CN114192793A - Spheroidizing process for refractory metal powder - Google Patents
Spheroidizing process for refractory metal powder Download PDFInfo
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- CN114192793A CN114192793A CN202111617166.4A CN202111617166A CN114192793A CN 114192793 A CN114192793 A CN 114192793A CN 202111617166 A CN202111617166 A CN 202111617166A CN 114192793 A CN114192793 A CN 114192793A
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- 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
The invention discloses a spheroidizing process of refractory metal powder, and relates to the technical field of metal processing. The invention uses hydrogen peroxide and polyhydric alcohol to pretreat the nanometer refractory metal oxide, and then uses the plasma spheroidizing device to reduce and spheroidize the pretreated refractory metal oxide, thereby obtaining the nanometer refractory metal spherical particles. The treatment process can obtain refractory metal spherical particles with the diameter of 50-350nm, and the refractory metal spherical particles have high sphericity and high dispersity among particles.
Description
Technical Field
The invention belongs to the technical field of metal processing, and particularly relates to a spheroidizing process of refractory metal powder.
Background
The refractory metal is a metal element such as titanium, zirconium, or hafnium in the IV subgroup, vanadium, niobium, or tantalum in the V subgroup, chromium, tungsten, or molybdenum in the VI subgroup, or rhenium in the VII subgroup in the periodic table. The refractory metals, as a group with a melting point higher than 1650 ℃, have variable valence and play an important role in national economy by virtue of outstanding physical, chemical, mechanical and nuclear properties, and particularly play a more important role in the advanced scientific field.
The spherical metal powder material has excellent physical and chemical properties, which are mainly reflected in good powder flowability, low powder particle porosity, high density, effectively improved surface smoothness and brittleness, and thus is more and more widely applied. For example, the spherical tungsten powder and the titanium powder replace the conventional common powder materials used in the fields of aerospace and the like, so that the performance of the equipment is greatly improved. Spheroidization of metallic powder materials is an important basis for technological advances and industry upgrades in powder metallurgy and equipment manufacturing.
At present, the spheroidization technology of refractory metals is mainly a plasma spheroidization technology, and the refractory metals are rapidly spheroidized by taking plasma as a heat source and by virtue of the characteristics of high temperature, high break and large temperature gradient. The procedure for the preparation of spherical powders was as follows:
a stable argon plasma torch was first set up and then the raw powder was injected into the torch with a carrier gas (argon) through a charging gun. The powder particles absorb a large amount of heat in a plasma torch within a very short time and are rapidly melted, and in the flying process of the particles, ions with high sphericity are formed under the action of surface tension, enter a heat exchange chamber at a very high speed, are cooled and solidified, and then enter a gas-solid separation chamber to be collected. Because the metal powder particles are melted at high temperature, the grain diameter of the prepared spheroidized metal is relatively high and is generally in a micron level, and the spheroidized metal powder in a nanometer level is difficult to prepare by utilizing a plasma technology.
For example, chinese patent CN111097919A discloses a method for preparing multi-component refractory metal spherical powder, which comprises ball-milling refractory metal hydride, mixing with refractory metal simple substance, adding solvent and binder, mixing and granulating, and spheroidizing spherical particles in a plasma spheroidizing powder-making device to obtain particles with a particle size of 10-60 microns.
Therefore, the preparation of nanoscale spherical metal powder is a new direction of current research.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a spheroidizing process of refractory metal powder. The nanometer refractory metal oxide is treated by hydrogen peroxide and polyhydric alcohol, and then the treated refractory metal oxide is subjected to reduction spheroidization by using a plasma technology, so that the nanometer refractory metal spherical particles are obtained.
The spheroidizing process of the refractory metal powder comprises the following steps:
(1) putting refractory metal oxide (with particle size of 1-100 nm) with particle size of 10-100nm into ethanol, adding hydrogen peroxide and polyalcohol, mixing, and ball milling;
(2) filtering the ball-milled slurry, spray drying, and mechanically grinding and screening;
(3) carrying out plasma spheroidizing treatment on the powder treated in the step (2) to obtain refractory metal spherical particles with the diameter of 50-350 nm; wherein the hydrogen flow in the plasma spheroidization process is 40-50scfh, the argon flow is 5-10scfh, and the power is 50-100 kw.
Preferably, the refractory metal oxide of the present invention is an oxide of vanadium, niobium, tantalum, chromium, tungsten or molybdenum, specifically one of vanadium pentoxide, niobium pentoxide, tantalum pentoxide, chromium trioxide, tungsten trioxide or molybdenum trioxide.
Preferably, the adding amount of the hydrogen peroxide in the step (1) accounts for 1-3% of the mass of the refractory metal oxide.
Preferably, said polyol of step (1) is added in an amount of 5 to 10% by mass of said refractory metal oxide.
More preferably, the polyol in the step (1) is one of ethylene glycol and glycerol.
Preferably, the temperature of said spray drying of step (2) is below 150 ℃.
Further preferred. The temperature of the spray drying in the step (2) is 100-120 ℃.
Preferably, in the step (2), the powder after spray drying is ground for 30min-150 min. Compared with the prior art, the invention has the following beneficial effects:
according to the invention, the nanometer refractory metal oxide particles are pretreated, so that agglomeration among the particles is avoided when the pretreated refractory metal oxide is subjected to plasma spheroidization, and meanwhile, parameters of a spheroidization process are adjusted, so that hydrogen is used as a main atmosphere, and reduction treatment is simultaneously carried out in the spheroidization process, thereby obtaining the nanometer refractory metal spherical particles. The treatment method effectively avoids the occurrence of the agglomeration phenomenon of the nano particles during the rapid high-temperature spheroidizing treatment, thereby ensuring the dispersity and the sphericity of the spherical particles.
Detailed Description
The invention provides a spheroidization process of refractory metal powder, which comprises the steps of treating a nanoscale refractory metal oxide by using hydrogen peroxide and polyhydric alcohol, and then carrying out reduction spheroidization on the treated refractory metal oxide by using a plasma technology, thereby obtaining nanoscale refractory metal spherical particles.
The present invention will be further described with reference to the following specific examples.
Example 1
A spheroidizing process for refractory metal powder comprises the following specific steps
(1) Putting vanadium pentoxide with the average particle size of 20nm into ethanol, adding hydrogen peroxide accounting for 2% of the mass of the vanadium pentoxide and ethylene glycol accounting for 5% of the mass of the vanadium pentoxide, mixing, and performing ball milling treatment;
(2) filtering the slurry after ball milling, and performing spray drying at the drying temperature of 120 ℃ for 100min by mechanical grinding;
(3) carrying out plasma spheroidizing treatment on the powder treated in the step (2) to obtain refractory metal spherical particles with the average diameter of 75 nm; wherein the hydrogen flow rate in the plasma spheroidization process is 45scfh, the argon flow rate is 5scfh, and the power is 80 kw.
Examples 2 to 6
According to the method of the embodiment 1, the vanadium pentoxide in the embodiment 1 is replaced by niobium pentoxide, tantalum pentoxide, chromium sesquioxide, tungsten sesquioxide and molybdenum trioxide, and the rest of the processes are not changed. Specifically, the results are shown in Table 1.
TABLE 1
| Refractory metal oxides | Average diameter of refractory metal spherical particles | |
| Example 1 | Vanadium pentoxide | 75nm |
| Example 2 | Niobium pentoxide | 70nm |
| Example 3 | Tantalum pentoxide | 72nm |
| Example 4 | Chromium oxide | 63nm |
| Example 5 | Tungsten sesquioxide | 65nm |
| Example 6 | Molybdenum trioxide | 60nm |
Examples 7 to 10
The average particle size of the vanadium pentoxide in example 1 was adjusted to 10nm, 50nm, 80nm, and 100nm by the method of example 1, and the rest of the process was not changed. Specifically, as shown in table 2.
TABLE 2
| Average particle diameter of refractory metal oxide | Average diameter of refractory metal spherical particles | |
| Example 7 | 10nm | 50nm |
| Example 1 | 20nm | 75nm |
| Example 8 | 50nm | 130nm |
| Example 9 | 80nm | 210nm |
| Example 10 | 100nm | 300nm |
Example 11
A spheroidizing process for refractory metal powder comprises the following specific steps
(1) Putting vanadium pentoxide with the average particle size of 20nm into ethanol, adding hydrogen peroxide accounting for 1% of the mass of the vanadium pentoxide and ethylene glycol accounting for 10% of the mass of the vanadium pentoxide, mixing, and performing ball milling treatment;
(2) filtering the slurry after ball milling, and performing spray drying at the drying temperature of 110 ℃ for mechanical grinding for 80 min;
(3) carrying out plasma spheroidizing treatment on the powder treated in the step (2) to obtain refractory metal spherical particles with the average diameter of 80 nm; wherein the hydrogen flow rate in the plasma spheroidization process is 45scfh, the argon flow rate is 5scfh, and the power is 80 kw.
Example 12
A spheroidizing process for refractory metal powder comprises the following specific steps
(1) Putting vanadium pentoxide with the average particle size of 20nm into ethanol, adding hydrogen peroxide accounting for 3% of the mass of the vanadium pentoxide and ethylene glycol accounting for 8% of the mass of the vanadium pentoxide, mixing, and performing ball milling treatment;
(2) filtering the slurry after ball milling, and performing spray drying at the drying temperature of 120 ℃ for 100min by mechanical grinding;
(3) carrying out plasma spheroidizing treatment on the powder treated in the step (2) to obtain refractory metal spherical particles with the average diameter of 60 nm; wherein the hydrogen flow rate in the plasma spheroidization process is 45scfh, the argon flow rate is 5scfh, and the power is 80 kw.
Examples 13 to 16
The process of example 1 was followed with the temperature of the spray drying of step (2) being adjusted and the rest of the process being unchanged. Specifically, the results are shown in Table 3.
TABLE 3
| Temperature of spray drying | Average diameter of refractory metal spherical particles | |
| Example 1 | 120℃ | 75nm |
| Example 13 | 110℃ | 70nm |
| Example 14 | 100℃ | 65nm |
| Example 15 | 150℃ | 1.0µm |
| Example 16 | 200℃ | 1.8µm |
Comparative example 1
A spheroidizing process for refractory metal powder comprises the following specific steps
(1) Putting vanadium pentoxide with the average particle size of 20nm into ethanol, adding hydrogen peroxide accounting for 2% of the mass of the vanadium pentoxide, mixing, and performing ball milling treatment;
(2) filtering the slurry after ball milling, and performing spray drying at the drying temperature of 120 ℃ for 100min by mechanical grinding;
(3) carrying out plasma spheroidizing treatment on the powder treated in the step (2) to obtain refractory metal spherical particles with the average diameter of 1.0 mu m; wherein the hydrogen flow rate in the plasma spheroidization is 45scfh, the argon flow rate is 5scfh, and the power is 80 kw.
Comparative example 2
A spheroidizing process for refractory metal powder comprises the following specific steps
(1) Putting vanadium pentoxide with the average particle size of 20nm into ethanol, adding ethylene glycol accounting for 5% of the mass of the vanadium pentoxide, mixing, and performing ball milling treatment;
(2) filtering the slurry after ball milling, and performing spray drying at the drying temperature of 120 ℃ for 100min by mechanical grinding;
(3) carrying out plasma spheroidizing treatment on the powder treated in the step (2) to obtain refractory metal spherical particles with the average diameter of 1.2 mu m; wherein the hydrogen flow rate in the plasma spheroidization process is 45scfh, the argon flow rate is 5scfh, and the power is 80 kw.
Comparative example 3
A spheroidization process of refractory metal powder comprises the specific steps of carrying out plasma spheroidization on vanadium pentoxide with the average particle size of 20nm to obtain refractory metal spherical particles with the average diameter of 2.0 mu m; wherein the hydrogen flow rate in the plasma spheroidization is 45scfh, the argon flow rate is 5scfh, and the power is 80 kw.
Examples 17 to 20
The plasma spheronization parameters of step (3) were adjusted according to the procedure of example 1, with the remaining steps unchanged, as shown in table 4.
TABLE 4
| Flow rate of hydrogen | Argon flow rate | Average diameter of refractory metal spherical particles | |
| Example 1 | 45scfh | 5scfh | 75nm |
| Example 17 | 50scfh | 10scfh | 75nm |
| Example 18 | 40scfh | 15scfh | 120nm |
| Example 19 | 10scfh | 50scfh | 750nm |
| Example 20 | 5scfh | 60scfh | 920nm |
In some embodiments, the reduction in the flow rate of hydrogen gas as the flow rate of argon gas is increased causes the average diameter of the refractory metal spherical particles produced to exhibit a tendency to increase. Due to the reduction of the hydrogen flow rate, the reduction reaction can not be effectively carried out in the spheroidization process, so that the prepared spherical particles can not be completely reduced, and simultaneously, the agglomeration phenomenon is easy to occur, and finally, the metal powder with larger particles is obtained.
In some examples, the ethylene glycol of example 1 was replaced with glycerol to produce refractory metal spherical particles having substantially the same size as example 1.
It should be noted that the above-mentioned embodiments are merely examples of the present invention, and it is obvious that the present invention is not limited to the above-mentioned embodiments, and other modifications are possible. All modifications directly or indirectly derivable by a person skilled in the art from the present disclosure are to be considered within the scope of the present invention.
Claims (8)
1. A process for spheroidizing refractory metal powder is characterized in that the spheroidizing process is to use hydrogen peroxide and polyhydric alcohol to pretreat a nanoscale refractory metal oxide, then use a plasma spheroidizing device to reduce and spheroidize the pretreated refractory metal oxide, thereby obtaining nanoscale refractory metal spherical particles, and the process comprises the following steps:
putting refractory metal oxide with the particle size of 10-100nm into ethanol, adding hydrogen peroxide and polyhydric alcohol, mixing and performing ball milling treatment;
filtering the ball-milled slurry, spray drying and mechanically grinding;
carrying out plasma spheroidizing treatment on the powder treated in the step (2) to obtain refractory metal spherical particles with the diameter of 50-350 nm; wherein the hydrogen flow in the plasma spheroidization process is 40-50scfh, the argon flow is 5-10scfh, and the power is 50-100 kw.
2. The spheroidization process of the refractory metal powder of claim 1, wherein the refractory metal oxide is one of vanadium oxide, niobium oxide, tantalum oxide, chromium oxide, tungsten oxide, or molybdenum oxide.
3. The spheroidization process of the refractory metal powder of claim 1, wherein the addition amount of the hydrogen peroxide in the step (1) accounts for 1-3% of the mass of the refractory metal oxide.
4. The process for spheroidizing refractory metal powder according to claim 1, wherein the polyol added in step (1) accounts for 5-10% by mass of the refractory metal oxide.
5. The spheroidization process of the refractory metal powder of claim 4, wherein the polyol in step (1) is one of ethylene glycol and glycerol.
6. The refractory metal powder spheroidization process of claim 1, wherein the temperature of the spray drying of step (2) is less than 150 ℃.
7. The spheroidization process of the refractory metal powder of claim 6, wherein the temperature of the spray drying in the step (2) is 100-120 ℃.
8. The spheroidization process of the refractory metal powder of claim 7, wherein in the step (2), the spray-dried powder is mechanically ground for 30min to 150 min.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115041699A (en) * | 2022-07-22 | 2022-09-13 | 华材(山东)新材料有限公司 | Production method of spherical zirconium powder for 3D printing |
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