CN107988539A - A kind of quick method for preparing high-compactness fine grained texture xenon flash lamp electrode - Google Patents
A kind of quick method for preparing high-compactness fine grained texture xenon flash lamp electrode Download PDFInfo
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- CN107988539A CN107988539A CN201711215547.3A CN201711215547A CN107988539A CN 107988539 A CN107988539 A CN 107988539A CN 201711215547 A CN201711215547 A CN 201711215547A CN 107988539 A CN107988539 A CN 107988539A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
- C22C27/04—Alloys based on tungsten or molybdenum
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
- C22C1/051—Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
- C22C1/058—Mixtures of metal powder with non-metallic powder by reaction sintering (i.e. gasless reaction starting from a mixture of solid metal compounds)
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/001—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J9/00—Apparatus or processes specially adapted for the manufacture, installation, removal, maintenance of electric discharge tubes, discharge lamps, or parts thereof; Recovery of material from discharge tubes or lamps
- H01J9/02—Manufacture of electrodes or electrode systems
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Abstract
A kind of quick method for preparing high-compactness fine grained texture xenon flash lamp electrode, belongs to electrode technology field.It is to adulterate by APT and carry out secondary hydrogen reduction in reduction furnace to produce powder first；Take out quantitative above-mentioned powder, abrading-ball and absolute ethyl alcohol and be put into by a certain percentage in ball grinder and carry out ball-milling treatment, the powder before being sintered；Powder is fitted into the mould of discharge plasma hero and is sintered, wherein sintering condition is：Vacuum≤10Pa is sintered, sintering pressure is 10 60Mpa, and sintering temperature is 1,000 1600 DEG C, 3 10min of soaking time, 100 DEG C/min of the rate of heat addition.Prepared high-compactness fine grained texture xenon flash lamp tungsten electrode out of the invention can increase substantially the service life of xenon lamp in xenon lamp test, and preparation process is comparatively fairly simple, and sintering time is short, and energy consumption is than relatively low.
Description
Technical field
The present invention relates to a kind of preparation method of material, is sintered more particularly, to a kind of discharge plasma and prepares pulsed xenon
The method of lamp electrode, belongs to electrode technology field.
Technical background
Xenon flash lamp is a kind of device that radiation energy is converted electrical energy into by pulsed discharge form, and storage is on the capacitor
Energy discharged in a short period of time by fluorescent tube in the form of gas discharge, establish the high-temperature plasma in fluorescent tube, produce
The radiation of raw high brightness, so as to encourage operation material.Pulse atmosphere lamp is a kind of new type light source, has that ultraviolet continuous spectrum is good, light
Intensity is big, high luminous efficiency and other features, oneself through being widely used in the optical pumping of solid state laser, also with it is small,
Brightness is high, the features such as need not preheating, and has obtained widely should in water quality monitoring, soil analysis and medical treatment, chemical industry process field
With.
It is mainly thorium tungsten, barium tungsten and cerium tungsten that xenon flash lamp, which uses electrode material, at present, the load energy of cerium tungsten cathode, defeated
Go out the technical indicators such as power and light efficiency and be higher than thoriated-tungsten cathode, the light efficiency of cerium tungsten cathode is higher than thoriated-tungsten cathode by 5%, so generally
Xenon flash lamp selects cerium tungsten as its cathode at present.As requirement of the people to xenon flash lamp cathode is higher and higher, send out in recent years
The multielement rare earth tungsten electrode that exhibition is got up provides some thinkings to improve the performance of xenon lamp, how to study and select suitable component
Being used as xenon lamp cathode becomes the hot spot of a research.
The characteristics of this kind of electrode product is that demand is small, and species complexity is various, it usually needs is customized towards electrode manufacturer, specially
Door, which feeds intake, to be sintered, and prepared by pressure processing, complex process, cost is higher, the unit prepared by traditional electrode fabrication
Rare-earth tungsten electrode cannot increasingly meet requirement of the xenon flash lamp to tungsten electrode, how quickly prepare consistency higher crystal grain
The more tiny rare-earth tungsten electrode of enterprise schema becomes demand urgent always for improving the service life of xenon flash lamp and performance.This
Invention selection determines the component of most suitable xenon lamp electrode, and La is added in tungsten powder2O3、Y2O3、Zr2O3Three kinds of rare-earth oxidations
Thing, and the xenon lamp electrode for preparing high-compactness fine grained texture is sintered by discharge plasma.
The content of the invention
It is an object of the invention to pass through La2o3、Y2o3、Zr2o3Three kinds of rare earth oxides, and burnt by discharge plasma
Knot prepares the xenon lamp electrode of high-compactness fine grained texture.The present invention provides a kind of discharge plasma sintering to prepare xenon lamp electricity
The method of pole, prepared by powder, pre-molding, discharge plasma sintering and etc., prepare consistency and be up to 99%, firmly
Angle value is up to the multielement rare earth tungsten electrode of 496.7HV, and the preparation method is simple, and sintering time is short, and cost obtains certain control
System, energy consumption are low.
A kind of W-La-Y-Zr electrodes provided by the invention, it is characterised in that it is dilute that tri- kinds of La, Y, Zr is added in tungsten basal body
Native oxide La2O3、Y2O3、Zr2O3, its middle rare earth La2O3、Y2O3、Zr2O3Weight hundred in W-La-Y-Zr electrodes
Point ratio is：1.2-1.8%.It is preferred that the molar ratio of La, Y, Zr are (10-30):(0.5-1.5)：(0.5-1.5).
The preparation method of above-mentioned W-La-Y-Zr electrodes, it is characterised in that using solid-liquid doping way, including following step
Suddenly：
(1) add deionized water in doping machine, add the nitrate of tri- kinds of rare earths of La, Y, Zr, heating (such as steam heating),
Stirring, treats that nitrate is completely dissolved, and stirs evenly to be doped after addition sodium paratungstate and (is such as mixed with the speed stirring of 100r/min
Miscellaneous 2h), drying box is put into after water evaporating completely, is then carried out successively at a temperature of 620 DEG C -680 DEG C and 780 DEG C -980 DEG C
Hydrogen reduction twice, produces powder raw material；
(2) powder raw material, ball milling ball and the absolute ethyl alcohol produced upper step, which are put into ball grinder, carries out ball-milling treatment, from
And obtain mixing tungsten powder powder；Then mixing tungsten powder powder is wrapped with graphite tinfoil, be loaded into graphite jig, and
It is pressed into fine and close idiosome；
(3) above-mentioned fine and close idiosome is fitted into discharge plasma sintering furnace and be sintered, sintering current is DC pulse
Electric current, pulse ratio are set to 12:2, vacuum≤10Pa, sintering pressure 10-70Mpa, sintering temperature is 1000-1800 DEG C, is protected
The warm time is 3-15min, and the electrode of obtained xenon lamp remembers E3 electrodes.
The mass ratio of the raw material, abrading-ball and the absolute ethyl alcohol that are put into further preferred step (2) in ball grinder is 1:25:2,
The diameter of abrading-ball differs；Ball milling ball used is agate ball, and ball grinder used is agate pot.
The rotating speed of ball-milling treatment is 300-500r/min, Ball-milling Time 10-20h described in further preferred step (2).
Heating rate described in further preferred step (3) is 100 DEG C/min；The optimal sintering temperature is 1450
℃；The optimal soaking time is 5min；The optimal sintering pressure is 50Mpa.
Compared to the unit rare-earth tungsten electrode used in present xenon lamp electrode, prepared by discharge plasma sintering provided by the invention
Xenon lamp can reach 99% with the consistency of E3 electrodes, sintered body of the hardness number in 450HV-600HV, this system can be obtained
Preparation Method is easy to operate, and sintering time is short, design mould can be removed according to the demand of oneself, so as to obtain the sintering of oneself demand
Body, energy consumption are low.
Brief description of the drawings
Fig. 1 is the W-La-Y-Zr tungsten alloy electrode SEM photographs obtained in present example；
a.1350℃b.1400℃c.1450℃。
Fig. 2 is the relation of the W-La-Y-Zr tungsten alloy electrode temperature hardness obtained in present example.
Embodiment
Clear, complete description is carried out to the technical solution in the embodiment of the present invention below, it is clear that described embodiment
Only be the present invention part of the embodiment, rather than the present invention whole embodiments.
The method that discharge plasma sintering of the present invention prepares xenon lamp electrode, specifically implements according to following steps：
Prepare component and contain La2O3、Y2O3、Zr2O3Three kinds of rare earth oxides, the molar ratio of three kinds of oxides is 20:1:
1.The total content weight ratio of three kinds of rare earth oxides is 1.8% in such scheme.
By rare earth nitrades and deionized water wiring solution-forming containing three kinds of rare earth oxides, it is added in a manner of vaporific secondary
In wolframic acid salt powder dry after through 620 DEG C -680 DEG C (preferably 650 DEG C) and 780 DEG C -980 DEG C (800 DEG C) at a temperature of carry out two
Secondary hydrogen reduction；Then by raw material, abrading-ball and absolute ethyl alcohol made from above-mentioned steps according to 1:25:2 mass ratio is put into ball milling
In tank, ball grinder is put into ball mill after sealing, rotating speed 300-500r/min, continuous ball milling 4-48h, it is cold to remove ball grinder
But, mixing tungsten powder powder is taken out to spontaneously dry, ask described in ball milling ball be agate ball, ball grinder is agate pot；Then will be mixed
Close tungsten powder powder to be wrapped with the graphite tinfoil of 2mm, be loaded into graphite jig, and be pressed into fine and close idiosome；Finally will
Mould is put into discharge plasma sintering furnace, is closed fire door, is extracted out indoor gas with vacuum pump, until vacuum drops to
Below 10pa is sintered again, wherein the condition of the sintering processes is：Sintering current is DC pulse current, sintering
Pressure is 10-60Mpa, and sintering temperature is 1200-1800 DEG C, and heating rate is 100 DEG C/min, soaking time 3-10min, is burnt
Less than about 200 DEG C are cooled to mould after knot, is then removed from the molds sintered body, you can obtains W-La-Y-
Zr electrodes.
The specific embodiment of the present invention is illustrated below：
Embodiment 1
50g is chosen from being reduced twice in produced tungsten alloy powder by APT+, is put into after being sufficiently mixed in ball grinder,
The non-uniform agate ball of 1.25kg sizes and 100ml absolute ethyl alcohols are placed into, ball grinder is put into ball mill after sealing completely
In, ball grinder is removed after rotating speed 450r/min, continuous ball milling 18h, is cooled down, tungsten alloy powder is taken out and spontaneously dries；Again will
Obtained tungsten alloy powder after flexible carbon paper parcel with being fitted into the graphite jig used in discharge plasma sintering, then by mould
Tool be put into discharge plasma sintering furnace, shut fire door, then carry out vacuum drawn, until vacuum drop to 10pa with
Under, using DC pulse current, under the sintering pressure of 50Mpa, 1350 DEG C are heated to 100 DEG C/min, keeps the temperature 5min, sintering
After with mould be together cooled to less than about 150 DEG C when, mould is taken out from sintering furnace, obtains sintered tungsten
Alloy electrode.As shown in fig. 1A, Fig. 2 is the W-La-Y- obtained in present example to the SEM figures of the tungsten alloy electrode
The relation of Zr tungsten alloy electrodes temperature, hardness and the porosity.It can be seen that the grain size of the tungsten alloy electrode is big
About 2.2 μm, and in the case where obtaining tiny crystallite dimension tissue, the consistency of tungsten alloy electrode has reached 94%.Fig. 2 is this hair
W-La-Y-Zr tungsten alloy electrodes temperature, the relation of hardness obtained in bright example, as can be seen from the figure comes prepared by 1350 DEG C
The hardness of W-La-Y-Zr tungsten alloy electrodes be also not reaching to highest.
Embodiment 2
50g is chosen from being reduced twice in produced tungsten alloy powder by APT+, is put into after being sufficiently mixed in ball grinder,
The non-uniform agate ball of 1.25kg sizes and 100ml absolute ethyl alcohols are placed into, ball grinder is put into ball mill after sealing completely
In, ball grinder is removed after rotating speed 450r/min, continuous ball milling 18h, is cooled down, tungsten alloy powder is taken out and spontaneously dries；Again will
Obtained tungsten alloy powder after flexible carbon paper parcel with being fitted into the graphite jig used in discharge plasma sintering, then by mould
Tool be put into discharge plasma sintering furnace, shut fire door, then carry out vacuum drawn, until vacuum drop to 10pa with
Under, using DC pulse current, under the sintering pressure of 50Mpa, 1400 DEG C are heated to 100 DEG C/min, keeps the temperature 7min, sintering
After with mould be together cooled to less than about 150 DEG C when, mould is taken out from sintering furnace, obtains sintered tungsten
Alloy electrode.The SEM of the tungsten alloy electrode is schemed as shown in fig. ib, it can be seen that the crystalline substance of the tungsten alloy electrode
Particle size size is about 3 μm, and in the case where obtaining tiny crystallite dimension tissue, the consistency of tungsten alloy electrode reaches
97%.Fig. 2 is the relation of the W-La-Y-Zr tungsten alloy electrodes temperature and hardness obtained in present example, can from figure
Out the hardness of the W-La-Y-Zr tungsten alloy electrodes prepared by 1400 DEG C is also not reaching to highest.
Embodiment 3
50g is chosen from being reduced twice in produced tungsten alloy powder by APT+, is put into after being sufficiently mixed in ball grinder,
The non-uniform agate ball of 1.25kg sizes and 100ml absolute ethyl alcohols are placed into, ball grinder is put into ball mill after sealing completely
In, ball grinder is removed after rotating speed 450r/min, continuous ball milling 18h, is cooled down, tungsten alloy powder is taken out and spontaneously dries；Again will
Obtained tungsten alloy powder after flexible carbon paper parcel with being fitted into the graphite jig used in discharge plasma sintering, then by mould
Tool be put into discharge plasma sintering furnace, shut fire door, then carry out vacuum drawn, until vacuum drop to 10pa with
Under, using DC pulse current, under the sintering pressure of 50Mpa, 1450 DEG C are heated to 100 DEG C/min, keeps the temperature 5min, sintering
After with mould be together cooled to less than about 150 DEG C when, mould is taken out from sintering furnace, obtains sintered tungsten
Alloy electrode.The SEM of the tungsten alloy electrode is schemed as shown in the c in Fig. 1, it can be seen that the crystalline substance of the tungsten alloy electrode
Particle size size is about 3.5 μm, and in the case where obtaining tiny crystallite dimension tissue, the consistency of tungsten alloy electrode reaches
99%.Fig. 2 is the relation of the W-La-Y-Zr tungsten alloy electrodes temperature and hardness obtained in present example, can from figure
Out the hardness of the W-La-Y-Zr tungsten alloy electrodes prepared by 1450 DEG C reaches highest, its performance is also best.
The foregoing is merely the embodiment of the present invention, is not intended to limit the scope of the invention, every to utilize this Shen
Please the equivalent structure or equivalent flow shift made of invention book content, be directly or indirectly used in the technologies of other correlation techniques
Field, is included within the scope of the present invention.
Claims (10)
1. a kind of W-La-Y-Zr electrodes, it is characterised in that tri- kinds of rare earth oxide La of La, Y, Zr are added in tungsten basal body2O3、
Y2O3、Zr2O3, its middle rare earth La2O3、Y2O3、Zr2O3Percentage by weight in W-La-Y-Zr electrodes is：1.2-
1.8%.
2. a kind of W-La-Y-Zr electrodes described in accordance with the claim 1, it is characterised in that the molar ratio of La, Y, Zr are (10-
30):
(0.5-1.5)：(0.5-1.5).
3. prepare the method for the W-La-Y-Zr electrodes described in claim 1 or 2, it is characterised in that comprise the following steps：
(1) deionized water is added in doping machine, adds the nitrate of tri- kinds of rare earths of La, Y, Zr, heating (such as steam heating), stir
Mix, treat that nitrate is completely dissolved, stir evenly to be doped after addition ammonium paratungstate and (doping is such as stirred with the speed of 100r/min
2h), drying box is put into after water evaporating completely, then carries out two at a temperature of 620 DEG C -680 DEG C and 780 DEG C -980 DEG C successively
Secondary hydrogen reduction, produces powder raw material；
(2) powder raw material, ball milling ball and the absolute ethyl alcohol produced upper step, which are put into ball grinder, carries out ball-milling treatment, so that
To mixing tungsten powder powder；Then mixing tungsten powder powder is wrapped with graphite tinfoil, be loaded into graphite jig, and suppress
Into fine and close idiosome；
(3) above-mentioned fine and close idiosome being fitted into discharge plasma sintering furnace and be sintered, sintering current is DC pulse current,
Pulse ratio is set to 12:2, vacuum≤10Pa, sintering pressure 10-70Mpa, sintering temperature is 1000-1800 DEG C, soaking time
For 3-15min, the electrode of obtained xenon lamp.
4. in accordance with the method for claim 3, it is characterised in that raw material, abrading-ball and the nothing being put into step (2) in ball grinder
The mass ratio of water-ethanol is 1:25:2.
5. in accordance with the method for claim 3, it is characterised in that ball milling ball used is agate ball, and ball grinder used is
Agate pot.
6. in accordance with the method for claim 3, it is characterised in that the rotating speed of ball-milling treatment described in step (2) is 300-
500r/min, Ball-milling Time 10-20h.
7. in accordance with the method for claim 3, it is characterised in that the heating rate described in step (3) is 100 DEG C/min.
8. in accordance with the method for claim 3, it is characterised in that step (3) sintering temperature is 1450 DEG C.
9. in accordance with the method for claim 3, it is characterised in that step (3) soaking time is 5min.
10. in accordance with the method for claim 3, it is characterised in that step (3) sintering pressure is 50Mpa.
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| CN109385547A (en) * | 2018-10-15 | 2019-02-26 | 北京工业大学 | A kind of carbon nano tube-doped rare-earth tungsten electrode material and preparation method |
| CN110587176A (en) * | 2019-09-20 | 2019-12-20 | 北京矿冶科技集团有限公司 | Zirconium oxide micro-doped tungsten electrode material, zirconium oxide micro-doped tungsten electrode, preparation method and application of zirconium oxide micro-doped tungsten electrode material |
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| CN110587176A (en) * | 2019-09-20 | 2019-12-20 | 北京矿冶科技集团有限公司 | Zirconium oxide micro-doped tungsten electrode material, zirconium oxide micro-doped tungsten electrode, preparation method and application of zirconium oxide micro-doped tungsten electrode material |
| CN110587176B (en) * | 2019-09-20 | 2020-11-20 | 北京矿冶科技集团有限公司 | Zirconium oxide micro-doped tungsten electrode material, zirconium oxide micro-doped tungsten electrode, preparation method and application of zirconium oxide micro-doped tungsten electrode material |
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Application publication date: 20180504 |