CN110227826A - A method of preparing high-purity nm molybdenum powder - Google Patents
A method of preparing high-purity nm molybdenum powder Download PDFInfo
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- CN110227826A CN110227826A CN201810826127.7A CN201810826127A CN110227826A CN 110227826 A CN110227826 A CN 110227826A CN 201810826127 A CN201810826127 A CN 201810826127A CN 110227826 A CN110227826 A CN 110227826A
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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
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Abstract
A method of preparing high-purity nm molybdenum powder.Using molybdenum trioxide or ammonium molybdate as molybdenum source, by molybdenum trioxide and carbon black, 1:0.5-1:2.0 ingredient is mixed in molar ratio, prepare the extremely low molybdenum dioxide containing a certain amount of nanometer molybdenum core of carbon content, then the molybdenum dioxide containing nanometer molybdenum core is restored with hydrogen, the extremely low high-purity nm molybdenum powder of carbon content can be obtained.The present invention solves the problems, such as to be difficult to prepare nano Mo powder during tradition prepares molybdenum dioxide and molybdenum powder using hydrogen reducing molybdenum trioxide.In the present invention, the use of thinner carbon black is reducing agent, the nanometer molybdenum core of a certain amount of dispersion is generated in molybdenum dioxide, the tiny nanometer molybdenum core of these dispersions can assist hydrogen reducing molybdenum dioxide to generate molybdenum nano particle.For the nano Mo powder average particle size that the present invention prepares in 40-200nm, carbon content is smaller than 0.01%.Cost of material of the present invention is low, and product purity is high, and granularity is small, simple process, high production efficiency, is suitble to large-scale industrial production high-purity nm molybdenum powder.
Description
Technical field
The invention belongs to nano-powder material preparation fields, disclose a kind of method for preparing high-purity nm molybdenum powder.
Background technique
Molybdenum has many excellent characteristics, such as: high-melting-point, high-wearing feature, low thermal coefficient of expansion, excellent is led high rigidity
Conductance hot property and good corrosion resistance.Therefore, molybdenum and its alloy are widely used in many fields.Such as: change
The fields such as work, metallurgy, electronics, military project and aerospace.And the molybdenum powder of nano-scale, there are many unique properties, it is such as high
Specific surface area, the chemical activity enhancing of interface atom, these all may significant its physics of change, mechanically and chemically property.
In addition, sintering temperature can be significantly reduced in nano Mo powder, obtain that consistency is higher and the lesser production of crystal grain at a lower temperature
Product.So with nano Mo powder be sintered synthesis molybdenum base and its alloy be improve molybdenum system alloy physics mechanical property optimal path it
One.
Currently, industrially preparing the technique that molybdenum powder mainly uses two sections of hydrogen reduction molybdenum trioxides.But it is used in tradition
During hydrogen reducing molybdenum trioxide prepares molybdenum dioxide and molybdenum powder, since molybdenum dioxide and molybdenum dispersion forming core are difficult, and
The presence of gas-migration mechanism makes it difficult to prepare nano Mo powder.Although there is a lot of other methods to be used to prepare a nanometer molybdenum
Powder, including high-energy ball milling, heat plasma technology, molybdenum carbonyl thermal decomposition method, low-temperature molten salt preparation etc., still, these methods
Industrialized production nano Mo powder is difficult to use in due to cost, production efficiency, complex process etc..
Summary of the invention
The object of the present invention is to provide a kind of new low cost, simple process, efficiently, be suitable for large-scale industrial production
The method for preparing high-purity nm molybdenum powder.
To achieve the above object, the present invention adopts the following technical scheme:
A method of preparing high-purity nm molybdenum powder, which is characterized in that the present invention is using molybdenum trioxide as molybdenum source, carbon black and hydrogen
Gas is reducing agent；Molybdenum trioxide is reduced to then to be contained with hydrogen containing the molybdenum dioxide of a certain amount of nanometer molybdenum core with carbon black
There is the molybdenum dioxide of nanometer molybdenum core to restore, obtains high-purity nm molybdenum powder.
Further, the molybdenum trioxide can be substituted with ammonium molybdate.
Further, specific step is as follows by the present invention:
(1) molybdenum trioxide and carbon black 1:0.5-1:2.0 ingredient and are uniformly mixed in molar ratio, are carried out at 400-750 DEG C
Reduction, obtains the ultra-fine molybdenum dioxide containing a certain amount of carbon black.
(2) by the ultra-fine molybdenum dioxide obtained in step (1) containing a certain amount of carbon black 800 DEG C -1150 DEG C at a temperature of
Reaction, obtains the molybdenum dioxide containing a certain amount of nanometer molybdenum core.
(3) molybdenum dioxide of a certain amount of nanometer molybdenum core will be contained obtained in step (2) in 600-1100 DEG C of progress hydrogen
Gas reduction, obtains high-purity nm molybdenum powder, average particle size is in 40-200nm.
It is possible to further contain the molybdenum dioxide of a certain amount of nanometer molybdenum core using the reduction of hydrogen alternative carbon black, in turn
Prepare high-purity nm molybdenum powder.
Compared with prior art, the present invention having the advantage that
1. solving tradition the present invention provides a kind of new technique for preparing high-purity nm molybdenum powder and using hydrogen reducing three
Molybdenum oxide is difficult to the problem of preparing nano Mo powder during preparing molybdenum dioxide and molybdenum powder.
2. raw material molybdenum trioxide (or ammonium molybdate), carbon black and hydrogen that the present invention uses all are industrial common raw materials,
Production cost can be effectively reduced and improve production efficiency.
3. present invention process is simple and low for equipment requirements.Carbon black and molybdenum oxide reaction do not need special installation, controlling party
Just and formation efficiency is high；The molybdenum dioxide of the hydrogen reducing core of molybdenum containing nanometer can use the equipment of existing industrial production molybdenum powder.
Therefore, the present invention is suitble to industrialization large-scale production nano Mo powder.
4. nano Mo powder prepared by the present invention, average particle size is smaller than in 40nm-200nm, epigranular, carbon content
0.01%.
Specific embodiment
To further appreciate that the contents of the present invention.Further statement is made to the present invention below with reference to example.
Embodiment one:
The ratio of high-purity molybdenum trioxide and carbon black 1:0.8 in molar ratio are uniformly mixed.By the raw material of mixing at 600 DEG C
Inert gas atmosphere roasts 1 hour, then in 1000 DEG C of 1 hours of roasting, then by the product after roasting in 900 DEG C of progress hydrogen
Gas reduction, obtains high-purity nm molybdenum powder.
Embodiment two:
The ratio of high-purity molybdenum trioxide and carbon black 1:1.4 in molar ratio are uniformly mixed.By the raw material of mixing at 550 DEG C
Inert gas atmosphere roasts 1.5 hours, then in 900 DEG C of 1 hours of roasting, then by the product after roasting in 800 DEG C of progress
Hydrogen reducing obtains high-purity nm molybdenum powder.
Embodiment three:
Ammonium molybdate is uniformly mixed in the ratio of molybdenum contained therein and carbon black molar ratio 1:1.0.By the raw material of mixing 530
At DEG C inert gas atmosphere roast 2 hours, then in 950 DEG C of 1 hours of roasting, then by the product after roasting 850 DEG C into
Row hydrogen reducing obtains high-purity nm molybdenum powder.
Claims (4)
1. a kind of method for preparing high-purity nm molybdenum powder, which is characterized in that the present invention is using molybdenum trioxide as molybdenum source, carbon black and hydrogen
For reducing agent；Molybdenum trioxide is reduced to then to be contained with hydrogen containing the molybdenum dioxide of a certain amount of nanometer molybdenum core with carbon black
The molybdenum dioxide reduction of nanometer molybdenum core, obtains high-purity nm molybdenum powder.
2. a kind of method for preparing high-purity nm molybdenum powder according to claim 1, which is characterized in that the molybdenum trioxide
It can be substituted with ammonium molybdate.
3. a kind of method for preparing high-purity nm molybdenum powder according to claim 1, which is characterized in that specific step is as follows:
(1) molybdenum trioxide and carbon black 1:0.5-1:2.0 ingredient and are uniformly mixed in molar ratio, are restored at 400-750 DEG C,
Obtain the ultra-fine molybdenum dioxide containing a certain amount of carbon black；
(2) by the ultra-fine molybdenum dioxide obtained in step (1) containing a certain amount of carbon black 800 DEG C -1150 DEG C at a temperature of react,
Obtain the molybdenum dioxide containing a certain amount of nanometer molybdenum core；
(3) by obtained in step (2) contain a certain amount of nanometer molybdenum core molybdenum dioxide 600-1100 DEG C of progress hydrogen also
Original obtains high-purity nm molybdenum powder, and average particle size is in 40-200nm.
4. a kind of method for preparing high-purity nm molybdenum powder according to claim 1 or 3, it is characterised in that substituted using hydrogen
Carbon black reduction contains the molybdenum dioxide of a certain amount of nanometer molybdenum core, and then prepares high-purity nm molybdenum powder.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112207287A (en) * | 2020-12-07 | 2021-01-12 | 西安稀有金属材料研究院有限公司 | Preparation method and application of yttrium oxide nanoparticle-doped nano molybdenum powder |
| CN112222419A (en) * | 2020-12-07 | 2021-01-15 | 西安稀有金属材料研究院有限公司 | Method for preparing nano molybdenum powder by regulating nucleation and growth processes and application |
| CN112222420A (en) * | 2020-12-07 | 2021-01-15 | 西安稀有金属材料研究院有限公司 | Nano tungsten powder doped with metal oxide nano particles and preparation method thereof |
| CN113234940A (en) * | 2021-04-13 | 2021-08-10 | 郑州大学 | Method for preparing molybdenum metal product from molybdenum concentrate in short process |
| CN115233022A (en) * | 2022-09-23 | 2022-10-25 | 西安稀有金属材料研究院有限公司 | Ultrahigh-hardness nano-structure molybdenum-aluminum alloy and preparation method thereof |
| CN115229181A (en) * | 2022-09-23 | 2022-10-25 | 西安稀有金属材料研究院有限公司 | Method for preparing superfine molybdenum dioxide and molybdenum powder based on nano-scale solid-liquid mixed deposition |
| CN115321598A (en) * | 2022-09-23 | 2022-11-11 | 西安稀有金属材料研究院有限公司 | Preparation method of low-cost, high-dispersion, high-porosity and high-purity ultrafine molybdenum trioxide |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112207287A (en) * | 2020-12-07 | 2021-01-12 | 西安稀有金属材料研究院有限公司 | Preparation method and application of yttrium oxide nanoparticle-doped nano molybdenum powder |
| CN112222419A (en) * | 2020-12-07 | 2021-01-15 | 西安稀有金属材料研究院有限公司 | Method for preparing nano molybdenum powder by regulating nucleation and growth processes and application |
| CN112222420A (en) * | 2020-12-07 | 2021-01-15 | 西安稀有金属材料研究院有限公司 | Nano tungsten powder doped with metal oxide nano particles and preparation method thereof |
| CN112222420B (en) * | 2020-12-07 | 2021-03-16 | 西安稀有金属材料研究院有限公司 | Nano tungsten powder doped with metal oxide nano particles and preparation method thereof |
| CN113234940A (en) * | 2021-04-13 | 2021-08-10 | 郑州大学 | Method for preparing molybdenum metal product from molybdenum concentrate in short process |
| CN115233022A (en) * | 2022-09-23 | 2022-10-25 | 西安稀有金属材料研究院有限公司 | Ultrahigh-hardness nano-structure molybdenum-aluminum alloy and preparation method thereof |
| CN115229181A (en) * | 2022-09-23 | 2022-10-25 | 西安稀有金属材料研究院有限公司 | Method for preparing superfine molybdenum dioxide and molybdenum powder based on nano-scale solid-liquid mixed deposition |
| CN115321598A (en) * | 2022-09-23 | 2022-11-11 | 西安稀有金属材料研究院有限公司 | Preparation method of low-cost, high-dispersion, high-porosity and high-purity ultrafine molybdenum trioxide |
| CN115321598B (en) * | 2022-09-23 | 2023-10-20 | 西安稀有金属材料研究院有限公司 | Preparation method of low-cost, high-dispersion, high-porosity and high-purity superfine molybdenum trioxide |
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