CN111790915B - Preparation method of potassium-doped superfine low-potassium tungsten powder - Google Patents
Preparation method of potassium-doped superfine low-potassium tungsten powder Download PDFInfo
- Publication number
- CN111790915B CN111790915B CN202010138979.4A CN202010138979A CN111790915B CN 111790915 B CN111790915 B CN 111790915B CN 202010138979 A CN202010138979 A CN 202010138979A CN 111790915 B CN111790915 B CN 111790915B
- Authority
- CN
- China
- Prior art keywords
- potassium
- reduction
- tungsten
- controlled
- tungsten powder
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
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
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The invention discloses a preparation method of potassium-doped superfine low-potassium tungsten powder, which comprises the steps of taking ammonium paratungstate as a raw material, carrying out primary reduction to prepare blue tungsten, doping silicon, aluminum and potassium elements in the blue tungsten, carrying out secondary reduction to prepare tungsten dioxide, carrying out tertiary reduction on the tungsten dioxide to generate superfine low-potassium tungsten powder, and carrying out acid washing to obtain the tungsten powder with the average potassium content of 20-40 ppm, the silicon content of 200-400 ppm, the aluminum content of 10-20 ppm and the tungsten powder particle size of 1.0-1.5 mu m. The preparation method can ensure the effective potassium content in the tungsten crystal lattice, has good forming and sintering properties, is beneficial to later forging processing, and is suitable for large-scale production of potassium-containing tungsten bars and plates.
Description
Technical Field
The invention belongs to the technical field of metal powder metallurgy, and particularly relates to a preparation method of potassium-doped superfine low-potassium tungsten powder.
Background
Tungsten is an important rare metal, has the characteristics of high melting point, high density, high hardness, low thermal expansion coefficient, excellent corrosion resistance and high-temperature strength, determines that the metal tungsten can become an optimal material used under high-temperature and ultrahigh-temperature conditions, and is widely applied to the fields of aerospace, military industry, medical treatment, semiconductors, high-temperature furnaces and special light sources.
The potassium-doped tungsten material with potassium bubbles in crystal lattices has excellent high-temperature creep resistance due to the dispersion strengthening effect of the potassium bubbles. However, the granularity of the potassium-doped tungsten powder prepared by the traditional process is generally between 2.5 and 5.0 microns, even though the deliberately prepared fine-grained doped tungsten powder has the granularity of generally between 2.3 and 2.8 microns, the potassium content is 120 to 160ppm, the powder has coarse granularity and high potassium content, is not beneficial to sintering of potassium-doped tungsten bars and plates, the potassium existing on the grain boundary in the powder is difficult to volatilize out in the sintering process, the density of the sintered bars and plates is low, the subsequent thermal deformation processing performance is poor, and the problems of splitting, layering and the like are easy to occur, so the use of the potassium-doped tungsten material is greatly limited.
Therefore, how to improve the existing preparation process of the potassium-doped tungsten powder so as to improve the hot-working performance of the sintered bar and the sintered plate is a technical problem to be solved urgently by the technical personnel in the field.
Disclosure of Invention
The invention aims to provide a preparation method of potassium-doped superfine low-potassium tungsten powder, which aims to solve the technical problems in the prior art. Therefore, the preparation method of the potassium-doped superfine low-potassium tungsten powder comprises the following steps:
primary reduction: heating and reducing ammonium paratungstate to generate blue tungsten, wherein the reduction temperature is controlled to be 400-550 ℃, the reduction hydrogen flow is controlled to be 300-700L/h, and the reduction time is controlled to be 2-3 h;
doping elements: doping three additive elements of silicon, aluminum and potassium in blue tungsten, and preparing potassium silicate, aluminum nitrate and potassium hydroxide aqueous solution containing the three additive elements, wherein the aqueous solution is prepared to contain 0.18-0.24% of K in weight percentage relative to the blue tungsten according to equivalent weight2O, 0.001 to 0.003% of Al2O30.2 to 0.4 percent of SiO; soaking blue tungsten in the aqueous solution, putting the water solution into a stirring pot, fully stirring, introducing steam into an interlayer of the stirring pot, heating the water solution under the condition that the steam pressure is controlled to be 0.3MPa, stirring and heating the water solution until the water in the blue tungsten is completely evaporated to dryness, and then sieving the dried blue tungsten for later use;
and (3) secondary reduction: carrying out secondary reduction on the blue tungsten doped with the elements to produce tungsten dioxide, wherein the reduction temperature is controlled to be 500-700 ℃, and the flow of reduction hydrogen is controlled to be 3-4 m3The reduction time is controlled to be 8-9 h, and the oxygen content of the tungsten dioxide is controlled to be 11-13 percent in the secondary reductionTo (c) to (d);
and (3) carrying out third reduction: carrying out three times of reduction on tungsten dioxide to produce tungsten powder, wherein the reduction temperature is controlled to be 700-950 ℃, and the flow of reduction hydrogen is controlled to be 5-6 m3Controlling the reduction time to be 8-9 h, and preparing superfine potassium-doped tungsten powder, wherein the granularity of the tungsten powder is controlled to be 1.0-1.5 mu m;
acid washing: and (2) stirring and cleaning the tungsten powder twice by using hydrochloric acid and hydrofluoric acid respectively to remove redundant trace additive elements on the surface of the tungsten powder, wherein the content of doping elements of the cleaned tungsten powder is controlled to be 20-40 ppm of potassium, 200-400 ppm of silicon and 10-20 ppm of aluminum.
Preferably, in the preparation method of the potassium-doped ultra-fine low-potassium tungsten powder, a drying step is further included after the acid washing step, wherein the cleaned tungsten powder is dried in a vacuum drying oven, the drying temperature is controlled to be 60-80 ℃, the drying time is controlled to be 18h, and the vacuum degree of the vacuum drying oven is controlled to be less than-0.1 Kpa.
Preferably, in the above method for preparing potassium-doped ultra-fine low-potassium tungsten powder, the primary reduction, the secondary reduction and the tertiary reduction are all performed in a tubular pusher furnace filled with the reducing hydrogen.
Preferably, in the preparation method of the potassium-doped ultrafine low-potassium tungsten powder, the pressure in the tubular pusher furnace is controlled to be 1-2 Kpa in the secondary reduction.
Preferably, in the preparation method of the potassium-doped superfine low-potassium tungsten powder, the dew point of the reducing hydrogen is controlled to be-40 to-70 ℃ and the purity of the reducing hydrogen is controlled to be more than 99.99% in the primary reduction, the secondary reduction and the tertiary reduction.
The preparation method of the potassium-doped superfine low-potassium tungsten powder adopts solid-liquid doping and three-time reduction processes, and can prepare the superfine tungsten powder with the granularity of 1.0-1.5 mu m by controlling the reduction temperature, the hydrogen flow, the hydrogen purity and the pressure in the furnace, wherein the potassium content of the tungsten powder is 20-40 ppm.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be clearly and completely described below with reference to the specific embodiments of the present invention. It is to be understood that the described embodiments are merely a few embodiments of the invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments of the present invention without making any creative effort, shall fall within the protection scope of the present invention.
In general, the preparation method of the potassium-doped superfine low-potassium tungsten powder adopts solid-liquid doping and three-time reduction processes, and the superfine tungsten powder with the particle size of 1.0-1.5 mu m is prepared by controlling the reduction temperature, the hydrogen flow, the hydrogen purity and the pressure in the furnace, wherein the potassium content of the tungsten powder is 20-40 ppm. Specifically, the preparation method of the potassium-doped superfine low-potassium tungsten powder comprises the following steps:
primary reduction: pushing ammonium paratungstate into a tubular push boat furnace filled with reduction hydrogen, heating and reducing to generate blue tungsten, controlling the reduction temperature to be 400-550 ℃, controlling the flow of the reduction hydrogen filled into the tubular push boat furnace to be 300-700L/h, and controlling the reduction time to be 2-3 h;
doping elements: doping three additive elements of silicon, aluminum and potassium in blue tungsten, and concretely comprises preparing potassium silicate, aluminum nitrate and potassium hydroxide aqueous solution containing the three additive elements, wherein the aqueous solution is prepared to contain 0.18-0.24 wt% of K relative to the blue tungsten according to equivalent weight2O, 0.001 to 0.003% of Al2O30.2 to 0.4 percent of SiO; soaking blue tungsten in the aqueous solution, putting the water solution into a stirring pot, fully stirring, introducing steam into an interlayer of the stirring pot, heating the water solution under the condition that the steam pressure is controlled to be 0.3MPa, stirring and heating the water solution until the water in the blue tungsten is completely evaporated to dryness, and then sieving the dried blue tungsten for later use;
and (3) secondary reduction: pushing the blue tungsten doped with the elements into a tubular pusher furnace for secondary reduction to produce tungsten dioxide, wherein the reduction temperature is controlled to be 500-700 ℃, and the tubular pusher furnace is used for tubular reductionThe flow of the reducing hydrogen in the pusher furnace is controlled to be 3-4 m3The pressure in the tubular pusher furnace is controlled to be 1-2 KPa, the reduction time is controlled to be 8-9 h, and the oxygen content of the tungsten dioxide is controlled to be 11-13% in the secondary reduction;
and (3) carrying out third reduction: pushing tungsten dioxide into a tubular pusher furnace for carrying out tertiary reduction to produce tungsten powder, wherein the reduction temperature is controlled to be 700-950 ℃, and the reduction hydrogen flow in the tubular pusher furnace is controlled to be 5-6 m3Controlling the reduction time to be 8-9 h, and preparing superfine potassium-doped tungsten powder, wherein the granularity of the tungsten powder is controlled to be 1.0-1.5 mu m;
acid washing and drying: stirring and cleaning tungsten powder twice by using hydrochloric acid and hydrofluoric acid respectively, removing redundant trace additive elements on the surface of the tungsten powder, controlling the content of doping elements of the cleaned tungsten powder to be 20-40 ppm of potassium, 200-400 ppm of silicon and 10-20 ppm of aluminum, then drying the cleaned tungsten powder in a vacuum drying oven, controlling the drying temperature to be 60-80 ℃, controlling the drying time to be 18h, and controlling the vacuum degree of the vacuum drying oven to be less than-0.1 KPa; drying and sieving to obtain the potassium-doped superfine low-potassium tungsten powder.
Preferably, in the above-mentioned primary reduction, secondary reduction and tertiary reduction, the dew point of the reducing hydrogen is controlled to be-40 to-70 ℃, and the purity of the reducing hydrogen is controlled to be more than 99.99%.
The preparation method of the potassium-doped ultra-fine low-potassium tungsten powder of the present invention is described in detail below with reference to specific examples.
Example 1
The method comprises the following steps: weighing 300kg of ammonium paratungstate, pushing the ammonium paratungstate into a tubular push boat furnace according to a boat loading amount of 500 g/boat and a boat pushing speed of 20 min/boat for primary reduction, controlling the reduction temperature to be 400-550 ℃, controlling the flow of reduction hydrogen introduced into the tubular push boat furnace to be 300-700L/h until the reduction is finished, and generating blue tungsten;
step two: weighing 250kg of blue tungsten and putting the blue tungsten into an aqueous solution of potassium silicate, aluminum nitrate and potassium hydroxide, wherein the aqueous solution contains 0.20 percent of K relative to the weight of the blue tungsten by weight according to equivalent calculation2O, 0.002% of Al2O30.3 percent of SiO, and stirringStirring by a stirring paddle of a stirring pot, then starting steam for heating, controlling the steam pressure to be 0.3MPa, heating while stirring until the steam is dried, and then sieving the dried blue tungsten for later use;
step three: pushing the doped blue tungsten into a tubular push boat furnace according to the boat loading amount of 150 g/boat and the push boat speed of 20 min/boat for secondary reduction, wherein the reduction temperature is controlled to be 500-700 ℃, and the reduction hydrogen flow in the tubular push boat furnace is controlled to be 3-3.5 m3The reduction time of the single boat in the furnace is controlled to be 8-9 h, brown tungsten dioxide is generated by reduction, and the oxygen content of the tungsten dioxide is controlled to be 11-12% in secondary reduction;
step four: pushing tungsten dioxide into a tubular push-boat furnace according to the boat loading amount of 300 g/boat and the push-boat speed of 30 min/boat for three-time reduction, wherein the reduction temperature is controlled to be 700-950 ℃, and the reduction hydrogen flow in the tubular push-boat furnace is controlled to be 5-5.5 m3The reduction time of the single boat in the furnace is controlled to be 8-9 h, the gray potassium-doped ultra-fine granularity tungsten powder is generated by reduction, and the granularity of the tungsten powder is controlled to be 1.0-1.5 mu m;
step five: stirring and cleaning tungsten powder twice by using hydrochloric acid and hydrofluoric acid to remove redundant doping elements adhered to the surface of the tungsten powder, and then putting the tungsten powder into a vacuum drying oven for drying, wherein the drying temperature is controlled to be 60-80 ℃, and the drying time is controlled to be 18 h; drying and sieving to obtain the potassium-doped superfine low-potassium tungsten powder.
Example 2
The method comprises the following steps: weighing 300kg of ammonium paratungstate, pushing the ammonium paratungstate into a tubular push boat furnace according to a boat loading amount of 500 g/boat and a boat pushing speed of 20 min/boat for primary reduction, controlling the reduction temperature to be 400-550 ℃, controlling the flow of reduction hydrogen introduced into the tubular push boat furnace to be 300-500L/h until the reduction is finished, and generating blue tungsten;
step two: weighing 250kg of blue tungsten and putting the blue tungsten into an aqueous solution of potassium silicate, aluminum nitrate and potassium hydroxide, wherein the aqueous solution contains 0.18 percent of K relative to the weight of the blue tungsten by weight according to equivalent calculation2O, 0.0015% Al2O30.4 percent of SiO, starting a stirring paddle of the stirring pot for stirring, then starting steam for heating, and controlling the steam pressureHeating under stirring with a force of 0.3MPa until the powder is dried, and sieving the dried blue tungsten for later use;
step three: pushing the doped blue tungsten into a tubular push boat furnace according to the boat loading amount of 200 g/boat and the push boat speed of 20 min/boat for secondary reduction, controlling the reduction temperature to be 500-700 ℃, and controlling the reduction hydrogen flow in the tubular push boat furnace to be 3-3.5 m3The reduction time of the single boat in the furnace is controlled to be 8-9 h, brown tungsten dioxide is generated by reduction, and the oxygen content of the tungsten dioxide is controlled to be 12-13% in secondary reduction;
step four: pushing the tungsten dioxide into a tubular push-boat furnace according to the boat loading amount of 250 g/boat and the push-boat speed of 30 min/boat for three-time reduction, wherein the reduction temperature is controlled to be 700-950 ℃, and the reduction hydrogen flow in the tubular push-boat furnace is controlled to be 5-5.5 m3The reduction time of the single boat in the furnace is controlled to be 8-9 h, the gray potassium-doped ultra-fine granularity tungsten powder is generated by reduction, and the granularity of the tungsten powder is controlled to be 1.0-1.5 mu m;
step five: stirring and cleaning tungsten powder twice by using hydrochloric acid and hydrofluoric acid to remove redundant doping elements adhered to the surface of the tungsten powder, and then putting the tungsten powder into a vacuum drying oven for drying, wherein the drying temperature is controlled to be 60-80 ℃, and the drying time is controlled to be 18 h; drying and sieving to obtain the potassium-doped superfine low-potassium tungsten powder.
In summary, the preparation method of the potassium-doped ultra-fine low-potassium tungsten powder provided by the invention uses ammonium paratungstate as a raw material, ammonium paratungstate is subjected to primary reduction to prepare blue tungsten, a certain amount of potassium oxide, aluminum oxide and silicon oxide are added into the blue tungsten, then the blue tungsten is subjected to secondary reduction to prepare tungsten dioxide, the tungsten dioxide is subjected to tertiary reduction to generate ultra-fine low-potassium tungsten powder, and after acid washing, the tungsten powder has the average potassium content of 20-40 ppm, the silicon content of 200-400 ppm, the aluminum content of 10-20 ppm and the particle size of 1.0-1.5 μm.
It should be noted that the above embodiments are only used for illustrating the technical solution of the present invention, and not for limiting the same; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or alterations do not depart from the spirit of the invention.
Claims (5)
1. The preparation method of the potassium-doped superfine low-potassium tungsten powder is characterized by comprising the following steps of:
primary reduction: heating and reducing ammonium paratungstate to generate blue tungsten, wherein the reduction temperature is controlled to be 400-550 ℃, the reduction hydrogen flow is controlled to be 300-700L/h, and the reduction time is controlled to be 2-3 h;
doping elements: doping three additive elements of silicon, aluminum and potassium in blue tungsten, wherein the element doping step comprises the step of preparing potassium silicate, aluminum nitrate and potassium hydroxide aqueous solution containing the three additive elements, and the aqueous solution is prepared to contain 0.18-0.24 wt% of K relative to the blue tungsten according to equivalent weight2O, 0.001 to 0.003% of Al2O30.2 to 0.4 percent of SiO; soaking blue tungsten in the aqueous solution, putting the water solution into a stirring pot, fully stirring, introducing steam into an interlayer of the stirring pot, heating the water solution under the condition that the steam pressure is controlled to be 0.3MPa, stirring and heating the water solution until the water in the blue tungsten is completely evaporated to dryness, and then sieving the dried blue tungsten for later use;
and (3) secondary reduction: carrying out secondary reduction on the blue tungsten doped with the elements to produce tungsten dioxide, wherein the reduction temperature is controlled to be 500-700 ℃, and the flow of reduction hydrogen is controlled to be 3-4 m3The reduction time is controlled to be 8-9 h, and the oxygen content of the tungsten dioxide is controlled to be 11-13% in the secondary reduction;
and (3) carrying out third reduction: carrying out three times of reduction on tungsten dioxide to produce tungsten powder, wherein the reduction temperature is controlled to be 700-950 ℃, and the flow of reduction hydrogen is controlled to be 5-6 m3Controlling the reduction time to be 8-9 h, and preparing superfine potassium-doped tungsten powder, wherein the granularity of the tungsten powder is controlled to be 1.0-1.5 mu m;
acid washing: and (2) stirring and cleaning the tungsten powder twice by using hydrochloric acid and hydrofluoric acid respectively to remove redundant trace additive elements on the surface of the tungsten powder, wherein the content of doping elements of the cleaned tungsten powder is controlled to be 20-40 ppm of potassium, 200-400 ppm of silicon and 10-20 ppm of aluminum.
2. The method for preparing potassium-doped ultra-fine low-potassium tungsten powder according to claim 1, wherein the acid washing step is followed by a drying step, wherein the cleaned tungsten powder is dried in a vacuum drying oven, the drying temperature is controlled to be 60-80 ℃, the drying time is controlled to be 18h, and the vacuum degree of the vacuum drying oven is controlled to be < -0.1 Kpa.
3. The method for preparing potassium-doped ultra-fine low-potassium tungsten powder as claimed in claim 1 or 2, wherein the primary reduction, the secondary reduction and the tertiary reduction are all performed in a tube-type pusher furnace through which the reducing hydrogen gas is passed.
4. The method of claim 3, wherein the pressure inside the tube pusher furnace is controlled to be 1 to 2Kpa during the secondary reduction.
5. The method for preparing potassium-doped ultra-fine low-potassium tungsten powder as claimed in claim 3, wherein the dew point of the reducing hydrogen is controlled to be-40 to-70 ℃ and the purity of the reducing hydrogen is controlled to be more than 99.99% in the primary reduction, the secondary reduction and the tertiary reduction.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010138979.4A CN111790915B (en) | 2020-03-03 | 2020-03-03 | Preparation method of potassium-doped superfine low-potassium tungsten powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010138979.4A CN111790915B (en) | 2020-03-03 | 2020-03-03 | Preparation method of potassium-doped superfine low-potassium tungsten powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN111790915A CN111790915A (en) | 2020-10-20 |
| CN111790915B true CN111790915B (en) | 2021-09-24 |
Family
ID=72806684
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010138979.4A Active CN111790915B (en) | 2020-03-03 | 2020-03-03 | Preparation method of potassium-doped superfine low-potassium tungsten powder |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111790915B (en) |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6057481B2 (en) * | 1979-12-18 | 1985-12-16 | 日本タングステン株式会社 | Method for adjusting potassium content in tungsten powder |
| 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 |
| CN1757466A (en) * | 2005-10-11 | 2006-04-12 | 自贡硬质合金有限责任公司 | Method for producing potassium-contd. metal tungsten bars |
| CN102198507A (en) * | 2011-05-16 | 2011-09-28 | 赣州虹飞钨钼材料有限公司 | Method for producing tungsten bar serving as halogen tungsten lamp tungsten filament |
| CN103290296A (en) * | 2013-06-20 | 2013-09-11 | 威海多晶钨钼科技有限公司 | Superfine-crystal large-size tungsten bar and preparation method thereof |
| CN105903977A (en) * | 2016-05-02 | 2016-08-31 | 陈昌和 | Production method of potassium-dopedmetal tungsten powder and method for producing tungsten bar through tungsten powder |
| CN106906396A (en) * | 2017-03-06 | 2017-06-30 | 威海多晶钨钼科技有限公司 | A kind of uniform fine grain Tungsten Bar and preparation method thereof |
| CN107068514A (en) * | 2017-04-18 | 2017-08-18 | 江苏圣亚有色金属材料有限公司 | A kind of preparation method of electron gun filament |
-
2020
- 2020-03-03 CN CN202010138979.4A patent/CN111790915B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6057481B2 (en) * | 1979-12-18 | 1985-12-16 | 日本タングステン株式会社 | Method for adjusting potassium content in tungsten powder |
| 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 |
| CN1757466A (en) * | 2005-10-11 | 2006-04-12 | 自贡硬质合金有限责任公司 | Method for producing potassium-contd. metal tungsten bars |
| CN102198507A (en) * | 2011-05-16 | 2011-09-28 | 赣州虹飞钨钼材料有限公司 | Method for producing tungsten bar serving as halogen tungsten lamp tungsten filament |
| CN103290296A (en) * | 2013-06-20 | 2013-09-11 | 威海多晶钨钼科技有限公司 | Superfine-crystal large-size tungsten bar and preparation method thereof |
| CN105903977A (en) * | 2016-05-02 | 2016-08-31 | 陈昌和 | Production method of potassium-dopedmetal tungsten powder and method for producing tungsten bar through tungsten powder |
| CN106906396A (en) * | 2017-03-06 | 2017-06-30 | 威海多晶钨钼科技有限公司 | A kind of uniform fine grain Tungsten Bar and preparation method thereof |
| CN107068514A (en) * | 2017-04-18 | 2017-08-18 | 江苏圣亚有色金属材料有限公司 | A kind of preparation method of electron gun filament |
Also Published As
| Publication number | Publication date |
|---|---|
| CN111790915A (en) | 2020-10-20 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108145156B (en) | Preparation method of high-performance TZM molybdenum alloy bar | |
| WO2018214830A1 (en) | Method for preparing high melting point metal powder via multi-stage deep reduction | |
| CN111320177B (en) | Method for removing hydroxyl groups in quartz sand powder | |
| CN115287499B (en) | High-strength corrosion-resistant Zr702L alloy with low stress corrosion sensitivity | |
| CN103978224A (en) | Method for preparing tungsten nano-powder from arsenic-doped ammonium paratungstate or ammonium metatungstate | |
| JP5837636B2 (en) | Ferritic oxide dispersion strengthened alloy and method for producing the same | |
| CN113427008A (en) | Tantalum-tungsten alloy powder and preparation method thereof | |
| WO2014101658A1 (en) | Zirconium alloy for nuclear power | |
| CN110791671B (en) | Al-Ti-C-SiC composite material and preparation method thereof | |
| CN102181749B (en) | Zirconium alloy for nuclear pressurized water reactor and preparation method thereof | |
| CN111790915B (en) | Preparation method of potassium-doped superfine low-potassium tungsten powder | |
| CN111570784A (en) | Preparation method of iron-copper alloy diffusion powder | |
| CN101891217B (en) | Method for preparing high-purity rare earth boride 6 (REB6) nano-powder | |
| CN114309631B (en) | Preparation method of rhenium powder | |
| CN114351007B (en) | High-temperature-resistant fastener and manufacturing method thereof | |
| CN110066952A (en) | A kind of preparation method of zirconium oxide enhancing molybdenum alloy bar material | |
| CN102181750B (en) | Zirconium alloy material and preparation method thereof | |
| CN114921686B (en) | Nickel-based alloy with high corrosion resistance and preparation method thereof | |
| CN110872661A (en) | High-temperature-resistant titanium alloy plate and preparation method thereof | |
| CN115652161B (en) | Preparation method of polymer carbonized porous coated nano carbide strengthening and toughening molybdenum alloy | |
| CN114703397B (en) | Zirconium-based alloy with corrosion resistance and creep resistance for nuclear reactor fuel cladding and method for preparing zirconium-based alloy pipe by using zirconium-based alloy | |
| CN110606742B (en) | TiO for nuclear power2-Gd2O3Burnable poison ceramic material and preparation method thereof | |
| CN113333739B (en) | Method for improving nitrogen content in powdery vanadium-nitrogen alloy | |
| WO2022174608A1 (en) | Large-size deformation-resistant molybdenum alloy bar and preparation method therefor | |
| CN115198163B (en) | Preparation method of multi-nano-phase reinforced ODS alloy with tensile plasticity |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |