CN105788996B - A kind of submicron film scandium tungsten cathode and preparation method thereof - Google Patents
A kind of submicron film scandium tungsten cathode and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of preparation method of submicron film scandium tungsten cathode, including tungsten powder suppressed, is sintered, obtain cathode base；Cathode base is impregnated into active material barium calcium aluminium compound；Cathode base impregnated of active material is assembled in the cathode support cylinder containing heater；Sub-micron scandium W film is deposited on cathode base surface with magnetically controlled DC sputtering, obtains submicron film scandium tungsten cathode.The current density of negative electrode produced by the present invention is big, and operating temperature is low, longevity of service, and manufacture method is simple, workable, reproducible.
Description
Technical field
The present invention relates to electrovacuum component field.More particularly, to a kind of submicron film scandium tungsten cathode and its system
Preparation Method.
Background technology
Cathode electronics emitter pass through a nearly century development, many science and technologies Disciplinary Frontiers in occupation of not
Alternative status.In military, space technology, the technical field such as electron accelerator and free-electron laser, to low temperature, big electricity
The demand of the electron emitter of current density, high uniform emission and long-life is very urgent all the time.Emission p erformance, process stabilizing
Property and reliability obviously also the development to costly electronic device with production it is particularly significant.In fact, cathode emitter
Improve can also serve impetus to vacuum electron device development and performance boost.Vacuum electron device includes microwave vacuum electricity
Sub- device, the theory of relativity vacuum electron device, vacuum electronic display, vacuum electronic illuminating device and the ion using electron source
Device etc..
Occupied using tungsten basal body, alkaline-earth metal barium as the diffused negative electrode of active material in current all kinds of vacuum electron devices
First choice, it is widely used.The seventies latter stage, rare earth Sc Sc are introduced into this electron emitter and illustrated to dispenser cathode
Emitting performance significantly improves, and extensive must be paid close attention to so as to cause.In more than 20 years thereafter, countries in the world are developed in succession
The scandium-containing diffusion cathode of various variants, work function is set finally to be reduced to 1.5-1.6 electron-volts；Obtaining same current density
When, the operating temperature than M type dispenser cathodes declines 200 DEG C or so, greatly increases the performance of electron emitter.
The type of scandium-containing diffusion cathode substantially has following a few classes：
1) by Sc2O3Add the immersion-type Scandate cathode in dispenser cathode aluminic acid barium salt.1977 public by Philips
Department proposes that emitting performance is：During 1000 DEG C of operating temperature, emission 5A/cm2, about 3000 hours life-spans
(US4007393)。
2) by Sc2O3Add the mixed base negative electrode containing scandium in tungsten basal body.Generally by Sc in this kind of negative electrode2O3With tungsten powder machine
Tool mixes, and the substrate of POROUS TUNGSTEN containing scandium is made in repressed, sintering, then impregnates barium aluminate and forms diffused negative electrode containing scandium.This moon
Polar form was proposed first in 1984 by Japanese Hitachi, and for the negative electrode in 850 DEG C of operating temperature, pulsed emission current is close
Spend 10A/cm2(S.Yamamoto,S.Taguchi,T.Aida,Appl.Surf.Sci.17(1984)504-516)。
3) mixed base " top layer " negative electrode containing scandium.By Philips companies (J.Hasker, J.Van were announced in 1986
Esdonk and J.E.Crombeen.Appl.Surface Sci.26(1986)173.).This negative electrode is that 0.1mm is thick
Porous tungsten body containing scandium is placed on common porous tungsten body, forms " top layer " containing scandium, then impregnate aluminate.It has favourable to launching
Surface containing scandium, while remain and ample supply and the common porous tungsten substrate of active barium can be stored, so as to improve the property of negative electrode
Energy.But due to its complex process, technique productions are not suitable for it.Then, Philips companies are transferred to mixed base again in nineteen ninety
Negative electrode studies (U.van Slooten, Peter A.Duine Appl.Surf.Sci.111 (1997) 24-29), obtained negative electrode
Impulse ejection ability operating temperature be 1000 DEG C reached 100A/cm2。
4) film-type " top layer " negative electrode containing scandium.It is with one layer of film containing scandium of deposition on conventional impregnation type dispenser cathode
Method realize containing scandium " top layer " addition.The method of deposition can be radio-frequency sputtering (Yamamoto S, Taguchi S and
Aida T et al.Appl.Surface Sci.17 (1986) 517) or laser evaporation (CN1128403A), the film of deposition can
To be W+Sc2O3、W+Sc2W3O12(S.Yamamoto,I.Watanabe,S.Taguchi et al,Jpn.J.Appl.Phys.28
(1989) 490-494.) or W/Sc2O3+Re(G.Gartner,P.Geittner,H.Lydton,A.Ritz,
Appl.Surf.Sci.111(1997)11-17).Film-type " top layer " negative electrode containing scandium can be introduced with certain thickness uniformly heavy
Long-pending film containing scandium.Research to scandium series cathode shows, is no tribute to transmitting if the Sc of cathode surface exists with elementary state
Offer, only when Sc is oxidation state, the work function of negative electrode can be made reduce in subsequent activation.So film
The technology key of type scandium series cathode must is fulfilled at following 2 points：1) covering of film can not change the conduction on former impregnated cathode surface
Characteristic；2) Sc in film must be existing for oxidation state[.Existing film-type " top layer " negative electrode containing scandium, which introduces, has certain thickness
The film containing scandium of the uniform deposition of degree, but radio-frequency sputtering can cause the decomposition of scandium oxide in target, in order that obtaining in film
Sc is oxidation state, it is necessary to system is oxygenated and strict control partial pressure, this causes the control to the condition of spatter film forming
Become extremely difficult；And although laser evaporization method has without that Sc can be made to keep complete in film system introducing active gases
Oxidation state, but its complex manufacturing technology, poor controllability.In addition, JP Laid-Open 6-260084 and CN102522281 disclose use
D.c. sputtering is made film-type scandium series cathode.
The above negative electrode containing scandium is present：1) diffusion of scandium and its oxide is bad, makes supplement difficult.Work as high temperature
When evaporating or bearing Ions Bombardment and lose, it is difficult to be restored, directly affect transmitting and the life-span of negative electrode；2) addition scandium or
Its oxide skewness, it is uneven so as to cause to launch；3) complex process, and poor repeatability.
Therefore, it is necessary to which a kind of method of new preparation negative electrode containing scandium, avoids aforementioned defect.
The content of the invention
It is an object of the present invention to provide a kind of submicron film scandium tungsten cathode.
It is another object of the present invention to provide the preparation method of above-mentioned submicron film scandium tungsten cathode.
To reach above-mentioned purpose, the present invention uses following technical proposals：
A kind of preparation method of submicron film scandium tungsten cathode, comprises the following steps：
1) tungsten powder is suppressed, sintered, obtain cathode base；
2) cathode base is impregnated into active material barium calcium aluminium compound；
3) cathode base impregnated of active material is assembled in the cathode support cylinder containing heater；
4) sub-micron scandium W film is deposited on cathode base surface with magnetically controlled DC sputtering；During magnetically controlled DC sputtering, target
Raw material be submicron-scale made from sol-gal process Scandia doped tungsten powder；Using ladder making alive mode, first splashing
Radio pressure 350-450V is kept for 4-6 minutes；Kept for 4-6 minutes in sputtering voltage 750-850V again；Finally in sputtering voltage 1150-
1250V is kept for 40-60 minutes, obtains submicron film scandium tungsten cathode.
In step 1), tungsten powder is high-purity micron order tungsten powder；The compacting is to use isostatic pressing technology, and press temperature is room
Temperature, pressing pressure are 2-2.5 tons；The sintering is sintered in hydrogen atmosphere, and sintering temperature is 1900-2000 DEG C, during sintering
Between be 40-60 minutes.
Porous tungsten basal body is obtained after sintering, porous tungsten basal body is passed through and soaks copper, is machined, removes copper, obtains cathode base；
The leaching copper is that copper is melted under the conditions of 1400-1500 DEG C of temperature, and copper is impregnated into POROUS TUNGSTEN base using capillarity afterwards
In body；The machining is leaching copper tungsten basal body to be processed into required shape, tool using processing methods such as car system, electric sparks
Body step and condition refer to existing literature；It is described that to remove copper be that the leaching processed is removed using chemical method or high temperature evaporation method
Copper in copper tungsten basal body, specific steps and condition refer to existing literature.
In step 2), barium calcium aluminium compound can be barium calcium-aluminate or the barium calcium aluminium compound of other stabilizations.
When barium calcium aluminium compound is barium calcium-aluminate, BaO：CaO：Al2O3Mol ratio be 5：3：2,4：1：1 or 6：1：
2。
The dipping temperature is 1500 DEG C -1700 DEG C, and dip time is the 10-120 seconds.After dipping, gone with turning processing method
Except the remaining dipping thing on cathode base surface.
In step 3), heater is indirect-heating heater.
Cathode base and cathode support cylinder are brazed together by brazing material.
Preferably, in the cathode base one side relative with heater coated with suppression evaporation material.Suppress evaporation material and the moon
Brazing material between pole matrix and cathode support cylinder is identical, is molybdenum ruthenium solder.Pricker between cathode base and cathode support cylinder
Weldering, the coating of suppression evaporation material are while completed in hydrogen stove.Suppress the hole that evaporation material is used to seal the cathode base back side
Gap, prevent barium calcium aluminium compound from being evaporated to heater.
Preferably, the space filling high purity aluminium oxide between cathode base and heater.High purity aluminium oxide filler is through burning
Cathode base is directly transferred heat to by heat exchange pattern after knot, improves the efficiency of heating surface and temperature homogeneity.
In step 4), the target raw material used in magnetically controlled DC sputtering does not use the mechanical mixture of general tungsten powder and scandium oxide powder
Thing, but use the Scandia doped tungsten powder of submicron-scale made from sol-gal process.
The preparation of the target is by the Scandia doped tungsten powder elder generation compression molding of submicron-scale, then low-temperature sintering.Institute
It is that the Scandia doped tungsten powder powder of appropriate submicron-scale is inserted target holder at room temperature to state compression molding, uses manual pressure
Power machine carries out just one-step forming, and pressing pressure is 2-2.5 tons；The low-temperature sintering is in a vacuum furnace to burn the target of first one-step forming
Knot makes to target type to 850-950 DEG C.This is due to that must assure that the chemical state of scandium and powder size are almost unchanged in sputtering,
And the surface-active between the powder granule of submicron-scale strengthens, between the frictional force, powder and mold wall between powder
Frictional force and the relative increase of viscosity resistance, are molded relative difficulty.
During magnetically controlled DC sputtering, atmosphere gas is nitrogen, and background vacuum is 5 × 10-4Pa；The diameter 50mm of target；Target
Distance with cathode base surface is 40-50mm；Sputtering power is 100-120W.
Deposit by specific dc sputtering processes to obtain scandium W film using the pressed by powder target of the present invention, oxidation can be made
Scandium is more evenly distributed cathode surface, significantly reduces the work function of cathode surface, improves the emission of negative electrode
And emission uniformity.
Preferably, percentage by weight of the scandium oxide in tungsten powder is 3-10%, more preferably 5%.Scandium oxide content is high, energy
The anti-Ions Bombardment ability of negative electrode is improved, so as to improve the life-span of negative electrode.
Preferably, using ladder making alive mode, first kept for 5 minutes in sputtering voltage 400V；Again in sputtering voltage 800V
Kept for 5 minutes；Finally kept for 45 minutes in sputtering voltage 1200V, obtain submicron film scandium tungsten cathode.
The present invention also provides the submicron film scandium tungsten cathode as made from above-mentioned preparation method, and it includes：Cathode support cylinder,
Heater, cathode base, active material, sub-micron scandium W film, the active material is immersed in cathode base, the sub-micro
Rice scandium W film is to sputter at cathode base surface, and the cathode base and heater are arranged in cathode support cylinder.
Preferably, the negative electrode also includes suppressing evaporation material, suppresses evaporation material and is coated in the cathode base back side, face
Heater.
Preferably, the negative electrode also includes high purity aluminium oxide filler, and high purity aluminium oxide filler is filled in suppression evaporation
Space between material and heater.
Preferably, the thickness of sub-micron scandium W film is 200-400nm.
Beneficial effects of the present invention are as follows：
The present invention prepares direct magnetic control by using the repressed sintering of submicron material for keeping granular size almost unchanged
The target of sputtering, and the parameters of each step are strictly controlled to make scandium oxide be evenly distributed on cathode base surface,
The current density of negative electrode produced by the present invention is big, is believed that highest current density is about 85.08A/cm at 1000 DEG C2, and
Operating temperature ratio can be made to cover osmium film negative electrode under same current density reduces by 200 DEG C or so, and the activationary time needed is only 10-30
Minute, the seasoned time is only about 24 hours, and the working time reduces 0.2- up to 3000 hours, by the work function of cathode surface
0.4eV。
The controllability of the present invention is strong, without being filled with active gases such as O to system2Protected etc. the scandium element that can make in scandium tungsten film
Hold complete oxidation state.
The manufacture method of the present invention is simple, workable, reproducible.
Brief description of the drawings
The embodiment of the present invention is described in further detail below in conjunction with the accompanying drawings.
Fig. 1 is the schematic diagram of submicron film negative electrode containing scandium produced by the present invention.
Fig. 2 is the powder granularity distribution map of obtained Scandia doped tungsten powder in embodiment 1.
Fig. 3 is the powder XRD of obtained Scandia doped tungsten powder in embodiment 1.
Fig. 4 is the SEM figures of sub-micron scandium W film.
Fig. 5 is the XPS spectrum figure of scandium oxide in sub-micron scandium W film.
Fig. 6 is the emission figure that the negative electrode of embodiment 1 is tested in water cooling anode diode.
Fig. 7 is to cover the emission figure that osmium film negative electrode is tested in water cooling anode diode
Fig. 8 is the emission figure that the negative electrode of embodiment 1 is tested in electron gun.
In Fig. 1,1- cathode support cylinders, 2- indirect-heating heaters, 3- cathode bases, 4- active materials, 5- sub-micron scandium tungsten is thin
Film, 6- suppress evaporation material, 7- high purity aluminium oxide fillers.
Embodiment
In order to illustrate more clearly of the present invention, with reference to preferred embodiment, the present invention is described further.Ability
Field technique personnel should be appreciated that following specifically described content is illustrative and be not restrictive, and this should not be limited with this
The protection domain of invention.
Embodiment 1
A kind of preparation method of submicron film scandium tungsten cathode, comprises the following steps：
1) high-purity micron order tungsten powder is first used into isostatic pressing technology at room temperature, suppressed under 2 tons of pressing pressures；Afterwards in hydrogen
It it is 1900 DEG C in sintering temperature, sintering time is to obtain porous tungsten basal body in 40 minutes in gas atmosphere；Copper in 1400 DEG C of bars of temperature
Melt under part, copper is impregnated into porous tungsten basal body using capillarity afterwards；Using processing methods such as car system, electric sparks leaching
Copper tungsten basal body is processed into required shape；Removed using chemical method or high temperature evaporation method in the leaching copper tungsten basal body processed
Copper, obtain cathode base；
2) cathode base is impregnated into active material barium calcium aluminium compound (barium calcium-aluminate, BaO：CaO：Al2O3Mol ratio
For 5：3：2), dipping temperature is 1500 DEG C, and dip time is 10 seconds, and cathode base table is removed with turning processing method after the completion of dipping
The remaining dipping thing in face；
3) molybdenum ruthenium solder pricker will be passed through impregnated of the cathode support cylinder of the cathode base of active material and the heater containing indirect-heating
It is welded together, coat molybdenum ruthenium solder in the cathode base one side relative with heater；Space between cathode base and heater is filled out
Fill high purity aluminium oxide；
4) sub-micron scandium W film is deposited on cathode base surface with magnetically controlled DC sputtering；Will be sub- made from sol-gal process
The Scandia doped tungsten powder of micro-meter scale is at room temperature with 2 tons of pressing pressure elder generation compression moldings, afterwards in 850 DEG C of low-temperature sinterings,
Target as magnetically controlled DC sputtering；Atmosphere gas is nitrogen, and background vacuum is 5 × 10-4Pa；The diameter 50mm of target；Target
Distance with cathode base surface is 40mm；Sputtering power is 100W, is first kept for 5 minutes in sputtering voltage 400V；Sputtering again
Voltage 800V keeps 4 clocks；Finally kept for 45 minutes in sputtering voltage 1200V, obtain submicron film scandium tungsten cathode.
Fig. 1 is the schematic diagram of submicron film negative electrode containing scandium produced by the present invention.
Fig. 2 is the powder granularity distribution map of obtained Scandia doped tungsten powder in embodiment 1.It can be seen that adopt
The even particle size distribution of the Scandia doped tungsten powder of the submicron-scale made from sol-gal process, powder granule shape are defined ball
Shape, diameter of particle distribution meet preferable quasi normal distribution.
Fig. 3 is the powder XRD of obtained Scandia doped tungsten powder in embodiment 1.As can be seen that Sc is oxidation from figure
State (scandium oxide) and temperature independent (collection of illustrative plates is all at 1100 DEG C, 1200 DEG C, 1300 DEG C, 1500 DEG C and 1700 DEG C when temperature
It is to overlap).
Fig. 4 is the SEM figures of sub-micron scandium W film.
Fig. 5 is the XPS spectrum figure of scandium oxide in sub-micron scandium W film, and spectral peak is located near 402.2eV, shows scandium to aoxidize
Titanium is present in film.
Under conditions of pulsewidth 5-25 μ s, repetition rate 100-500Hz, the cathode current emission of the negative electrode of the present invention is tested
Density, as shown in Figure 6：At 900 DEG C, its keen current density launched is better than 30A/cm after cathode stabilization2；Corresponding to 1000 DEG C
Curve, because test power supply can only achieve 2700V, therefore keen current density is not obtained, highest current density is about
85.08A/cm2.It can be seen that the negative electrode has very high emission current densities, hence it is evident that higher than M types negative electrode and Scandate cathode.
Fig. 7 is to cover the emission figure that osmium film negative electrode is tested in water cooling anode diode, it can be seen that is commonly covered
Osmium film negative electrode is at 1100 DEG C, its keen current density about 30A/cm launched2。
U.S. SLAC is tested using electron gun to the negative electrode of the present invention, test result such as Fig. 8：It is cloudy at 1050 DEG C
Its keen current density launched is better than 100A/cm after stabilizer pole2。
The work function of cathode surface is reduced 0.2-0.4eV by the method for the present invention, during the activation that obtained negative electrode needs
Between be only 10-30 minutes, the seasoned time is only about 24 hours, but the working time was up to 3000 hours.
Embodiment 2
A kind of preparation method of submicron film scandium tungsten cathode, comprises the following steps：
1) high-purity micron order tungsten powder is first used into isostatic pressing technology at room temperature, suppressed under 2 tons of pressing pressures；Afterwards in hydrogen
It it is 2000 DEG C in sintering temperature, sintering time is to obtain porous tungsten basal body in 60 minutes in gas atmosphere；Copper in 1500 DEG C of bars of temperature
Melt under part, copper is impregnated into porous tungsten basal body using capillarity afterwards；Using processing methods such as car system, electric sparks leaching
Copper tungsten basal body is processed into required shape；Removed using chemical method or high temperature evaporation method in the leaching copper tungsten basal body processed
Copper, obtain cathode base；
2) cathode base is impregnated into active material barium calcium aluminium compound (barium calcium-aluminate, BaO：CaO：Al2O3Mol ratio
For 4：1：1), dipping temperature is 1700 DEG C, and dip time is 120 seconds, and cathode base is removed with turning processing method after the completion of dipping
The remaining dipping thing on surface；
3) molybdenum ruthenium solder pricker will be passed through impregnated of the cathode support cylinder of the cathode base of active material and the heater containing indirect-heating
It is welded together, coat molybdenum ruthenium solder in the cathode base one side relative with heater；Space between cathode base and heater is filled out
Fill high purity aluminium oxide；
4) sub-micron scandium W film is deposited on cathode base surface with magnetically controlled DC sputtering；Will be sub- made from sol-gal process
The Scandia doped tungsten powder of micro-meter scale with 2.5 tons of pressing pressure elder generation compression moldings, burns in 950 DEG C of low temperature afterwards at room temperature
Knot, the target as magnetically controlled DC sputtering；Atmosphere gas is nitrogen, and background vacuum is 5 × 10-4Pa；The diameter 50mm of target；Target
Material and the distance on cathode base surface are 50mm；Sputtering power is 120W, is first kept for 6 minutes in sputtering voltage 350V；Splashing again
Radio pressure 750V is kept for 6 minutes；Finally kept for 60 minutes in sputtering voltage 1150V, obtain submicron film scandium tungsten cathode.Performance
Test result is similar to Example 1.
Embodiment 3
A kind of preparation method of submicron film scandium tungsten cathode, comprises the following steps：
1) high-purity micron order tungsten powder is first used into isostatic pressing technology at room temperature, suppressed under 2.5 tons of pressing pressures；Exist afterwards
It it is 2000 DEG C in sintering temperature, sintering time is to obtain porous tungsten basal body in 50 minutes in hydrogen atmosphere；Copper in 1500 DEG C of temperature
Under the conditions of melt, copper is impregnated into porous tungsten basal body using capillarity afterwards；Utilize the processing method handle such as car system, electric spark
Leaching copper tungsten basal body is processed into required shape；The leaching copper tungsten basal body processed is removed using chemical method or high temperature evaporation method
In copper, obtain cathode base；
2) cathode base is impregnated into active material barium calcium aluminium compound (barium calcium-aluminate, BaO：CaO：Al2O3Mol ratio
For 6：1：2), dipping temperature is 1600 DEG C, and dip time is 60 seconds, and cathode base table is removed with turning processing method after the completion of dipping
The remaining dipping thing in face；
3) molybdenum ruthenium solder pricker will be passed through impregnated of the cathode support cylinder of the cathode base of active material and the heater containing indirect-heating
It is welded together, coat molybdenum ruthenium solder in the cathode base one side relative with heater；Space between cathode base and heater is filled out
Fill high purity aluminium oxide；
4) sub-micron scandium W film is deposited on cathode base surface with magnetically controlled DC sputtering；Will be sub- made from sol-gal process
The Scandia doped tungsten powder of micro-meter scale with 2.5 tons of pressing pressure elder generation compression moldings, burns in 900 DEG C of low temperature afterwards at room temperature
Knot, the target as magnetically controlled DC sputtering；Atmosphere gas is nitrogen, and background vacuum is 5 × 10-4Pa；The diameter 50mm of target；Target
Material and the distance on cathode base surface are 40-50mm；Sputtering power is 120W, is first kept for 4 minutes in sputtering voltage 450V；Exist again
Sputtering voltage 850V is kept for 4 minutes；Finally kept for 40 minutes in sputtering voltage 1250V, obtain submicron film scandium tungsten cathode.Property
Energy test result is similar to Example 1.
Obviously, the above embodiment of the present invention is only intended to clearly illustrate example of the present invention, and is not pair
The restriction of embodiments of the present invention, for those of ordinary skill in the field, may be used also on the basis of the above description
To make other changes in different forms, all embodiments can not be exhaustive here, it is every to belong to this hair
Row of the obvious changes or variations that bright technical scheme is extended out still in protection scope of the present invention.
Claims (13)
1. a kind of preparation method of submicron film scandium tungsten cathode, it is characterised in that comprise the following steps：
1）Tungsten powder is suppressed, sintered, obtains porous tungsten basal body, porous tungsten basal body is passed through and soaks copper, is machined, removes copper, is obtained
Cathode base；
2）Cathode base is impregnated into active material barium calcium aluminium compound；
3）Cathode base impregnated of active material is assembled in the cathode support cylinder containing heater；
4）With magnetically controlled DC sputtering sub-micron scandium W film is deposited on cathode base surface；During magnetically controlled DC sputtering, the original of target
Expect for the Scandia doped tungsten powder of submicron-scale made from sol-gal process；Using ladder making alive mode, first in sputtering electricity
350-450 V are pressed to be kept for 4-6 minutes；Kept for 4-6 minutes in sputtering voltage 750-850V again；Finally in sputtering voltage 1150-
1250V is kept for 40-60 minutes, obtains submicron film scandium tungsten cathode；
Step 1）In, the compacting is to use isostatic pressing technology, and press temperature is room temperature, pressing pressure is 2-2.5 tons；The burning
Knot is sintered in hydrogen atmosphere, and sintering temperature is 1900-2000 DEG C, and sintering time is 40-60 minutes.
A kind of 2. preparation method of submicron film scandium tungsten cathode according to claim 1, it is characterised in that step 2）
In, the barium calcium aluminium compound is barium calcium-aluminate, BaO：CaO：Al2O3Mol ratio be 5：3：2,4：1：1 or 6：1：2；It is described
Dipping temperature is 1500 DEG C -1700 DEG C, and dip time is the 10-120 seconds.
A kind of 3. preparation method of submicron film scandium tungsten cathode according to claim 1, it is characterised in that step 3）
In, suppress evaporation material in the cathode base one side coating relative with heater.
4. the preparation method of a kind of submicron film scandium tungsten cathode according to claim 3, it is characterised in that in negative electrode base
Space filling high purity aluminium oxide between body and heater.
A kind of 5. preparation method of submicron film scandium tungsten cathode according to claim 1, it is characterised in that step 4）
In, the preparation of the target be at room temperature by the Scandia doped tungsten powder of submicron-scale under 2-2.5 ton pressing pressures first
Compression molding, obtained afterwards in 850-950 DEG C of sintering.
A kind of 6. preparation method of submicron film scandium tungsten cathode according to claim 1, it is characterised in that step 4）
In, during magnetically controlled DC sputtering, atmosphere gas is nitrogen, and background vacuum is 5 × 10-4 Pa；The diameter 50mm of target；Target and the moon
The distance of pole matrix surface is 40-50mm；Sputtering power is 100-120W.
A kind of 7. preparation method of submicron film scandium tungsten cathode according to claim 1, it is characterised in that step 4）
In, percentage by weight of the scandium oxide in tungsten powder is 3-10%.
A kind of 8. preparation method of submicron film scandium tungsten cathode according to claim 1, it is characterised in that step 4）
In, using ladder making alive mode, first kept for 5 minutes in sputtering voltage 400V；Kept for 5 minutes in sputtering voltage 800V again；Most
Kept for 45 minutes in sputtering voltage 1200V afterwards, obtain submicron film scandium tungsten cathode.
9. the preparation method of a kind of submicron film scandium tungsten cathode according to claim 1, it is characterised in that including following
Step：
1）High-purity micron order tungsten powder is used into isostatic pressing technology at room temperature, suppressed under 2-2.5 ton pressing pressures；Afterwards in hydrogen
It it is 1900-2000 DEG C in sintering temperature in atmosphere, sintering time is 40-60 minutes to obtain porous tungsten basal body；Copper in temperature
Melt under the conditions of 1400-1500 DEG C, copper is impregnated into porous tungsten basal body using capillarity afterwards；Utilize machining process
Leaching copper tungsten basal body is processed into required shape；The leaching copper tungsten base processed is removed using chemical method or high temperature evaporation method
Copper in body, obtains cathode base；
2）Cathode base is impregnated into active material barium calcium-aluminate, BaO：CaO：Al2O3Mol ratio be 5：3：2,4：1：1 or 6：
1：2, dipping temperature is 1500-1700 DEG C, and dip time is the 10-120 seconds；
3）It will be existed impregnated of the cathode support cylinder of the cathode base of active material and the heater containing indirect-heating by molybdenum ruthenium solder soldering
Together, molybdenum ruthenium solder is coated in the cathode base one side relative with heater；Space filling between cathode base and heater is high
Pure alumina；
4）With magnetically controlled DC sputtering sub-micron scandium W film is deposited on cathode base surface；By sub-micron made from sol-gal process
The Scandia doped tungsten powder of yardstick with the compression molding of 2-2.5 ton pressing pressures elder generation, sinters at 850-950 DEG C afterwards at room temperature,
Target as magnetically controlled DC sputtering；Atmosphere gas is nitrogen, and background vacuum is 5 × 10-4 Pa；The diameter 50mm of target；Target
Distance with cathode base surface is 40-50mm；Sputtering power is 100-120w；First 4-6 is kept in sputtering voltage 350-450 V
Minute；Kept for 4-6 minutes in sputtering voltage 750-850V again；Finally kept for 40-60 minutes in sputtering voltage 1150-1250V, obtained
To submicron film scandium tungsten cathode.
10. the submicron film scandium tungsten cathode as made from claim 1-9 any described preparation methods, it is characterised in that its
Including：Cathode support cylinder, heater, cathode base, active material, sub-micron scandium W film, the active material is to be immersed in the moon
In the matrix of pole, the sub-micron scandium W film is to sputter at cathode base surface, and the cathode base and heater are arranged on negative electrode
Support in cylinder.
11. submicron film scandium tungsten cathode according to claim 10, it is characterised in that the negative electrode also includes suppressing evaporation
Material, suppress evaporation material and be coated in the cathode base back side, face heater.
12. the submicron film scandium tungsten cathode according to claim 11, it is characterised in that the negative electrode also includes high pure zirconia
Aluminium filler, high purity aluminium oxide filler are filled in the space suppressed between evaporation material and heater.
13. submicron film scandium tungsten cathode according to claim 10, it is characterised in that the thickness of sub-micron scandium W film is
200-400nm。
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| CN109390195B (en) * | 2018-11-29 | 2020-11-27 | 北京工业大学 | Scandium-containing cathode at top layer of submicron structure and preparation method thereof |
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