CN108394922A - A kind of simple preparation method of hot cathode aluminate electronic emitting material - Google Patents
A kind of simple preparation method of hot cathode aluminate electronic emitting material Download PDFInfo
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- CN108394922A CN108394922A CN201810307397.7A CN201810307397A CN108394922A CN 108394922 A CN108394922 A CN 108394922A CN 201810307397 A CN201810307397 A CN 201810307397A CN 108394922 A CN108394922 A CN 108394922A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/16—Preparation of alkaline-earth metal aluminates or magnesium aluminates; Aluminium oxide or hydroxide therefrom
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J1/00—Details of electrodes, of magnetic control means, of screens, or of the mounting or spacing thereof, common to two or more basic types of discharge tubes or lamps
- H01J1/02—Main electrodes
- H01J1/13—Solid thermionic cathodes
- H01J1/14—Solid thermionic cathodes characterised by the material
- H01J1/142—Solid thermionic cathodes characterised by the material with alkaline-earth metal oxides, or such oxides used in conjunction with reducing agents, as an emissive material
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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Abstract
A kind of simple preparation method of hot cathode aluminate electronic emitting material, belongs to the preparing technical field of hot-cathode electric emissive material, with Ba (NO3)2、Ca(NO3)2·4H20 and Al (NO3)3·9H2O is raw material, and using EDTA as complexing agent, the Precursor Powder of salt is made by sol-gal process, Precursor Powder is roasted to obtain final aluminate, cathode is after fully activation at 950 DEG CbUnder, pulsed emission current density can reach 100A/cm2More than, emit 1.4 or more slope.Have many advantages, such as that preparation process is simple, ingredient is uniform, object is mutually single, fusing point is low, emitting performance is good using the aluminate that the method is prepared.It is expected to be applied to the fields such as microwave vacuum electronic device.
Description
Technical field
The present invention relates to a kind of hot cathode simple preparation methods of aluminate electronic emitting material, and in particular to it is a kind of with
EDTA is the preparation method for the aluminate that complexing agent provides excellent primary electron emitting performance using sol-gel and roasting,
Belong to the preparing technical field of primary electron transmitting hot cathode material.
Background technology
Vacuum electron device is in broadcast, TV, radio communication, space navigation, electronic countermeasure, modern industry sensing heating
Etc. play an important role in national economy field.Electron source of the cathode as vacuum electron device, directly decides vacuum
The characteristic and service life of electronic device.Currently, vacuum electron device usually uses hot cathode material, but China's system at present
There are a certain distance compared with external for standby emission p erformance, are mainly reflected in the preparation of aluminate electronic emitting material
On, cause emitting performance relatively poor, evaporation is very fast, seriously affects the overall performance of device.For aluminate, front axle shell
Last common preparation method mainly has solid phase mechanical mixture and coprecipitation, using different preparation methods for finally preparing
Obtained object phase composition has prodigious influence, and when the aluminate that roasting obtains is closer to a kind of only object phase,
There can be better emission p erformance.The aluminate of different formulations can obtain low melting point eutectic using preparation process appropriate
Body --- calcium aluminate barium salt, such as Ba3CaAl2O7, Ba5CaAl4O12, the work function of cathode can be effectively reduced, is ensureing that cathode is good
Make the evaporation rate of cathode lower while emitting performance.Identical in aluminate formula, main phase is
Ba5CaAl4O12Calcium aluminate barium salt have dipping temperature it is low, activationary time is short, evaporates small feature, this be also weigh aluminate
A good and bad standard.Experiment shows the aluminate synthesized using mechanical mixing due to being influenced by initial feed granularity,
So that product particle size is big and more uneven, reactivity is relatively low, and it is very uniformly, significantly to be mixed during mechanical batch mixing not
Influence the emitting performance of cathode.Compared with mechanical mixing, the advantages of liquid-phase coprecipitation, is embodied in each component mixing more
Uniformly, the particle of mixed powder is more tiny, specific surface area bigger, and reactivity higher is conducive to firing stage solid phase reaction
Abundant progress, and the structure of synthetic product, than more uniform, still, liquid-phase coprecipitation disadvantage is that use scope is narrow,
When being co-precipitated aluminate Precursor Powder, the Al (OH) of generation is precipitated3Yi Shuan is hydrolyzed, so needing stringent note when adding precipitating reagent
Meaning additive amount, solution, which crosses alkali, can make Al3+It dissolves again.
Invention content
The aluminate granularity that is finally prepared for traditional mechanical mixing and coprecipitation is larger, object is not mutually single
One and the deficiencies of relatively low more and emitting performance, the present invention uses sol-gel process, with Ba (NO3)2、Ca(NO3)2·
4H20 and Al (NO3)3·9H2O is raw material, and using EDTA as complexing agent, the Precursor Powder of salt is made by sol-gel method, will before
Powder is driven to roast to obtain final aluminate.By adjusting suitable solution concentration, bath temperature and sintering temperature etc., finally
Successfully prepare that ingredient is uniform, fusing point is low, product structure aluminate more good than more uniform and emitting performance.The present invention provides
A kind of preparation process is simple, fusing point is low, phase structure is single and the preparation side of the good emission of cathode material of emitting performance
Method.
A kind of hot cathode provided by the present invention is passed through with the simple preparation method of aluminate electronic emitting material with lower section
Formula is realized：
A. by Ba (NO3)2、Ca(NO3)2·4H20 and Al (NO3)3·9H2O raw materials are dissolved in deionization respectively by a certain percentage
It is uniform that respective solution ＆ stir is configured in water；Complexing agent EDTA is dissolved in ammonium hydroxide；
B. scandium nitrate solution, calcium nitrate solution and aluminum nitrate solution that step A is prepared are mixed and puts mixed solution
Enter in water-bath and heat, then EDTA solution is gradually added into wherein, is stirred continuously in heating process, until leucosol is formed, it will
This colloidal sol, which is fully dried, goes moisture removal to form xerogel；
C. the obtained xerogel of step B is positioned in Muffle furnace and carries out preliminary exposition and removes ammonium hydroxide and uncomplexed
EDTA；
D. the Precursor Powder that step C is decomposed is sintered in high temperature tungsten net hydrogen furnace pure hydrogen atmosphere, final
To emission of cathode substance aluminate.
In above method step A, the preferably described raw material Ba (NO3)2、Ca(NO3)2·4H20 and Al (NO3)3·9H2O's rubs
You are than being 4：1：2 or 6：1：4 or 5：3：4, purity is that analysis is pure.
In above method step A, the barium nitrate solution of the preparation, calcium nitrate solution, aluminum nitrate solution concentration control
System is conducive to dissolve full and uniform within the scope of 0.2mol/L~0.5mol/L；EDTA per 100g, which is corresponded to, uses 50~100ml
Ammonium hydroxide fully dissolved.
In above method step B, the heating water bath is to control bath temperature within the scope of 70 DEG C~90 DEG C, will after colloidal sol
It is positioned in 120 DEG C of baking ovens and is dried into gel；Ba (NO in mixed solution3)2、Ca(NO3)2·4H20 and Al (NO3)3·9H2O
The molar ratio of comprehensive molal quantity and EDTA are (0.8-1.2):1.
In above method step C, the decomposition step is to adjust decomposition temperature to 700 DEG C~900 DEG C ranges, when heat preservation
Between determined according to product is how many, main purpose is that ammonium hydroxide and remaining EDTA are decomposed and is discharged；By the powder after decomposition
End is ground, sieves, and is stored in after 100 mesh excessively or 200 mesh sieve to be used in drying cupboard.
In above method step D, the step that is sintered in high temperature tungsten net hydrogen furnace is to adjust sintering temperature
Within the scope of 1300 DEG C~1600 DEG C, soaking time is 2~8h.
In above method step D, the high-purity hydrogen a concentration of 99.999% of the pure hydrogen atmosphere.
With preparation process, simple, ingredient is uniformly, object is mutually single, fusing point is low for the aluminate that the present invention is finally prepared,
The advantages that emitting performance is good impregnates the cathode after this kind of aluminate after fully activation at 950 DEG CbUnder, pulsed emission current is close
Degree can reach 100A/cm2More than, emit 1.4 or more slope.
Description of the drawings
Fig. 1 is the SEM patterns of the made aluminate Precursor Powder of embodiment 1；
Fig. 2 is the SEM patterns of the made aluminate of embodiment 1；
Fig. 3 is the SEM patterns of the made aluminate of embodiment 3；
Fig. 4 is the XRD diagram of the made aluminate of embodiment 2；
Fig. 5 is the XRD diagram of the made aluminate of embodiment 4；
Fig. 6 be embodiment 1 dipping after cathode pulsed emission current density I-V characteristic curve；
Fig. 7 be embodiment 2 dipping after cathode pulsed emission current density I-V characteristic curve；
Fig. 8 be embodiment 3 dipping after cathode pulsed emission current density I-V characteristic curve；
Fig. 9 be embodiment 4 dipping after cathode pulsed emission current density I-V characteristic curve.
Specific implementation mode
With reference to embodiment, the invention will be further described, but the present invention is not limited to following embodiments.
Embodiment 1
Ba (the NO of 52.3g are weighed respectively3)2, 11.8g Ca (NO3)2·4H2Al (the NO of 0 and 37.5g3)3·9H2O etc.
Raw material, three's molar ratio are 4：1：2, it is dissolved into the deionized water of 2L and forms nitrate solution, and weigh 102.3g
EDTA and be dissolved in the ammonium hydroxide of 100ml.Nitrate solution is put into water-bath and is heated to 80 DEG C, while EDTA is molten
Liquid is slowly added into wherein, is heated and is stirred continuously to form colloidal sol, is positioned in 120 DEG C of baking ovens and moisture removal is gone to form xerogel, and
It is put in Muffle furnace and is decomposed again, decomposition temperature is 800 DEG C, keeps the temperature 4h.Obtained Precursor Powder pattern such as Fig. 1 institutes
Show, 200 mesh standard sieve of polished mistake, after put it into high temperature hydrogen furnace hydrogen environment and be sintered, 1400 DEG C of setting
Sintering temperature, keep the temperature 4h after take out obtain aluminate, microscopic appearance is as shown in Figure 2.The cathode dipping aluminate only needs 1600
DEG C, and after cathode fully activates, at 950 DEG CbUnder, pulsed emission current density has reached 102.29A/cm2, emitting slope is
1.423 as shown in Figure 6.
Embodiment 2
Ba (the NO of 52.3g are weighed respectively3)2, 11.8g Ca (NO3)2·4H2Al (the NO of 0 and 37.5g3)3·9H2O etc.
Raw material, three's molar ratio are 4：1：2, it is dissolved into the deionized water of 2L and forms nitrate solution, and weigh 102.3g
EDTA and be dissolved in the ammonium hydroxide of 100ml.Nitrate solution is put into water-bath and is heated to 80 DEG C, while EDTA is molten
Liquid is slowly added into wherein, is heated and is stirred continuously to form colloidal sol, is positioned in 120 DEG C of baking ovens and moisture removal is gone to form xerogel, and
It is put in Muffle furnace and is decomposed again, decomposition temperature is 800 DEG C, keeps the temperature 4h.The polished mistake of obtained Precursor Powder 200
Mesh standard sieve, after put it into high temperature hydrogen furnace hydrogen environment and be sintered, the sintering temperature of 1500 DEG C of setting, after keeping the temperature 4h
Taking-up obtains aluminate, and material phase analysis is as shown in Figure 4.The cathode dipping aluminate only needs 1600 DEG C, and cathode fully swashs
After work, at 950 DEG CbUnder, pulsed emission current density has reached 107.81A/cm2, transmitting slope is 1.423, as shown in Figure 7.
Embodiment 3
Ba (the NO of 52.3g are weighed respectively3)2, 7.9g Ca (NO3)2·4H2Al (the NO of 0 and 50.0g3)3·9H2O etc.
Raw material, three's molar ratio are 6：1：4, it is dissolved into the deionized water of 2L and forms nitrate solution, and weigh 102.3g
EDTA and be dissolved in the ammonium hydroxide of 100ml.Nitrate solution is put into water-bath and is heated to 80 DEG C, while EDTA is molten
Liquid is slowly added into wherein, is heated and is stirred continuously to form colloidal sol, is positioned in 120 DEG C of baking ovens and moisture removal is gone to form xerogel, and
It is put in Muffle furnace and is decomposed again, decomposition temperature is 800 DEG C, keeps the temperature 4h.The polished mistake of obtained Precursor Powder 200
Mesh standard sieve, after put it into high temperature hydrogen furnace hydrogen environment and be sintered, the sintering temperature of 1400 DEG C of setting, after keeping the temperature 4h
Taking-up obtains aluminate, and microscopic appearance is as shown in Figure 3.The cathode dipping aluminate only needs 1625 DEG C, and cathode fully swashs
After work, at 950 DEG CbUnder, pulsed emission current density has reached 101.75A/cm2, transmitting slope is 1.430, as shown in Figure 8.
Embodiment 4
Ba (the NO of 52.3g are weighed respectively3)2, 7.9g Ca (NO3)2·4H2Al (the NO of 0 and 50.0g3)3·9H2O etc.
Raw material, three's molar ratio are 6：1：4, it is dissolved into the deionized water of 2L and forms nitrate solution, and weigh 102.3g
EDTA and be dissolved in the ammonium hydroxide of 100ml.Nitrate solution is put into water-bath and is heated to 80 DEG C, while EDTA is molten
Liquid is slowly added into wherein, is heated and is stirred continuously to form colloidal sol, is positioned in 120 DEG C of baking ovens and moisture removal is gone to form xerogel, and
It is put in Muffle furnace and is decomposed again, decomposition temperature is 800 DEG C, keeps the temperature 4h.The polished mistake of obtained Precursor Powder 200
Mesh standard sieve, after put it into high temperature hydrogen furnace hydrogen environment and be sintered, the sintering temperature of 1500 DEG C of setting, after keeping the temperature 4h
Taking-up obtains aluminate, and material phase analysis is as shown in Figure 5.The cathode dipping aluminate only needs 1625 DEG C, and cathode fully swashs
After work, at 950 DEG CbUnder, pulsed emission current density has reached 101.95A/cm2, transmitting slope is 1.418, as shown in Figure 9.
The foregoing is merely the main scheme for implementing said method of the present invention, however the present invention is not limited to this, all not depart from this
Any modification, equivalent replacement or improvement for being made in the case of invention core etc., should be included within the scope of the present invention.
Claims (10)
1. a kind of hot cathode simple preparation method of aluminate electronic emitting material, which is characterized in that include the following steps：
A. by Ba (NO3)2、Ca(NO3)2·4H20 and Al (NO3)3·9H2O raw materials are dissolved in deionized water respectively by a certain percentage
It is uniform to be configured to respective solution ＆ stir；Complexing agent EDTA is dissolved in ammonium hydroxide；
B. scandium nitrate solution, calcium nitrate solution and aluminum nitrate solution that step A is prepared are mixed and mixed solution is put into water
It is heated in bath, then EDTA solution is gradually added into wherein, be stirred continuously in heating process, until leucosol is formed, this is molten
Glue, which is fully dried, goes moisture removal to form xerogel；
C. the obtained xerogel of step B is positioned in Muffle furnace and carries out preliminary exposition removing ammonium hydroxide and uncomplexed EDTA；
D. the Precursor Powder that step C is decomposed is sintered in high temperature tungsten net hydrogen furnace pure hydrogen atmosphere, finally obtains the moon
Pole emitting material aluminate.
2. a kind of hot cathode simple preparation method of aluminate electronic emitting material described in accordance with the claim 1, feature
Be, in above method step A, the barium nitrate solution of the preparation, calcium nitrate solution, aluminum nitrate solution concentration control
Within the scope of 0.2mol/L~0.5mol/L.
3. a kind of hot cathode simple preparation method of aluminate electronic emitting material described in accordance with the claim 1, feature
It is, in above method step A, the EDTA per 100g is corresponded to fully to be dissolved using the ammonium hydroxide of 50~100ml.
4. a kind of hot cathode simple preparation method of aluminate electronic emitting material described in accordance with the claim 1, feature
It is, in above method step B, the heating water bath is to control bath temperature within the scope of 70 DEG C~90 DEG C, by it after colloidal sol
It is positioned in 120 DEG C of baking ovens and is dried into gel.
5. a kind of hot cathode simple preparation method of aluminate electronic emitting material described in accordance with the claim 1, feature
It is, in above method step B, Ba (NO in mixed solution3)2、Ca(NO3)2·4H20 and Al (NO3)3·9H2O integrates molal quantity
Molar ratio with EDTA is (0.8-1.2):1.
6. a kind of hot cathode simple preparation method of aluminate electronic emitting material described in accordance with the claim 1, feature
It is, in above method step C, the decomposition step is to adjust decomposition temperature to 700 DEG C~900 DEG C ranges；After decomposing
Powder be ground, sieve, cross 100 mesh or 200 mesh sieve after be stored in it is to be used in drying cupboard.
7. a kind of hot cathode simple preparation method of aluminate electronic emitting material described in accordance with the claim 1, feature
It is, in above method step D, the step that is sintered in high temperature tungsten net hydrogen furnace is to adjust sintering temperature 1300
DEG C~1600 DEG C within the scope of, soaking time be 2~8h.
8. a kind of hot cathode simple preparation method of aluminate electronic emitting material described in accordance with the claim 1, feature
It is, in above method step D, the high-purity hydrogen a concentration of 99.999% of the pure hydrogen atmosphere.
9. a kind of hot cathode simple preparation method of aluminate electronic emitting material described in accordance with the claim 1, feature
It is, in above method step A, the raw material Ba (NO3)2、Ca(NO3)2·4H20 and Al (NO3)3·9H2The molar ratio of O is 4：
1：2 or 6：1：4 or 5：3：4, purity is that analysis is pure.
10. the hot cathode aluminate electronic emitting material being prepared according to claim 1-9 any one of them methods.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109704377A (en) * | 2019-01-24 | 2019-05-03 | 北京工业大学 | A kind of preparation method of 411 aluminate electronic emitting material of microwave sintering |
| CN112374882A (en) * | 2020-11-12 | 2021-02-19 | 中国科学院空天信息创新研究院 | Emitting material, preparation method and application |
| CN113044864A (en) * | 2021-03-05 | 2021-06-29 | 北京工业大学 | Method for preparing alkaline earth metal aluminate for cathode by freeze drying method |
| CN114644517A (en) * | 2022-03-29 | 2022-06-21 | 南京三乐集团有限公司 | High-performance aluminate source for terahertz traveling wave tube and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109704377A (en) * | 2019-01-24 | 2019-05-03 | 北京工业大学 | A kind of preparation method of 411 aluminate electronic emitting material of microwave sintering |
| CN109704377B (en) * | 2019-01-24 | 2021-06-04 | 北京工业大学 | Preparation method of 411 aluminate electron emission material by microwave sintering |
| CN112374882A (en) * | 2020-11-12 | 2021-02-19 | 中国科学院空天信息创新研究院 | Emitting material, preparation method and application |
| CN113044864A (en) * | 2021-03-05 | 2021-06-29 | 北京工业大学 | Method for preparing alkaline earth metal aluminate for cathode by freeze drying method |
| CN113044864B (en) * | 2021-03-05 | 2022-06-24 | 北京工业大学 | Method for preparing alkaline earth metal aluminate for cathode by freeze drying method |
| CN114644517A (en) * | 2022-03-29 | 2022-06-21 | 南京三乐集团有限公司 | High-performance aluminate source for terahertz traveling wave tube and preparation method thereof |
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