CN117086321A - Preparation method of superfine tungsten powder - Google Patents
Preparation method of superfine tungsten powder Download PDFInfo
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- CN117086321A CN117086321A CN202311350667.XA CN202311350667A CN117086321A CN 117086321 A CN117086321 A CN 117086321A CN 202311350667 A CN202311350667 A CN 202311350667A CN 117086321 A CN117086321 A CN 117086321A
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- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 title claims abstract description 63
- 238000002360 preparation method Methods 0.000 title claims abstract description 31
- 239000000843 powder Substances 0.000 claims abstract description 55
- 238000006243 chemical reaction Methods 0.000 claims abstract description 36
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 claims abstract description 35
- 229910001930 tungsten oxide Inorganic materials 0.000 claims abstract description 35
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 31
- 239000010937 tungsten Substances 0.000 claims abstract description 31
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 30
- -1 tungsten nitride Chemical class 0.000 claims abstract description 25
- 239000002994 raw material Substances 0.000 claims abstract description 18
- 229910052786 argon Inorganic materials 0.000 claims abstract description 15
- 238000001816 cooling Methods 0.000 claims abstract description 15
- 238000002161 passivation Methods 0.000 claims abstract description 15
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 14
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000001257 hydrogen Substances 0.000 claims abstract description 14
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 14
- 230000035484 reaction time Effects 0.000 claims abstract description 11
- 238000001354 calcination Methods 0.000 claims description 23
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 10
- 239000002245 particle Substances 0.000 abstract description 9
- 239000000956 alloy Substances 0.000 abstract description 7
- 229910045601 alloy Inorganic materials 0.000 abstract description 7
- 229910021529 ammonia Inorganic materials 0.000 abstract description 5
- 239000013078 crystal Substances 0.000 abstract description 4
- 230000002159 abnormal effect Effects 0.000 abstract description 3
- 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 abstract 1
- 239000013067 intermediate product Substances 0.000 abstract 1
- 229910052708 sodium Inorganic materials 0.000 abstract 1
- 239000011734 sodium Substances 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- XAYGUHUYDMLJJV-UHFFFAOYSA-Z decaazanium;dioxido(dioxo)tungsten;hydron;trioxotungsten Chemical compound [H+].[H+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O XAYGUHUYDMLJJV-UHFFFAOYSA-Z 0.000 description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 239000002159 nanocrystal Substances 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 238000011217 control strategy Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 150000001247 metal acetylides Chemical class 0.000 description 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000005245 sintering Methods 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
- 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
- B22F9/22—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds using gaseous reductors
-
- 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
- B22F1/054—Nanosized 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
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
- B22F1/056—Submicron particles having a size above 100 nm up to 300 nm
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Composite Materials (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Materials Engineering (AREA)
- Crystallography & Structural Chemistry (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The invention relates to the technical field of powder preparation, in particular to a preparation method of superfine tungsten powder, which comprises the following steps: pretreating raw material sodium metatungstate to obtain tungsten oxide powder; in an ammonia atmosphere, carrying out deoxidization treatment on tungsten oxide powder in a tubular atmosphere furnace; after deoxidation is finished, introducing a high-purity argon set into the tubular atmosphere furnace for passivation treatment, and cooling the powder to room temperature for collection; placing the collected powder into a tubular atmosphere furnace for chemical reaction under the hydrogen atmosphere; according to the invention, the purpose of introducing the intermediate product tungsten nitride is realized by adopting different atmospheres in different preparation stages, and the prepared tungsten powder has the particle size range of 50-120nm and good powder dispersity by controlling the reaction temperature and the reaction time in each stage, so that the structure and the performance of the superfine crystal/nanocrystalline hard alloy can be effectively improved, and the problems of rapid tungsten oxide volatilization and abnormal tungsten powder growth caused by steam generation in the preparation process can be avoided.
Description
Technical Field
The invention relates to the technical field of powder preparation, in particular to a preparation method of superfine tungsten powder.
Background
The nano tungsten powder is the key for preparing the superfine crystal/nano crystal hard alloy. The development of the hard alloy forming technology and the sintering technology has greatly broken through today, and the use requirement of the ultra-fine grain/nano-crystal hard alloy can be basically met. However, further improvements in the performance of ultra-fine/nanocrystalline cemented carbides are more dependent on tungsten powder quality. Therefore, the preparation of high-quality nano tungsten powder becomes a necessary way for improving the performance of the ultra-fine grain/nano crystal hard alloy.
At present, the preparation method of the nano tungsten powder mainly comprises a tungsten oxide hydrogen reduction method and a carbon-assisted hydrogen reduction method, and is essentially to reduce the tungsten oxide powder into metal tungsten by utilizing reducing gas. A large amount of water vapor is formed in the process of reducing tungsten oxide into metal tungsten, and the volatilization of the tungsten oxide is accelerated by the water vapor, so that tungsten powder rapidly grows up, and even abnormal growth occurs. Therefore, reducing the water vapor content in the reaction stage becomes a key point for preparing high-quality nano tungsten powder.
Disclosure of Invention
The invention provides a preparation method of superfine tungsten powder, which overcomes the defects of the prior art, and can effectively solve the problems that the volatilization of tungsten oxide is accelerated by water vapor generated in the existing process of preparing tungsten powder by adopting a reduction method, so that the tungsten powder grows up rapidly and even an abnormal growth phenomenon occurs.
In order to solve the problems, the preparation method of the superfine tungsten powder comprises the following steps:
s101, pretreating raw material ammonium metatungstate to obtain tungsten oxide powder;
s201, in an ammonia gas atmosphere, carrying out deoxidization treatment on tungsten oxide powder in a tubular atmosphere furnace to obtain tungsten nitride powder;
s301, after deoxidation is finished, introducing a high-purity argon set into a tubular atmosphere furnace for passivation treatment, and cooling tungsten nitride powder to room temperature for collection;
s401, placing the tungsten nitride powder collected in the S301 in a tubular atmosphere furnace for chemical reaction in a hydrogen atmosphere to obtain tungsten powder;
s501, introducing high-purity argon into a tubular atmosphere furnace after the chemical reaction is finished for passivation treatment, and cooling tungsten powder to room temperature for collection.
The pretreatment of the raw material ammonium metatungstate to obtain tungsten oxide powder comprises the steps of calcining the raw material ammonium metatungstate in a muffle furnace at the temperature of 650 ℃ for 2-4 h.
The deoxidizing treatment in the step S201 is performed at 550-650deg.C for 1.5-3 h.
The reaction temperature of the chemical reaction in the step S401 is 800-900 ℃ and the reaction time is 1.5-3 h.
The embodiment of the invention discloses a preparation method of superfine tungsten powder, which is characterized in that a phase element control strategy is adopted to prepare tungsten powder, namely different atmospheres are adopted in different preparation phases, the aim of introducing intermediate tungsten nitride is fulfilled, the coexistence of hydrogen and oxygen elements in the preparation phase of tungsten powder is avoided in the form of N-generation O, the particle size range of the prepared tungsten powder is between 50 and 120nm by controlling the reaction temperature and the reaction time of each phase, the powder dispersity is better, the tissue and the performance of superfine crystal/nanocrystalline hard alloy can be effectively improved, and the problems that tungsten oxide is volatilized quickly due to steam generated in the preparation process, and the tungsten powder grows rapidly and grows abnormally are avoided; meanwhile, the raw materials required in the preparation process are easy to obtain, the reaction process is zero in pollution, and the green low-carbon high-quality development of the superfine tungsten powder preparation process is promoted.
Detailed Description
The present invention is not limited by the following examples, and specific embodiments can be determined according to the technical scheme and practical situations of the present invention.
Example 1: the embodiment discloses a preparation method of superfine tungsten powder, which comprises the following steps:
s101, pretreating raw material ammonium metatungstate to obtain tungsten oxide powder;
s201, in an ammonia gas atmosphere, carrying out deoxidization treatment on tungsten oxide powder in a tubular atmosphere furnace to obtain tungsten nitride powder;
s301, after deoxidation is finished, introducing a high-purity argon set into a tubular atmosphere furnace for passivation treatment, and cooling tungsten nitride powder to room temperature for collection;
s401, placing the tungsten nitride powder collected in the S301 in a tubular atmosphere furnace for chemical reaction in a hydrogen atmosphere to obtain tungsten powder;
s501, introducing high-purity argon into a tubular atmosphere furnace after the chemical reaction is finished for passivation treatment, and cooling tungsten powder to room temperature for collection.
In the step S101, the raw material ammonium metatungstate is pretreated to obtain tungsten oxide powder, which includes calcining the raw material ammonium metatungstate in a muffle furnace at 650 ℃ for 2-4 h.
Wherein, the calcination temperature is 650 ℃ because when the calcination temperature is lower, the ammonium metatungstate is difficult to decompose to form tungsten oxide powder; the energy consumption is high when the calcining temperature is too high; the tungsten oxide powder was obtained by calcining the raw material ammonium metatungstate as described above.
In the above step S201, the deoxidizing temperature of the deoxidizing treatment is 550-650 ℃ and the deoxidizing time is 1.5-3 h.
Wherein the deoxidization treatment aims at introducing intermediate tungsten nitride, avoiding the simultaneous existence of hydrogen element and oxygen element in the preparation stage of tungsten powder in the form of N-generation O, and avoiding the formation of water molecules because the water molecules react with tungsten oxide to generate volatile hydrate, WO X H 2 O→WO X .nH 2 O (g) ≡, tungsten oxide in the gas phase is deposited on tungsten particles by hydrogen reduction, so that the tungsten particles grow up; the deoxidization temperature is 550-650 ℃ to promote the decomposition of ammonia gas to generate hydrogen-nitrogen mixed gas, promote the process of using N generation O, and the reaction process is slow or even incomplete when the temperature is too low, and the tungsten oxide powder grows up when the temperature is too high.
In the step S401, the reaction temperature for performing the chemical reaction is 800-900 ℃ and the reaction time is 1.5-3 h.
Wherein, the reaction temperature of the chemical reaction is 800-900 ℃, so that the problem that the powder is difficult to decompose due to the too low temperature can be avoided, and the powder grows up due to the too high temperature.
In the above examples, the reason for selecting ammonium metatungstate as the raw material is specifically as follows: (1) Ammonium paratungstate or ammonium paratungstate is only a tungsten source, and yellow tungsten oxide is generated by dehydration at high temperature, but compared with ammonium paratungstate, the appearance structure of the ammonium paratungstate is more complex (the appearance structure of the ammonium paratungstate is flaky and needle-shaped), inheritance of the appearance structure can occur in the tungsten oxide, the appearance of the tungsten oxide powder is diversified, and the single appearance powder is not beneficial to obtaining; (2) Ammonium metatungstate is readily soluble in water, while ammonium paratungstate is slightly soluble in water, so that ammonium metatungstate has unique advantages in the development of new products in the later period as a tungsten source.
Example 2: the embodiment discloses a preparation method of superfine tungsten powder, which comprises the following steps:
s201, calcining a raw material ammonium metatungstate in a muffle furnace to obtain tungsten oxide powder; wherein the calcination temperature is 650 ℃ and the calcination time is 3 h;
s202, placing the tungsten oxide powder obtained by calcination in a tubular atmosphere furnace for deoxidization treatment in an ammonia atmosphere to obtain tungsten nitride powder; wherein the deoxidizing temperature is 650 ℃ and the deoxidizing time is 3 h;
s203, introducing high-purity argon into the tubular atmosphere furnace for passivation treatment after deoxidation is finished, and cooling tungsten nitride powder to room temperature for collection;
s204, placing the tungsten nitride powder obtained in the step S203 in a tubular atmosphere furnace for chemical reaction in a hydrogen atmosphere to obtain tungsten powder; wherein the reaction temperature is 850 ℃, and the reaction time is 2 h;
and S205, introducing high-purity argon into a tubular atmosphere furnace for passivation treatment after the chemical reaction is finished, cooling tungsten powder to room temperature, and collecting tungsten powder with the particle size of about 50 nm.
Example 3: the embodiment discloses a preparation method of superfine tungsten powder, which comprises the following steps:
s301, calcining a raw material ammonium metatungstate in a muffle furnace to obtain tungsten oxide powder; wherein the calcination temperature is 650 ℃ and the calcination time is 3 h;
s302, placing the tungsten oxide powder obtained by calcination in a tubular atmosphere furnace for deoxidization treatment in an ammonia atmosphere to obtain tungsten nitride powder; wherein the deoxidizing temperature is 650 ℃ and the deoxidizing time is 3 h;
s303, introducing high-purity argon into the tubular atmosphere furnace for passivation treatment after deoxidation is finished, and cooling tungsten nitride powder to room temperature for collection;
s304, placing the tungsten nitride powder obtained in the step S303 into a tubular atmosphere furnace for chemical reaction in a hydrogen atmosphere to obtain tungsten powder; wherein the reaction temperature is 850 ℃, and the reaction time is 3 h;
and S305, introducing high-purity argon into the tubular atmosphere furnace for passivation treatment after the chemical reaction is finished, cooling the tungsten powder to room temperature, and collecting the tungsten powder with the particle size of 63 nm.
Example 4: the embodiment discloses a preparation method of superfine tungsten powder, which comprises the following steps:
s401, calcining a raw material ammonium metatungstate in a muffle furnace to obtain tungsten oxide powder; wherein the calcination temperature is 650 ℃ and the calcination time is 3 h;
s402, placing the tungsten oxide powder obtained by calcination in a tubular atmosphere furnace for deoxidization treatment in an ammonia atmosphere to obtain tungsten nitride powder; wherein the deoxidizing temperature is 650 ℃ and the deoxidizing time is 3 h;
s403, introducing high-purity argon into the tubular atmosphere furnace for passivation treatment after deoxidation is finished, and cooling tungsten nitride powder to room temperature for collection;
s404, placing the tungsten nitride powder obtained in the step S403 in a tubular atmosphere furnace for chemical reaction in a hydrogen atmosphere to obtain tungsten powder; wherein the reaction temperature is 900 ℃, and the reaction time is 2 h;
and S405, introducing high-purity argon into a tubular atmosphere furnace for passivation treatment after the chemical reaction is finished, cooling tungsten powder to room temperature, and collecting tungsten powder with the particle size of 89 nm.
Example 5: the embodiment discloses a preparation method of superfine tungsten powder, which comprises the following steps:
s501, calcining a raw material ammonium metatungstate in a muffle furnace to obtain tungsten oxide powder; wherein the calcination temperature is 650 ℃ and the calcination time is 3 h;
s502, placing the tungsten oxide powder obtained by calcination in a tubular atmosphere furnace for deoxidization treatment in an ammonia atmosphere to obtain tungsten nitride powder; wherein the deoxidizing temperature is 650 ℃ and the deoxidizing time is 3 h;
s503, introducing high-purity argon into the tubular atmosphere furnace for passivation treatment after deoxidation is finished, and cooling tungsten nitride powder to room temperature for collection;
s504, placing the tungsten nitride powder obtained in the step (3) in a tubular atmosphere furnace for chemical reaction in a hydrogen atmosphere to obtain tungsten powder; the reaction temperature is 900 ℃ and the reaction time is 3 h;
and S505, after the chemical reaction is finished, introducing high-purity argon into a tubular atmosphere furnace for passivation treatment, cooling tungsten powder to room temperature, and collecting tungsten powder with the particle size of about 110 and nm.
In summary, the embodiment of the invention discloses a preparation method of superfine tungsten powder, which adopts a stage element control strategy to prepare tungsten powder, namely different atmospheres are adopted in different preparation stages, so that the aim of introducing intermediate tungsten nitride is fulfilled, the coexistence of hydrogen and oxygen elements in the preparation stage of tungsten powder is avoided in the form of N-generation O, the particle size range of the prepared tungsten powder is 50-120nm by controlling the reaction temperature and the reaction time of each stage, the powder dispersity is better, the structure and the performance of superfine crystal/nanocrystalline hard alloy can be effectively improved, and the problems that tungsten oxide volatilizes quickly due to steam generated in the preparation process, and the tungsten powder grows rapidly and grows abnormally can be avoided; meanwhile, the raw materials required in the preparation process are easy to obtain, the reaction process is zero in pollution, and the green low-carbon high-quality development of the superfine tungsten powder preparation process is promoted.
Claims (5)
1. The preparation method of the superfine tungsten powder is characterized by comprising the following steps of:
s101, pretreating raw material ammonium metatungstate to obtain tungsten oxide powder;
s201, in an ammonia gas atmosphere, carrying out deoxidization treatment on tungsten oxide powder in a tubular atmosphere furnace to obtain tungsten nitride powder;
s301, after deoxidation is finished, introducing a high-purity argon set into a tubular atmosphere furnace for passivation treatment, and cooling tungsten nitride powder to room temperature for collection;
s401, placing the tungsten nitride powder collected in the S301 in a tubular atmosphere furnace for chemical reaction in a hydrogen atmosphere to obtain tungsten powder;
s501, introducing high-purity argon into a tubular atmosphere furnace after the chemical reaction is finished for passivation treatment, and cooling tungsten powder to room temperature for collection.
2. The method for preparing ultrafine tungsten powder according to claim 1, wherein the pretreatment of the raw material ammonium meta-tungstate to obtain tungsten oxide powder comprises calcining the raw material ammonium meta-tungstate in a muffle furnace at 650 ℃ for 2-4 h.
3. The method for preparing ultrafine tungsten powder according to claim 1 or 2, wherein the deoxidizing treatment in the step S201 has a deoxidizing temperature of 550-650 ℃ and a deoxidizing time of 1.5-3 h.
4. The method for preparing ultrafine tungsten powder according to claim 1 or 2, wherein the reaction temperature for the chemical reaction in the step S401 is 800-900 ℃ and the reaction time is 1.5-3 h.
5. The method for preparing ultrafine tungsten powder according to claim 3, wherein the reaction temperature for the chemical reaction in the step S401 is 800-900 ℃ and the reaction time is 1.5-3 h.
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| JP2018165391A (en) * | 2017-03-28 | 2018-10-25 | 日本新金属株式会社 | Method for producing tungsten fine powder |
| CN109622989A (en) * | 2019-02-26 | 2019-04-16 | 江钨世泰科钨品有限公司 | A kind of preparation method of high-purity homogeneous needle-shaped purple tungsten powder |
| CN110496969A (en) * | 2019-09-23 | 2019-11-26 | 江西理工大学 | Nano-tungsten powder and preparation method thereof |
-
2023
- 2023-10-18 CN CN202311350667.XA patent/CN117086321A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1593822A (en) * | 2003-09-10 | 2005-03-16 | 厦门金鹭特种合金有限公司 | Preparation method of high performance nanometer sized and superfine tungsten powder |
| CN101985356A (en) * | 2010-12-10 | 2011-03-16 | 中国科学院上海硅酸盐研究所 | Method for preparing tungsten carbide nano-powder |
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| CN104743529A (en) * | 2015-03-23 | 2015-07-01 | 北京科技大学 | Synthesis method of tungsten nitride with high catalytic performance |
| JP2018165391A (en) * | 2017-03-28 | 2018-10-25 | 日本新金属株式会社 | Method for producing tungsten fine powder |
| CN109622989A (en) * | 2019-02-26 | 2019-04-16 | 江钨世泰科钨品有限公司 | A kind of preparation method of high-purity homogeneous needle-shaped purple tungsten powder |
| CN110496969A (en) * | 2019-09-23 | 2019-11-26 | 江西理工大学 | Nano-tungsten powder and preparation method thereof |
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