CN101966593A - Submicron molybdenum powder production method - Google Patents
Submicron molybdenum powder production method Download PDFInfo
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- CN101966593A CN101966593A CN2010105327666A CN201010532766A CN101966593A CN 101966593 A CN101966593 A CN 101966593A CN 2010105327666 A CN2010105327666 A CN 2010105327666A CN 201010532766 A CN201010532766 A CN 201010532766A CN 101966593 A CN101966593 A CN 101966593A
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Abstract
The invention relates to a submicron molybdenum powder production method, which is characterized in that: in the production process of the submicron molybdenum powder, X-octamolybdic acid serves as a raw material and two times of low-temperature reduction by hydrogen are adopted for producing the submicron molybdenum powder. The molybdenum powder produced by the submicron molybdenum powder production method of the invention is submicron molybdenum powder of which the granularity is between 0.5 and 1 micrometer. In the invention, fine-grain molybdenum blanks with granularity ranging from 300 to 800 nano meters and density ranging from 9.8 to 10.0g/cm<3> can be prepared by using the molybdenum powder as the raw material and by profiling and sintering.
Description
Technical field
The present invention relates to a kind of submicron molybdenum powder production method.
Background technology
Molybdenum powder mainly is the method preparation of raw material by hydrogen reduction with the ammonium molybdate, and ammonium molybdate mainly contains ammonium tetramolybdate, ammonium dimolybdate, ammonium heptamolybdate and ammonium octamolybdate etc., and the ammonium molybdate of different cultivars, structure difference, crystal formation particle size range are also different.The ammonium molybdate of different grain size and distribution influences very big to granularity and distribution, the density of sintered article and the size of crystal grain of molybdenum powder.Industrial common employing ammonium tetramolybdate and ammonium dimolybdate are the feedstock production molybdenum powder, and between the general 2～5um of the Fisher particle size of molybdenum powder, this molybdenum powder is difficult to satisfy production fine grain molybdenum base, the i.e. needs of crystal grain between 300～800nm.
Summary of the invention
Purpose of the present invention is exactly the deficiency that exists at above-mentioned prior art, provides a kind of energy to satisfy the needs of producing fine grain molybdenum base, large-scale production submicron molybdenum powder method.
The objective of the invention is to be achieved through the following technical solutions.
A kind of submicron molybdenum powder production method is characterized in that it is raw material that its production process adopts the X-ammonium octamolybdate, adopts hydrogen to carry out the submicron molybdenum powder of twice low-temperature reduction production Fisher particle size between 0.5～1um.
A kind of submicron molybdenum powder production method of the present invention is characterized in that the production process step comprises:
(1) X-ammonium octamolybdate raw material is packed in the alloy boat;
(2) under 400～500 ℃ of temperature, carry out hydrogen reducing one time, the recovery time is 240～360min;
(3) under 750～900 ℃ of temperature, carry out the secondary hydrogen reducing, the recovery time is 240～360min.
A kind of submicron molybdenum powder production method of the present invention, the hydrogen that it is characterized in that carrying out hydrogen reducing is the hydrogen that pressure swing adsorption method makes, hydrogen flowing quantity is 12～16m
3/ h, dew point≤-40 ℃.
A kind of submicron molybdenum powder production method of the present invention, the molybdenum powder of the submicron order of molybdenum powder Fisher particle size between 0.5～1um of production.
The specific embodiment
A kind of submicron molybdenum powder production method, it is raw material that its production process adopts the X-ammonium octamolybdate, adopts hydrogen to carry out also original production submicron molybdenum powder twice; The production process step comprises: pack X-ammonium octamolybdate raw material in the alloy boat (1); (2) under 500～550 ℃ of temperature, carry out hydrogen reducing 240～360min; (3) again under 750～900 ℃ of temperature, carrying out the hydrogen reducing time is 240～360min.
Embodiment 1
Getting 500 gram particle mean sizes is the 1.0um X-ammonium octamolybdate material boat of packing into, paves, and thickness is 20mm, carries out low-temperature reduction in four pipe Muffle furnace stoves, and pushing away boat speed is 20min two boats, and reduction temperature is 500 ℃, and reducing agent is transformation absorption hydrogen manufacturing, and hydrogen flowing quantity is 12m
3/ h, dew point≤-40 ℃, the recovery time is 300min, obtains molybdenum dioxide.Molybdenum dioxide is crossed 80 mesh sieves.Get molybdenum dioxide 1000 grams, pave, thickness is 25mm, carries out high temperature reduction in four pipe Muffle furnace stoves, and reduction temperature is 750 ℃, and reducing agent is transformation absorption hydrogen manufacturing, and hydrogen flowing quantity is 12～16m
3/ h, dew point≤-40 ℃, the recovery time is 300min, obtains the sub-micron molybdenum powder, crosses 160 mesh sieves, the molybdenum powder Fisher particle size is 0.6um.Molybdenum powder through moulding, sintering, is obtained fine grain molybdenum base, and its density can reach 9.85g/cm
3, crystallite dimension is 350～500nm.
Embodiment 2
Getting 500 gram particle mean sizes is the 0.6um X-ammonium octamolybdate material boat of packing into, paves, and thickness is 20mm, carries out low-temperature reduction in four pipe Muffle furnace stoves, and pushing away boat speed is 20min two boats, and reduction temperature is 500 ℃, and reducing agent is transformation absorption hydrogen manufacturing, and hydrogen flowing quantity is 15m
3/ h, dew point≤-40 ℃, the recovery time is 240min, obtains molybdenum dioxide.Molybdenum dioxide is crossed 80 mesh sieves.Get molybdenum dioxide 1000 grams, pave, thickness is 25mm, carries out high temperature reduction in four pipe Muffle furnace stoves, and reduction temperature is 800 ℃, and reducing agent is transformation absorption hydrogen manufacturing, and hydrogen flowing quantity is 16m
3/ h, dew point≤-40 ℃, the recovery time is 300min, obtains the sub-micron molybdenum powder, crosses 160 mesh sieves, the molybdenum powder Fisher particle size is 0.8um.This molybdenum powder is repressed, sintering can obtain fine grain molybdenum base, and its density can reach 9.8g/cm
3, crystallite dimension is 500～700nm.
Embodiment 3
Getting 500 gram particle mean sizes is the 0.6um X-ammonium octamolybdate material boat of packing into, paves, and thickness is 20mm, carries out low-temperature reduction in four pipe Muffle furnace stoves, and pushing away boat speed is 20min two boats, and reduction temperature is 500 ℃, and reducing agent is transformation absorption hydrogen manufacturing, and hydrogen flowing quantity is 14m
3/ h, dew point≤-40 ℃, the recovery time is 300min, obtains molybdenum dioxide.Molybdenum dioxide is crossed 80 mesh sieves.Get molybdenum dioxide 1000 grams, pave, thickness is 25mm, carries out high temperature reduction in four pipe Muffle furnace stoves, and reduction temperature is 900 ℃, and reducing agent is transformation absorption hydrogen manufacturing, and hydrogen flowing quantity is 12～16m
3/ h, dew point≤-40 ℃, the recovery time is 240min, obtains the sub-micron molybdenum powder, crosses 160 mesh sieves, the molybdenum powder Fisher particle size is 1.0um.This molybdenum powder through moulding, sintering, is obtained fine grain molybdenum base, and its density can reach 9.85g/cm
3, crystallite dimension is 600～750nm.
Claims (3)
1. submicron molybdenum powder production method, it is characterized in that it is raw material that its production process adopts the X-ammonium octamolybdate, adopt hydrogen to carry out the submicron molybdenum powder between low-temperature reduction production Fisher particle size 0.5～1um twice, through moulding, sintering, can prepare crystallite dimension is 300～800nm, density 9.8～10.0g/cm with this molybdenum powder
3Fine grain molybdenum base, be used to prepare high-quality molybdenum materials
2. a kind of submicron molybdenum powder production method according to claim 1 is characterized in that the production process step comprises:
(1) X-ammonium octamolybdate raw material is packed in the alloy boat;
(2) under 500～550 ℃ of temperature, to carry out hydrogen and once reduce, the recovery time is 240～360min;
(3) under 750～850 ℃ of temperature, carry out the hydrogen secondary reduction, the recovery time is 240～360min.
3. a kind of submicron molybdenum powder production method according to claim 1, the hydrogen that it is characterized in that carrying out hydrogen reducing is the hydrogen that pressure swing adsorption method makes, hydrogen flowing quantity is 12～16m
3/ h, dew point≤-40 ℃.
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| CN2010105327666A CN101966593A (en) | 2010-11-01 | 2010-11-01 | Submicron molybdenum powder production method |
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| CN2010105327666A CN101966593A (en) | 2010-11-01 | 2010-11-01 | Submicron molybdenum powder production method |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102601385A (en) * | 2012-04-18 | 2012-07-25 | 金堆城钼业股份有限公司 | Preparation method of molybdenum powder |
| CN104070176A (en) * | 2014-07-11 | 2014-10-01 | 青岛裕华电子科技有限公司 | Production method for preparing superfine molybdenum powder in low temperature reduction mode |
| CN110899690A (en) * | 2019-12-12 | 2020-03-24 | 金堆城钼业股份有限公司 | Method for reducing oxygen content of molybdenum powder |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JPS6345310A (en) * | 1986-08-12 | 1988-02-26 | Tokyo Tungsten Co Ltd | Molybdenum powder and its production |
| CN1038232A (en) * | 1988-06-09 | 1989-12-27 | 天津大学冶金分校 | The manufacturing technology of ultrafine molybdenum powder |
| CN101323021A (en) * | 2008-07-14 | 2008-12-17 | 姜堰市光明化工厂 | Preparation method of nano-grade molybdenum powder |
| CN101758241A (en) * | 2010-02-05 | 2010-06-30 | 金堆城钼业股份有限公司 | Method for preparing submicron molybdenum powder |
-
2010
- 2010-11-01 CN CN2010105327666A patent/CN101966593A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6345310A (en) * | 1986-08-12 | 1988-02-26 | Tokyo Tungsten Co Ltd | Molybdenum powder and its production |
| CN1038232A (en) * | 1988-06-09 | 1989-12-27 | 天津大学冶金分校 | The manufacturing technology of ultrafine molybdenum powder |
| CN101323021A (en) * | 2008-07-14 | 2008-12-17 | 姜堰市光明化工厂 | Preparation method of nano-grade molybdenum powder |
| CN101758241A (en) * | 2010-02-05 | 2010-06-30 | 金堆城钼业股份有限公司 | Method for preparing submicron molybdenum powder |
Non-Patent Citations (1)
| Title |
|---|
| 《中国钼业》 20080831 黄晓玲等 钼细晶材料制备工艺研究 第32卷, 第4期 2 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102601385A (en) * | 2012-04-18 | 2012-07-25 | 金堆城钼业股份有限公司 | Preparation method of molybdenum powder |
| CN104070176A (en) * | 2014-07-11 | 2014-10-01 | 青岛裕华电子科技有限公司 | Production method for preparing superfine molybdenum powder in low temperature reduction mode |
| CN110899690A (en) * | 2019-12-12 | 2020-03-24 | 金堆城钼业股份有限公司 | Method for reducing oxygen content of molybdenum powder |
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Application publication date: 20110209 |