CN107470639B - 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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- CN107470639B CN107470639B CN201710842720.6A CN201710842720A CN107470639B CN 107470639 B CN107470639 B CN 107470639B CN 201710842720 A CN201710842720 A CN 201710842720A CN 107470639 B CN107470639 B CN 107470639B
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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, provide a kind of narrow size distribution globular tungsten powder preparation method.It handles and combines with plasma spheroidization by dispersion, the classification to commercially available serious tungsten powder (3-20 μm) of reuniting, prepare the globular tungsten powder of narrow size distribution.Concrete technology is: high degree of agglomeration, the raw material tungsten powder that in irregular shape, size distribution is wide being completely dispersed by airflow milling realization and are effectively classified, then treated tungsten powder is realized by radio frequency plasma torch to the spheroidising of tungsten powder, obtain globular tungsten powder.The invention has the advantages that airflow milling dispersion, classification processing are combined with radio frequency plasma nodularization, solve the problems, such as the single globular tungsten powder obtained using radio frequency plasma nodularization due to reunion agglomeration, fine powder gasification disappears, size distribution is wide and technique is difficult to control, 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, are 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 for thermal spraying, filtering material,
The fields such as cathode 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 more 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 green compact that end is prepared is shunk more controllably during the sintering process, and microstructure is more uniform, is able to achieve inherent porosity and aperture
The accurate control of size.In cathode preparation field, for the emitting performance for guaranteeing cathode, American scientist proposition should use granularity group
At narrow, good sphericity, the round and smooth tungsten powder of particle surface makees raw material.Soviet Union scholar has studied the particle size of tungsten powder, distribution
Influence with pattern to dipped cathode emissivities and service life.The result shows that the tungsten powder of best cathodes emitting performance average
Particle size is 4.1~6 μm, and powder morphology has influence to emission p erformance, is had using the cathode that globular tungsten powder is prepared
There are hole more evenly, the better emitting performance of Xiang Yingyou.
The method for preparing globular tungsten powder at present mainly has following methods: tungsten powder re-oxidation-reduction method: patent (CN
101983804) subsphaeroidal powder is obtained by adding repeatedly cleaning-drying after abrasion or alkali cleaning using after selective oxidation, however
Environment is polluted in the addition of alkali, and needs to aoxidize alkali cleaning flushing repeatedly；Patent (CN 102935515A) is by by irregular shape
After tungsten powder is dry, the wedge angle of tungsten powder in irregular shape and seamed edge oxidation is made to be crushed and form sphere-like tungsten powder by internal oxidation,
It needs to obtain the tungsten powder of good sphericity by repeatedly processing；Tungstates precipitating reduction, patent (Chinese patent
200810239760.2) wolframic acid is obtained by concentrated acid using wolframic acid amine bonus point powder to precipitate, then by drying precipitate and restore
Spherical tungsten particle is prepared, concentrated acid is serious using environmental pollution in this method.
Plasma spheroidization has energy density high, and heating intensity is big, and there is no pollutions, to refractory metals such as tungsten powders
Reason has good effect, can obtain Oxygen potential height, good sphericity, spherical powder with high purity.Patent (CN
101391307A) commercially tungsten powder is handled using plasma spheroidization, has obtained good sphericity and the high powder of Oxygen potential,
However 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 the nodularization of argon plasma torch after grinding, and granularity is larger after nodularization and broad particle distribution size is uneven
And Oxygen potential is not high.Patent (CN 102259186A) combines realization tungsten with radio frequency plasma torch using airflow milling dispersion classification
The nodularization of powder, the tungsten powder good sphericity that the powder after dispersion classification is obtained through radio frequency plasma nodularization, Oxygen potential is high, due to
Dispersion de-agglomerated only is carried out to starting powder in airflow milling treatment process, powder is not classified effectively, powder after processing
Size distribution it is wide, obtained spherical powder particle size is uneven after nodularization.Since 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 the high-power Oxygen potential to improve powder is mentioned, necessarily lead to fine granularity ball in this process
The gasification of shape tungsten powder disappears, and the meso-position radius of powder increases, and shows as the powder size distribution width that plasma spheroidization is handled, powder
Easy agglomeration.Since powder diameter is distributed width, so that entire technological parameter is difficult to control, and the gasification of fine powder is caused to disappear,
Influence the stability of technique and the recovery rate of powder.
Summary of the invention
It is an object of the invention at present due to raw material tungsten powder reunite and cause nodularization process be difficult to control and
Particle growth after nodularization, the deficiency that powder size distribution is wide, recovery rate is low, take air-flow dispersion, classification technique and radio frequency etc. from
Daughter powder processing techniques combine 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 dispersion, is classified and radio frequency plasma nodularization phase
In conjunction with being first completely dispersed to powder, collect superfines of the removal commercially in tungsten powder, then carry out fine graded place to tungsten powder
Reason, then by treated, powder carries out radio frequency plasma spheroidising, has obtained narrow particle size distribution, surface is smooth, Oxygen potential
High globular tungsten powder.
Specific process step are as follows:
1) it is dried: powder being 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: being filled with high purity inert gas into equipment and removes air and equipment is carried out
Inflation cleaning；
3) gas shock is crushed powder: adjusting pressure appropriate and starts grinding valve and be crushed to powder, grinding pressure exists
0.50-0.80MPa；
4) collect fine powder: adjustment sorting wheel speed to 7200r/min collects the molecule in tungsten powder；
5) separation wheel adjusting is classified powder: adjusting revolving speed starts separation wheel and carries out classification processing to powder, sorts
Wheel speed is 3000-6000r/min；
6) feed separation and collection: the powder by broken classification is collected；
7) powder feeding nodularization: sending powder into powder feeder, is pressed to form plasmatorch, and powder feeding carries out spheroidising to powder,
Power is 40-60kw；
8) cooling to collect: to be collected after supercooling through the powder of plasmatorch.
The invention has the advantages that
1. airflow milling processing is mutually to be collided under high pure nitrogen or argon atmosphere by powder, pollution-free；
2. tungsten powder, which is reunited, to be opened, and granularity narrows, and mobility improves, and pattern becomes rule after airflow milling is handled；
3. radio frequency plasma energy density is high, heating intensity is big, and by axial powder feed, it is pure to obtain powder for electrodeless pollution
Degree is high, and Oxygen potential is high, good sphericity, is suitble to the processing of refractory metal powder；
4. nodularization process parameter is controllable, due to tungsten powder through airflow milling treated tungsten powder through radio frequency plasma nodularization
Mobility it is more preferable, can effectively avoid the agglomeration of agglomerate particle, tungsten powder good sphericity after nodularization, nodularization is abundant, grain
Narrowly distributing is spent, recovery rate is high.
Detailed description of the invention
Fig. 1 is process flow chart of the 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.
Specific embodiment
Embodiment:
Step 1 is dried: Fisher particle size being placed in drying oven for 8 μm of powder and is heated under inert gas atmosphere
100 DEG C of heat preservation 1h；
Step 2 is filled with gas shield and cleaning equipment: be filled with into equipment high pure nitrogen remove air and to equipment into
Row inflation cleaning；
Step 3 gas shock is crushed powder: it adjusts pressure appropriate and starts grinding valve powder is crushed, grinding pressure
Power is 0.70MPa；
Step 4 collects fine powder: adjustment sorting wheel speed to 7200r/min collects the molecule in tungsten powder；
The adjusting of step 5 separation wheel is classified powder: adjusting revolving speed starts separation wheel and carries out classification processing to powder,
Sorting wheel speed is 6000r/min；
Step 6 feed separation and collection: the powder by broken classification is collected；
Step 7 powder feeding nodularization: sending powder into powder feeder, is pressed to form plasmatorch, and powder feeding carries out nodularization to powder
Processing, power 50kw；
Step 8 is cooling to be collected: being collected after supercooling through the powder of plasmatorch.
Comparative example:
Step 1 is dried: Fisher particle size being placed in drying oven for 8 μm of powder and is heated under inert gas atmosphere
100 DEG C are dried；
Step 2 powder feeding nodularization: sending powder into powder feeder, is pressed to form plasmatorch, and powder feeding carries out nodularization to powder
Processing, power 60kw；
Step 3 is cooling to be collected: being collected after supercooling through the powder of plasmatorch.
Claims (1)
1. a kind of method for preparing narrow size distribution globular tungsten powder, it is characterised in that will be commercially available in irregular shape, size distribution is wide,
The tungsten powder of high degree of agglomeration disperses raw material tungsten powder as raw material, using gas shock method, classification is handled, then will processing
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 are as follows:
1) it is dried: the raw material tungsten powder that Fisher particle size is 8 μm being placed in drying oven and is heated under inert gas atmosphere
100 DEG C are dried；
2) gas shield and cleaning equipment are filled with: being filled with high purity inert gas into equipment and removes air and equipment is inflated
Cleaning；
3) gas shock is crushed powder: adjusting pressure appropriate and starts grinding valve and be crushed to powder, grinding pressure is 0.70
MPa；
4) collect fine powder: adjustment sorting wheel speed to 7200 r/min of maximum speed collects the molecule in tungsten powder；
5) separation wheel adjusting is classified powder: adjusting revolving speed starts separation wheel and carries out classification processing, sorting rotation to powder
Speed is 6000 r/min；
6) feed separation and collection: the powder by broken classification is collected；
7) powder feeding nodularization: sending powder into powder feeder, is pressed to form plasmatorch, and powder feeding carries out spheroidising, power to powder
For 50 kw；
8) cooling to collect: to be collected after supercooling through the powder of plasma spheroidization；
3) step 2 and use 99.9% high pure nitrogen or argon gas for working gas in step 5), step 7) uses 99.9% high
Pure argon is work gas；
Tungsten powder after decentralized processing, reunion are unlocked, and mobility improves, and collect removal superfines, then carry out essence to tungsten powder
Subfractionation processing, then by treated, powder carries out radio frequency plasma spheroidising, obtains the close of the narrow size distribution of individual particle
Globular tungsten powder；Preparation gained spherical powder Oxygen potential is 95% or more, good sphericity, narrow particle size distribution, and powder yield is high.
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| CN107470639B true CN107470639B (en) | 2019-10-18 |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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 |
| CN112091228B (en) * | 2020-09-23 | 2022-09-30 | 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 |
| CN114289722B (en) * | 2021-12-08 | 2023-08-29 | 北京科技大学 | Preparation method of fine-grained spherical tungsten powder |
Citations (4)
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|---|---|---|---|---|
| CN101391307A (en) * | 2008-11-20 | 2009-03-25 | 核工业西南物理研究院 | Preparation method of fine globular tungsten powder |
| 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 |
| CN102259186A (en) * | 2011-07-28 | 2011-11-30 | 北京科技大学 | Method for producing thin spherical tungsten powder |
| CN104070173A (en) * | 2014-06-23 | 2014-10-01 | 陕西斯瑞工业有限责任公司 | Preparation method of spherical tungsten powder |
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2017
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Patent Citations (4)
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|---|---|---|---|---|
| CN101391307A (en) * | 2008-11-20 | 2009-03-25 | 核工业西南物理研究院 | Preparation method of fine globular tungsten powder |
| 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 |
| CN102259186A (en) * | 2011-07-28 | 2011-11-30 | 北京科技大学 | Method for producing thin spherical tungsten powder |
| CN104070173A (en) * | 2014-06-23 | 2014-10-01 | 陕西斯瑞工业有限责任公司 | Preparation method of spherical tungsten powder |
Non-Patent Citations (3)
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