CN107470639A - A kind of preparation method of narrow size distribution globular tungsten powder - Google Patents
A kind of preparation method of narrow size distribution globular tungsten powder Download PDFInfo
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- CN107470639A CN107470639A CN201710842720.6A CN201710842720A CN107470639A CN 107470639 A CN107470639 A CN 107470639A CN 201710842720 A CN201710842720 A CN 201710842720A CN 107470639 A CN107470639 A CN 107470639A
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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
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
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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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/06—Metallic powder characterised by the shape of the particles
- B22F1/065—Spherical particles
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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
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/044—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by jet milling
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Abstract
A kind of narrow size distribution globular tungsten powder preparation method, the invention belongs to field of powder metallurgy preparation, there is provided a kind of narrow size distribution globular tungsten powder preparation method.By being combined to commercially available the scattered of serious tungsten powder (3 20 μm) of reuniting, classification with plasma spheroidization processing, the globular tungsten powder of narrow size distribution is prepared.Concrete technology is：High degree of agglomeration, the raw material tungsten powder that in irregular shape, size distribution is wide are realized by airflow milling and be completely dispersed and be effectively classified, then the tungsten powder after processing is realized to the spheroidising of tungsten powder by radio frequency plasma torch, obtain globular tungsten powder.It is an advantage of the invention that：Airflow milling is disperseed, classification processing is combined with radio frequency plasma nodularization, the single globular tungsten powder obtained using radio frequency plasma nodularization is solved the problems, such as because of reunion and agglomeration, fine powder gasification disappears, size distribution is wide and technique is unmanageable, obtained powder good sphericity, narrow particle size distribution, Oxygen potential is high, surface is smooth, and recovery rate is high.
Description
Technical field
The invention belongs to field of powder metallurgy, is related to a kind of preparation method of narrow size distribution globular tungsten powder.
Technical background
Globular tungsten powder is because of its good sphericity and mobility, and high tap density is mainly used in thermal spraying, filtering material,
The field such as negative electrode and porous material.It is growing day by day for the demand of the globular tungsten powder of high quality at present, it is spherical in field of thermal spray
Powder is evenly fine and close because of the coating that its good mobility and high tap density obtain.In field of powder metallurgy, spherical powder
The pressed compact that end is prepared shrinks more controllable in sintering process, and microstructure is more uniform, can realize inherent porosity and aperture
The accurate control of size.In negative electrode preparation field, to ensure the emitting performance of negative electrode, American scientist proposes that granularity group should be used
Into narrow, good sphericity, the round and smooth tungsten powder of particle surface makees raw material.The Soviet Union's scholar's research particle size of tungsten powder, distribution
With influence of the pattern to dipped cathode emissivities and life-span.As a result show, average of the tungsten powder of best cathodes emitting performance
Particle size is 4.1~6 μm, and powder morphology has influence to emission p erformance, and the negative electrode being prepared using globular tungsten powder is had
There are hole evenly, the more preferable emitting performances of Xiang Yingyou.
The method for preparing globular tungsten powder at present mainly has following methods：Tungsten powder re-oxidation-reducing process：Patent (CN
101983804) it is cleaned and dried repeatedly to obtain subsphaeroidal powder using after selective oxidation by adding after abrasion or alkali cleaning, but
The addition pollution environment of alkali, and need to aoxidize alkali cleaning flushing repeatedly；Patent (CN 102935515A) is by by irregular shape
After tungsten powder is dried, sphere-like tungsten powder is formed by the way that wedge angle and the seamed edge oxidation of internal oxidation tungsten powder in irregular shape are broken,
Needed to obtain the tungsten powder of good sphericity by repeatedly processing；Tungstates precipitation reduction, patent (Chinese patent
200810239760.2) obtain wolframic acid by concentrated acid using wolframic acid amine bonus point powder to precipitate, then by drying precipitate and reduce
Prepare spherical tungsten particle, concentrated acid is serious using environmental pollution in this method.
Plasma spheroidization has energy density high, and heating intensity is big, and in the absence of pollution, to refractory metals such as tungsten powders
Reason has good effect, can obtain Oxygen potential height, good sphericity, the high spherical powder of purity.Patent (CN
101391307A) commercially tungsten powder is handled using plasma spheroidization, has obtained good sphericity and the high powder of Oxygen potential,
But size of powder particles is uneven, size distribution is wide, hardly results in thin globular tungsten powder；Patent (CN 104070173A) proposes to use
5-27 μm of tungsten powder is by argon plasma torch nodularization after grinding, and granularity is larger after nodularization and broad particle distribution size is uneven
And Oxygen potential is not high.Patent (CN 102259186A) is combined with radio frequency plasma torch using the scattered classification of airflow milling and realizes tungsten
The nodularization of powder, the tungsten powder good sphericity that the powder after scattered classification obtains through radio frequency plasma nodularization, Oxygen potential is high, due to
Scattered de-agglomerated is only carried out to starting powder in airflow milling processing procedure, powder is not classified effectively, powder after processing
Size distribution it is wide, after nodularization obtained by spherical powder particle size it is uneven.Because commercially tungsten powder is reunited seriously, and through penetrating
The particle size and its distribution for the powder received after the processing of frequency plasma spheroidization is mainly determined by the particle size and its distribution of feeding powder
It is fixed, in this case through carry it is high-power improve the Oxygen potential of powder, necessarily cause fine granularity ball in this process
The gasification of shape tungsten powder disappears, the meso-position radius increase of powder, shows as the powder size distribution width that plasma spheroidization handles to obtain, powder
Easy agglomeration.Because powder diameter is distributed width so that whole technological parameter is difficult to control, and causes the gasification of fine powder to disappear,
Influence the stability of technique and the recovery rate of powder.
The content of the invention
It is an object of the invention to at present due to raw material tungsten powder is reunited and cause nodularization process unmanageable and
Particle growth after nodularization, the deficiency that powder size distribution is wide, recovery rate is low, take scattered air-flow, classification technique and radio frequency etc. from
Daughter powder processing techniques are combined to prepare the high narrow size distribution globular tungsten powder of Oxygen potential.
A kind of preparation method of narrow size distribution globular tungsten powder, using gas is scattered, classification and radio frequency plasma nodularization phase
With reference to, first powder is completely dispersed, collects the superfines removed in commercially tungsten powder, then to the fine graded place of tungsten powder progress
Reason, the powder after processing is then subjected to radio frequency plasma spheroidising, has obtained narrow particle size distribution, surface is smooth, Oxygen potential
High globular tungsten powder.
Concrete technology step is：
1) drying process：Powder is placed in drying oven and is heated to 50-100 DEG C under inert gas atmosphere place is dried
Reason；
2) gas shield and cleaning equipment are filled with：High purity inert gas is filled with into equipment to remove air and carry out equipment
Inflation cleaning；
3) gas shock crushes powder：Adjust appropriate pressure and start grinding valve and powder is crushed, grinding pressure exists
0.50-0.80MPa；
4) fine powder is collected：Adjustment sorting wheel speed collects the molecule in tungsten powder to 7200r/min；
5) separation wheel regulation is classified to powder：Regulation rotating speed starts separation wheel and classification processing is carried out to powder, sorts
Wheel speed is 3000-6000r/min；
6) feed separation is with collecting：Powder by broken classification is collected；
7) powder feeding nodularization:Powder to be sent into powder feeder, is pressed to form plasmatorch, powder feeding carries out spheroidising to powder,
Power is 40-60kw；
8) cooling is collected：Collected through the powder of plasmatorch after supercooling.
It is an advantage of the invention that：
1. airflow milling processing is mutually collided by powder under high pure nitrogen or argon gas atmosphere, pollution-free；
2. after airflow milling is handled, tungsten powder, which is reunited, to be opened, and granularity narrows, and mobility improves, and pattern becomes rule；
3. radio frequency plasma energy density is high, heating intensity is big, by axial powder feed, electrodeless pollution, it is pure to obtain powder
Degree is high, and Oxygen potential is high, good sphericity, is adapted to the processing of refractory metal powder；
4. the tungsten powder after airflow milling is handled is through radio frequency plasma nodularization, nodularization process parameter is controllable, due to tungsten powder
Mobility it is more preferable, the agglomeration of agglomerate particle can be effectively prevent, tungsten powder good sphericity after nodularization, nodularization is abundant, grain
Narrowly distributing is spent, recovery rate is high.
Brief description of the drawings
Fig. 1 is the process chart of the present invention,
Fig. 2 is original tungsten powder pattern,
Fig. 3 is that airflow milling handles tungsten powder pattern,
Fig. 4 is powder morphology after original tungsten powder nodularization,
Fig. 5 is powder morphology after tungsten powder nodularization after processing.
Embodiment
Embodiment：
Step 1 drying process：Fisher particle size is placed in drying oven for 8 μm of powder and is heated under inert gas atmosphere
100 DEG C of insulation 1h；
Step 2 is filled with gas shield and cleaning equipment：High pure nitrogen is filled with into equipment to remove air and enter equipment
Row inflation cleaning；
Step 3 gas shocks crush powder：Adjust appropriate pressure and start grinding valve and powder is crushed, grinding pressure
Power is 0.70MPa；
Step 4 collects fine powder：Adjustment sorting wheel speed collects the molecule in tungsten powder to 7200r/min；
The regulation of step 5 separation wheels is classified to powder：Regulation rotating speed starts separation wheel and carries out classification processing to powder,
Sorting wheel speed is 6000r/min；
Step 6 feed separations are with collecting：Powder by broken classification is collected；
Step 7 powder feeding nodularizations:Powder is sent into powder feeder, is pressed to form plasmatorch, powder feeding carries out nodularization to powder
Processing, power 50kw；
Step 8 coolings are collected：Collected through the powder of plasmatorch after supercooling.
Comparative example：
Step 1 drying process：Fisher particle size is placed in drying oven for 8 μm of powder and is heated under inert gas atmosphere
100 DEG C are dried processing；
Step 2 powder feeding nodularizations:Powder is sent into powder feeder, is pressed to form plasmatorch, powder feeding carries out nodularization to powder
Processing, power 60kw；
Step 3 coolings are collected：Collected through the powder of plasmatorch after supercooling.
Claims (3)
- A kind of 1. method for preparing narrow size distribution globular tungsten powder, it is characterised in that in irregular shape by commercially available from, size distribution is wide, The tungsten powder of high degree of agglomeration is disperseed, classification processing to raw material tungsten powder using gas shock method, then will handled as raw material Tungsten powder afterwards prepares globular tungsten powder through radio frequency plasma processing, realizes the preparation of narrow size distribution globular tungsten powder, concrete technology Step is：1) drying process：Powder is placed in drying oven and is heated to 50-100 DEG C under inert gas atmosphere processing is dried；2) gas shield and cleaning equipment are filled with：High purity inert gas is filled with into equipment to remove air and be inflated equipment Cleaning；3) gas shock crushes powder：Adjust appropriate pressure and start grinding valve and powder is crushed, grinding pressure is in 0.50- 0.80MPa；4) fine powder is collected：Adjustment sorting wheel speed collects the molecule in tungsten powder to maximum speed 7200r/min；5) separation wheel regulation is classified to powder：Regulation rotating speed starts separation wheel and classification processing, sorting rotation is carried out to powder Speed is 3000-6000r/min；6) feed separation is with collecting：Powder by broken classification is collected；7) powder feeding nodularization:Powder is sent into powder feeder, is pressed to form plasmatorch, powder feeding carries out spheroidising, power to powder For 40-60kw；8) cooling is collected：Collected through the powder of plasma spheroidization after supercooling.
- 2. the method according to claim 1 for preparing trickle globular tungsten powder, it is characterised in that：3) and step 5) step 2), For working gas, step 7) uses 99.9% high-purity argon gas as work gas for the middle high pure nitrogen for using 99.9% or argon gas.
- 3. the method according to claim 1 for preparing trickle globular tungsten powder, it is characterised in that：Tungsten after decentralized processing Powder, reunion are untied, and mobility improves, and after collecting fine powder and classification processing, the fine grained tungsten powder in original tungsten powder are removed, obtained Obtain the sphere-like tungsten powder of the narrow size distribution of individual particle；Gained spherical powder Oxygen potential is prepared more than 95%, good sphericity, granularity Narrowly distributing, powder yield are high.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110732676A (en) * | 2019-11-11 | 2020-01-31 | 重庆材料研究院有限公司 | Preparation method of spherical tungsten-rhenium alloy powder |
| CN112091228A (en) * | 2020-09-23 | 2020-12-18 | 矿冶科技集团有限公司 | Preparation method of large-particle spherical tungsten powder |
| CN112626404A (en) * | 2020-11-19 | 2021-04-09 | 北京科技大学 | 3D printing high-performance WMoTaTi high-entropy alloy and low-cost powder preparation method thereof |
| CN113492211A (en) * | 2020-04-08 | 2021-10-12 | 安泰科技股份有限公司 | Preparation method of high-uniformity metal powder with controllable particle size |
| CN114247894A (en) * | 2020-09-25 | 2022-03-29 | 安泰天龙钨钼科技有限公司 | Method for preparing large-particle-size spherical tungsten powder by radio frequency plasma method |
| CN114289722A (en) * | 2021-12-08 | 2022-04-08 | 北京科技大学 | Preparation method of fine-grained spherical tungsten powder |
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| CN101850424A (en) * | 2010-05-26 | 2010-10-06 | 北京科技大学 | Method for largely preparing superfine spherical titanium aluminium-based alloyed powder |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110732676A (en) * | 2019-11-11 | 2020-01-31 | 重庆材料研究院有限公司 | Preparation method of spherical tungsten-rhenium alloy powder |
| CN110732676B (en) * | 2019-11-11 | 2022-08-02 | 重庆材料研究院有限公司 | Preparation method of spherical tungsten-rhenium alloy powder |
| CN113492211A (en) * | 2020-04-08 | 2021-10-12 | 安泰科技股份有限公司 | Preparation method of high-uniformity metal powder with controllable particle size |
| CN113492211B (en) * | 2020-04-08 | 2023-11-14 | 安泰科技股份有限公司 | Preparation method of high-uniformity granularity-controllable metal powder |
| CN112091228A (en) * | 2020-09-23 | 2020-12-18 | 矿冶科技集团有限公司 | Preparation method of large-particle spherical tungsten powder |
| CN114247894A (en) * | 2020-09-25 | 2022-03-29 | 安泰天龙钨钼科技有限公司 | Method for preparing large-particle-size spherical tungsten powder by radio frequency plasma method |
| CN112626404A (en) * | 2020-11-19 | 2021-04-09 | 北京科技大学 | 3D printing high-performance WMoTaTi high-entropy alloy and low-cost powder preparation method thereof |
| CN114289722A (en) * | 2021-12-08 | 2022-04-08 | 北京科技大学 | Preparation method of fine-grained spherical tungsten powder |
| CN114289722B (en) * | 2021-12-08 | 2023-08-29 | 北京科技大学 | Preparation method of fine-grained spherical tungsten powder |
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