Method for preparing pressed scandia-doped dispenser cathodes using microwave sintering

Patent metadata

Field	Value
Publication number	US-10651000-B2
Application number	US-201715409888-A
Country	US
Kind code	B2
Filing date	Jan 19, 2017
Priority date	May 27, 2016
Publication date	May 12, 2020
Grant date	May 12, 2020

Abstract

The present disclosure discloses a preparation method of pressed Scandia-doped dispenser cathode using microwave sintering. Embodiments of the present disclosure include dissolving some nitrates and ammonium metatungstate with deionized water to prepare a homogeneous solution. Precursor powder with uniform size is obtained by spray drying, the precursor powder is decomposed, and two-step reduction may be proceeded to form doped tungsten powder with uniform element distribution. The cathode is prepared by one-time microwave sintering. One-time forming of cathode sintering is realized, and sintering shrinkage and sintering time are reduced significantly. The method has excellent repeatability, and the cathode has a homogeneous structure and excellent emission performance at 950° C.

First claim

What is claimed is:

1. A method of preparing a pressed scandia-doped dispenser cathode using microwave sintering, the method comprising:
preparing precursor powders by:
dissolving ammonium metatungstate hydrate, scandium nitrate, aluminum nitrate, barium nitrate and calcium nitrate in water under a room temperature to obtain solutions, respectively;
mixing a solution of the ammonium metatungstate hydrate and a solution of the scandium nitrate to obtain a mixture;
mixing a solution of the barium nitrate, a solution of the calcium nitrate, and a solution of the aluminum nitrate to obtain a nitrate solution;
adding the nitrate solution, while performing constant agitation, to the mixture; and
obtaining precursor powder by spray drying, wherein a feeding rate is 200 ml/h-600 ml/h, a blast rate is 0.4 m 3 /min-0.6 m 3 /min, an inlet temperature is 150° C., and an outlet temperature is 90-96° C.;

performing decomposition and reduction of the precursor powder by:
decomposing the precursor powder in a muffle furnace for 3 hours to remove powder containing C and N in the precursor powder under a condition including a temperature of 550° C. and air or oxygen atmosphere to obtain oxide powder; and

performing a reduction process of the oxide powder in a tube or furnace under hydrogen atmosphere by:
keeping the temperature at 450-550° C. and maintaining it for 2-3 h; and
raising the temperature to 800-850° C. and maintaining it for 2-3 h to obtain doped tungsten powder; and

pressing and sintering a cathode by:
pressing the decomposed powder under a certain pressure using molds;
placing green bodies in an auxiliary heating and insulation combining device;
placing the auxiliary heating and insulation combining device in a microwave cavity of a microwave source;
turning on the microwave source and raising the temperature in the microwave cavity with a constant rate until 800-850° C.;
maintaining the temperature for 5 minutes;
raising the temperature with a rate of 10˜15° C./min until 1400-1500° C.;
maintaining the temperature for 10-30 min; and
obtaining the cathode after cooling the cathode to the room temperature.

2. The method of claim 1 , wherein the composition of the powder generated from the reduction process is W (85%); Sc 2 O 3 (5%); BaO, CaO, and Al 2 O 3 (10%), and a molar ratio of Ba:Ca:Al is 4:1:1.

3. The method of claim 1 , wherein a composition of the powder generated from the reduction process is W, Sc 2 O 3 , BaO, CaO, and Al 2 O 3 .

4. The method of claim 1 , further comprising:
filtering the powder through a 200-mesh screen after the preparing of the precursor powders and the performing of the decomposition and reduction of the precursor powder, respectively.

5. The method of claim 1 , wherein a pressing pressure in the pressing and sintering of the cathode is 0.8-1.2 t/cm 2 .

6. The method of claim 1 , wherein an auxiliary heating material of the auxiliary heating and insulation combining device is SiC, and an insulation material of the insulation combining device is Mullite Fiber.

Assignees

• Univ Beijing Technology

Inventors

• Liu Wei
• Tian Mingchaung
• Wang Jinshu
• Zhou Fan
• Wang Yiman
• Dong Liran
• Yang Yunfei
• Zhang Quan

Classifications

• H01J1/28

  Dispenser-type cathodes, e.g. L-cathode · CPC title

• B22F3/105

  by using electric current {other than for infrared radiant energy}, laser radiation or plasma (B22F3/11 takes precedence){; by ultrasonic bonding (B22F3/115 takes precedence)} · CPC title

• B22F9/30

  with decomposition of metal compounds, e.g. by pyrolysis · CPC title

• B22F9/22

  using gaseous reductors · CPC title

• C22B34/36

  Obtaining tungsten · CPC title