CN103050347A - Method for preparing nickel-scandium (Ni-Sc) sponge oxide cathode - Google Patents
Method for preparing nickel-scandium (Ni-Sc) sponge oxide cathode Download PDFInfo
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- CN103050347A CN103050347A CN2011103099903A CN201110309990A CN103050347A CN 103050347 A CN103050347 A CN 103050347A CN 2011103099903 A CN2011103099903 A CN 2011103099903A CN 201110309990 A CN201110309990 A CN 201110309990A CN 103050347 A CN103050347 A CN 103050347A
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Abstract
The invention discloses a method for preparing a nickel-scandium (Ni-Sc) sponge oxide cathode, and relates to an electro-vacuum technology. The method comprises the following steps of: grinding and mixing Sc powder and Ni powder according to the mass percent of less than 5 percent to prepare Ni and Sc mixed metal powder; spraying a layer of adhesive on a cathode Ni substrate; covering the Ni and Sc mixed metal powder on the adhesive to form a Ni and Sc sponge layer; removing floating powder of the Ni and Sc mixed metal powder from the adhesive after drying; placing the cathode Ni substrate adhered to the Ni and Sc sponge layer in an H2 furnace; sintering for 10 to 20 minutes at the temperature of 1,300+/-10 DEG C; filling triplex carbonate of BaCO3, SrCO3 and CaCO3 in the Ni and Sc sponge layer; and spraying the triplex carbonate on the surface of the Ni and Sc sponge layer to prepare the Sc-Ni sponge oxide cathode. By the method, the emission current density of the sponge oxide cathode is improved; the working temperature of the cathode is reduced; and the service life of the cathode is prolonged.
Description
Technical field
The present invention relates to the electric vacuum technology field, is the method that employing Ni, Sc mixed-powder sponge prepare the Ni sponge oxide cathode, to improve Ni sponge oxide cathode emission, reduce the negative electrode working temperature, to prolong cathode life.
Background technology
Oxide coated cathode is to be applied to the most widely one of hot cathode of electron tube.In the development of oxide coated cathode, bonding for the mechanical strength that strengthens negative electrode and cathode surface oxide and Base Metal is generally at the Ni spongy layer of surface, cathode base metal sintering last layer thickness less than 400 μ m.The Ni spongy layer of this porous can increase the stockage of emitting material and the path that electric current passes through in the oxide coating is shortened, so the Ni sponge oxide cathode can be drawn larger emission than ordinary oxide negative electrode, is widely used in the vacuum electron device.Yet after negative electrode work a period of time, because the increase of intermediate layer resistance, cathode activity can reduce gradually, causes cathode life to finish.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of nickel scandium sponge oxide cathode, with emission, reduction negative electrode working temperature, the prolongation cathode life that improves the nickel sponge oxide coated cathode.
For achieving the above object, technical solution of the present invention is:
A kind of preparation method who prepares nickel scandium sponge oxide cathode the steps include:
A) with the Sc powder by Ni opaque amount percentage less than 5% with Ni powder ground and mixed, make Ni, Sc mixed metal powder;
B) at negative electrode Ni substrate spray one deck bonding agent, be covered with Ni, the Sc mixed metal powder that step a) prepares at bonding agent, form Ni, Sc spongy layer, remove the floating powder of top Ni, Sc mixed metal powder after the drying;
C) with step b) preparation the negative electrode Ni substrate that is stained with Ni, Sc spongy layer put into H
2In the stove, in 1300 ± 10 ℃ of sintering 10-20 minutes; Normal pressure, H
2Flow 5～8L/min;
D) at step c) insert triplex carbonate among the Ni, Sc spongy layer of preparation after, spray the identical triplex carbonate of one deck in Ni, Sc spongy layer surface again, prepare nickel scandium sponge oxide cathode.
Described preparation method, its described step grinding in a) is to grind in the alms bowl at agate to grind.
Described preparation method, its described step b) bonding agent in is guncotton solution; Ni, Sc spongy layer thickness are 100 μ m-200 μ m.
Described preparation method, its described step b) Ni that is covered with at bonding agent in, Sc mixed metal powder particle diameter are for can pass through 325 order mesh screens.
The thickness of the triplex carbonate that sprays described preparation method, its described steps d) is 20 μ m-40 μ m.
Described preparation method, its described steps d) triplex carbonate in is BaCO
3, SrCO
3And CaCO
3
The beneficial effect of the inventive method is: can improve emission, the reduction negative electrode working temperature of common Ni sponge oxide cathode, prolong cathode life, realize the oxide coated cathode Ni-Sc spongy layer of synthetic function admirable.And adopt the negative electrode of Ni-Sc sponge preparation because Sc is conducive to the storage of surplus Ba with Ni effect in the negative electrode course of work and to the diffusion of coating, thus improve the emission of Ni sponge oxide cathode, reduce cathode temperature, prolongation cathode life.
Description of drawings
Fig. 1 a is the nickel scandium sponge oxide cathode structural representation of the inventive method preparation;
Fig. 1 b is the negative electrode partial cutaway schematic among Fig. 1 a;
Fig. 2 is the dc voltage current characteristic curve of the Ni-Sc sponge oxide cathode of the inventive method preparation;
Fig. 3 is the Pulse Voltammetry characteristic curve of the Ni-Sc sponge oxide cathode of the inventive method preparation;
Fig. 4 is the life curve of the Ni-Sc sponge oxide cathode of the inventive method preparation.
Specific implementation method
Preparation method of the present invention, its key step is:
A) at first with purity be the 99.9wt% particle mean size be 30 μ m～40 μ m the Sc powder by Ni opaque amount percentage less than 5% with put into agate after the Ni powder of same purity, granularity mixes and grind alms bowl;
B) above-mentioned mixed-powder was ground in the agate alms bowl more than 2 hours, guarantee that two kinds of powder mix;
C) be negative electrode Ni net surface spray one deck guncotton solution of 3mm at diameter, with the above-mentioned Ni that mixes of 325 purpose sieves sieve one deck, Sc metal dust, dry, remove top floating powder, form the Ni-Sc spongy layer, the thickness of this spongy layer is 100 μ m-200 μ m;
D) with the above-mentioned negative electrode Ni net that is stained with the Ni-Sc spongy layer, put into H
2Carry out sintering in the stove, sintering temperature is 1300 ± 10 ℃, 15 minutes time.
E) the Ni net with the above-mentioned Ni-Sc of preparing spongy layer is welded on the little cylinder of the negative electrode that is filled with Reservoir active material, inserts BaCO in the Ni-Sc spongy layer
3, SrCO
3And CaCO
3Triplex carbonate after guaranteeing to fill up carbonate in the hole of spongy layer, is this triplex carbonate of 20 μ m-40 μ m in cathode surface spray a layer thickness, finishes the preparation of negative electrode, and cathode construction schematic diagram and negative electrode partial cutaway schematic are respectively shown in Fig. 1 a, Fig. 1 b.
Negative electrode is respectively charged in water-cooled anode diode dynamic test system and the conventional test diode, between the anode and cathode apart from 0.9m～1.1mm, negative electrode decomposition, activation and ageing carry out respectively negative electrode direct current, Pulse Voltammetry characteristic and life test after 30 hours.The cathode temperature that in the test electronics cooling effect is caused descends and does not carry out temperature-compensating.Test result such as Fig. 2, Fig. 3 and shown in Figure 4.
This Ni-Sc sponge oxide cathode is respectively 0.65A/cm in 700 ℃ of cathode temperatures, negative electrode direct current deviation point emission 750 ℃, 800 ℃, 850 ℃ the time as can be seen from Figure 2
2, 1.2A/cm
2, 2.3A/cm
2, 4.5A/cm
2, greater than the emission of common Ni sponge oxide cathode.
This negative electrode is at pulse duration 10 μ s as can be seen from Figure 3, during repetition rate 100Hz, is respectively 6.4A/cm in 800 ℃ of cathode temperatures, cathode pulse deviation point emission 820 ℃, 850 ℃ the time
2, 15.5A/cm
2, 33A/cm
2, greater than the impulse ejection current density of common Ni sponge oxide cathode.
Fig. 4 be this negative electrode 780 ℃ of temperature, initial transmissions current density 2.3A/cm
2The time life curve, this negative electrode descends at 1350 hours after-currents and is no more than 5% of initial current density as can be seen from Figure 4, the life performance of this negative electrode obviously is better than the life performance of common Ni sponge oxide cathode.
In addition, negative electrode does not detect that coating is overheated, emission current is unstable, the phenomenon of striking sparks and evapotranspire in voltage-current characteristic and life test process, illustrate that the Ni-Sc sponge oxide cathode of the inventive method manufacturing has preferably reliability.
Claims (6)
1. a preparation method who prepares nickel scandium sponge oxide cathode is characterized in that, step is:
A) with the Sc powder by Ni opaque amount percentage less than 5% with Ni powder ground and mixed, make Ni, Sc mixed metal powder;
B) at negative electrode Ni substrate spray one deck bonding agent, be covered with Ni, the Sc mixed metal powder that step a) prepares at bonding agent, form Ni, Sc spongy layer, remove the floating powder of top Ni, Sc mixed metal powder after the drying;
C) with step b) preparation the negative electrode Ni substrate that is stained with Ni, Sc spongy layer put into H
2In the stove, in 1300 ± 10 ℃ of sintering 10-20 minutes; Normal pressure, H
2Flow 5～8L/min;
D) at step c) insert triplex carbonate among the Ni, Sc spongy layer of preparation after, spray the identical triplex carbonate of one deck in Ni, Sc spongy layer surface again, prepare nickel scandium sponge oxide cathode.
2. preparation method as claimed in claim 1 is characterized in that, the grinding of described step in a) is to grind in the alms bowl at agate to grind.
3. preparation method as claimed in claim 1 is characterized in that, described step b) in bonding agent, be guncotton solution; Ni, Sc spongy layer thickness are 100 μ m-200 μ m.
4. such as claim 1 or 3 described preparation methods, it is characterized in that described step b) in the Ni, Sc mixed metal powder particle diameter that are covered with at bonding agent for can pass through 325 order mesh screens.
5. preparation method as claimed in claim 1 is characterized in that, described steps d) in the thickness of the triplex carbonate that sprays be 20 μ m-40 μ m.
6. such as claim 1 or 5 described preparation methods, it is characterized in that described steps d) in triplex carbonate be BaCO
3, SrCO
3And CaCO
3
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108054069A (en) * | 2017-11-06 | 2018-05-18 | 昆山国力大功率器件工业技术研究院有限公司 | A kind of oxide-coated cathode powder filling device and its application method |
| CN110649208A (en) * | 2018-09-29 | 2020-01-03 | 合肥工业大学 | Lithium-sulfur battery composite diaphragm and preparation method thereof |
Citations (4)
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|---|---|---|---|---|
| CN85106573A (en) * | 1985-09-03 | 1987-01-21 | 中国科学院电子学研究所 | Reliable and long life-time cathode |
| KR970077003A (en) * | 1996-05-11 | 1997-12-12 | 엄길용 | Cathode for electron emission and manufacturing method thereof |
| CN1395737A (en) * | 2000-09-19 | 2003-02-05 | 皇家菲利浦电子有限公司 | Cathode ray tube having oxide cathode |
| CN101794697A (en) * | 2009-02-04 | 2010-08-04 | 中国科学院电子学研究所 | Ni-Re-Ir mixed sponge oxide cathode |
-
2011
- 2011-10-13 CN CN2011103099903A patent/CN103050347A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85106573A (en) * | 1985-09-03 | 1987-01-21 | 中国科学院电子学研究所 | Reliable and long life-time cathode |
| KR970077003A (en) * | 1996-05-11 | 1997-12-12 | 엄길용 | Cathode for electron emission and manufacturing method thereof |
| CN1395737A (en) * | 2000-09-19 | 2003-02-05 | 皇家菲利浦电子有限公司 | Cathode ray tube having oxide cathode |
| CN101794697A (en) * | 2009-02-04 | 2010-08-04 | 中国科学院电子学研究所 | Ni-Re-Ir mixed sponge oxide cathode |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108054069A (en) * | 2017-11-06 | 2018-05-18 | 昆山国力大功率器件工业技术研究院有限公司 | A kind of oxide-coated cathode powder filling device and its application method |
| CN108054069B (en) * | 2017-11-06 | 2019-05-14 | 昆山国力大功率器件工业技术研究院有限公司 | A kind of oxide-coated cathode powder filling device and its application method |
| CN110649208A (en) * | 2018-09-29 | 2020-01-03 | 合肥工业大学 | Lithium-sulfur battery composite diaphragm and preparation method thereof |
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Application publication date: 20130417 |