CN115229199B - Method for preparing high-dispersion high-porosity superfine molybdenum dioxide and molybdenum powder by induced nucleation - Google Patents
Method for preparing high-dispersion high-porosity superfine molybdenum dioxide and molybdenum powder by induced nucleation Download PDFInfo
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Abstract
The invention discloses a method for preparing high-dispersion high-porosity ultrafine molybdenum dioxide and molybdenum powder by inducing nucleation, which comprises the following steps: 1. carrying out active site, particle size adjustment and modification treatment on the amorphous cracked carbon to obtain high-activity-site amorphous cracked carbon, and carrying out crushing, agglomeration and dispersion treatment on molybdenum trioxide to obtain dispersed molybdenum trioxide; 2. stirring and dispersing high-activity-site amorphous cracked carbon and dispersed molybdenum trioxide, and performing low-energy ball milling to obtain uniformly mixed slurry; 3. drying the uniformly mixed slurry and then stirring; 4. reducing with hydrogen to obtain high-dispersion high-porosity superfine molybdenum dioxide powder; 5. and performing hydrogen reduction treatment to obtain the high-dispersion high-porosity ultrafine molybdenum powder. The method improves carbon defects and active sites through active site and particle size adjustment and modification treatment, realizes the control of the particle sizes of molybdenum dioxide powder and molybdenum powder by taking the carbon defects and the active sites as an inducer for molybdenum trioxide nucleation and molybdenum source directional transmission in the hydrogen reduction process, and sequentially obtains superfine molybdenum dioxide and molybdenum powder.
Description
Technical Field
The invention belongs to the technical field of preparation of nano powder materials, and particularly relates to a method for preparing high-dispersion high-porosity superfine molybdenum dioxide and molybdenum powder by induced nucleation.
Background
Molybdenum has the advantages of high melting point, higher strength and elastic modulus, low expansion coefficient, good electric conductivity and thermal conductivity, excellent corrosion resistance and the like. By virtue of these excellent characteristics, molybdenum and its alloy materials have important applications in many fields. Most molybdenum products are indispensable key materials for national defense and national economy departments, and have important application in the fields of aerospace, military, chemistry, nuclear energy, metallurgy and the like. Although the metal molybdenum material has a series of excellent physical, chemical and mechanical properties, the molybdenum material with a common structure has the defects of low recrystallization temperature, low strength, toughness, hardness, low wear resistance and the like, and the increasing requirements of the fields of civil use, military industry, national defense and the like on the superior comprehensive properties of the molybdenum material are difficult to meet. The design and preparation of the ultra-fine grain nano-structure alloy material become an important development trend of high-performance powder metallurgy molybdenum materials. Among them, the ultra-fine/nano molybdenum powder is considered as a key raw material for preparing ultra-fine grain nano-structured molybdenum and its alloy material by powder metallurgy due to its excellent characteristics.
The particle size and morphology of the molybdenum powder are mainly determined by MoO 2 Reduction to Mo to refine MoO 2 The granularity of the Mo powder is beneficial to preparing the finer Mo powder. However, it is difficult to reduce commercial micron-sized MoO using conventional hydrogen 3 Reduced to ultrafine/nano MoO 2 Mainly because the number of nuclei formed in the reduction process is too small and difficult to regulate. The hydrogen reduction of molybdenum trioxide is the main process for industrially preparing molybdenum dioxide at present, but the reduction of commercial micron-sized molybdenum trioxide hydrogen into superfine molybdenum dioxide is always a difficult problem.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a method for preparing high-dispersion high-porosity superfine molybdenum dioxide and molybdenum powder by inducing nucleation, aiming at the defects of the prior art. According to the method, active sites, particle size adjustment and modification treatment are carried out on amorphous cracked carbon, so that carbon defects and active sites are improved, the high-activity-site amorphous cracked carbon is obtained and is used as an inducer for molybdenum trioxide nucleation and molybdenum source directional transmission in a hydrogen reduction process, effective control over the particle size of molybdenum dioxide is achieved, control over the particle size of molybdenum powder is further achieved, and the problems of small nucleation quantity, poor dispersibility, large particle size and the like in the traditional process of reducing molybdenum trioxide by hydrogen are solved.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows: the method for preparing the high-dispersion high-porosity superfine molybdenum dioxide and molybdenum powder by inducing nucleation is characterized by comprising the following steps:
step one, carrying out active site, particle size adjustment and modification treatment on amorphous cracking carbon to obtain high-active-site amorphous cracking carbon, and carrying out crushing agglomeration and dispersion treatment on molybdenum trioxide to obtain dispersed molybdenum trioxide;
step two, adding the high-activity-site amorphous cracked carbon and the dispersed molybdenum trioxide obtained in the step one into a solvent and a dispersing agent for stirring and dispersing, and then putting the mixture into a ball milling tank for low-energy ball milling and mixing to obtain uniform mixing slurry;
step three, drying the uniformly mixed slurry obtained in the step two, then putting the dried uniformly mixed slurry into an ultrahigh-speed stirrer, and stirring the slurry to disperse and adjust the porosity, so as to obtain the high-activity site amorphous cracked carbon particle-coated molybdenum trioxide nano composite powder with a core-shell structure and high dispersion and low apparent density;
step four, performing hydrogen reduction on the high-activity site amorphous cracked carbon particle coated molybdenum trioxide nano composite powder with the core-shell structure with high dispersion and low apparent density obtained in the step three to obtain high-dispersion high-porosity superfine molybdenum dioxide powder;
and step five, carrying out hydrogen reduction treatment on the superfine molybdenum dioxide powder with high dispersion and high porosity obtained in the step four to obtain the superfine molybdenum powder with high dispersion and high porosity.
The method comprises the steps of carrying out active site, particle size adjustment and modification treatment on amorphous cracked carbon, improving carbon defects and active sites, obtaining high-activity-site amorphous cracked carbon, then taking the high-activity-site amorphous cracked carbon as an inducer for molybdenum trioxide nucleation and molybdenum source directional transmission in a hydrogen reduction process, dispersing the high-activity-site amorphous cracked carbon and dispersed molybdenum trioxide under the assistance of a dispersing agent, carrying out ball-milling mixing, and carrying out ultrahigh-speed stirring treatment to obtain the molybdenum trioxide nano composite powder coated by the high-activity-site amorphous cracked carbon particles with a core-shell structure, further improving the dispersibility and the porosity, and providing necessary conditions for gas phase migration transmission and dispersed nucleation growth in the hydrogen reduction process; in the hydrogen reduction process, as a nucleation inducer, a large number of active sites in the high-activity-site amorphous cracking carbon induce gas-phase dissolution and directional transmission of molybdenum trioxide, and the molybdenum trioxide in pores is transferred to amorphous cracking carbon distributed around the molybdenum trioxide through gas-phase migration to react to form heterogeneous nucleation and deposition growth of molybdenum dioxide, so that large-particle molybdenum trioxide is dissolved, transferred and converted into ultrafine molybdenum dioxide with high activity sites, and the molybdenum dioxide with high activity sites is reduced into ultrafine molybdenum powder through further hydrogen reduction treatment, thereby solving the problems of small number of nucleation of molybdenum dioxide, poor dispersibility, large particle size and the like in the traditional process of reducing molybdenum trioxide by hydrogen.
The method for preparing the high-dispersion high-porosity ultrafine molybdenum dioxide and molybdenum powder by inducing nucleation is characterized in that in the step one, the amorphous cracking carbon is generated by cracking a gas-phase carbon source, a liquid-phase carbon source or a solid-phase carbon source, and the active site, particle size and modification treatment methods comprise ultrasonic treatment, friction treatment, plasma treatment or microwave treatment; the mass purity of the molybdenum trioxide is more than 99%, and the average particle size of the primary particles is less than 5 mu m. The invention adopts common micron-sized molybdenum trioxide as a raw material, and the raw material has wide source and low cost, thereby reducing the preparation cost.
The method for preparing the high-dispersion high-porosity superfine molybdenum dioxide and molybdenum powder by induced nucleation is characterized in that the mass of the high-activity-site amorphous cracked carbon in the second step is less than 3% of the mass of the dispersed molybdenum trioxide. The method adopts the high-activity site amorphous cracking carbon as the nucleation inducer, provides a great number of heterogeneous nucleation sites for reducing the ultrafine molybdenum dioxide powder, can meet the requirement of controlling the granularity of the molybdenum dioxide only by using very little carbon, and reduces the addition amount of the high-activity site amorphous cracking carbon.
The method for preparing the high-dispersion high-porosity superfine molybdenum dioxide and molybdenum powder by induced nucleation is characterized in that in the third step, the rotating speed of the ultra-high speed stirrer is more than 5000 revolutions per minute, the stirring time is more than 60 seconds, and the loose density of the high-activity site amorphous cracked carbon particle-coated molybdenum trioxide nano composite powder with the core-shell structure of the high-dispersion and low-loose density is less than 1.0g/cm 3 The porosity is greater than 80%. The invention improves the dispersion degree and porosity of the nano composite powder and reduces the apparent density by controlling the rotating speed and time of ultrahigh-speed stirring, thereby providing conditions for obtaining the superfine molybdenum dioxide powder and the molybdenum powder by subsequent preparation.
The method for preparing the high-dispersion high-porosity superfine molybdenum dioxide and molybdenum powder by inducing nucleation is characterized in that the hydrogen is reduced in the step fourThe temperature is 500-700 ℃, the average particle size of the superfine molybdenum dioxide powder is less than 500nm, and the loose packed density is less than 1.0g/cm 3 The porosity is greater than 90%. By controlling the temperature of hydrogen reduction, the invention ensures the generation of gas-phase molybdenum-containing hydrate in the nano composite powder and the gas-phase transmission and migration from the oxide to the nucleation inducer on the one hand, and effectively controls the concentration of generated water vapor on the other hand, and ensures the stability of the molybdenum dioxide powder particles obtained by reduction.
The method for preparing the high-dispersion high-porosity ultrafine molybdenum dioxide and molybdenum powder by induced nucleation is characterized in that the temperature of hydrogen reduction treatment in the fifth step is 700-900 ℃, the average particle size of the high-dispersion high-porosity ultrafine molybdenum powder is less than 500nm, and the apparent density is less than 1.0g/cm 3 The porosity is greater than 90%. The invention reduces the concentration of generated water vapor and reduces the gas phase dissolution and coarsening of molybdenum by controlling the temperature of hydrogen reduction treatment, realizes the control of the ultrafine granularity of molybdenum dioxide and ensures that the ultrafine molybdenum powder with high dispersion and high porosity is obtained.
Compared with the prior art, the invention has the following advantages:
1. according to the invention, the active site, the particle size and the modification treatment are carried out on the amorphous cracked carbon, so that the carbon defect and the active site are improved, the high-activity-site amorphous cracked carbon is obtained and is used as an inducer for molybdenum trioxide nucleation and molybdenum source directional transmission in the hydrogen reduction process, the effective control of the particle size of molybdenum dioxide is realized, the particle size of molybdenum powder is further controlled, and the superfine molybdenum dioxide and molybdenum powder are sequentially obtained.
2. The invention constructs the nano composite powder with a core-shell structure by ball milling and mixing the high-activity site amorphous cracking carbon and the dispersed molybdenum trioxide, combines with ultrahigh-speed stirring treatment, further improves the dispersibility and the porosity, and provides necessary conditions for gas phase migration transmission and dispersed nucleation growth in the hydrogen reduction process.
3. The method utilizes the high-activity-site amorphous cracking carbon in the nano composite powder of the molybdenum trioxide coated by the high-activity-site amorphous cracking carbon particles with the core-shell structure as a nucleating agent to induce and promote gas phase dissolution, transmission migration, nucleation and deposition growth of the molybdenum trioxide to form ultrafine molybdenum dioxide with high activity sites, and solves the problems of small number of molybdenum dioxide nucleation, poor dispersibility, large particle size and the like in the traditional process of reducing the molybdenum trioxide by hydrogen.
4. The invention performs hydrogen reduction treatment on the ultrafine molybdenum dioxide powder with high dispersion, high porosity and high active sites, obviously improves the nucleation number of the molybdenum powder by utilizing each site with high activity, obviously improves the dispersibility of the molybdenum powder by utilizing high dispersibility, and obviously improves the gas phase migration efficiency by utilizing high porosity, thereby improving the dispersibility and the reaction efficiency of the molybdenum powder.
5. The invention adopts common micron-sized molybdenum trioxide as a raw material, has wide sources and low cost, and reduces the preparation cost.
The technical solution of the present invention is further described in detail by the accompanying drawings and examples.
Drawings
Fig. 1 is an SEM image of a high-activity-site amorphous cracked carbon particle-coated molybdenum trioxide nanocomposite powder having a core-shell structure prepared in example 1 of the present invention.
FIG. 2 is an SEM photograph of the ultrafine molybdenum dioxide powder prepared in example 1 of the present invention.
FIG. 3 is an SEM image of the ultrafine molybdenum dioxide powder prepared in example 2 of the present invention.
Detailed Description
Example 1
The embodiment comprises the following steps:
firstly, carrying out active site, particle size adjustment and modification treatment on amorphous cracked carbon generated by cracking glucose through ultrasonic irradiation to obtain high-activity-site amorphous cracked carbon, and carrying out high-speed stirring on molybdenum trioxide with the mass purity of 99.95% and the average particle size of primary particles of 2 mu m at the rotating speed of 15000 r/min to carry out crushing, agglomeration and dispersion treatment to obtain dispersed molybdenum trioxide;
step two, adding the high-activity-site amorphous cracked carbon and the dispersed molybdenum trioxide obtained in the step one into solvent ethanol and a dispersing agent PEG-1000 for stirring and dispersing, and then putting the mixture into a ball milling tank for low-energy ball milling and mixing at the rotating speed of 200 revolutions per minute to obtain uniform mixing slurry; the mass of the high-activity-site amorphous cracking carbon is 1.25% of that of the dispersed molybdenum trioxide;
step three, drying the uniformly mixed slurry obtained in the step two at 80 ℃, and then putting the dried uniformly mixed slurry into an ultrahigh-speed stirrer to stir at the rotating speed of 20000 revolutions per minute for 160 seconds to disperse and adjust the porosity, so as to obtain the high-activity-site amorphous cracking carbon particles of the core-shell structure coated with the molybdenum trioxide nano composite powder; the loose packing density of the high-activity-site amorphous cracked carbon particle-coated molybdenum trioxide nano composite powder with the core-shell structure is 0.6g/cm 3 The porosity is 90%;
fourthly, carrying out hydrogen reduction on the high-activity-site amorphous cracked carbon particle-coated molybdenum trioxide nano composite powder with the core-shell structure obtained in the third step at 500-700 ℃ to obtain superfine molybdenum dioxide powder; the average particle size of the superfine molybdenum dioxide powder is 400nm, and the apparent density is 0.6g/cm 3 Porosity of 91%;
step five, performing hydrogen reduction treatment on the superfine molybdenum dioxide powder obtained in the step four at the temperature of 700-800 ℃ to obtain superfine molybdenum powder; the average particle diameter of the ultrafine molybdenum powder is 400nm, and the apparent density is 0.8g/cm 3 The porosity was 92%.
In the first step of this embodiment, the amorphous cracked carbon may be generated by cracking a gas-phase or liquid-phase carbon source, and the methods of active site and particle size adjustment and modification treatment may be replaced by friction treatment, plasma treatment or microwave treatment.
Fig. 1 is an SEM image of the molybdenum trioxide nano-composite powder coated with the highly active site amorphous cracking carbon particles of the core-shell structure prepared in this example, and it can be seen from fig. 1 that the highly active site amorphous cracking carbon particles are uniformly coated around the molybdenum trioxide particles with a larger particle size to construct the micro-nano core-shell structure.
FIG. 2 is an SEM photograph of the ultrafine molybdenum dioxide powder prepared in this example, and it can be seen from FIG. 2 that the average particle size of the ultrafine molybdenum dioxide powder is about 400nm.
Example 2
The embodiment comprises the following steps:
firstly, carrying out active site, particle size adjustment and modification treatment on amorphous cracking carbon generated by cracking sucrose by ultrasonic irradiation to obtain high-activity-site amorphous cracking carbon, and carrying out high-speed stirring on molybdenum trioxide with the mass purity of 99.95% and the average particle size of primary particles of 2 mu m at the rotating speed of 15000 r/min to carry out crushing, agglomeration and dispersion treatment to obtain dispersed molybdenum trioxide;
step two, adding the high-activity-site amorphous cracked carbon and the dispersed molybdenum trioxide obtained in the step one into solvent ethanol and a dispersing agent PEG-1000 for stirring and dispersing, and then putting the mixture into a ball milling tank for low-energy ball milling and mixing at the rotating speed of 200 revolutions per minute to obtain uniform mixing slurry; the mass of the high-activity-site amorphous cracking carbon is 2.5% of that of the dispersed molybdenum trioxide;
step three, drying the uniformly mixed slurry obtained in the step two at 80 ℃, then putting the uniformly mixed slurry into an ultrahigh-speed stirrer, and stirring the uniformly mixed slurry for 120 seconds at the rotating speed of 15000 revolutions per minute to disperse and adjust the porosity, so as to obtain the high-activity-site amorphous cracked carbon particle-coated molybdenum trioxide nano composite powder with a core-shell structure; the loose packing density of the high-activity-site amorphous cracking carbon particle-coated molybdenum trioxide nano composite powder with the core-shell structure is 0.55g/cm 3 Porosity of 88%;
fourthly, carrying out hydrogen reduction on the high-activity-site amorphous cracked carbon particle-coated molybdenum trioxide nano composite powder with the core-shell structure obtained in the third step at the temperature of 500-600 ℃ to obtain superfine molybdenum dioxide powder; the average particle size of the superfine molybdenum dioxide powder is less than 300nm, and the apparent density is 0.5g/cm 3 Porosity 92%;
step five, performing hydrogen reduction treatment on the superfine molybdenum dioxide powder obtained in the step four at 800-900 ℃ to obtain superfine molybdenum powder; the average grain diameter of the superfine molybdenum powder is less than 400nm, and the apparent density is 0.8g/cm 3 The porosity was 92.2%.
In the first step of this embodiment, the amorphous cracked carbon may be generated by cracking a gas-phase or liquid-phase carbon source, and the methods of adjusting the active sites and the particle size and modifying may be replaced by friction treatment, plasma treatment or microwave treatment.
Fig. 3 is an SEM image of the ultra-fine molybdenum dioxide powder prepared in this example, and it can be seen from fig. 3 that the average particle size of the ultra-fine molybdenum dioxide powder is less than 300nm.
Example 3
The embodiment comprises the following steps:
firstly, carrying out active site, particle size adjustment and modification treatment on amorphous cracking carbon generated by glucose cracking through ultrasonic irradiation to obtain high-active-site amorphous cracking carbon, and carrying out high-speed stirring on molybdenum trioxide with the mass purity of 99.9% and the average particle size of 4 mu m of primary particles at the rotating speed of 15000 r/min to carry out crushing agglomeration and dispersion treatment to obtain dispersed molybdenum trioxide;
step two, adding the high-activity-site amorphous cracking carbon and the dispersed molybdenum trioxide obtained in the step one into solvent ethanol and a dispersing agent PEG-1000 for stirring and dispersing, and then putting into a ball milling tank for low-energy ball milling and mixing at a rotating speed of 200 revolutions per minute to obtain uniform mixing slurry; the mass of the high-activity-site amorphous cracking carbon is 2% of that of the dispersed molybdenum trioxide;
step three, drying the uniformly mixed slurry obtained in the step two at 80 ℃, then putting the uniformly mixed slurry into an ultrahigh-speed stirrer, and stirring the uniformly mixed slurry for 160 seconds at the rotating speed of 10000 revolutions per minute to disperse and adjust the porosity, so as to obtain the core-shell structure high-activity-site amorphous cracked carbon particle-coated molybdenum trioxide nano composite powder; the loose packing density of the high-activity-site amorphous cracked carbon particle-coated molybdenum trioxide nano composite powder with the core-shell structure is 0.6g/cm 3 Porosity of 85%;
fourthly, carrying out hydrogen reduction on the high-activity-site amorphous cracked carbon particle-coated molybdenum trioxide nano composite powder with the core-shell structure obtained in the third step at 500-700 ℃ to obtain superfine molybdenum dioxide powder; the average particle size of the superfine molybdenum dioxide powder is less than 350nm, and the apparent density is 0.55g/cm 3 Porosity 91.5%;
step five, performing the superfine molybdenum dioxide powder obtained in the step four at the temperature of 800-900 DEG CReducing with hydrogen to obtain superfine molybdenum powder; the average particle diameter of the superfine molybdenum powder is 390nm, and the apparent density is 0.9g/cm 3 The porosity was 91.2%.
In the first step of this embodiment, the amorphous cracked carbon may be generated by cracking a gas-phase or liquid-phase carbon source, and the methods of adjusting the active sites and the particle size and modifying may be replaced by friction treatment, plasma treatment or microwave treatment.
The above description is only for the preferred embodiment of the present invention, and is not intended to limit the present invention in any way. Any simple modification, change and equivalent changes of the above embodiments according to the technical essence of the invention are still within the protection scope of the technical solution of the invention.
Claims (3)
1. The method for preparing the high-dispersion high-porosity superfine molybdenum dioxide and molybdenum powder by inducing nucleation is characterized by comprising the following steps:
step one, carrying out active site, particle size adjustment and modification treatment on amorphous pyrolysis carbon to obtain high-activity-site amorphous pyrolysis carbon, and carrying out crushing, agglomeration and dispersion treatment on molybdenum trioxide to obtain dispersed molybdenum trioxide;
step two, adding the high-activity-site amorphous cracking carbon and the dispersed molybdenum trioxide obtained in the step one into a solvent and a dispersing agent for stirring and dispersing, and then putting into a ball-milling tank for low-energy ball-milling mixing to obtain uniform mixing slurry;
step three, drying the uniformly mixed slurry obtained in the step two, then putting the dried uniformly mixed slurry into an ultrahigh-speed stirrer, and stirring the slurry to disperse and adjust the porosity, so as to obtain the high-activity site amorphous cracked carbon particle-coated molybdenum trioxide nano composite powder with a core-shell structure and high dispersion and low apparent density; the rotation speed of the ultra-high speed stirrer is more than 5000 revolutions per minute, the stirring time is more than 60 seconds, and the apparent density of the molybdenum trioxide-coated nano composite powder coated by the high-activity site amorphous cracked carbon particles with the core-shell structure with high dispersion and low apparent density is less than 1.0g/cm 3 Porosity is greater than 80%;
step four, the high dispersion and low apparent density obtained in the step threeThe high-activity-site amorphous cracked carbon particles of the core-shell structure coat the molybdenum trioxide nano-composite powder to carry out hydrogen reduction, so as to obtain high-dispersion high-porosity superfine molybdenum dioxide powder; the temperature of hydrogen reduction is 500-700 ℃, the average particle size of the superfine molybdenum dioxide powder is less than 500nm, and the apparent density is less than 1.0g/cm 3 Porosity greater than 90%;
step five, performing hydrogen reduction treatment on the high-dispersion high-porosity superfine molybdenum dioxide powder obtained in the step four to obtain high-dispersion high-porosity superfine molybdenum powder; the temperature of the hydrogen reduction treatment is 700-900 ℃, the average particle size of the high-dispersion high-porosity ultrafine molybdenum powder is less than 500nm, and the apparent density is less than 1.0g/cm 3 The porosity is greater than 90%.
2. The method for preparing high-dispersion high-porosity superfine molybdenum dioxide and molybdenum powder through induced nucleation according to claim 1, wherein the amorphous cracked carbon is generated through cracking of a gas-phase, liquid-phase or solid-phase carbon source in the step one, and the active site, particle size adjustment and modification treatment are ultrasonic treatment, friction treatment, plasma treatment or microwave treatment; the mass purity of the molybdenum trioxide is more than 99%, and the average particle size of the primary particles is less than 5 mu m.
3. The method for preparing ultra-fine molybdenum dioxide and molybdenum powder with high dispersion and high porosity by induced nucleation as claimed in claim 1, wherein the mass of the high active site amorphous cracked carbon in the second step is less than 3% of the mass of the dispersed molybdenum trioxide.
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| DE10253399A1 (en) * | 2002-11-15 | 2004-05-27 | Eramet & Comilog Chemicals S.A. | Metal-coated carbon black, useful as ferromagnetic material or in e.g. medical valve applications, involve use of nickel, iron, cobalt, yttrium, copper or iridium as the metal |
| DE102006057004A1 (en) * | 2006-12-02 | 2008-06-05 | H.C. Starck Gmbh | metal powder |
| CN102350506A (en) * | 2011-10-31 | 2012-02-15 | 西南石油大学 | Preparation method of nano-structure WC-Co composite powder |
| JP2014534348A (en) * | 2011-11-25 | 2014-12-18 | アーベー フェアロイレジェリンガーＡｂ Ｆｅｒｒｏｌｅｇｅｒｉｎｇａｒ | Pellets containing iron and molybdenum |
| SE1650211A1 (en) * | 2016-02-18 | 2017-08-19 | Process for producing molybdenum-containing units | |
| CN109317665B (en) * | 2018-12-03 | 2020-07-17 | 中南大学 | Copper/carbon composite material and preparation method thereof |
| CN111495402B (en) * | 2020-04-20 | 2023-03-24 | 嘉兴学院 | Molybdenum-based composite material prepared by microwave spark and preparation method and application thereof |
| CN112222418B (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 tungsten powder by regulating nucleation and growth processes and application |
| 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 |
| CN114425616B (en) * | 2022-03-31 | 2022-06-24 | 南通领跑者新材料科技有限公司 | Silver-coated copper composite powder with core-shell structure and preparation method thereof |
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