4) is 1 × 10-3～1×10-2Pa, e.g. 1X 10-3Pa、3×10-3Pa、5×10-3Pa、6×10-3Pa、8×10-3Pa or 1X 10-2Pa, etc., but are not limited to the recited values, and other values not recited within the range of values are also applicable.
In a preferred embodiment of the present invention, the hot isostatic pressing temperature in step (4) is 1000 to 1250 ℃, for example, 1000 ℃, 1050 ℃, 1100 ℃, 1150 ℃, 1200 ℃ or 1250 ℃, but the temperature is not limited to the above-mentioned values, and other values not shown in the above-mentioned range are also applicable.
Preferably, the hot isostatic pressing in step (4) is performed at a pressure of 170 to 190MPa, such as 170MPa, 175MPa, 180MPa, 185MPa or 190MPa, but not limited to the recited values, and other values not recited in the range of values are also applicable.
Preferably, the hot isostatic pressing in step (4) is performed for 3 to 6 hours, such as 3 hours, 3.5 hours, 4 hours, 4.5 hours, 5 hours, 5.5 hours, or 6 hours, but not limited to the recited values, and other values not recited in the range of the values are also applicable.
As a preferred technical scheme of the invention, the preparation method comprises the following steps:
(1) placing tantalum ingots with the purity of more than or equal to 99.99% as a high-purity tantalum source in a hydrogenation furnace for vacuumizing to obtain the vacuum environment, filling hydrogen and heating at 600-700 ℃ to obtain a hydrogenated high-purity tantalum source;
(2) crushing the hydrogenated high-purity tantalum source obtained in the step (1) by adopting a pair-roller machine and a jet mill in sequence, wherein the pair-roller machine and the jet mill are both provided with inner liners made of tantalum with the purity of more than or equal to 99.99%, screening to obtain hydrogenated high-purity tantalum powder with the granularity of 180-325 meshes, then placing the hydrogenated high-purity tantalum powder in a hydrogenation furnace, and carrying out dehydrogenation treatment at the temperature of 750-850 ℃ to obtain the dehydrogenated high-purity tantalum powder;
(3) mixing the dehydrogenized high-purity tantalum powder obtained in the step (2) with magnesium powder, wherein the magnesium powder accounts for 0.8-1.5 wt% of the dehydrogenized high-purity tantalum powder obtained in the step (2), preserving heat at 780-860 ℃ for 3-5 hours to perform oxygen reduction treatment, firstly performing acid washing on the mixed powder obtained by the oxygen reduction treatment by using nitric acid with the concentration of 10-15 wt%, then performing water washing by using deionized water until washing liquid obtained by the water washing is neutral, placing the tantalum powder obtained by the washing in a vacuum drying oven, and drying at 55-65 ℃ for 11-13 hours to obtain high-purity low-oxygen tantalum powder;
(4) sealing the high-purity low-oxygen tantalum powder obtained in the step (3) in a rubber sleeve, and carrying out cold isostatic pressing for 20-30 min under 160-190 MPa to obtain a cold-pressed blank; placing the cold-pressed blank into a stainless steel sheath for welding, and degassing at 400-600 ℃ for 6-9 h until the vacuum degree in the stainless steel sheath is 1 multiplied by 10-3～1×10-2Pa; and hot isostatic pressing for 3-6 h at 1000-1250 ℃ and 170-190 MPa, removing the stainless steel sleeve and machining to obtain the high-purity low-oxygen tantalum target material.
Compared with the prior art, the invention has at least the following beneficial effects:
(1) according to the preparation method, a hydrogenation-dehydrogenation process is firstly adopted for the high-purity tantalum source, various oxide or chloride impurities in the high-purity tantalum source are reduced, but the oxygen content in the high-purity tantalum powder is increased in the crushing and screening processes, then the oxygen is converted into magnesium oxide by adopting oxygen reduction treatment of magnesium powder, and then the redundant magnesium powder and the magnesium oxide can be removed by acid pickling and drying, so that the high-purity low-oxygen tantalum powder with the oxygen content of less than or equal to 400ppm and more preferably less than or equal to 300ppm is obtained;
(2) according to the preparation method, the high-purity low-oxygen tantalum powder is subjected to cold isostatic pressing to obtain a tightly combined cold-pressed blank, impurity gas is further removed through degassing treatment, the density is improved, finally, the high-purity low-oxygen tantalum target with the standard density is prepared through hot isostatic pressing, the oxygen content in the tantalum target is controlled to be less than or equal to 400ppm, preferably less than or equal to 300ppm, and the yield of the target is improved.
Detailed Description
For the purpose of facilitating an understanding of the present invention, the present invention will now be described by way of examples. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
Example 1
The embodiment provides a preparation method of a high-purity low-oxygen tantalum target material, which comprises the following steps:
(1) placing tantalum ingots with the purity of more than or equal to 99.99% as a high-purity tantalum source in a hydrogenation furnace, vacuumizing to obtain the vacuum environment, filling hydrogen and heating at 650 ℃ to obtain a hydrogenated high-purity tantalum source;
(2) crushing the hydrogenated high-purity tantalum source obtained in the step (1) by adopting a pair-roller machine and a jet mill in sequence, wherein the pair-roller machine and the jet mill are both provided with inner liners made of tantalum with the purity of more than or equal to 99.99%, screening to obtain hydrogenated high-purity tantalum powder with the granularity of 250 meshes, then placing the hydrogenated high-purity tantalum powder in a hydrogenation furnace, and carrying out dehydrogenation treatment at 800 ℃ to obtain the dehydrogenated high-purity tantalum powder;
(3) mixing the dehydrogenized high-purity tantalum powder obtained in the step (2) with magnesium powder, wherein the magnesium powder accounts for 1.0 wt% of the dehydrogenized high-purity tantalum powder obtained in the step (2), preserving heat at 800 ℃ for 4 hours to perform oxygen reduction treatment, firstly performing acid washing on the mixed powder obtained by the oxygen reduction treatment by using nitric acid with the concentration of 15 wt%, then performing water washing by using deionized water until washing liquid obtained by the water washing is neutral, placing the tantalum powder obtained by the washing in a vacuum drying box, and drying at 60 ℃ for 12 hours to obtain high-purity low-oxygen tantalum powder;
(4) sealing the high-purity low-oxygen tantalum powder obtained in the step (3) in a rubber sleeve, and carrying out cold isostatic pressing for 25min under 180MPa to obtain a cold-pressed blank; welding the cold-pressed blank in a stainless steel sheath, degassing at 500 deg.C for 8 hr until the vacuum degree in the stainless steel sheath is 5 × 10-3(ii) a Hot isostatic pressing at 1200 deg.C under 180MPa for 6 hr, removing stainless steel jacket, and machiningAnd obtaining the high-purity low-oxygen tantalum target material.
Example 2
The embodiment provides a preparation method of a high-purity low-oxygen tantalum target material, which comprises the following steps:
(1) placing tantalum ingots with the purity of more than or equal to 99.99% as a high-purity tantalum source in a hydrogenation furnace for vacuumizing to obtain a vacuum environment, filling hydrogen and heating at 600 ℃ to obtain a hydrogenated high-purity tantalum source;
(2) crushing the hydrogenated high-purity tantalum source obtained in the step (1) by adopting a pair-roller machine and a jet mill in sequence, wherein the pair-roller machine and the jet mill are both provided with inner liners made of tantalum with the purity of more than or equal to 99.99%, screening to obtain hydrogenated high-purity tantalum powder with the granularity of 180 meshes, then placing the hydrogenated high-purity tantalum powder in a hydrogenation furnace, and carrying out dehydrogenation treatment at 750 ℃ to obtain the dehydrogenated high-purity tantalum powder;
(3) mixing the dehydrogenized high-purity tantalum powder obtained in the step (2) with magnesium powder, wherein the magnesium powder accounts for 0.8 wt% of the dehydrogenized high-purity tantalum powder obtained in the step (2), preserving heat at 780 ℃ for 5 hours to perform oxygen reduction treatment, firstly performing acid washing on the mixed powder obtained by the oxygen reduction treatment by using nitric acid with the concentration of 10 wt%, then performing water washing by using deionized water until washing liquid obtained by the water washing is neutral, placing the tantalum powder obtained by the washing in a vacuum drying box, and drying at 60 ℃ for 12 hours to obtain high-purity low-oxygen tantalum powder;
(4) sealing the high-purity low-oxygen tantalum powder obtained in the step (3) in a rubber sleeve, and carrying out cold isostatic pressing for 30min under 160MPa to obtain a cold-pressed blank; welding the cold-pressed blank in a stainless steel sheath, degassing at 400 deg.C for 9 hr until the vacuum degree in the stainless steel sheath is 1 × 10-3(ii) a And hot isostatic pressing for 6h at 1000 ℃ and 170MPa, removing the stainless steel ladle sleeve and machining to obtain the high-purity low-oxygen tantalum target material.
Example 3
The embodiment provides a preparation method of a high-purity low-oxygen tantalum target material, which comprises the following steps:
(1) placing tantalum ingots with the purity of more than or equal to 99.99% as a high-purity tantalum source in a hydrogenation furnace for vacuumizing to obtain a vacuum environment, filling hydrogen and heating at 700 ℃ to obtain a hydrogenated high-purity tantalum source;
(2) crushing the hydrogenated high-purity tantalum source obtained in the step (1) by adopting a pair-roller machine and a jet mill in sequence, wherein the pair-roller machine and the jet mill are both provided with inner liners made of tantalum with the purity of more than or equal to 99.99%, screening to obtain hydrogenated high-purity tantalum powder with the granularity of 325 meshes, then placing the hydrogenated high-purity tantalum powder in a hydrogenation furnace, and carrying out dehydrogenation treatment at 850 ℃ to obtain the dehydrogenated high-purity tantalum powder;
(3) mixing the dehydrogenized high-purity tantalum powder obtained in the step (2) with magnesium powder, wherein the magnesium powder accounts for 1.5 wt% of the dehydrogenized high-purity tantalum powder obtained in the step (2), preserving heat at 860 ℃ for 3 hours to perform oxygen reduction treatment, firstly performing acid washing on the mixed powder obtained by the oxygen reduction treatment by using nitric acid with the concentration of 15 wt%, then performing water washing by using deionized water until washing liquid obtained by the water washing is neutral, placing the tantalum powder obtained by the washing in a vacuum drying box, and drying at 60 ℃ for 12 hours to obtain high-purity low-oxygen tantalum powder;
(4) sealing the high-purity low-oxygen tantalum powder obtained in the step (3) in a rubber sleeve, and carrying out cold isostatic pressing for 20min at 190MPa to obtain a cold-pressed blank; welding the cold-pressed blank in a stainless steel sheath, degassing at 600 deg.C for 6 hr until the vacuum degree in the stainless steel sheath is 1 × 10-2Pa; and hot isostatic pressing for 3h at 1250 ℃ and 190MPa, removing the stainless steel ladle sleeve and machining to obtain the high-purity low-oxygen tantalum target material.
Example 4
The present example provides a method for preparing a high-purity tantalum target material with low oxygen content, which is different from the method of example 1 only in that: the temperature of the oxygen reduction treatment in the step (3) is 750 ℃.
Example 5
The present example provides a method for preparing a high-purity tantalum target material with low oxygen content, which is different from the method of example 1 only in that: the temperature of the oxygen reduction treatment in the step (3) is 900 ℃.
Example 6
The present example provides a method for preparing a high-purity tantalum target material with low oxygen content, which is different from the method of example 1 only in that: in the step (3), the magnesium powder accounts for 0.5 wt% of the dehydrogenated high-purity tantalum powder in the step (2).
Example 7
The present example provides a method for preparing a high-purity tantalum target material with low oxygen content, which is different from the method of example 1 only in that: in the step (3), the magnesium powder accounts for 2.0 wt% of the dehydrogenated high-purity tantalum powder in the step (2).
Comparative example 1
The present comparative example provides a method for preparing a high-purity tantalum target material with low oxygen content, which is different from the method of example 1 only in that: and (3) directly putting the dehydrogenated high-purity tantalum powder in the step (2) into a rubber sleeve for sealing, and sequentially carrying out cold isostatic pressing, degassing treatment, hot isostatic pressing and machining to obtain the high-purity low-oxygen tantalum target material.
Comparative example 2
The present comparative example provides a method for preparing a high-purity tantalum target material with low oxygen content, which is different from the method of example 1 only in that: and (4) omitting the cold isostatic pressing in the step (4), directly putting the high-purity low-oxygen tantalum powder in the step (3) into a stainless steel sheath for welding, and sequentially performing degassing treatment, hot isostatic pressing and machining to obtain the high-purity low-oxygen tantalum target material.
The high-purity low-oxygen tantalum target materials prepared by the preparation methods in the above examples and comparative examples are respectively subjected to measurement of oxygen content, compactness and yield, wherein the yield refers to the mass M of the high-purity low-oxygen tantalum target material after machining is completed1The feed quantity M of the high-purity low-oxygen tantalum powder0The specific results are shown in table 1.
TABLE 1
| Item | Oxygen content/ppm | Density/% | Yield per cent |
| Example 1 | 245ppm | 99.41％ | 85.5％ |
| Example 2 | 259ppm | 99.31％ | 85.4％ |
| Example 3 | 389ppm | 99.45％ | 86.8％ |
| Example 4 | 365ppm | 99.35％ | 84.5％ |
| Example 5 | 321ppm | 99.50％ | 85.1％ |
| Example 6 | 412ppm | 99.32％ | 84.6％ |
| Example 7 | 241ppm | 99.42％ | 85.1％ |
| Comparative example 1 | 2132ppm | 98.20％ | 82.5％ |
| Comparative example 2 | 297ppm | 98.60％ | 63.7％ |
From table 1, the following points can be seen:
(1) according to the preparation method of the high-purity low-oxygen tantalum target material, a high-purity tantalum source is subjected to hydrogenation, crushing, screening, dehydrogenation, oxygen reduction treatment by adding magnesium powder, washing and drying in sequence to obtain high-purity low-oxygen tantalum powder, the high-purity low-oxygen tantalum powder is subjected to cold isostatic pressing, degassing treatment, hot isostatic pressing and machining in sequence to obtain the high-purity low-oxygen tantalum target material, the oxygen content is effectively reduced under the condition that the purity of the target material is ensured, the oxygen content in the tantalum target material is controlled to be less than or equal to 400ppm, preferably less than or equal to 300ppm, and meanwhile, the yield of the target material is improved;
(2) comparing example 1 with examples 4 and 5, since example 4 reduces the temperature of the oxygen reduction treatment in step (3) to 750 ℃, the reaction rate of magnesium powder and oxygen is reduced, so that the oxygen content of the high-purity tantalum powder obtained by washing and drying is higher, and finally the oxygen content of the high-purity tantalum target material is up to 365 ppm; in the embodiment 5, the temperature of the oxygen reduction treatment in the step (3) is increased to 900 ℃, so that oxygen reacts with trace impurities in the dehydrogenated high-purity tantalum powder under a high-temperature environment, but the oxygen content of the high-purity low-oxygen tantalum powder obtained by washing and drying is slightly increased, and finally the oxygen content of the high-purity low-oxygen tantalum target is increased to 321ppm, and the energy consumption cost is increased by the oxygen reduction treatment at a higher temperature;
(3) comparing the example 1 with the examples 6 and 7, since the content of the magnesium powder in the oxygen reduction treatment is reduced to 0.5 wt% in the example 6, the reaction degree of the magnesium powder and the oxygen is obviously weakened, so that the oxygen content of the high-purity low-oxygen tantalum powder obtained by washing and drying is higher, and finally the oxygen content of the high-purity low-oxygen tantalum target material is as high as 412 ppm; although the content of the magnesium powder in the oxygen reduction treatment is increased to 2.0 wt%, the reaction degree of the magnesium powder and the oxygen is not obviously improved, the oxygen content of the high-purity low-oxygen tantalum target material is only reduced to 241ppm, and the raw material cost is greatly increased by adopting the magnesium powder with higher content in the oxygen reduction treatment;
(4) comparing the embodiment 1 with the comparative example 1, wherein the oxygen reduction treatment in the step (3) is omitted in the comparative example 1, the dehydrogenated high-purity tantalum powder in the step (2) is directly placed into a rubber sleeve for sealing, and cold isostatic pressing, degassing treatment, hot isostatic pressing and machining are sequentially carried out, so that the oxygen content of the dehydrogenated high-purity tantalum powder in the step (2) is higher, the oxygen content of the high-purity low-oxygen tantalum target material is increased to 2132ppm, and the prepared high-purity low-oxygen tantalum target material cannot meet the qualified quality requirement;
(5) comparing the embodiment 1 with the comparative example 2, as the comparative example 2 omits the cold isostatic pressing in the step (4), the high-purity low-oxygen tantalum powder in the step (3) is directly put into a stainless steel sheath for welding, and degassing treatment, hot isostatic pressing and machining are sequentially carried out, although the oxygen content and the density of the obtained high-purity low-oxygen tantalum target can meet the requirements, the loose packing density of the tantalum powder is low, the tantalum powder is easy to escape, the subsequent hot isostatic pressing is influenced, the deformation amount of the sintered target is large, the yield is only 63.7%, and the production cost is increased.
The invention relates to a preparation method of a high-purity low-oxygen tantalum target material, which comprises the steps of firstly adopting a hydrogenation-dehydrogenation process for a high-purity tantalum source, reducing various oxide or chloride impurities in the high-purity tantalum source by using hydrogen to ensure that the high-purity tantalum source becomes brittle, crushing and dehydrogenating to prepare high-purity tantalum powder, wherein in the crushing and screening processes, the oxygen content in the high-purity tantalum powder is increased, then adopting oxygen reduction treatment of magnesium powder to convert oxygen into magnesium oxide, and then removing redundant magnesium powder and magnesium oxide by using acid pickling and drying to obtain the high-purity low-oxygen tantalum powder; and then, carrying out cold isostatic pressing on the high-purity low-oxygen tantalum powder to obtain a tightly combined cold-pressed blank, further removing impurity gas through degassing treatment and improving the density, and finally, preparing the high-purity low-oxygen tantalum target material with the density reaching the standard by means of hot isostatic pressing, wherein the oxygen content in the tantalum target material is controlled to be less than or equal to 400ppm, preferably less than or equal to 300ppm, and meanwhile, the yield of the target material is improved.
The applicant states that the present invention is illustrated by the above examples to show the detailed process equipment and process flow of the present invention, but the present invention is not limited to the above detailed process equipment and process flow, i.e. it does not mean that the present invention must rely on the above detailed process equipment and process flow to be implemented. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
Claims (10)
1. The preparation method of the high-purity low-oxygen tantalum target material is characterized by comprising the following steps:
(1) placing a high-purity tantalum source with the purity of more than or equal to 99.99% in a vacuum environment, filling hydrogen and heating to obtain a hydrogenated high-purity tantalum source;
(2) sequentially crushing, screening and dehydrogenating the hydrogenated high-purity tantalum source in the step (1) to obtain dehydrogenated high-purity tantalum powder;
(3) mixing magnesium powder with the dehydrogenated high-purity tantalum powder in the step (2), and sequentially performing oxygen reduction treatment, washing and drying to obtain high-purity low-oxygen tantalum powder;
(4) and (4) sequentially carrying out cold isostatic pressing, degassing treatment, hot isostatic pressing and machining on the high-purity low-oxygen tantalum powder in the step (3) to obtain the high-purity low-oxygen tantalum target material.
2. The method of claim 1, wherein the high purity tantalum source of step (1) comprises an ingot of tantalum;
preferably, the heating temperature in the step (1) is 600-700 ℃.
3. The production method according to claim 1 or 2, wherein the crushing of step (2) comprises rolling and jet milling which are carried out in this order;
preferably, after the screening in the step (2), obtaining hydrogenated high-purity tantalum powder with the granularity of 180-325 meshes;
preferably, the temperature of the dehydrogenation treatment in the step (2) is 750-850 ℃.
4. The method according to any one of claims 1 to 3, wherein in the step (3), the magnesium powder accounts for 0.8 to 1.5 wt% of the dehydrogenated high-purity tantalum powder in the step (2).
5. The method according to any one of claims 1 to 4, wherein the temperature of the oxygen reduction treatment in the step (3) is 780 to 860 ℃;
preferably, the heat preservation time of the oxygen reduction treatment in the step (3) is 3-5 h.
6. The method according to any one of claims 1 to 5, wherein the washing in step (3) comprises acid washing and water washing sequentially;
preferably, the acid washing is performed by using nitric acid with a concentration of 10-15 wt.%;
preferably, the water washing is performed by using deionized water;
preferably, the end point of the water washing is that the washing liquid is neutral;
preferably, the drying of step (3) is vacuum drying;
preferably, the drying temperature in the step (3) is 55-65 ℃;
preferably, the drying time in the step (3) is 11-13 h.
7. The production method according to any one of claims 1 to 6, wherein the cold isostatic pressing in step (4) is carried out at a pressure of 160 to 190 MPa;
preferably, the time of the cold isostatic pressing in the step (4) is 20-30 min.
8. The method according to any one of claims 1 to 7, wherein the degassing treatment in step (4) is carried out at a temperature of 400 to 600 ℃;
preferably, the time of the degassing treatment in the step (4) is 6-9 h;
preferably, the vacuum degree of the degassing treatment in the step (4) is 1 × 10-3～1×10-2Pa。
9. The production method according to any one of claims 1 to 8, wherein the hot isostatic pressing in step (4) is performed at a temperature of 1000 to 1250 ℃;
preferably, the hot isostatic pressing pressure in the step (4) is 170-190 MPa;
preferably, the hot isostatic pressing time in the step (4) is 3-6 h.
10. The method according to any one of claims 1 to 9, characterized by comprising the steps of:
(1) placing tantalum ingots with the purity of more than or equal to 99.99% as a high-purity tantalum source in a hydrogenation furnace for vacuumizing to obtain the vacuum environment, filling hydrogen and heating at 600-700 ℃ to obtain a hydrogenated high-purity tantalum source;
(2) crushing the hydrogenated high-purity tantalum source obtained in the step (1) by adopting a pair-roller machine and a jet mill in sequence, wherein the pair-roller machine and the jet mill are both provided with inner liners made of tantalum with the purity of more than or equal to 99.99%, screening to obtain hydrogenated high-purity tantalum powder with the granularity of 180-325 meshes, then placing the hydrogenated high-purity tantalum powder in a hydrogenation furnace, and carrying out dehydrogenation treatment at the temperature of 750-850 ℃ to obtain the dehydrogenated high-purity tantalum powder;
(3) mixing the dehydrogenized high-purity tantalum powder obtained in the step (2) with magnesium powder, wherein the magnesium powder accounts for 0.8-1.5 wt% of the dehydrogenized high-purity tantalum powder obtained in the step (2), preserving heat at 780-860 ℃ for 3-5 hours to perform oxygen reduction treatment, firstly performing acid washing on the mixed powder obtained by the oxygen reduction treatment by using nitric acid with the concentration of 10-15 wt%, then performing water washing by using deionized water until washing liquid obtained by the water washing is neutral, placing the tantalum powder obtained by the washing in a vacuum drying oven, and drying at 55-65 ℃ for 11-13 hours to obtain high-purity low-oxygen tantalum powder;
(4) sealing the high-purity low-oxygen tantalum powder obtained in the step (3) in a rubber sleeve, and carrying out cold isostatic pressing for 20-30 min under 160-190 MPa to obtain a cold-pressed blank; placing the cold-pressed blank into a stainless steel sheath for welding, and degassing at 400-600 ℃ for 6-9 h until the vacuum degree in the stainless steel sheath is 1 multiplied by 10-3～1×10-2Pa; and hot isostatic pressing for 3-6 h at 1000-1250 ℃ and 170-190 MPa, removing the stainless steel sleeve and machining to obtain the high-purity low-oxygen tantalum target material.
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