CN105788996A - Sub-micron film scandium-tungsten cathode and preparation method thereof - Google Patents
Sub-micron film scandium-tungsten cathode and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a preparation method of a sub-micron film scandium-tungsten cathode. The preparation method comprises the following steps: pressing and sintering tungsten powder to obtain a cathode matrix; dipping the cathode matrix into an active material barium-calcium-aluminum compound; assembling the cathode matrix dipped with the active material into a cathode support cylinder containing a heater; and depositing a sub-micron scandium-tungsten film on the surface of the cathode matrix in a DC magnetron sputtering manner to obtain the sub-micron film scandium-tungsten cathode. The prepared cathode is high in current density, low in working temperature, long in working time, simple in manufacturing method, high in operability and good in repeatability.
Description
Technical field
The present invention relates to electrovacuum components and parts field.More particularly, to a kind of submicron film scandium tungsten cathode and preparation method thereof.
Background technology
Cathode electronics emitter is through the development in a nearly century, at the Disciplinary Frontiers of many science and technologies in occupation of irreplaceable status.In military, space technology, in the technical field such as electron accelerator and free-electron laser, the demand of low temperature, high current density, high uniform emission and long-life electron emitter is very urgent all the time.Emission p erformance, technology stability and reliability are obviously also particularly significant with production to the development of the electronic device of cost intensive.It is true that vacuum electron device development and performance boost also can be served impetus by the improvement of cathode emitter.Vacuum electron device includes microwave vacuum electronic device, the Theory of Relativity vacuum electron device, vacuum electronic display, vacuum electronic illuminating device and adopts the ionic device etc. of electron source.
In current all kinds of vacuum electron devices, occupy first-selection with the diffused negative electrode that tungsten basal body, alkaline-earth metal barium are active substance, be widely used.The seventies latter stage, rare earth Sc Sc is introduced into this electron emitter and illustrates significantly improving dispenser cathode emitting performance, extensive must pay close attention to thus causing.In more than 20 year thereafter, countries in the world have developed the scandium-containing diffusion cathode of various variant in succession, make work function finally be reduced to 1.5-1.6 electron-volt；When obtaining same electric current density, decline about 200 DEG C than the operating temperature of M type dispenser cathode, greatly increase the performance of electron emitter.
The type of scandium-containing diffusion cathode substantially has following a few class:
1) by Sc2O3It is added on the immersion-type Scandate cathode in dispenser cathode aluminic acid barium salt.Within 1977, being proposed by Philips company, emitting performance is: during operating temperature 1000 DEG C, emission 5A/cm2, about 3000 hours life-spans (US4007393).
2) by Sc2O3It is added on the mixed base in tungsten basal body containing scandium negative electrode.Generally by Sc in this kind of negative electrode2O3With tungsten powder mechanical mixture, repressed, sintering is made containing scandium POROUS TUNGSTEN substrate, and dipping barium aluminate constitutes diffused containing scandium negative electrode subsequently.This cathode form be by Japan Hitachi first proposed in 1984, this negative electrode when operating temperature 850 DEG C, pulsed emission current density 10A/cm2(S.Yamamoto,S.Taguchi,T.Aida,Appl.Surf.Sci.17(1984)504-516)。
3) mixed base " top layer " is containing scandium negative electrode.(J.Hasker, J.VanEsdonkandJ.E.Crombeen.Appl.SurfaceSci.26 (1986) 173.) was announced in 1986 by Philips company.This negative electrode is to be placed on common porous tungsten body by the porous tungsten body containing scandium that 0.1mm is thick, constitutes containing scandium " top layer ", then impregnates aluminate.It has launching favourable containing scandium surface, remain simultaneously can ample supply and at the bottom of storing the common porous tungstenio of activity barium, thus improving the performance of negative electrode.But due to its complex process, it is not suitable for explained hereafter.Then, Philips company proceeds to mixed base negative electrode research (U.vanSlooten again in nineteen ninety, PeterA.DuineAppl.Surf.Sci.111 (1997) 24-29), the impulse ejection ability of the negative electrode obtained is 1000 DEG C in operating temperature and has reached 100A/cm2。
4) film type " top layer " is containing scandium negative electrode.It is with depositing the one layer of method realization containing the scandium thin film interpolation containing scandium " top layer " on conventional impregnation type dispenser cathode.The method of deposition can be radio-frequency sputtering (YamamotoS, TaguchiSandAidaTetal.Appl.SurfaceSci.17 (1986) 517) or laser evaporation (CN1128403A), and the thin film of deposition can be W+Sc2O3、W+Sc2W3O12(S.Yamamoto, I.Watanabe, S.Taguchietal, 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 " can introduce containing scandium negative electrode have certain thickness uniform deposition containing scandium thin film.The research of scandium series cathode is shown, if the Sc of cathode surface exists with elementary state, is do not have contributive to transmitting, only when Sc is oxidation state, the work function of negative electrode can be made in activation process subsequently to reduce.So, the technology key of film type scandium series cathode must is fulfilled for following 2 points: 1) covering of thin film can not change the conductive characteristic on former impregnated cathode surface；2) Sc in thin film must be that oxidation state exists[.Existing film type " top layer " containing scandium negative electrode introduce have certain thickness uniform deposition containing scandium thin film, but radio-frequency sputtering can cause the decomposition of Scia in target, so that the Sc in thin film is oxidation state, system must being filled oxygen and strict control partial pressure, this makes the control of the condition to spatter film forming become extremely difficult；And although laser evaporization method has and Sc can be made to keep complete oxidation state in film without system is introduced active gases, but its complex manufacturing technology, poor controllability.Additionally, JP Laid-Open 6-260084 and CN102522281 discloses the use of d.c. sputtering to prepare film type scandium series cathode.
The above negative electrode containing scandium all exists: 1) diffusion of scandium and oxide thereof is bad, makes to supplement difficulty.When high temperature evaporation or when bearing ion bom bardment and lose, it is difficult to be restored, directly affect transmitting and the life-span of negative electrode；2) scandium added or its oxide skewness, thus causing transmitting uneven；3) complex process, and poor repeatability.
Accordingly, it would be desirable to a kind of method that new preparation is containing scandium negative electrode, it is to avoid aforementioned defect.
Summary of the invention
It is an object of the present invention to provide a kind of submicron film scandium tungsten cathode.
Further object is that the preparation method that above-mentioned submicron film scandium tungsten cathode is provided.
For reaching above-mentioned purpose, the present invention adopts following technical proposals:
The preparation method of a kind of submicron film scandium tungsten cathode, comprises the following steps:
1) tungsten powder suppressed, sinter, obtain cathode base；
2) by impregnated activated for cathode base material barium calcium aluminium compound；
3) cathode base that impregnated of active substance is assembled in the cathode support cylinder containing heater；
4) with magnetically controlled DC sputtering at cathode base surface deposition submicron scandium W film；During magnetically controlled DC sputtering, the raw material of target is the Scandia doped tungsten powder of the submicron-scale that sol-gal process prepares；Adopt ladder making alive mode, first keep 4-6 minute at sputtering voltage 350-450V；Keep 4-6 minute at sputtering voltage 750-850V again；Last sputtering voltage 1150-1250V maintenance 40-60 minute, obtain submicron film scandium tungsten cathode.
Step 1) in, tungsten powder is high-purity micron order tungsten powder；Described compacting is to adopt isostatic pressing technology, and press temperature is room temperature, pressing pressure is 2-2.5 ton；Described sintering is to sinter in hydrogen atmosphere, and sintering temperature is 1900-2000 DEG C, and sintering time is 40-60 minute.
Obtain POROUS TUNGSTEN matrix after sintering, by POROUS TUNGSTEN matrix through soaking copper, machining, removing copper, obtain cathode base；Described leaching copper is that copper is melted under temperature 1400-1500 DEG C of condition, utilizes capillarity to be impregnated in POROUS TUNGSTEN matrix by copper afterwards；Described machining is to utilize the processing method such as car system, electric spark that leaching copper tungsten basal body is processed into required shape, concrete steps and condition to be referred to existing document；Described to remove copper be the copper utilizing chemical method or high temperature evaporation method to remove in the leaching copper tungsten basal body processed, and concrete steps and condition are referred to existing document.
Step 2) in, barium calcium aluminium compound can be barium calcium-aluminate, it is also possible to be other stable barium calcium aluminium compound.
When barium calcium aluminium compound is barium calcium-aluminate, BaO:CaO:Al2O3Mol ratio be 5:3:2,4:1:1 or 6:1:2.
Described dipping temperature is 1500 DEG C-1700 DEG C, and dip time is the 10-120 second.After dipping, the remnants removing cathode base surface with turning processing method impregnate thing.
Step 3) in, heater is indirect-heating heater.
Cathode base and cathode support cylinder are to be brazed together by brazing material.
Preferably, it is coated with suppression evaporation material in the one side that cathode base is relative with heater.Suppress evaporation material identical with the brazing material between cathode base and cathode support cylinder, for molybdenum ruthenium solder.Soldering between cathode base and cathode support cylinder, the coating of suppression evaporation material are to complete in hydrogen stove simultaneously.Suppress evaporation material for sealing the hole at the cathode base back side, it is prevented that barium calcium aluminium compound evaporates to heater.
Preferably, high purity aluminium oxide is filled in the space between cathode base and heater.Directly transfer heat to cathode base by heat exchange pattern after high purity aluminium oxide implant is sintered, improve the efficiency of heating surface and temperature homogeneity.
Step 4) in, the target raw material used by magnetically controlled DC sputtering does not adopt the mechanical impurity of general tungsten powder and Scia powder, but adopts the Scandia doped tungsten powder of submicron-scale that sol-gal process prepares.
Being prepared by the Scandia doped tungsten powder elder generation compression molding of submicron-scale of described target, then low-temperature sintering.Described compression molding is at room temperature the Scandia doped tungsten powder powder body of appropriate submicron-scale to be inserted target holder, uses hand press to carry out just one-step forming, and pressing pressure is 2-2.5 ton；Described low-temperature sintering is in a vacuum furnace the target of first one-step forming to be sintered to 850-950 DEG C, makes to target type.This is almost constant owing to must assure that the chemical state of scandium and powder body size in sputtering, and the surface activity between the powder granule of submicron-scale strengthens, frictional force between powder, the frictional force between powder and mold wall is relative with viscosity resistance increases, molding relative difficulty.
During magnetically controlled DC sputtering, atmosphere gas is nitrogen, and background vacuum is 5 × 10-4Pa；The diameter 50mm of target；The distance on target and cathode base surface is 40-50mm；Sputtering power is 100-120W.
The pressed by powder target adopting the present invention obtains scandium W film by specific dc sputtering processes deposition, can make Scia being more evenly distributed at cathode surface, significantly reduce the work function of cathode surface, improve emission and the emission uniformity of negative electrode.
Preferably, Scia percentage by weight in tungsten powder is 3-10%, more preferably 5%.Scia content is high, can improve the anti-ion bom bardment ability of negative electrode, thus improving the life-span of negative electrode.
Preferably, adopt ladder making alive mode, first keep 5 minutes at sputtering voltage 400V；Keep 5 minutes at sputtering voltage 800V again；Last sputtering voltage 1200V maintenance 45 minutes, obtain submicron film scandium tungsten cathode.
The present invention also provides for the submicron film scandium tungsten cathode prepared by above-mentioned preparation method, comprising: cathode support cylinder, heater, cathode base, active substance, submicron scandium W film, described active substance is to be immersed in cathode base, described submicron scandium W film is to sputter at cathode base surface, and described cathode base and heater are arranged in cathode support cylinder.
Preferably, described negative electrode also includes suppressing evaporation material, it is suppressed that evaporation material is coated in the cathode base back side, faces heater.
Preferably, described negative electrode also includes high purity aluminium oxide implant, and high purity aluminium oxide implant is filled in the space suppressed between evaporation material and heater.
Preferably, the thickness of submicron scandium W film is 200-400nm.
Beneficial effects of the present invention is as follows:
The present invention prepares the target of magnetically controlled DC sputtering by adopting the repressed sintering of submicron material keeping granular size almost constant, and strictly control the parameters of each step to make Scia evenly be distributed on cathode base surface, the electric current density of the negative electrode that the present invention prepares is big, it is believed that the highest electric current density is about 85.08A/cm when 1000 DEG C2And operating temperature ratio can be made under same electric current density to cover osmium film negative electrode reduction about 200 DEG C, and the activationary time needed is only 10-30 minute, the seasoned time is only about 24 hours, the work function of cathode surface, up to 3000 hours, is reduced 0.2-0.4eV by the working time.
The controllability of the present invention is strong, it is not necessary to be filled with active gases such as O to system2Complete oxidation state is kept etc. the scandium element that can make in scandium tungsten film.
The manufacture method of the present invention is simple, workable, reproducible.
Accompanying drawing explanation
Below in conjunction with accompanying drawing, the specific embodiment of the present invention is described in further detail.
Fig. 1 is the submicron film for preparing of the present invention schematic diagram containing scandium negative electrode.
Fig. 2 is the powder granularity scattergram of the Scandia doped tungsten powder prepared in embodiment 1.
Fig. 3 is the powder body XRD figure of the Scandia doped tungsten powder prepared in embodiment 1.
Fig. 4 is the SEM figure of submicron scandium W film.
Fig. 5 is the XPS spectrum figure of Scia in submicron scandium W film.
Fig. 6 is the emission figure that the negative electrode of embodiment 1 is tested in water-cooled anode diode.
Fig. 7 covers the emission figure that osmium film negative electrode is tested in water-cooled 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 cylinder, 2-indirect-heating heater, 3-cathode base, 4-active substance, 5-submicron scandium W film, 6-suppresses evaporation material, 7-high purity aluminium oxide implant.
Detailed description of the invention
In order to be illustrated more clearly that the present invention, below in conjunction with preferred embodiment, the present invention is described further.It will be appreciated by those skilled in the art that following specifically described content is illustrative and be not restrictive, should not limit the scope of the invention with this.
Embodiment 1
The preparation method of a kind of submicron film scandium tungsten cathode, comprises the following steps:
1) high-purity micron order tungsten powder is first adopted isostatic pressing technology at room temperature, suppress under 2 tons of pressing pressures；Afterwards in hydrogen atmosphere, being 1900 DEG C in sintering temperature, sintering time is obtain POROUS TUNGSTEN matrix in 40 minutes；Copper is melted under 1400 DEG C of conditions of temperature, utilizes capillarity to be impregnated in POROUS TUNGSTEN matrix by copper afterwards；The processing method such as the car system of utilization, electric spark is processed into required shape leaching copper tungsten basal body；Utilize chemical method or high temperature evaporation method to remove the copper in the leaching copper tungsten basal body processed, obtain cathode base；
2) by impregnated activated for cathode base material barium calcium aluminium compound (barium calcium-aluminate, BaO:CaO:Al2O3Mol ratio be 5:3:2), dipping temperature is 1500 DEG C, and dip time is 10 seconds, after having impregnated with turning processing method remove cathode base surface remnants impregnate thing；
3) cathode base of active substance will be impregnated of and the cathode support cylinder containing indirect-heating heater is brazed together by molybdenum ruthenium solder, at the one side coating molybdenum ruthenium solder that cathode base is relative with heater；High purity aluminium oxide is filled in space between cathode base and heater；
4) with magnetically controlled DC sputtering at cathode base surface deposition submicron scandium W film；The Scandia doped tungsten powder of the submicron-scale prepared by sol-gal process is at room temperature with the compression molding of 2 tons of pressing pressure elder generations, afterwards 850 DEG C of low-temperature sinterings, as the target of magnetically controlled DC sputtering；Atmosphere gas is nitrogen, and background vacuum is 5 × 10-4Pa；The diameter 50mm of target；The distance on target and cathode base surface is 40mm；Sputtering power is 100W, first keeps 5 minutes at sputtering voltage 400V；4 clocks are kept again at sputtering voltage 800V；Last sputtering voltage 1200V maintenance 45 minutes, obtain submicron film scandium tungsten cathode.
Fig. 1 is the submicron film for preparing of the present invention schematic diagram containing scandium negative electrode.
Fig. 2 is the powder granularity scattergram of the Scandia doped tungsten powder prepared in embodiment 1.It can be seen that adopt the even particle size distribution of Scandia doped tungsten powder of submicron-scale that sol-gal process prepares, powder granule is shaped as torispherical, and diameter of particle distribution meets desirable quasi normal distribution.
Fig. 3 is the powder body XRD figure of the Scandia doped tungsten powder prepared in embodiment 1.It can be seen that Sc is oxidation state (Scia) and temperature independent (when temperature, when 1100 DEG C, 1200 DEG C, 1300 DEG C, 1500 DEG C and 1700 DEG C, collection of illustrative plates is all overlap) from figure.
Fig. 4 is the SEM figure of submicron scandium W film.
Fig. 5 is the XPS spectrum figure of Scia in submicron scandium W film, and spectral peak is positioned near 402.2eV, it was shown that scandium is present in thin film with titanium oxide.
At pulsewidth 5-25 μ s, when repetition rate 100-500Hz, the cathode emission current density of the negative electrode of the test present invention, as shown in Figure 6: when 900 DEG C, the keen current density of its transmitting after cathode stabilization is better than 30A/cm2；Curve 1000 DEG C corresponding, owing to test power supply can only achieve 2700V, does not therefore obtain keen current density, and the highest electric current density is about 85.08A/cm2.Visible, this negative electrode has significantly high emission current densities, hence it is evident that higher than M type negative electrode and Scandate cathode.
Fig. 7 covers the emission figure that osmium film negative electrode is tested in water-cooled anode diode, it can be seen that the common osmium film negative electrode that covers is when 1100 DEG C, and the keen current density of its transmitting is about 30A/cm2。
U.S. SLAC adopt electron gun the negative electrode of the present invention is tested, test result such as Fig. 8: 1050 DEG C time, the keen current density of its transmitting after cathode stabilization is better than 100A/cm2。
The work function of cathode surface is reduced 0.2-0.4eV by the method for the present invention, and the activationary time that prepared negative electrode needs is only 10-30 minute, and the seasoned time is only about 24 hours, but the working time was up to 3000 hours.
Embodiment 2
The preparation method of a kind of submicron film scandium tungsten cathode, comprises the following steps:
1) high-purity micron order tungsten powder is first adopted isostatic pressing technology at room temperature, suppress under 2 tons of pressing pressures；Afterwards in hydrogen atmosphere, being 2000 DEG C in sintering temperature, sintering time is obtain POROUS TUNGSTEN matrix in 60 minutes；Copper is melted under 1500 DEG C of conditions of temperature, utilizes capillarity to be impregnated in POROUS TUNGSTEN matrix by copper afterwards；The processing method such as the car system of utilization, electric spark is processed into required shape leaching copper tungsten basal body；Utilize chemical method or high temperature evaporation method to remove the copper in the leaching copper tungsten basal body processed, obtain cathode base；
2) by impregnated activated for cathode base material barium calcium aluminium compound (barium calcium-aluminate, BaO:CaO:Al2O3Mol ratio be 4:1:1), dipping temperature is 1700 DEG C, and dip time is 120 seconds, after having impregnated with turning processing method remove cathode base surface remnants impregnate thing；
3) cathode base of active substance will be impregnated of and the cathode support cylinder containing indirect-heating heater is brazed together by molybdenum ruthenium solder, at the one side coating molybdenum ruthenium solder that cathode base is relative with heater；High purity aluminium oxide is filled in space between cathode base and heater；
4) with magnetically controlled DC sputtering at cathode base surface deposition submicron scandium W film；The Scandia doped tungsten powder of the submicron-scale prepared by sol-gal process is at room temperature with the compression molding of 2.5 tons of pressing pressure elder generations, afterwards 950 DEG C of low-temperature sinterings, as the target of magnetically controlled DC sputtering；Atmosphere gas is nitrogen, and background vacuum is 5 × 10-4Pa；The diameter 50mm of target；The distance on target and cathode base surface is 50mm；Sputtering power is 120W, first keeps 6 minutes at sputtering voltage 350V；Keep 6 minutes at sputtering voltage 750V again；Last sputtering voltage 1150V maintenance 60 minutes, obtain submicron film scandium tungsten cathode.The performance test results is similar to Example 1.
Embodiment 3
The preparation method of a kind of submicron film scandium tungsten cathode, comprises the following steps:
1) high-purity micron order tungsten powder is first adopted isostatic pressing technology at room temperature, suppress under 2.5 tons of pressing pressures；Afterwards in hydrogen atmosphere, being 2000 DEG C in sintering temperature, sintering time is obtain POROUS TUNGSTEN matrix in 50 minutes；Copper is melted under 1500 DEG C of conditions of temperature, utilizes capillarity to be impregnated in POROUS TUNGSTEN matrix by copper afterwards；The processing method such as the car system of utilization, electric spark is processed into required shape leaching copper tungsten basal body；Utilize chemical method or high temperature evaporation method to remove the copper in the leaching copper tungsten basal body processed, obtain cathode base；
2) by impregnated activated for cathode base material barium calcium aluminium compound (barium calcium-aluminate, BaO:CaO:Al2O3Mol ratio be 6:1:2), dipping temperature is 1600 DEG C, and dip time is 60 seconds, after having impregnated with turning processing method remove cathode base surface remnants impregnate thing；
3) cathode base of active substance will be impregnated of and the cathode support cylinder containing indirect-heating heater is brazed together by molybdenum ruthenium solder, at the one side coating molybdenum ruthenium solder that cathode base is relative with heater；High purity aluminium oxide is filled in space between cathode base and heater；
4) with magnetically controlled DC sputtering at cathode base surface deposition submicron scandium W film；The Scandia doped tungsten powder of the submicron-scale prepared by sol-gal process is at room temperature with the compression molding of 2.5 tons of pressing pressure elder generations, afterwards 900 DEG C of low-temperature sinterings, as the target of magnetically controlled DC sputtering；Atmosphere gas is nitrogen, and background vacuum is 5 × 10-4Pa；The diameter 50mm of target；The distance on target and cathode base surface is 40-50mm；Sputtering power is 120W, first keeps 4 minutes at sputtering voltage 450V；Keep 4 minutes at sputtering voltage 850V again；Last sputtering voltage 1250V maintenance 40 minutes, obtain submicron film scandium tungsten cathode.The performance test results is similar to Example 1.
Obviously; the above embodiment of the present invention is only for clearly demonstrating example of the present invention; and be not the restriction to embodiments of the present invention; for those of ordinary skill in the field; can also make other changes in different forms on the basis of the above description; here cannot all of embodiment be given exhaustive, every belong to apparent change that technical scheme extended out or the variation row still in protection scope of the present invention.
Claims (10)
1. the preparation method of a submicron film scandium tungsten cathode, it is characterised in that comprise the following steps:
1) tungsten powder suppressed, sinter, obtain cathode base；
2) by impregnated activated for cathode base material barium calcium aluminium compound；
3) cathode base that impregnated of active substance is assembled in the cathode support cylinder containing heater；
4) with magnetically controlled DC sputtering at cathode base surface deposition submicron scandium W film；During magnetically controlled DC sputtering, the raw material of target is the Scandia doped tungsten powder of the submicron-scale that sol-gal process prepares；Adopt ladder making alive mode, first keep 4-6 minute at sputtering voltage 350-450V；Keep 4-6 minute at sputtering voltage 750-850V again；Last sputtering voltage 1150-1250V maintenance 40-60 minute, obtain submicron film scandium tungsten cathode.
2. the preparation method of a kind of submicron film scandium tungsten cathode according to claim 1, it is characterised in that step 1) in, described compacting is to adopt isostatic pressing technology, and press temperature is room temperature, pressing pressure is 2-2.5 ton；Described sintering is to sinter in hydrogen atmosphere, and sintering temperature is 1900-2000 DEG C, and sintering time is 40-60 minute.
3. the preparation method of a kind of submicron film scandium tungsten cathode according to claim 1, it is characterised in that step 2) in, described barium calcium aluminium compound is barium calcium-aluminate, BaO:CaO:Al2O3Mol ratio be 5:3:2,4:1:1 or 6:1:2；Described dipping temperature is 1500 DEG C-1700 DEG C, and dip time is the 10-120 second.
4. the preparation method of a kind of submicron film scandium tungsten cathode according to claim 1, it is characterised in that step 3) in, the one side coating relative with heater at cathode base suppresses evaporation material；
Preferably, high purity aluminium oxide is filled in the space between cathode base and heater.
5. the preparation method of a kind of submicron film scandium tungsten cathode according to claim 1, it is characterized in that, step 4) in, being prepared by of described target, at room temperature by the first compression molding under 2-2.5 ton pressing pressure of the Scandia doped tungsten powder of submicron-scale, obtains at 850-950 DEG C of sintering afterwards.
6. the preparation method of a kind 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 × 10-4Pa；The diameter 50mm of target；The distance on target and cathode base surface is 40-50mm；Sputtering power is 100-120W.
7. the preparation method of a kind of submicron film scandium tungsten cathode according to claim 1, it is characterised in that step 4) in, Scia percentage by weight in tungsten powder is 3-10%, more preferably 5%.
8. the preparation method of a kind of submicron film scandium tungsten cathode according to claim 1, it is characterised in that step 4) in, adopt ladder making alive mode, first keep 5 minutes at sputtering voltage 400V；Keep 5 minutes at sputtering voltage 800V again；Last sputtering voltage 1200V maintenance 45 minutes, 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 comprise the following steps:
1) high-purity micron order tungsten powder is adopted isostatic pressing technology at room temperature, suppress under 2-2.5 ton pressing pressure；Afterwards in hydrogen atmosphere, being 1900-2000 DEG C in sintering temperature, sintering time is within 40-60 minute, obtain POROUS TUNGSTEN matrix；Copper is melted under temperature 1400-1500 DEG C of condition, utilizes capillarity to be impregnated in POROUS TUNGSTEN matrix by copper afterwards；Utilize machining process that leaching copper tungsten basal body is processed into required shape；Utilize chemical method or high temperature evaporation method to remove the copper in the leaching copper tungsten basal body processed, obtain cathode base；
2) by impregnated activated for cathode base 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 second；
3) cathode base of active substance will be impregnated of and the cathode support cylinder containing indirect-heating heater is brazed together by molybdenum ruthenium solder, at the one side coating molybdenum ruthenium solder that cathode base is relative with heater；High purity aluminium oxide is filled in space between cathode base and heater；
4) with magnetically controlled DC sputtering at cathode base surface deposition submicron scandium W film；The Scandia doped tungsten powder of the submicron-scale prepared by sol-gal process is at room temperature with the compression molding of 2-2.5 ton pressing pressure elder generation, afterwards at 850-950 DEG C of sintering, as the target of magnetically controlled DC sputtering；Atmosphere gas is nitrogen, and background vacuum is 5 × 10-4Pa；The diameter 50mm of target；The distance on target and cathode base surface is 40-50mm；Sputtering power is 100-120w；First keep 4-6 minute at sputtering voltage 350-450V；Keep 4-6 minute at sputtering voltage 750-850V again；Last sputtering voltage 1150-1250V maintenance 40-60 minute, obtain submicron film scandium tungsten cathode.
10. the submicron film scandium tungsten cathode prepared by the arbitrary described preparation method of claim 1-9, it is characterized in that, comprising: cathode support cylinder, heater, cathode base, active substance, submicron scandium W film, described active substance is to be immersed in cathode base, described submicron scandium W film is to sputter at cathode base surface, and described cathode base and heater are arranged in cathode support cylinder；
Preferably, described negative electrode also includes suppressing evaporation material, it is suppressed that evaporation material is coated in the cathode base back side, faces heater；
Preferably, described negative electrode also includes high purity aluminium oxide implant, and high purity aluminium oxide implant is filled in the space suppressed between evaporation material and heater；
Preferably, the thickness of submicron scandium W film is 200-400nm.
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| CN108436079A (en) * | 2018-03-15 | 2018-08-24 | 北京矿冶科技集团有限公司 | A kind of preparation method of hole even porous tungsten |
| CN109390195A (en) * | 2018-11-29 | 2019-02-26 | 北京工业大学 | A kind of submicrometer structure top layer cathode containing scandium and preparation method thereof |
| CN114340124A (en) * | 2021-12-30 | 2022-04-12 | 中国科学院合肥物质科学研究院 | Sodium ion emitter and preparation method thereof |
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