Method for preparing high-density ultrafine-grained rare earth oxide doped tungsten alloy

A technology of rare earth oxides and tungsten alloys, applied in the field of powder metallurgy, can solve the problems of unfavorable preparation of high-density ultra-fine grain W-based alloys, difficulty in obtaining high density, and grain growth. The effect of low temperature required for sintering and high sintering activity

Active Publication Date: 2019-12-13
UNIV OF SCI & TECH BEIJING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] W is a difficult-to-sinter material. Using traditional sintering methods, it is difficult to obtain high density, and it needs to be sintered at high tem

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Put 31.18g of ammonium metatungstate, 0.295g of lanthanum nitrate, 12.75g of glycine, and 32.04g of ammonium nitrate into a beaker and add an appropriate amount of deionized water to dissolve to obtain a clear solution. Place the solution on an electric furnace and heat until the reaction occurs. A fluffy precursor powder is obtained. Put the precursor powder into a tube furnace for reduction. The reduction temperature is 700°C, the hydrogen flow rate is 1L / min, the holding time is 3h, and the heating rate is 5°C / min. 0.5wt%La 2 o 3 alloy powder.

[0023] Nano W-0.5wt% La 2 o 3 The alloy powder was subjected to multi-step discharge plasma sintering. The sintering temperature was 600°C and the holding time was 3 minutes; the sintering temperature was 900°C and the holding time was 3 minutes; Rare earth oxide doped tungsten alloy with a grain size of 250nm.

Embodiment 2

[0025] Put 31.20g of ammonium metatungstate, 0.60g of lanthanum nitrate, 13.05g of urea, and 32.34g of ammonium nitrate into a beaker and add an appropriate amount of deionized water to dissolve to obtain a clear solution. Place the solution on an electric furnace and heat it until the reaction occurs. A fluffy precursor powder is obtained. Put the precursor powder into a tube furnace for reduction. The reduction temperature is 700°C, the hydrogen flow rate is 1L / min, the holding time is 3h, and the heating rate is 5°C / min. 1wt% La 2 o 3 alloy powder.

[0026] Nano W-1wt% La 2 o 3 The alloy powder was subjected to multi-step discharge plasma sintering. The sintering temperature was 600°C and the holding time was 3 minutes; the sintering temperature was 1000°C and the holding time was 5 minutes; Rare earth oxide doped tungsten alloy with a grain size of 280nm.

Embodiment 3

[0028] Put 31.10g of ammonium metatungstate, 0.52g of yttrium nitrate, 12.50g of thiourea, and 32.05g of ammonium nitrate into a beaker and add an appropriate amount of deionized water to dissolve to obtain a clear solution. Place the solution on an electric furnace and heat until the reaction occurs , to obtain a fluffy precursor powder. Put the precursor powder into a tube furnace for reduction. The reduction temperature is 700°C, the hydrogen flow rate is 1L / min, the holding time is 3h, and the heating rate is 5°C / min. 1wt%Y 2 o 3 alloy powder.

[0029] Nano W-1wt%Y 2 o 3 The alloy powder is subjected to multi-step discharge plasma sintering, the sintering temperature is 600°C, the holding time is 3min; the sintering temperature is 900°C, the holding time is 5min; the sintering temperature is 1400°C, the holding time is 0.5min, the relative density is 98%. Rare earth oxide doped tungsten alloy with an average grain size of 250nm.

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Abstract

The invention provides a method for preparing high-density ultrafine-grained rare earth oxide doped tungsten alloy, and belongs to the field of powder metallurgy. The preparation method comprises thefollowing steps: preparing an oxide composite powder precursor by using ammonium metatungstate, rare earth nitrate, fuel and ammonium nitrate as raw materials and adopting a low-temperature solution combustion synthesis method, and then reducing by using H2 to prepare nano rare earth oxide doped tungsten alloy powder; and preparing the high-density ultrafine-grained rare earth oxide doped tungstenalloy by adopting multi-step discharge plasma sintering. According to the method, a low-temperature solution combustion synthesis method adopted can achieve the mixing at a molecular level, thus thetungsten oxide and the rare earth oxide in the obtained precursor are uniformly mixed, and the reduction product is alloy powder without subsequent special treatment; the SPS is suitable for rapid sintering of refractory metals and materials difficult to sinter, and the high-density ultrafine-grained rare earth oxide doped tungsten alloy can be obtained by adopting multi-step SPS; the relative density can reach 96-99%, and the average grain size is less than or equal to 300nm. The method has the advantages of simple and easily obtained raw materials, simple equipment and quick process, and issuitable for large-scale production.

Description

technical field [0001] The invention belongs to the field of powder metallurgy, and relates to a method for preparing a high-density ultrafine-grain rare earth oxide-doped tungsten alloy. Background technique [0002] Tungsten (W) has a high melting point, high hardness, good high-temperature strength, thermal conductivity, electrical conductivity, and low thermal expansion coefficient. It is widely used in national defense, nuclear industry, and high-temperature fields. However, the sintering temperature of W is usually higher than 2000 °C, which makes its densification difficult and causes grain growth. Refinement of W powder particle size to nanometer size can effectively reduce the sintering temperature of W, but the nano W powder will grow rapidly during the sintering process, which will reduce the mechanical properties of W alloy. Adding rare earth oxides (La 2 o 3 , Y 2 o 3 、Lu 2 o 3 、Ce 2 o 3 etc.) particles can prevent the movement of grain boundaries durin...

Claims

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Application Information

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IPC IPC(8): B22F9/22B22F3/105C22C1/05C22C1/10C22C27/04
CPCB22F3/105B22F9/22B22F2003/1051C22C1/051C22C27/04Y02P10/25
Inventor 秦明礼杨军军章雨峰陈铮王倩玉于瀛母晓东贾宝瑞曲选辉
Owner UNIV OF SCI & TECH BEIJING
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