CN110227826B - Method for preparing high-purity nano molybdenum powder - Google Patents
Method for preparing high-purity nano molybdenum powder Download PDFInfo
- Publication number
- CN110227826B CN110227826B CN201810826127.7A CN201810826127A CN110227826B CN 110227826 B CN110227826 B CN 110227826B CN 201810826127 A CN201810826127 A CN 201810826127A CN 110227826 B CN110227826 B CN 110227826B
- Authority
- CN
- China
- Prior art keywords
- molybdenum
- nano
- powder
- purity
- nano molybdenum
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
Abstract
A method for preparing high-purity nano molybdenum powder. Molybdenum trioxide or ammonium molybdate is used as a molybdenum source, molybdenum trioxide and carbon black are uniformly mixed according to the molar ratio of 1:0.5-1:2.0 to prepare molybdenum dioxide with extremely low carbon content and a certain amount of nano molybdenum core, and then the molybdenum dioxide with the nano molybdenum core is reduced by hydrogen to obtain high-purity nano molybdenum powder with extremely low carbon content. The method solves the problem that the nano molybdenum powder is difficult to prepare in the traditional process of preparing molybdenum dioxide and molybdenum powder by using hydrogen to reduce molybdenum trioxide. In the invention, fine carbon black is used as a reducing agent to generate a certain amount of dispersed nano molybdenum cores in molybdenum dioxide, and the dispersed nano molybdenum cores can assist hydrogen to reduce molybdenum dioxide to generate molybdenum nano particles. The average particle size of the nano molybdenum powder prepared by the method is 40-200nm, and the carbon content can be less than 0.01%. The method has the advantages of low raw material cost, high product purity, small particle size, simple process and high production efficiency, and is suitable for large-scale industrial production of high-purity nano molybdenum powder.
Description
Technical Field
The invention belongs to the field of preparation of nano powder materials, and discloses a method for preparing high-purity nano molybdenum powder.
Background
Molybdenum has many excellent characteristics, such as: high melting point, high hardness, high wear resistance, low thermal expansion coefficient, excellent electric and heat conductivity and good corrosion resistance. Molybdenum and its alloys have therefore found wide application in many fields. For example: chemical industry, metallurgy, electronics, military industry, aerospace and other fields. The nano-sized molybdenum powder has many unique properties such as extremely high specific surface area and enhanced chemical activity of atoms at the interface, which may significantly change the physical, mechanical and chemical properties. In addition, the nano molybdenum powder can obviously reduce the sintering temperature, and a product with higher density and smaller crystal grains can be obtained at lower temperature. Therefore, the sintering synthesis of the molybdenum blank and the molybdenum alloy by using the nano molybdenum powder is one of the best ways for improving the physical and mechanical properties of the molybdenum alloy.
Currently, the industrial preparation of molybdenum powder mainly adopts a process of reducing molybdenum trioxide by hydrogen in two stages. However, in the conventional process of preparing molybdenum dioxide and molybdenum powder by using hydrogen to reduce molybdenum trioxide, the nano molybdenum powder is difficult to prepare due to the difficulty in dispersing and nucleating molybdenum dioxide and molybdenum and the existence of a gas phase migration mechanism. Although there are many other methods for preparing nano molybdenum powder, including high energy ball milling, thermal plasma technology, carbonyl molybdenum thermal decomposition method, low temperature molten salt preparation, etc., these methods are difficult to be used for industrial production of nano molybdenum powder due to cost, production efficiency, complex process, etc.
Disclosure of Invention
The invention aims to provide a novel method for preparing high-purity nano molybdenum powder, which has low cost and simple and efficient process and is suitable for large-scale industrial production.
In order to achieve the purpose, the invention adopts the following technical scheme:
the method for preparing the high-purity nano molybdenum powder is characterized in that molybdenum trioxide is used as a molybdenum source, and carbon black and hydrogen are used as reducing agents; the molybdenum trioxide is reduced into molybdenum dioxide containing a certain amount of nano molybdenum cores by using carbon black, and then the molybdenum dioxide containing the nano molybdenum cores is reduced by using hydrogen to obtain high-purity nano molybdenum powder.
Further, the molybdenum trioxide may be replaced with ammonium molybdate.
Further, the method comprises the following specific steps:
(1) mixing molybdenum trioxide and carbon black according to the molar ratio of 1:0.5-1:2.0, uniformly mixing, and reducing at 400-750 ℃ to obtain the ultrafine molybdenum dioxide containing a certain amount of carbon black.
(2) And (2) reacting the superfine molybdenum dioxide containing a certain amount of carbon black obtained in the step (1) at the temperature of 800-1150 ℃ to obtain the molybdenum dioxide containing a certain amount of nano molybdenum cores.
(3) And (3) performing hydrogen reduction on the molybdenum dioxide containing a certain amount of nano molybdenum cores obtained in the step (2) at the temperature of 600-1100 ℃ to obtain high-purity nano molybdenum powder with the average particle size of 40-200 nm.
Furthermore, hydrogen can be used for replacing carbon black to reduce the molybdenum dioxide containing a certain amount of nano molybdenum cores, so that the high-purity nano molybdenum powder is prepared.
Compared with the prior art, the invention has the following advantages:
1. the invention provides a novel process for preparing high-purity nano molybdenum powder, which solves the problem that the nano molybdenum powder is difficult to prepare in the traditional process of preparing molybdenum dioxide and molybdenum powder by using hydrogen to reduce molybdenum trioxide.
2. The raw materials of molybdenum trioxide (or ammonium molybdate), carbon black and hydrogen used in the invention are all commonly used raw materials in industry, so that the production cost can be effectively reduced and the production efficiency can be improved.
3. The invention has simple process and low requirement on equipment. The reaction of the carbon black and the molybdenum oxide does not need special equipment, is convenient to control and has high generation efficiency; the hydrogen reduction of the molybdenum dioxide containing the nano molybdenum core can use the existing equipment for industrially producing molybdenum powder. Therefore, the method is suitable for industrial large-scale production of the nano molybdenum powder.
4. The nano molybdenum powder prepared by the invention has the average granularity of 40nm-200nm, uniform granularity and carbon content of less than 0.01 percent.
Detailed Description
For a further understanding of the present invention. The present invention will be further described with reference to examples.
The first embodiment is as follows:
uniformly mixing high-purity molybdenum trioxide and carbon black according to the molar ratio of 1: 0.8. Roasting the uniformly mixed raw materials at 600 ℃ for 1 hour in an inert gas atmosphere, then roasting at 1000 ℃ for 1 hour, and then performing hydrogen reduction on the roasted product at 900 ℃ to obtain the high-purity nano molybdenum powder.
Example two:
uniformly mixing high-purity molybdenum trioxide and carbon black according to the molar ratio of 1: 1.4. Roasting the uniformly mixed raw materials at 550 ℃ for 1.5 hours in an inert gas atmosphere, then roasting at 900 ℃ for 1 hour, and then performing hydrogen reduction on the roasted product at 800 ℃ to obtain the high-purity nano molybdenum powder.
Example three:
and uniformly mixing the ammonium molybdate according to the molar ratio of the molybdenum contained in the ammonium molybdate to the carbon black of 1: 1.0. Roasting the uniformly mixed raw materials at 530 ℃ for 2 hours in an inert gas atmosphere, then roasting at 950 ℃ for 1 hour, and then performing hydrogen reduction on the roasted product at 850 ℃ to obtain the high-purity nano molybdenum powder.
Claims (2)
1. A method for preparing high-purity nano molybdenum powder is characterized in that molybdenum trioxide is used as a molybdenum source, and carbon black and hydrogen are used as reducing agents; reducing molybdenum trioxide into molybdenum dioxide containing a certain amount of nano molybdenum cores by using carbon black, and then reducing the molybdenum dioxide containing the nano molybdenum cores by using hydrogen to obtain high-purity nano molybdenum powder;
the method comprises the following specific steps:
(1) mixing molybdenum trioxide and carbon black according to the molar ratio of 1:0.5-1:2.0, uniformly mixing, and reducing at 400-750 ℃ to obtain ultrafine molybdenum dioxide containing a certain amount of carbon black;
(2) reacting the superfine molybdenum dioxide containing a certain amount of carbon black obtained in the step (1) at the temperature of 800-1150 ℃ to obtain molybdenum dioxide containing a certain amount of nano molybdenum cores;
(3) and (3) performing hydrogen reduction on the molybdenum dioxide containing a certain amount of nano molybdenum cores obtained in the step (2) at the temperature of 600-1100 ℃ to obtain high-purity nano molybdenum powder with the average particle size of 40-200 nm.
2. The method for preparing high-purity nano molybdenum powder as claimed in claim 1, wherein the molybdenum trioxide can be replaced by ammonium molybdate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810826127.7A CN110227826B (en) | 2018-07-25 | 2018-07-25 | Method for preparing high-purity nano molybdenum powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810826127.7A CN110227826B (en) | 2018-07-25 | 2018-07-25 | Method for preparing high-purity nano molybdenum powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN110227826A CN110227826A (en) | 2019-09-13 |
| CN110227826B true CN110227826B (en) | 2020-06-12 |
Family
ID=67862272
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810826127.7A Active CN110227826B (en) | 2018-07-25 | 2018-07-25 | Method for preparing high-purity nano molybdenum powder |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110227826B (en) |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112222419B (en) * | 2020-12-07 | 2021-03-16 | 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 |
| 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 |
| CN112207287B (en) * | 2020-12-07 | 2021-03-16 | 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 |
| CN113234940B (en) * | 2021-04-13 | 2022-07-26 | 郑州大学 | Method for preparing molybdenum metal product from molybdenum concentrate in short process |
| 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 |
| CN115229181B (en) * | 2022-09-23 | 2022-12-09 | 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 |
| CN115233022B (en) * | 2022-09-23 | 2022-12-06 | 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 |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101200001A (en) * | 2007-12-17 | 2008-06-18 | 金堆城钼业股份有限公司 | Preparing process for ultrafine powder molybdenum |
| CN101966592A (en) * | 2010-11-01 | 2011-02-09 | 金堆城钼业股份有限公司 | Method for preparing molybdenum powder |
| CN106735282A (en) * | 2016-12-31 | 2017-05-31 | 湖南省华京粉体材料有限公司 | A kind of sodium molybdate organises the method for preparing nano Mo powder |
| CN107262733A (en) * | 2017-08-02 | 2017-10-20 | 北京科技大学 | A kind of method that two-part reduction prepares ultrafine molybdenum powder |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US9833765B2 (en) * | 2015-04-24 | 2017-12-05 | Georgia Tech Research Corporation | Carbide-derived carbons having incorporated metal chloride or metallic nanoparticles |
-
2018
- 2018-07-25 CN CN201810826127.7A patent/CN110227826B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101200001A (en) * | 2007-12-17 | 2008-06-18 | 金堆城钼业股份有限公司 | Preparing process for ultrafine powder molybdenum |
| CN101966592A (en) * | 2010-11-01 | 2011-02-09 | 金堆城钼业股份有限公司 | Method for preparing molybdenum powder |
| CN106735282A (en) * | 2016-12-31 | 2017-05-31 | 湖南省华京粉体材料有限公司 | A kind of sodium molybdate organises the method for preparing nano Mo powder |
| CN107262733A (en) * | 2017-08-02 | 2017-10-20 | 北京科技大学 | A kind of method that two-part reduction prepares ultrafine molybdenum powder |
Non-Patent Citations (1)
| Title |
|---|
| 钼粉的制备技术及其进展;林小芹等;《中国钼业》;20030228;第27卷(第01期);全文 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN110227826A (en) | 2019-09-13 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110227826B (en) | Method for preparing high-purity nano molybdenum powder | |
| CN108080649B (en) | Method for preparing superfine iron powder by low-temperature hydrocarbon duplex reduction | |
| CN104772473B (en) | A kind of preparation method of 3D printing fine grained sized spherical titanium powder | |
| CN108500283B (en) | Method for preparing nano tungsten powder by low-cost two-stage reduction | |
| CN102665972B (en) | The method of high-purity copper powder is produced by hot plasma | |
| CN112222419B (en) | Method for preparing nano molybdenum powder by regulating nucleation and growth processes and application | |
| CN106077695B (en) | A kind of preparation method of high-copper tungsten copper nano composite powder | |
| CN109336612B (en) | Preparation method of superfine titanium carbonitride powder | |
| CN110496969B (en) | Nano tungsten powder and preparation method thereof | |
| CN111187958A (en) | Mo powder/MoO2Method for preparing nano lanthanum-molybdenum oxide alloy by doping with lanthanum molybdate amine powder | |
| CN108543952A (en) | A kind of method of precursor process synthesis WC base nano composite powders | |
| CN109079151B (en) | Method for preparing ultra-coarse tungsten powder by high-temperature liquid-phase reduction of tungsten oxide | |
| WO2019227811A1 (en) | Ultrafine transition-metal boride powder, and preparation method therefor and application thereof | |
| CN108044126B (en) | Method for preparing plate-shaped WC-Co composite powder by using waste hard alloy | |
| CN107470646B (en) | Preparation method of superfine tungsten powder composite powder | |
| CN109128207B (en) | Superfine titanium powder and preparation method thereof | |
| CN103056376A (en) | Method for preparing spherical nanostructure tungsten/cobalt carbide compound powder | |
| CN102909389B (en) | Method for reducing and preparing nano molybdenum-copper composite powder with low temperature | |
| CN110014162B (en) | Method for preparing spherical molybdenum-based powder | |
| CN110014161B (en) | Method for preparing spherical tungsten-based powder | |
| CN109128143B (en) | Preparation method of nano tungsten-copper powder with core-shell structure | |
| CN107746057B (en) | Preparation method of superfine molybdenum carbide | |
| CN114853018B (en) | Preparation method of tantalum carbide powder | |
| CN112222420B (en) | Nano tungsten powder doped with metal oxide nano particles and preparation method thereof | |
| CN112338198B (en) | Micron-sized molybdenum powder and preparation method and application thereof |
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 |