Preparation method for rare earth oxide doped tungsten powder

A rare earth oxide and tungsten oxide technology, applied in the field of preparing rare earth oxide doped tungsten powder by low temperature combustion synthesis method, can solve the problems of rare earth oxide uniformity limitation, oxide segregation, easy particle growth, etc. Small, prevent agglomeration, evenly distributed effect

Active Publication Date: 2013-09-11
UNIV OF SCI & TECH BEIJING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, there are three main doping methods of rare earth oxides: solid-solid doping is directly introduced into rare earth oxides in the form of mechanical mixing, which has the problems of coarse structure and obvious oxide segregation; liquid-solid doping is mixed with rare earth nitrate solution The introduction of rare earth oxides in the form of solid refractory metal compounds refines the structure and improves the electron emission performance, but the uniformity of rare earth oxides is still limited; liquid-liquid doping (traditional sol-gel method) adds Rare earth nitrate solution and ammonium metatungstate solution to obtain oxide doped refractory metal, grain refinement and uniform distribution of rare earth elements improve electron emission performance, but there are problems of long time and low efficiency, tungsten powder and oxidation The particles are easy to grow

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  • Preparation method for rare earth oxide doped tungsten powder

Examples

Experimental program
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Effect test

Embodiment 1

[0016] Embodiment 1: One yuan rare earth oxide doped tungsten powder (W-0.05wt.%La 2 o 3 ) preparation

[0017] To analyze pure ammonium metatungstate, La(NO 3 ) 3 , urea and glucose as raw materials, (NH 4 ) 2 WO 4 and La(NO 3 ) 3 The molar ratio of the sum of the moles of the urea to the urea is 1:0.8, (NH 4 ) 2 WO 4 and La(NO 3 ) 3 The molar ratio of the sum of the molar amounts of the glucose to the glucose is 1: (0.5~2). Weigh according to the composition ratio, dissolve in a small amount of deionized water, and stir evenly to obtain a mixed solution; the mixed solution is heated in a temperature-controllable furnace to volatilize the aqueous solution. As the reaction proceeds, the heat released will cause pyrolysis and carbonization of the complexing agent, and the target element will be converted into extremely fine nano-sized oxide particles and tungsten oxide particles, thereby obtaining mono- or multi-element rare earth oxide particles, tungsten oxide an...

Embodiment 2

[0018] Embodiment 2: Unary rare earth oxide doped tungsten powder (W-1.5wt.%ZrO 2 ) preparation

[0019] To analyze pure ammonium metatungstate, Zr(NO 3 ) 4 , urea and glucose as raw materials, (NH 4 ) 2 WO 4 and Zr(NO 3 ) 4 The molar ratio of the sum of the moles of the urea to the urea is 1:0.8, (NH 4 ) 2 WO 4 and Zr(NO 3 ) 4 The molar ratio of the sum of the molar amounts of the glucose to the glucose is 1: (0.5~2). Weigh according to the composition ratio, dissolve in a small amount of deionized water, and stir evenly to obtain a mixed solution; the mixed solution is heated in a temperature-controllable furnace to volatilize the aqueous solution. As the reaction proceeds, the heat released will cause pyrolysis and carbonization of the complexing agent, and the target element will be converted into extremely fine nano-sized oxide particles and tungsten oxide particles, thereby obtaining mono- or multi-element rare earth oxide particles, tungsten oxide and Precu...

Embodiment 3

[0020] Embodiment 3: One elemental rare earth oxide doped tungsten powder (W-5wt.%Sc 2 o 3 ) preparation

[0021] To analyze pure ammonium metatungstate, Sc(NO 3 ) 3 , citric acid and glucose as raw materials, (NH 4 ) 2 WO 4 and Sc(NO 3 ) 3 The molar ratio of the sum of the moles of the citric acid to citric acid is 1:0.8, (NH 4 ) 2 WO 4 and Sc(NO 3 ) 3The molar ratio of the sum of the molar amounts of the sucrose to the sucrose is 1: (0.5~2). Weigh according to the composition ratio, dissolve in a small amount of deionized water, and stir evenly to obtain a mixed solution; the mixed solution is heated in a temperature-controllable furnace to volatilize the aqueous solution. As the reaction proceeds, the heat released will cause pyrolysis and carbonization of the complexing agent, and the target element will be converted into extremely fine nano-sized oxide particles and tungsten oxide particles, thereby obtaining mono- or multi-element rare earth oxide particles,...

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Abstract

The invention provides a preparation method of rare earth oxide doped tungsten powder, belonging to a technical field of rare earth refractory metal material. The process flow is that: firstly, a precursor powder is obtained by adopting low-temperature combustion synthesis, wherein the precursor powder is a uniform mixture of rare earth oxide (at least one of Sc2O3, Y2O3, La2O3, CeO2, ZrO2, Gd2O3 and Eu2O3) and tungsten oxide; secondly, the precursor powder undergoes calcination in a muffle furnace; lastly, two-step reduction is carried out in the atmosphere of hydrogen or dissociated ammonia. Easy-reduction tungsten oxide is reduced to tungsten matrix powder, and the rare earth oxide that can not be reduced is reserved, thereby the rare earth oxide doped tungsten powder is obtained. The content of the rare earth oxide in the rare earth oxide doped tungsten powder is 0.05-35 wt%. The advantage of the invention is that target element and organic carbon source are capable of forming a highly dispersed system, and particle sizes of the obtained oxide are uniform and fine. The method is suitable for industrialization production because of low cost of raw materials, quick reaction speed, low energy consumption and simple technology.

Description

technical field [0001] The invention belongs to the technical field of rare earth refractory metal materials, and particularly provides a method for preparing rare earth oxide doped tungsten powder by a low-temperature combustion synthesis method. Background technique [0002] Vacuum tube devices are essential equipment for national defense equipment such as radar, communications, electronic countermeasures, telemetry and remote control, and precision guidance, as well as civilian fields such as high-energy particle accelerators, weather radars, microwave communications, and satellite communications. Tungsten has a series of advantages such as high melting point, high specific gravity, high elastic modulus, high temperature strength, low vapor pressure and low expansion coefficient. etched electrode material. The cathode is the electron emission source of the vacuum tube device, and the performance of the cathode material is directly related to the performance and service l...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B22F9/22
Inventor 秦明礼章林刘烨曲选辉
Owner UNIV OF SCI & TECH BEIJING
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