CN103878378B - Preparation method and application of tungsten powder for cathode - Google Patents
Preparation method and application of tungsten powder for cathode Download PDFInfo
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- CN103878378B CN103878378B CN201410136089.4A CN201410136089A CN103878378B CN 103878378 B CN103878378 B CN 103878378B CN 201410136089 A CN201410136089 A CN 201410136089A CN 103878378 B CN103878378 B CN 103878378B
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Abstract
The invention discloses a preparation method and application of tungsten powder for a cathode, wherein the method comprises the following steps: (1) heating tungsten powder to 1850-2000 ℃ at the heating rate of 455-495 ℃/min under the hydrogen atmosphere, preserving the heat at the temperature for 100-140min, and then cooling; (2) ball-milling the cooled tungsten powder; (3) and screening the tungsten powder subjected to ball milling. The tungsten powder prepared by the method has the particle size of 3-5 mu m, the particle size distribution of the tungsten powder is concentrated, and the purity of the tungsten powder is 99.995-99.999%, which completely meets the quality requirement of the tungsten powder required by preparing the cathode.
Description
Technical field
The present invention relates to tungsten powder preparation field, be specifically related to a kind of tungsten powder for negative electrode preparation method and
Its application.
Background technology
Negative electrode is the key factor affecting the travelling-wave tubes life-span.During design negative electrode, need to fully take into account resistance to from
Son bombardment, poisoning high pressure resistant, resistance to, vibration resistance, impact resistance, anti-sparking, emissivities and life-span are long
Deng factors.
Barium-tungsten dispense cathode is as the one in negative electrode, and its body construction is by the active matter that can produce barium metal
Matter and the spongy body of tungsten as carrier form.Its working mechanism is monoatomic layer dipole theory, i.e. in work
When making temperature, the barium the most original in active material duct along spongy body of tungsten diffuses to surface, is formed single
The barium layer of atom, obtains the barium-oxygen-tungsten superficial layer with tungsten as substrate, thus reduces work function, increases
The emission of negative electrode.Meanwhile, during negative electrode works, the consume of barium can also obtain accordingly
Continuous supplementation, therefore it can maintain the transmitting of the stable electronics of high current density muchly.
As can be seen here, the tungsten powder as substrate is the most particularly significant, and traditional tungsten powder preparation method
The size distribution of the tungsten powder obtained is not concentrated, impurity is high and the most hygroscopic, it is difficult to reach preparation
The quality requirements of tungsten powder needed for negative electrode, therefore design a kind of tungsten powder prepared size distribution concentrate,
The method that purity is high is the problem that this area needs solution badly.
Summary of the invention
The invention aims to overcome the size distribution of tungsten powder in prior art not concentrate, impurity high with
And the most hygroscopic defect, it is provided that the size distribution of a kind of tungsten powder prepared is concentrated, purity is high
Method.
To achieve these goals, the present invention provides the preparation method of a kind of tungsten powder for preparing negative electrode,
Wherein, the method comprises the following steps:
(1) cool down after under an atmosphere of hydrogen, tungsten powder being heat-treated；
(2) tungsten powder after cooling is carried out ball milling；
(3) tungsten powder after ball milling is screened；
Wherein, described heat treatment is for be warming up to tungsten powder with 455-495 DEG C/min programming rate
1850-2000 DEG C, and it is incubated 100-140min at such a temperature.
Preferably, tungsten powder is placed in molybdenum bowl, molybdenum bowl is placed in drying bottle, and drying bottle is placed in tungsten
Net hydrogen stove is heat-treated.
Preferably, being 100 parts by volume with the capacity of molybdenum bowl, the consumption of described tungsten powder is 1-67 parts by volume.
It is highly preferred that be 100 parts by volume with the capacity of molybdenum bowl, the consumption of described tungsten powder is 20-50 volume
Part.
Preferably, the method for described ball milling includes: the tungsten powder through Overheating Treatment is ground to particle diameter is
The tungsten powder particles of 3-5mm, is placed in described tungsten powder particles in ball mill device, and ball mill device is placed in ball
In grinding machine, the rotating speed of ball mill is set to 90-110 rev/min, ball milling 15-20 minute.
Preferably, by concretely comprising the following steps that described tungsten powder particles is placed in ball mill device: by tungsten powder particles and
Agate ball is placed in agate tank, is placed on described agate tank by the first lid, and agate tank is placed in outer cover
In, and second lid with through hole is placed on described outer cover, then by described in fixing bolt-through second
The through hole of lid withstands described first lid, and is bolted to described second lid with nut by fixing
On.
Preferably, described agate ball includes 3-7 first agate ball of a diameter of 20-30mm, 5-15
Second agate ball of individual a diameter of 12-18mm and the 3rd agate ball of 3-10 a diameter of 5-10mm.
Preferably, the method carrying out screening by the tungsten powder after ball milling is: by the tungsten powder after ball milling
It is placed on the screen cloth of 200 mesh and carries out sieve and take.More preferably, for not being ground by the tungsten powder of screen cloth
And again sieve take, repeat until, on the basis of the tungsten powder before the heat treatment of 100 weight portions, do not lead to
The content of the tungsten powder crossing screen cloth is 1-10 weight portion.
The cathode base of travelling-wave tubes is being prepared according to the tungsten powder that the method described in above-mentioned any one prepares
In application.
Tungsten powder is heat-treated by the present invention in the presence of hydrogen gas, and the tungsten powder after cooling is carried out ball milling also
Screening, has just obtained size distribution and has relatively concentrated in 3-5 μm, size distribution, and purity exists
High-purity tungsten powder between 99.995%-99.999%.This method preparing tungsten powder is simple, and step is few, with
Time the tungsten powder for preparing comply fully with and prepare the quality requirements of tungsten powder needed for negative electrode.
Other features and advantages of the present invention will be described in detail in detailed description of the invention part subsequently.
Accompanying drawing explanation
Accompanying drawing is used to provide a further understanding of the present invention, and constitutes the part of specification, with
Detailed description below is used for explaining the present invention together, but is not intended that limitation of the present invention.?
In accompanying drawing:
Fig. 1 is the device schematic diagram that in the present invention, tungsten powder carries out ball milling.
Description of reference numerals
1, tungsten powder particles the 2, first agate ball
3, the second agate ball the 4, the 3rd agate ball
5, agate tank the 6, first lid
7, outer cover the 8, second lid
9, fixing bolt 10, nut.
Detailed description of the invention
Below in conjunction with accompanying drawing, the detailed description of the invention of the present invention is described in detail.It should be appreciated that
Detailed description of the invention described herein is merely to illustrate and explains the present invention, is not limited to this
Bright.
The preparation method of the tungsten powder for negative electrode that the present invention provides, wherein, the method comprises the following steps:
(1) cool down after under an atmosphere of hydrogen, tungsten powder being heat-treated；
(2) tungsten powder after cooling is carried out ball milling；
(3) tungsten powder after ball milling is screened；
Wherein, described heat treatment is for be warming up to tungsten powder with 455-495 DEG C/min programming rate
1850-2000 DEG C, and it is incubated 100-140min at such a temperature.
Tungsten powder under an atmosphere of hydrogen, is warming up to by the present invention with 455-495 DEG C/min programming rate
1850-2000 DEG C is heat-treated, and the oxide layer of tungsten powder surface is reduced under the effect of hydrogen, obtains
Highly purified tungsten powder, then the tungsten powder after cooling is carried out ball milling and screens, just obtain size distribution and existed
3-5 μm, purity high-purity tungsten powder between 99.995%-99.999%, this tungsten powder relatively carries out heat simultaneously
For tungsten powder before treatment, size distribution is relatively concentrated.This method preparing tungsten powder is simple, and step is few, with
Time the tungsten powder for preparing comply fully with and prepare the quality requirements of tungsten powder needed for negative electrode.
More thorough in order to what the oxide layer of tungsten powder surface was reduced, obtain the tungsten powder that quality is more excellent, at hydrogen
The step that atmosphere carries out under enclosing being heat-treated can be: is warming up to 470-485 DEG C/min programming rate
1900-1950 DEG C, and it is incubated 100-140min at such a temperature.
Tungsten powder carries out the most primary answering, in order to make the tungsten powder after being reduced be in the presence of hydrogen gas
In the environment being more dried, preferably tungsten powder is placed in molybdenum bowl, molybdenum bowl is placed in drying bottle, and will be dry
Dry bottle is placed in tungsten net hydrogen stove and is heat-treated.The step that operates with of described tungsten net hydrogen furnace is this area
Operating procedure known to technical staff.
In order to the tungsten powder in molybdenum bowl can sufficiently be contacted, so that what reduction reaction was carried out
More thorough, it is 100 parts by volume with the capacity of molybdenum bowl, the consumption of described tungsten powder is 1-67 parts by volume.
On the premise of ensureing that reduction reaction can be reacted completely, in order to the efficiency of tungsten powder is prepared in raising, it is preferable that
Being 100 parts by volume with the capacity of molybdenum bowl, the consumption of described tungsten powder is 20-50 parts by volume.
Tungsten powder can be pulverized by ball milling, so that the more concentration of the tungsten powder particles distribution after ball milling, ball
Tungsten powder after the method for mill comprises the steps that cooling is ground to the tungsten powder particles 1 that particle diameter is 3-5mm, by institute
State tungsten powder particles 1 to be placed in ball mill device, and ball mill device is placed in ball mill, turning ball mill
Speed is set to 90-110 rev/min, ball milling 15-20 minute.
In order to the further of tungsten powder particles distribution after making ball milling is concentrated, it is further preferred that described agate
Ball can include 3-7 first agate ball 2 of a diameter of 20-30mm, 5-15 a diameter of 12-18mm
The 3rd agate ball 4 of 3 and 3-10 a diameter of 5-10mm of the second agate ball.
Tungsten powder after ball milling yet suffers from some parts for fully pulverizing, in order to extract distribution of particles relatively
For the tungsten powder concentrated, the method carrying out the tungsten powder after ball milling screening can be: by after ball milling
Tungsten powder is placed on the screen cloth of 200 mesh and carries out sieve and take.In order to improve the productivity of the tungsten powder produced, it is highly preferred that
For be not ground by the tungsten powder of screen cloth and again sieve take, repeat until, with 100 weight portions
Heat treatment before tungsten powder on the basis of, be not 1-10 weight portion by the content of the tungsten powder of screen cloth.
The present invention also provides for tungsten powder the answering in the cathode base preparing travelling-wave tubes that above-mentioned method prepares
With.
Below in conjunction with specific embodiment, the invention will be further described:
Former to the detection of the granule size of the particle of tungsten powder and particle size distribution law in following each embodiment
Reason is: uses gamut Mie theory, takes into full account decentralized medium and the refractive index of tested particle,
In conjunction with measurement apparatus, it is finally inversed by according to the particle varied in size change of scattered light intensity in each angle
The granule size of grain group and particle size distribution law (particle size distribution law granularity weights width means), respectively
The measurement apparatus used in embodiment is Mastersizers2000 particle size analysis instrument, and testing conditions is:
Measuring grain graininess scope on analyzer is 0.02 μm-2000 μm, with water as dispersant, tungsten powder and water
Volume ratio is 0.0752:100.
In following each embodiment, the principle to the detection of the purity of tungsten powder is: by tungsten powder at X-ray irradiation
The principle of lower generation fluorescence, utilizes X-3600 noble metal detector to analyze the composition of tungsten powder, detects sample
Tungsten powder for Φ 30mm × 0.5mm suppresses sample.
Embodiment 1
Without hair paper on each pad on the pallet of balance left and right, weigh tungsten powder, with ox horn spoon, tungsten powder put into molybdenum bowl
In, and flatten, it is 100 parts by volume with the capacity of molybdenum bowl, the consumption of described tungsten powder is 20 parts by volume；
Then the molybdenum bowl that will be equipped with tungsten powder is inserted in drying bottle, is heat-treated, work gas in tungsten net hydrogen furnace
Atmosphere is hydrogen, is warming up to 1900 DEG C with 470 DEG C/min programming rate and is incubated 120min, cooling down subsequently
To 20 DEG C.
The tungsten powder obtained after carrying out high-temperature process in tungsten net hydrogen furnace and cool down is put in agate alms bowl, and
Smashed into pieces the tungsten powder particles 1 that particle diameter is 3mm-5mm with agate rod.Then as it is shown in figure 1, incite somebody to action
Second agate of first 2,11 Ф 15mm of agate ball of 1,5 Ф 25mm of 250g tungsten powder particles
3rd agate ball 4 of ball 3 and 6 Ф 10mm puts into the agate tank 5 of 0.4L, then with the first lid
Agate tank 5 is closed by son 6, is put into by agate tank 5 in outer cover 7, the second lid 8 is positioned on outer cover 7
Openend, with bottle opener fixing bolt 9 run through the second lid 8 and screw, then will be located in spiral shell with spanner
The nut 10 of bolt 9 one end screws, and is finally put on ball mill by the agate tank 5 of band outer cover 7.By ball
The rotating speed of grinding machine is set to 100 revs/min, is stirred and ball milling in 20 minutes, closes ball mill,
Take out agate tank 5 and open, and going out agate ball of the same race with ox horn bale-out, pouring out tungsten powder.
The paper without hair cutting (400 × 400) millimeter keeps flat on the table, with ox horn spoon by after ball milling
Tungsten powder pour in the screen cloth of 400 mesh, swing screen cloth with hand in the horizontal plane and screen, not over
The tungsten powder of screen cloth grid is poured in agate alms bowl, grinds them 15 minutes with agate rod, is again poured into
Screen in screen cloth, be repeated several times by, until not over screen cloth grid tungsten powder weight less than without
The weight 1/10 of the powder of Overheating Treatment.By pouring in clean measuring cup without the tungsten powder on hair paper, cover
Lid, pours in cup by the tungsten powder not sifted out from net, preserves as residue.
It is canescence that the present embodiment prepares tungsten powder, the present embodiment prepares tungsten powder and carries out the size of grain graininess
Detect with the purity of distribution of particles rule and tungsten powder, learn that the particle diameter of tungsten powder particles is 3-5 μm,
The granularity weighting width of tungsten powder is 57.31%, and the purity of tungsten powder is 99.998%.
Embodiment 2
Carry out according to the method for embodiment 1, except for the difference that by tungsten powder in the presence of hydrogen gas, with
480 DEG C/min programming rate is warming up to 1940 DEG C.The tungsten powder that the present embodiment prepares is canescence, to this reality
Execute example to prepare the purity of size and distribution of particles rule and tungsten powder that tungsten powder carries out grain graininess and examine
Surveying, learn that the particle diameter of tungsten powder particles is 3-5 μm, the granularity weighting width of tungsten powder is 57.33%, tungsten powder
Purity is 99.999%.
Embodiment 3
Carry out according to the method for embodiment 1, except for the difference that by tungsten powder in the presence of hydrogen gas, with
485 DEG C/min programming rate is warming up to 1950 DEG C.The tungsten powder that the present embodiment prepares is canescence, to this reality
Execute example to prepare the purity of size and distribution of particles rule and tungsten powder that tungsten powder carries out grain graininess and examine
Surveying, learn that the particle diameter of tungsten powder particles is 3-5 μm, the granularity weighting width of tungsten powder is 57.56%, tungsten powder
Purity is 99.998%.
Embodiment 4
Carry out according to the method for embodiment 1, except for the difference that by tungsten powder in the presence of hydrogen gas, with
460 DEG C/min programming rate is warming up to 1860 DEG C.The tungsten powder that the present embodiment prepares is canescence, to this reality
Execute example to prepare the purity of size and distribution of particles rule and tungsten powder that tungsten powder carries out grain graininess and examine
Surveying, learn that the particle diameter of tungsten powder particles is 3-5 μm, the granularity weighting width of tungsten powder is 56.10%, tungsten powder
Purity is 99.995%.
Embodiment 5
Carry out according to the method for embodiment 1, except for the difference that by tungsten powder in the presence of hydrogen gas, with
495 DEG C/min programming rate is warming up to 2000 DEG C.The tungsten powder that the present embodiment prepares is canescence, to this reality
Execute example to prepare the purity of size and distribution of particles rule and tungsten powder that tungsten powder carries out grain graininess and examine
Surveying, learn that the particle diameter of tungsten powder particles is 3-5 μm, the granularity weighting width of tungsten powder is 56.01%, tungsten powder
Purity is 99.996%.
Embodiment 6
Carry out according to the method for embodiment 1, be except for the difference that 100 parts by volume with the capacity of molybdenum bowl, described
The consumption of tungsten powder is 30 parts by volume.The tungsten powder that the present embodiment prepares is canescence, prepares the present embodiment
The purity of size and distribution of particles rule and tungsten powder that tungsten powder carries out grain graininess detects, and learns tungsten
The particle diameter of powder particles is 3-5 μm, and the granularity weighting width of tungsten powder is 57.34%, and the purity of tungsten powder is
99.999%
Embodiment 7
Carry out according to the method for embodiment 1, be except for the difference that 100 parts by volume with the capacity of molybdenum bowl, described
The consumption of tungsten powder is 50 parts by volume.The tungsten powder that the present embodiment prepares is canescence, prepares the present embodiment
The purity of size and distribution of particles rule and tungsten powder that tungsten powder carries out grain graininess detects, and learns tungsten
The particle diameter of powder particles is 3-5 μm, and the granularity weighting width of tungsten powder is 57.36%, and the purity of tungsten powder is
99.998%。
Embodiment 8
Carry out according to the method for embodiment 1, be except for the difference that 100 parts by volume with the capacity of molybdenum bowl, described
The consumption of tungsten powder is 10 parts by volume.The tungsten powder that the present embodiment prepares is canescence, prepares the present embodiment
The purity of size and distribution of particles rule and tungsten powder that tungsten powder carries out grain graininess detects, and learns tungsten
The particle diameter of powder particles is 3-5 μm, and the granularity weighting width of tungsten powder is 56.15%, and the purity of tungsten powder is
99.996%。
Embodiment 9
Carry out according to the method for embodiment 1, be except for the difference that 100 parts by volume with the capacity of molybdenum bowl, described
The consumption of tungsten powder is 60 parts by volume.The tungsten powder that the present embodiment prepares is canescence, prepares the present embodiment
The purity of size and distribution of particles rule and tungsten powder that tungsten powder carries out grain graininess detects, and learns tungsten
The particle diameter of powder particles is 3-5 μm, and the granularity weighting width of tungsten powder is 56.21%, and the purity of tungsten powder is
99.997%。
Comparative example 1
Carrying out according to the method for embodiment 1, except for the difference that tungsten powder is in the presence of hydrogen gas, with 440 DEG C/min
Programming rate is warming up to 1750 DEG C.This comparative example is prepared tungsten powder and carries out the size of grain graininess and particle divides
The purity of cloth rule and tungsten powder detects, and learns that the particle diameter of tungsten powder particles is 2-7 μm, the grain of tungsten powder
Degree weighting width is 34.51%, and the purity of tungsten powder is 99.982%.
Comparative example 2
Carrying out according to the method for embodiment 1, except for the difference that tungsten powder is in the presence of hydrogen gas, with 510 DEG C/min
Programming rate is warming up to 2060 DEG C.This comparative example is prepared tungsten powder and carries out the size of grain graininess and particle divides
The purity of cloth rule and tungsten powder detects, and learns that the particle diameter of tungsten powder particles is 2-8 μm, the grain of tungsten powder
Degree weighting width is 33.47%, and the purity of tungsten powder is 99.993%.
Comparative example 3
Carrying out according to the method for embodiment 1, different programming rates is 440 DEG C/min.To this comparative example
The purity of size and distribution of particles rule and tungsten powder that prepared tungsten powder carries out grain graininess detects,
The particle diameter knowing tungsten powder particles is 2-6 μm, and the granularity weighting width of tungsten powder is 36.81%, and the purity of tungsten powder is
99.994%。。
Comparative example 4
Carrying out according to the method for embodiment 1, different programming rates is 510 DEG C/min.To this comparative example
The purity of size and distribution of particles rule and tungsten powder that prepared tungsten powder carries out grain graininess detects,
The particle diameter knowing tungsten powder particles is 2-7 μm, and the granularity weighting width of tungsten powder is 35.96%, and the purity of tungsten powder is
99.992%。。
From above-described embodiment 1-9 and comparative example 1-4, prepared by the method provided by the present invention
Tungsten powder surface is canescence, and without oxide yellow layer, the particle diameter of tungsten powder particles is 3-5 μm simultaneously, tungsten powder
Granularity weighting width be more than 56%, size distribution concentrate, the purity of tungsten powder at 99.995-99.999%,
Comply fully with and prepare the quality requirements of tungsten powder needed for negative electrode.
The preferred embodiment of the present invention is described in detail above in association with accompanying drawing, but, the present invention does not limit
Detail in above-mentioned embodiment, in the technology concept of the present invention, can be to the present invention
Technical scheme carry out multiple simple variant, these simple variant belong to protection scope of the present invention.
It is further to note that each the concrete technology described in above-mentioned detailed description of the invention is special
Levy, in the case of reconcilable, can be combined by any suitable means, in order to avoid need not
The repetition wanted, various possible combinations are illustrated by the present invention the most separately.
Additionally, can also be combined between the various different embodiment of the present invention, as long as its
Without prejudice to the thought of the present invention, it should be considered as content disclosed in this invention equally.
Claims (10)
1. the preparation method for the tungsten powder of negative electrode, it is characterised in that the method includes following step
Rapid:
(1) cool down after under an atmosphere of hydrogen, tungsten powder being heat-treated；
(2) tungsten powder after cooling being ground to tungsten powder particles (1), the most described tungsten powder particles (1) is put
In ball mill device, and ball mill device is placed in ball mill carries out ball milling；
(3) tungsten powder after ball milling is screened；
Wherein, described heat treatment is for be warming up to 1850-2000 by tungsten powder with 455-495 DEG C/min programming rate
DEG C, and it is incubated 100-140min at such a temperature；Described tungsten powder particles (1) is placed in ball mill device
Concretely comprise the following steps: tungsten powder particles (1) and agate ball are placed in agate tank (5), by the first lid
(6) it is placed on described agate tank (5), and agate tank (5) is placed in outer cover (7), and will tool
The second lid (8) having through hole is placed on described outer cover (7), more fixing bolt (9) is run through institute
The through hole stating the second lid (8) withstands described first lid (6), and with nut (10) by fixing spiral shell
Bolt (9) is fixed on described second lid (8).
Method the most according to claim 1, wherein, described heat treatment be by tungsten powder with
470-485 DEG C/min programming rate is warming up to 1900-1950 DEG C, and is incubated 100-140min at such a temperature.
Method the most according to claim 1 and 2, wherein, is placed in tungsten powder in molybdenum bowl, by molybdenum
Bowl is placed in drying bottle, and is placed in by drying bottle in tungsten net hydrogen stove and is heat-treated.
Method the most according to claim 3, wherein, is 100 parts by volume with the capacity of molybdenum bowl,
The consumption of described tungsten powder is 1-67 parts by volume.
Method the most according to claim 4, wherein, is 100 parts by volume with the capacity of molybdenum bowl,
The consumption of described tungsten powder is 20-50 parts by volume.
6. according to the method described in any one in claim 1,4 and 5, wherein, described ball milling
Method includes: the particle diameter of described tungsten powder particles (1) is 3-5mm, and the rotating speed of described ball mill is arranged
For 90-110 rev/min, ball milling 15-20 minute.
7. according to the method described in any one in claim 1,4 and 5, wherein, described agate ball
Including 3-7 first agate ball (2) of a diameter of 20-30mm, 5-15 a diameter of 12-18mm
Second agate ball (3) and the 3rd agate ball (4) of 3-10 a diameter of 5-10mm.
8. according to the method described in any one in claim 1,4 and 5, wherein, will be through ball milling
After the tungsten powder method that carries out screening be: the tungsten powder after ball milling is placed on the screen cloth of 200 mesh and carries out
Sieve takes.
Method the most according to claim 8, wherein, for not grinding by the tungsten powder of screen cloth
Mill again sieve take, and repeat, until not leading on the basis of the tungsten powder before the heat treatment of 100 weight portions
The content of the tungsten powder crossing screen cloth is 1-10 weight portion.
10. the tungsten powder prepared according to the method described in any one in claim 1-9 is preparing row ripple
Application in the cathode base of pipe.
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| CN104485269A (en) * | 2014-11-11 | 2015-04-01 | 安徽华东光电技术研究所 | Multi-beam cathode rhenium powder treatment method |
| CN104525933B (en) * | 2014-11-17 | 2017-01-11 | 安徽华东光电技术研究所 | Cobalt powder treatment method for cathode brazing of dual-mode traveling wave tube |
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