CN117444193A - Tantalum powder and preparation method thereof - Google Patents
Tantalum powder and preparation method thereof Download PDFInfo
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- CN117444193A CN117444193A CN202311587838.0A CN202311587838A CN117444193A CN 117444193 A CN117444193 A CN 117444193A CN 202311587838 A CN202311587838 A CN 202311587838A CN 117444193 A CN117444193 A CN 117444193A
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- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 title claims abstract description 164
- 238000002360 preparation method Methods 0.000 title abstract description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 118
- 239000001301 oxygen Substances 0.000 claims abstract description 107
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 107
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 104
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 60
- 238000000034 method Methods 0.000 claims abstract description 42
- 238000002161 passivation Methods 0.000 claims abstract description 36
- 230000008569 process Effects 0.000 claims abstract description 19
- 239000002245 particle Substances 0.000 claims abstract description 18
- 238000005245 sintering Methods 0.000 claims description 63
- 238000011282 treatment Methods 0.000 claims description 46
- 238000005406 washing Methods 0.000 claims description 39
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims description 36
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 27
- 229910052708 sodium Inorganic materials 0.000 claims description 27
- 239000011734 sodium Substances 0.000 claims description 27
- 239000012535 impurity Substances 0.000 claims description 24
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 23
- 238000001914 filtration Methods 0.000 claims description 23
- 229910052700 potassium Inorganic materials 0.000 claims description 23
- 239000011591 potassium Substances 0.000 claims description 23
- 238000002156 mixing Methods 0.000 claims description 22
- 230000009467 reduction Effects 0.000 claims description 22
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 20
- 238000010521 absorption reaction Methods 0.000 claims description 20
- 239000007789 gas Substances 0.000 claims description 13
- 239000002243 precursor Substances 0.000 claims description 13
- 229910052786 argon Inorganic materials 0.000 claims description 10
- 238000004321 preservation Methods 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 9
- 238000002347 injection Methods 0.000 claims description 9
- 239000007924 injection Substances 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 8
- 239000011261 inert gas Substances 0.000 claims description 8
- 229910052804 chromium Inorganic materials 0.000 claims description 7
- 229910052742 iron Inorganic materials 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 238000005554 pickling Methods 0.000 claims description 5
- 239000010703 silicon Substances 0.000 claims description 5
- 229910052710 silicon Inorganic materials 0.000 claims description 5
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 4
- 229910052796 boron Inorganic materials 0.000 claims description 4
- 239000011573 trace mineral Substances 0.000 claims description 4
- 235000013619 trace mineral Nutrition 0.000 claims description 4
- 229910052785 arsenic Inorganic materials 0.000 claims description 3
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 claims description 3
- 229910052727 yttrium Inorganic materials 0.000 claims description 3
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims description 3
- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical compound [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 claims 1
- BPUBBGLMJRNUCC-UHFFFAOYSA-N oxygen(2-);tantalum(5+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ta+5].[Ta+5] BPUBBGLMJRNUCC-UHFFFAOYSA-N 0.000 abstract description 5
- 229910001936 tantalum oxide Inorganic materials 0.000 abstract description 5
- 239000006104 solid solution Substances 0.000 abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 26
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 description 17
- 229910000387 ammonium dihydrogen phosphate Inorganic materials 0.000 description 17
- 235000019837 monoammonium phosphate Nutrition 0.000 description 17
- 239000006012 monoammonium phosphate Substances 0.000 description 16
- 239000000126 substance Substances 0.000 description 13
- 239000002253 acid Substances 0.000 description 12
- 239000000463 material Substances 0.000 description 9
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 8
- 229910052751 metal Inorganic materials 0.000 description 7
- 239000002184 metal Substances 0.000 description 7
- 239000000047 product Substances 0.000 description 7
- 229910052715 tantalum Inorganic materials 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 238000011068 loading method Methods 0.000 description 5
- 238000007873 sieving Methods 0.000 description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 4
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 4
- 239000000706 filtrate Substances 0.000 description 4
- 229910017604 nitric acid Inorganic materials 0.000 description 4
- 229910052698 phosphorus Inorganic materials 0.000 description 4
- 239000011574 phosphorus Substances 0.000 description 4
- 238000011946 reduction process Methods 0.000 description 4
- 150000003839 salts Chemical class 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 238000001291 vacuum drying Methods 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 239000003990 capacitor Substances 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 230000003068 static effect Effects 0.000 description 2
- LWIHDJKSTIGBAC-UHFFFAOYSA-K tripotassium phosphate Chemical compound [K+].[K+].[K+].[O-]P([O-])([O-])=O LWIHDJKSTIGBAC-UHFFFAOYSA-K 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- -1 KBF 4 Inorganic materials 0.000 description 1
- 229910020808 NaBF Inorganic materials 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- 239000004115 Sodium Silicate Substances 0.000 description 1
- OLBVUFHMDRJKTK-UHFFFAOYSA-N [N].[O] Chemical compound [N].[O] OLBVUFHMDRJKTK-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 229910021538 borax Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000011534 incubation Methods 0.000 description 1
- 238000007885 magnetic separation Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- DOTMOQHOJINYBL-UHFFFAOYSA-N molecular nitrogen;molecular oxygen Chemical compound N#N.O=O DOTMOQHOJINYBL-UHFFFAOYSA-N 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000003921 particle size analysis Methods 0.000 description 1
- 235000014786 phosphorus Nutrition 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229910000160 potassium phosphate Inorganic materials 0.000 description 1
- 235000011009 potassium phosphates Nutrition 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000001488 sodium phosphate Substances 0.000 description 1
- 229910000162 sodium phosphate Inorganic materials 0.000 description 1
- 235000011008 sodium phosphates Nutrition 0.000 description 1
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
- 229910052911 sodium silicate Inorganic materials 0.000 description 1
- 239000004328 sodium tetraborate Substances 0.000 description 1
- 235000010339 sodium tetraborate Nutrition 0.000 description 1
- 238000005477 sputtering target Methods 0.000 description 1
- 230000026676 system process Effects 0.000 description 1
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 description 1
Classifications
-
- 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
- B22F1/05—Metallic powder characterised by the size or surface area of the 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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
- B22F1/142—Thermal or thermo-mechanical treatment
-
- 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
- B22F1/14—Treatment of metallic powder
- B22F1/145—Chemical treatment, e.g. passivation or decarburisation
-
- 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
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Powder Metallurgy (AREA)
Abstract
The application provides tantalum powder and a preparation method of the tantalum powder. The oxygen mass content of the tantalum powder is 20000-50000ppm, and the mass ratio of oxygen to nitrogen in the tantalum powder is (4-25): 1, the average particle size of the tantalum powder is below 0.7 mu m. Oxygen and nitrogen in the tantalum powder are also doped on the surface of the tantalum powder, nitrogen is dispersed on the surface of the tantalum powder in a solid solution mode, oxygen is dispersed on the surface of the tantalum powder in a tantalum oxide mode, and the particle size of the tantalum powder is smaller, so that the tantalum powder has higher specific surface area, and higher oxygen content and nitrogen content can be simultaneously realized when the tantalum powder and the nitrogen are doped simultaneously. And the influence of the nitrogen content in the tantalum powder on the oxygen content is also found, when the mass ratio of oxygen to nitrogen is controlled within the range, the oxygen content is improved, the stability of the tantalum powder is greatly improved, and the problem that the tantalum powder is easy to catch fire in the passivation process is well controlled.
Description
Technical Field
The application relates to the field of materials, in particular to tantalum powder and a preparation method of the tantalum powder.
Background
Tantalum is a rare metal that is considered an emerging strategic metal. The tantalum capacitor has the advantages of wide working temperature range, high reliability, shock resistance, long service life and the like, so that the tantalum capacitor is widely applied to electronic equipment such as communication, computers, mobile phones and the like, particularly has irreplaceable price in the fields of energy sources, national defense, high and new technology and the like, and greatly increases the usage amount along with the beneficial expansion of the application range.
The industrial process mainly uses sodium reduction method of potassium fluorotantalate to prepare metal tantalum powder, and is characterized by that NaCl, KCl, KF or the mixture of the above-mentioned two or three salts is mixed and placed into a reaction container, then the potassium fluorotantalate is added into the container, under the protection of argon gas, under the condition of above 700 deg.C sodium injection stirring and reduction are implemented. Removing soluble salt and excessive sodium from the reduction product after the reduction product is discharged out of the furnace by a static or dynamic water washing method, removing other impurities by acid washing by nitric acid, hydrochloric acid, hydrofluoric acid and the like, filtering and washing to be neutral by pure water, and carrying out vacuum drying, and obtaining the raw powder of sodium reduction tantalum powder by sieving and magnetic separation.
Tantalum powder is mainly used for preparing sputtering targets of various tantalum materials, barrier layers between integrated circuit copper wires and silicon, additives for alloys and tantalum powder applied to medical treatment, so that the quality of the tantalum powder is mainly measured by physical properties and chemical components. The performance parameters of the metallurgical grade tantalum powder comprise the granularity distribution, the particle morphology, the chemical impurities, the apparent specific gravity, the electrical performance and the like of the tantalum powder.
Tantalum metal has high affinity with oxygen, and tantalum is oxidized to generate Ta 2 O 5 Is exothermic reaction, and the tantalum powder surface is provided with a layer of compact tantalum oxide film to prevent the tantalum from being oxidized continuously. When (when)When the temperature is above 300 ℃, the tantalum oxide film is cracked and destroyed, part of oxygen is dissolved into the tantalum matrix, and part of oxygen escapes. The heated tantalum powder is cooled and then contacts with an oxygen-containing medium to oxidize the surface, absorb new oxygen and increase the oxygen content. Therefore, in order to improve the stability of the tantalum powder, passivation treatment is needed, but the oxygen absorption process of passivation treatment is an exothermic process, so that the ignition of the tantalum powder is easily caused, the oxygen absorption degree of the tantalum powder is limited, so that the production of the tantalum powder with high oxygen content is always a difficult point in the industry, and the performance research and the application development of the tantalum powder with high oxygen content are limited.
Disclosure of Invention
The application provides tantalum powder and a preparation method thereof, which are used for solving the problem of insufficient oxygen content of the tantalum powder.
The first aspect of the application provides tantalum powder, wherein the oxygen mass content of the tantalum powder is 20000-50000ppm, and the mass ratio of oxygen to nitrogen in the tantalum powder is (4-25): 1, the average particle size of the tantalum powder is below 0.7 mu m.
In any embodiment of the first aspect of the present application, the tantalum powder has an average particle size of 0.2 μm to 0.6 μm, optionally the tantalum powder has a nitrogen mass content of greater than or equal to 2000ppm, optionally the tantalum powder has a nitrogen mass content of 2000ppm to 4700ppm.
In any embodiment of the first aspect of the present application, the total mass content of the metallic impurities Fe, ni and Cr in the tantalum powder is <20ppm, and the mass content of c is <50ppm.
The second aspect of the present application provides a method for preparing tantalum powder, the method comprising: reducing potassium fluorotantalate in a reactor by adopting a sodium reduction method to prepare a nitrogen-containing tantalum powder precursor, and introducing high-purity nitrogen into the reactor after sodium injection of sodium reduction is started, wherein the flow of the high-purity nitrogen is greater than or equal to 60L/h relative to 80kg-100kg potassium fluorotantalate; washing, pickling, filtering, washing and drying the precursor of the nitrogen-containing tantalum powder to obtain nitrogen-containing tantalum powder; mixing the nitrogen-containing tantalum powder with a refiner, performing sintering treatment for n times, cooling to 10-40 ℃ in each sintering treatment, vacuumizing, and then starting to introduce oxygen-containing gas for oxygen absorption passivation treatment to obtain tantalum powder, wherein n is more than or equal to 1 and less than or equal to 5, and the oxygen absorption passivation time is 10-60 hours.
In any embodiment of the second aspect of the present application, the refiner comprises one or more of a phosphorus-containing refiner, a boron-containing refiner, an arsenic-containing refiner, an yttrium-containing refiner, and a silicon-containing refiner, optionally in a weight ratio of the refiner to tantalum powder of 50ppm to 300ppm.
In any embodiment of the second aspect of the present application, the process for preparing the nitrogen-containing tantalum powder precursor in the reactor by sodium reduction comprises: mixing KCl, KF and potassium fluotantalate in a reactor, heating to a preset temperature under the protection of inert gas after the mixing is completed, starting sodium injection, closing argon gas to introduce high-purity nitrogen until the heat preservation is finished, and obtaining a nitrogen-containing tantalum powder precursor, wherein the preset temperature is optionally 850-950 ℃, the flow of the high-purity nitrogen is optionally 60-100L/h relative to 80-100 kg potassium fluotantalate, and the heat preservation time is optionally 0.5-1.5 h.
In any of the embodiments of the second aspect of the present application, the process of mixing the nitrogen-containing tantalum powder with the refiner and then performing the sintering process n times includes: step A, sintering nitrogen-containing tantalum powder in reaction equipment under inert gas or vacuum condition, wherein the optional sintering temperature is 1000-1500 ℃, the heat preservation time is 0.5-3 h, then cooling to 10-40 ℃, vacuumizing, oxygen introducing and stopping oxygen introducing operation and circulating for 10-30 h to perform oxygen inhalation passivation treatment, wherein the duration of oxygen introducing is 10s-20s, and the duration of oxygen introducing stopping is 15-30min; step B, repeating the step A for n-1 times.
In any embodiment of the second aspect of the present application, the reaction apparatus is evacuated to a pressure of-0.03 MPa to-0.07 MPa.
In any embodiment of the second aspect of the present application, the operations of evacuating-oxygen-introducing-stopping oxygen-introducing are started when the temperature is lowered to 32-35 ℃.
In any of the embodiments of the second aspect of the present application, the potassium fluorotantalate has a mass content of C of <20ppm, and the mass contents of fe, ni, and Cr of <20 ppm; the mass content of Si is less than 10ppm, the mass content of Nb is less than 10ppm, and the trace element is less than 5ppm.
In any embodiment of the second aspect of the present application, the filtering and washing includes cold water filtering and washing and hot water filtering and washing performed sequentially, the temperature of the cold water being 10 ℃ to 20 ℃; and (3) when the temperature of the hot water is 50-80 ℃, the hot water is used for filtering and washing when the conductivity of the filtrate is smaller than 30 mu s/cm, and the hot water is used for filtering and washing when the conductivity of the filtrate is smaller than 30 mu s/cm, stopping filtering and washing.
In the tantalum powder, oxygen and nitrogen are doped on the surface of the tantalum powder, nitrogen is dispersed on the surface of the tantalum powder in a solid solution mode, oxygen is dispersed on the surface of the tantalum powder in a tantalum oxide mode, and the particle size of the tantalum powder is smaller, so that the tantalum powder has higher specific surface area, and higher oxygen content and nitrogen content can be simultaneously realized when the oxygen and the nitrogen are doped simultaneously. And the influence of the nitrogen content in the tantalum powder on the oxygen content is also found, when the mass ratio of oxygen to nitrogen is controlled within the range, the oxygen content is improved, the stability of the tantalum powder is greatly improved, and the problem that the tantalum powder is easy to catch fire in the passivation process is well controlled.
Detailed Description
Embodiments of the present application are described in further detail below in conjunction with examples. The following detailed description of the embodiments is provided to illustrate the principles of the present application and is not intended to limit the scope of the application, i.e., the application is not limited to the embodiments described.
As analyzed in the background of the present application, the tantalum powder of the prior art is deficient in oxygen content. In order to solve the problem, the application provides tantalum powder and a preparation method of the tantalum powder.
The first embodiment of the application provides tantalum powder, wherein the oxygen content of the tantalum powder is 20000-50000ppm, and the mass ratio of oxygen to nitrogen in the tantalum powder is (4-25): 1, and the average particle size of the tantalum powder is below 0.7 mu m.
In the tantalum powder, oxygen and nitrogen are doped on the surface of the tantalum powder, nitrogen is dispersed on the surface of the tantalum powder in a solid solution mode, oxygen is dispersed on the surface of the tantalum powder in a tantalum oxide mode, and the particle size of the tantalum powder is smaller, so that the tantalum powder has higher specific surface area, and higher oxygen content and nitrogen content can be simultaneously realized when the oxygen and the nitrogen are doped simultaneously. And the influence of the nitrogen content in the tantalum powder on the oxygen content is also found, when the mass ratio of oxygen to nitrogen is controlled within the range, the oxygen content is improved, the stability of the tantalum powder is greatly improved, and the problem that the tantalum powder is easy to catch fire in the passivation process is well controlled.
The oxygen content in the tantalum powder breaks through the limitation of the oxygen content in the prior art, so that the tantalum powder is favorable for being applied to the field of metallurgy, particularly for exploring the influence of the oxygen content on the performance of metallurgical products, and the application range of the high-oxygen tantalum powder is widened.
In some embodiments of the present application, the tantalum powder has an average particle size of 0.2 μm to 0.6 μm. Compared with conventional tantalum powder with the particle size of more than 1 micron, the particle size of the tantalum powder is greatly reduced, so that the specific surface area of the tantalum powder is larger, and a good foundation is provided for nitrogen-oxygen doping.
In some embodiments of the present application, the nitrogen content is greater than or equal to 2000ppm, optionally the tantalum powder has a nitrogen content of 2000ppm to 4700ppm.
To further increase the purity of the tantalum powder, in some embodiments of the present application, the total mass content of the metallic impurities Fe, ni, and Cr in the tantalum powder is <20ppm, and the mass content of c is <50ppm.
In a second embodiment of the present application, there is provided a method for preparing tantalum powder, the method comprising: reducing potassium fluorotantalate in a reactor by adopting a sodium reduction method to prepare a nitrogen-containing tantalum powder precursor, and introducing high-purity nitrogen into the reactor after sodium injection of sodium reduction is started, wherein the flow of the high-purity nitrogen is greater than or equal to 60L/h relative to 80kg-100kg potassium fluorotantalate; washing, pickling, filtering, washing and drying the precursor of the nitrogen-containing tantalum powder to obtain nitrogen-containing tantalum powder; mixing the nitrogen-containing tantalum powder with a refiner, performing sintering treatment for n times, cooling to 10-40 ℃ in each sintering treatment, vacuumizing, and then starting to introduce oxygen-containing gas for oxygen absorption passivation treatment to obtain tantalum powder, wherein n is more than or equal to 1 and less than or equal to 5, and the oxygen absorption passivation time is 10-60 hours.
Nitrogen is introduced into the sodium reduction process to carry out nitrogen doping, so that the nitrogen doping amount and the uniformity of nitrogen doping are improved; on the basis of high nitrogen doping, oxygen absorption passivation treatment is carried out for a plurality of times after sintering, so that the oxygen doping amount is increased. The grain refiner is doped before sintering, so that the growth of tantalum powder grains in the sintering process is effectively controlled, and the tantalum powder maintains higher specific surface area during oxygen inhalation passivation; meanwhile, the sintering treatment is repeated for n times, so that the oxygen doping amount is improved on the basis of improving the safety. And the nitrogen doping is performed firstly and then the oxygen doping is performed, the presence of the nitrogen is beneficial to the improvement of the oxygen doping amount, and the oxygen doping also has a certain adjusting effect on the content of the doped nitrogen, so that the reasonable oxygen-nitrogen ratio is obtained, and the stability of the tantalum powder is beneficial to improvement.
The n may be 1, 2, 3, 4 or 5.
The high-purity nitrogen is commercial gas in the field, and the higher the purity is, the better the purity is on the basis of meeting the basic purity requirement of the high-purity nitrogen, and the upper limit of the purity is not required.
The above oxygen-containing gas is mainly used for providing oxygen for passivation, and the oxygen-containing gas commonly used in passivation in this stage can be used, for example, air, or a mixed gas of air and an inert gas (such as argon), or a mixed gas of oxygen and an inert gas (such as argon) can be selected. In some embodiments, the concentration of oxygen in the oxygen-containing gas is preferably below 21vol%, and the lower the oxygen concentration, the easier the safety of the oxygen absorption passivation process can be controlled, but the oxygen absorption passivation efficiency can be affected. In order to improve the oxygen absorption passivation efficiency, the concentration of oxygen in the oxygen-containing gas is preferably 10Vol% to 21Vol%.
The refiner is mainly used for controlling the agglomeration of tantalum powder in the sintering process, and can effectively control the particle diameter of the tantalum powder. In some embodiments, the refiners include one or more of phosphorus-containing refiners, boron-containing refiners, arsenic-containing refiners, yttrium-containing refiners, and silicon-containing refiners. Such as phosphorus-containing refiners including but not limited to sodium phosphate, potassium phosphate, ammonium dihydrogen phosphate, phosphorus or phosphide, etc., boron-containing refiners including but not limited to borax, KBF 4 、NaBF 4 Silicon-containing refiners include, but are not limited to, silicic acid, sodium silicate, or silicon nitride, among others.
In order to enhance the control effect on the grain size of the tantalum powder and reduce the addition of the refiner resulting in excessive introduction of impurity elements, in some embodiments, the weight proportion of the refiner with respect to the tantalum powder is optionally 50ppm to 300ppm.
In some embodiments of the present application, the process for preparing a nitrogen-containing tantalum powder precursor in a reactor using a sodium reduction process comprises: and (3) mixing KCl, KF and potassium fluotantalate in a reactor, heating to a preset temperature under the protection of inert gas after the mixing is completed, starting sodium injection, and simultaneously closing argon to introduce high-purity nitrogen until the heat preservation is finished, so as to obtain the nitrogen-containing tantalum powder precursor. In addition to the introduction of high purity nitrogen, the implementation process of the sodium reduction method can be referred to by a conventional sodium reduction method, such as the proportion of KCl, KF and potassium fluorotantalate, a predetermined temperature and the like.
In some embodiments, the optional predetermined temperature is 850-950 ℃, and the optional incubation time is 0.5h-1.5h, thereby increasing sodium reduction efficiency. In some embodiments, to increase the utilization of high purity nitrogen, the flow rate of high purity nitrogen is optionally 60L/h to 100L/h relative to 80kg to 100kg potassium fluorotantalate.
In some embodiments, the process of mixing the nitrogen-containing tantalum powder with the refiner and then performing the n sintering treatments includes: step A, sintering nitrogen-containing tantalum powder in reaction equipment under inert gas or vacuum condition, wherein the optional sintering temperature is 1000-1500 ℃, the heat preservation time is 0.5-3 h, then cooling to 10-40 ℃, vacuumizing, oxygen introducing and stopping oxygen introducing operation and circulating for 10-30 h to perform oxygen inhalation passivation treatment, wherein the duration of oxygen introducing is 10s-20s, and the duration of oxygen introducing stopping is 15-30min; step B, repeating the step A for n-1 times.
The sintering improves the surface activity of tantalum powder and provides favorable conditions for oxygen inhalation passivation; and the sintering temperature can lead the oxide film formed each time to be fully broken and dispersed so as to form a compact and uniform oxide film on the surface of the tantalum powder. The oxygen absorption passivation is realized by adopting the process of circularly repeating the vacuumizing, oxygen introducing and oxygen introducing stopping processes, and the oxygen introduced before the oxygen introducing stopping period is subjected to oxidation reaction with the surface of the tantalum powder, so that the oxygen introducing stopping time is longer because the oxygen introducing time is shorter each time, the oxidation reaction degree can be controlled, and the oxidation uniformity can be improved. The sintering treatment can be carried out for a plurality of times, so that the compactness of the oxide film on the surface of the tantalum powder is further improved.
To further control safety, in some embodiments, the reaction apparatus is evacuated to a pressure of-0.03 MPa to-0.07 MPa.
In some embodiments, to increase passivation efficiency, the evacuation-oxygen-purging-stopping the oxygen purging operation is initiated when the temperature is reduced to 32-35 ℃.
To further increase the purity of the resulting tantalum powder, in some embodiments, the potassium fluorotantalate has a mass content of C of <20ppm, and a mass content of Fe, ni, and Cr of <20 ppm; the mass content of Si is less than 10ppm, the mass content of Nb is less than 10ppm, and the trace element is less than 5ppm.
The water washing, acid washing, filtering washing and drying processes in the preparation method can refer to the conventional operation.
After the reduction product containing the nitrogen-containing tantalum powder precursor is discharged from the furnace, soluble salts and excessive sodium are removed by a static or dynamic water washing method. The unopened particles in the water washing process are broken up by stirring and washing, so that other impurities are further removed.
Metal impurities such as Fe, ni, cr, C, si are removed by acid washing. In some embodiments, the acid used for the acid wash comprises nitric acid, hydrofluoric acid, and water in a mass ratio of (3.5-4.0): 0.4 (21-23). Thereby improving the removal efficiency of each metal impurity.
Acid used for acid washing is removed by filtration washing, so that corrosion of acid to subsequent processing equipment is avoided, and the content of metal impurities in tantalum powder is increased, and in some embodiments, the filtration washing comprises cold water filtration washing and hot water filtration washing which are sequentially carried out, and the temperature of cold water is 10-20 ℃; and (3) when the temperature of the hot water is 50-80 ℃, the hot water is used for filtering and washing when the conductivity of the filtrate is smaller than 30 mu s/cm, and the hot water is used for filtering and washing when the conductivity of the filtrate is smaller than 30 mu s/cm, stopping filtering and washing. Thereby removing the acid as clean as possible.
Drying may be performed using a vacuum oven, in some embodiments, at a temperature of 120-150 ℃. In order to further remove the influence of large-particle impurities, the powder is dried and then screened, wherein the number of the screened meshes is 50-100.
By using the preparation method of the application, the tantalum powder of any of the previous embodiments can be prepared.
The advantageous effects of the present application will be further described below with reference to examples and comparative examples, but the scope of the present invention is not limited to these examples.
The analysis equipment and the particle size analysis equipment of the main elements in the tantalum powder obtained in the following examples are recorded in table 1.
TABLE 1
In the potassium fluotantalate used in each example, the mass content of C is less than 20ppm, and the mass content of Fe, ni and Cr is less than 20ppm; the mass content of Si is less than 10ppm, the mass content of Nb is less than 10ppm, and the trace element is less than 5ppm.
Example 1
1) And (3) reduction: adding KCl, KF and potassium fluorotantalate into a reactor according to the weight ratio of 3.5:2.5:1, mixing (the mass of the potassium fluorotantalate is 90 kg), heating to 850 ℃ under the protection of argon, starting sodium injection, closing the argon, introducing high-purity nitrogen into the reactor at the flow rate of 60L/h-70L/h until the heat preservation is finished after 1h, and obtaining a nitrogen-containing reduction product.
2) Washing: after the reduction product is discharged from the furnace, soluble salt and excessive sodium are removed by a water washing method, unopened particles are broken up by stirring in the water system process, and other impurities are further removed, so that a water-washed material is obtained.
3) Acid washing: adding water into 65% nitric acid and 40% hydrofluoric acid to prepare an acid solution, wherein the ratio of the nitric acid solution to the hydrofluoric acid solution to the water is 6:1:20, and pickling the material after water washing by using the acid solution to obtain the material after pickling.
4) And (3) filtering and washing: placing the pickled material into a filtering and washing tank for filtering and washing, filtering and washing with cold water at 15-20 ℃ until the conductivity is less than 30 mu s/cm, then exchanging hot water at 50-60 ℃, filtering and washing with hot water until the conductivity is less than 30 mu s/cm, and discharging the filtered and washed material into a vacuum drying box.
5) And (3) drying: and drying the filtered and washed material by using a vacuum drying box at the drying temperature of 120-150 ℃.
6) And (3) screening: sieving the dried material with a sieve with 80 meshes to obtain the nitrogen-containing tantalum powder.
7) Sintering: mixing nitrogen-containing tantalum powder and monoammonium phosphate, and performing sintering treatment, wherein the weight proportion of monoammonium phosphate relative to the tantalum powder is 100ppm. The tray loading amount in the sintering treatment process is 0.7 kg/tray, the highest sintering temperature is 1100 ℃, the heating rate is 10 ℃/min, the temperature is kept for 3 hours, the temperature is reduced to be less than 34 ℃ and oxygen inhalation passivation is started: vacuumizing the furnace to-0.05 MPa, opening a valve, introducing air for 15s, and closing the valve for 15-30min; vacuumizing the furnace to-0.05 MPa, opening the valve again, introducing air, closing the valve, continuing for 15-30min, repeating the steps, taking out after oxygen absorption and passivation for 18h, and sieving with a 50-mesh sieve after taking out to obtain a sample A. The chemical impurity content is shown in Table 2.
Example 2
Steps 1) to 6) are the same as in example 1.
7) Sintering: mixing nitrogen-containing tantalum powder and monoammonium phosphate, and performing sintering treatment, wherein the weight proportion of monoammonium phosphate relative to the tantalum powder is 150ppm. The tray loading amount in the sintering treatment process is 0.7 kg/tray, the sintering temperature of the first sintering treatment is 1250 ℃, the heating rate is 10 ℃/min, the temperature is kept for 1 hour, and then the temperature is reduced to be less than 34 ℃ to start oxygen inhalation passivation: vacuumizing the furnace to-0.05 MPa, opening a valve, introducing air for 15s, and closing the valve for 15-30min; vacuumizing the furnace to-0.05 MPa, opening the valve, introducing air for 15s, closing the valve, and repeating the steps for 18h for 15-30 min. And (3) after oxygen absorption passivation is finished, the blank is not broken, secondary sintering treatment is directly carried out, the secondary sintering treatment flow is the same as that of the primary sintering treatment, the oxygen absorption passivation time in the secondary sintering treatment is 26 hours, and the sample B is obtained after the sample B is discharged from a furnace and is sieved by a 50-mesh sieve. The chemical impurity content is shown in Table 2.
Example 3
Steps 1) to 6) are the same as in example 1.
7) Sintering: mixing nitrogen-containing tantalum powder and monoammonium phosphate, and performing sintering treatment, wherein the weight proportion of monoammonium phosphate relative to the tantalum powder is 200ppm. The tray loading amount in the sintering treatment process is 0.7 kg/tray, the highest sintering temperature in the first sintering treatment is 1400 ℃, the heating rate is 10 ℃/min, the temperature is kept for 0.5 hour, the temperature is reduced to be less than 34 ℃ and oxygen absorption passivation is started: vacuumizing the furnace to-0.05 MPa, opening a valve, introducing air for 15s, closing the valve and keeping for 15-30min; vacuumizing the furnace to-0.05 MPa, opening a valve, introducing air for 15s, closing the valve for 15-30min, and repeating the steps for 18h. After passivation, the blank is not broken, secondary sintering treatment is directly carried out, the secondary sintering treatment flow is the same as the primary sintering treatment, and the oxygen absorption passivation time in the secondary sintering treatment is 26 hours; and after passivation, the blank is not broken, and then three times of sintering treatment are carried out, wherein the flow of the three times of sintering treatment is the same as that of the first sintering treatment, the oxygen absorption passivation time in the three times of sintering treatment is 12 hours, and the sample C is obtained by crushing and sieving with a 50-mesh sieve after discharging. The chemical impurity content is shown in Table 2.
Example 4
Steps 1) to 6) are the same as in example 1.
7) Sintering: mixing nitrogen-containing tantalum powder and monoammonium phosphate, and performing sintering treatment, wherein the weight proportion of monoammonium phosphate relative to the tantalum powder is 80ppm. The rest of the procedure is as in example 2. Sample D was obtained. The chemical impurity content is shown in Table 2.
Example 5
Steps 1) to 6) are the same as in example 1.
7) Sintering: mixing nitrogen-containing tantalum powder and monoammonium phosphate, and performing sintering treatment, wherein the weight proportion of monoammonium phosphate relative to the tantalum powder is 300ppm. The rest of the procedure is as in example 2. Sample E was obtained. The chemical impurity content is shown in Table 2.
Example 6
Steps 1) to 6) are the same as in example 1.
7) Sintering: mixing nitrogen-containing tantalum powder and monoammonium phosphate, and performing sintering treatment, wherein the weight proportion of monoammonium phosphate relative to the tantalum powder is 50ppm. The rest of the procedure is as in example 2. Sample F was obtained. The chemical impurity content is shown in Table 2.
Example 7
Steps 1) to 6) are the same as in example 1.
7) Sintering: mixing nitrogen-containing tantalum powder and monoammonium phosphate, and performing sintering treatment, wherein the weight proportion of monoammonium phosphate relative to the tantalum powder is 400ppm. The rest of the procedure is as in example 2. Sample G was obtained. The chemical impurity content is shown in Table 2.
Example 8
Steps 1) to 6) are the same as in example 1.
7) Sintering: mixing nitrogen-containing tantalum powder and monoammonium phosphate, and performing sintering treatment, wherein the weight proportion of monoammonium phosphate relative to the tantalum powder is 100ppm. The tray loading amount in the sintering treatment process is 0.7 kg/tray, the highest sintering temperature is 1100 ℃, the heating rate is 10 ℃/min, the temperature is kept for 3 hours, the temperature is reduced to be less than 34 ℃ and oxygen inhalation passivation is started: vacuumizing the furnace to-0.05 MPa, opening a valve, introducing air for 15s, and closing the valve for 5-10 min; vacuumizing the furnace to-0.05 MPa, opening the valve again, introducing air, closing the valve for 5-10 min, repeating the steps, taking out after oxygen absorption and passivation for 18H, and sieving with a 50-mesh sieve after taking out to obtain a sample H. The chemical impurity content is shown in Table 2.
Comparative example 1
Steps 1) to 6) are the same as in example 1.
7) Sintering: no refiner was used during sintering. The rest of the procedure is as in example 2. Sample I was obtained. The chemical impurity content is shown in Table 2.
Comparative example 2
1) And (3) reduction: adding KCl, KF and potassium fluorotantalate into a reactor according to the weight ratio of 3.5:2.5:1, mixing (the mass of the potassium fluorotantalate is 90 kg), heating to 800 ℃ under the protection of argon, starting sodium injection, closing the argon, and introducing high-purity nitrogen into the reactor at the flow rate of 40L/h-50L/h until the heat preservation is finished after 1, thus obtaining the nitrogen-containing reduction product.
Steps 2) to 7) are the same as in example 2. Sample J was obtained. The chemical impurity content is shown in Table 2.
Table 2: chemical impurity content of sample
It can be seen that the tantalum powder with high oxygen and high nitrogen is prepared in each example, the average granularity is below 1 mu m, the oxygen content is 20000-50000ppm, the nitrogen content is more than 2000ppm, the metal impurity content Sigma Fe+Ni+Cr is less than 20PPm, and the C content is less than 50 ppm; and the obtained high-oxygen high-nitrogen tantalum powder has no temperature rise phenomenon when being placed in the air for 24 hours, which proves that the high-oxygen high-nitrogen tantalum powder has better stability.
The reduction process of comparative example 2, without the use of a refiner, resulted in a lower oxygen content and a larger average particle size, and the reduction process of comparative example 1 had a lower nitrogen loading pressure, resulting in a lower nitrogen content, while also affecting the oxygen content.
The present application is not limited to the above embodiment. The above embodiments are merely examples, and embodiments having substantially the same configuration and the same effects as those of the technical idea within the scope of the present application are included in the technical scope of the present application. Further, various modifications that can be made to the embodiments and other modes of combining some of the constituent elements in the embodiments, which are conceivable to those skilled in the art, are also included in the scope of the present application within the scope not departing from the gist of the present application.
Claims (10)
1. The tantalum powder is characterized in that the oxygen mass content of the tantalum powder is 20000-50000ppm, and the mass ratio of oxygen to nitrogen in the tantalum powder is (4-25): 1, wherein the average particle size of the tantalum powder is below 0.7 mu m.
2. Tantalum powder according to claim 1, characterised in that the tantalum powder has an average particle size of 0.2 μm to 0.6 μm, optionally the nitrogen mass content of the tantalum powder is greater than or equal to 2000ppm, optionally the nitrogen mass content of the tantalum powder is 2000ppm to 4700ppm.
3. Tantalum powder according to claim 1, characterised in that the total mass content of metallic impurities Fe, ni and Cr in the tantalum powder is <20ppm, the mass content of c is <50ppm.
4. A method for preparing tantalum powder, comprising the steps of:
reducing potassium fluorotantalate in a reactor by adopting a sodium reduction method to prepare a nitrogen-containing tantalum powder precursor, and introducing high-purity nitrogen into the reactor after sodium injection of sodium reduction begins, wherein the flow of the high-purity nitrogen is greater than or equal to 60L/h relative to 80kg-100kg potassium fluorotantalate;
washing, pickling, filtering, washing and drying the nitrogen-containing tantalum powder precursor to obtain nitrogen-containing tantalum powder;
mixing the nitrogen-containing tantalum powder with a refiner, performing sintering treatment for n times, cooling to 10-40 ℃ in each sintering treatment, vacuumizing, and then starting to introduce oxygen-containing gas for oxygen absorption passivation treatment to obtain the tantalum powder, wherein n is more than or equal to 1 and less than or equal to 5, and the oxygen absorption passivation time is 10-60 hours.
5. The method of claim 4, wherein the refiner comprises one or more of a phosphorous-containing refiner, a boron-containing refiner, an arsenic-containing refiner, an yttrium-containing refiner, and a silicon-containing refiner, optionally in a weight ratio of 50ppm to 300ppm relative to the tantalum powder.
6. The method of claim 4 or 5, wherein the preparing the nitrogen-containing tantalum powder precursor in the reactor by sodium reduction comprises:
and mixing KCl, KF and potassium fluorotantalate in the reactor, heating to a preset temperature under the protection of inert gas after the mixing is completed, starting sodium injection, simultaneously closing argon gas to introduce the high-purity nitrogen until the heat preservation is finished, and obtaining the nitrogen-containing tantalum powder precursor, wherein the preset temperature is optionally 850-950 ℃, the flow of the high-purity nitrogen is optionally 60-100L/h relative to 80-100 kg potassium fluorotantalate, and the heat preservation time is optionally 0.5-1.5 h.
7. The method according to any one of claims 4 to 6, wherein the process of mixing the nitrogen-containing tantalum powder with a refiner and then performing sintering treatment n times comprises:
step A, sintering the nitrogen-containing tantalum powder in reaction equipment under inert gas or vacuum condition, wherein the optional sintering temperature is 1000-1500 ℃, the heat preservation time is 0.5-3 h, then the reaction equipment is subjected to vacuumizing-oxygen-introducing-stopping oxygen-introducing operation and circulation for 10-30 h when the temperature is reduced to 10-40 ℃ so as to perform oxygen-absorbing passivation treatment, and the duration of each oxygen-introducing is 10s-20s, and the duration of each oxygen-introducing-stopping time is 15-30min;
and B, repeating the step A for n-1 times.
8. The production method according to any one of claims 4 to 7, wherein the reaction apparatus is evacuated to a pressure of-0.03 MPa to-0.07 MPa.
9. The method according to any one of claims 4 to 8, wherein the operations of vacuum-oxygen-introducing and oxygen-introducing are started when the temperature is lowered to 32 ℃ to 35 ℃.
10. The production method according to any one of claims 4 to 9, wherein the potassium fluorotantalate has a mass content of C of <20ppm, and a mass content of fe, ni and Cr of <20 ppm; the mass content of Si is less than 10ppm, the mass content of Nb is less than 10ppm, and the trace element is less than 5ppm.
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