Method for preparing rare-earth oxide dispersion strengthened fine-grained tungsten material

A rare earth oxide, fine-grained tungsten material technology, applied in the field of nanomaterials, can solve the problems of uneven distribution of heterogeneous impurities, poor material properties, poor compatibility and other problems, and achieve simple process, large sintering activity, and uniform structure. Effect

Active Publication Date: 2016-04-20
长沙微纳坤宸新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are some problems in the above-mentioned preparation method: powders prepared by high-energy ball milling or mechanical alloying are prone to uneven distribution of components and introduction of heterogeneous impurities, while SPS and hot pressing sintering methods are not suitable for large-scale preparation of engineering
However, due to the poor compatibility between tungsten and the surface of rare earth oxide particles, tungsten materials containing trace rare earth oxides are directly prepared by sol-spray drying method, and the dispersion strengthening effect of rare earth oxide particles on tungsten is very limited, resulting in poor performance of the material , it is difficult to meet the requirements for the use of nuclear fusion tungsten materials

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] The preparation composition is W-0.1wt%Y 2 o 3 Take the dispersion strengthened fine-grained tungsten material as an example.

[0023] (1) First, according to the final mass fraction of rare earth oxides to be prepared, soluble rare earth salts and tungstates are weighed in proportion by mass, that is, 1.02g of yttrium nitrate and 411.27g of ammonium metatungstate are weighed to prepare 50g / L respectively Rare earth salt solution and 150g / L tungsten salt solution.

[0024] (2) First, slowly dropwise add ammonia water with a concentration of 10wt% in the yttrium nitrate solution, adjust the pH to 7.2, and add 0.2g PEG400 as a reaction dispersant, under the action of ultrasonic vibration and electric mixer stirring, the rare earth salt reacts with the alkali Form a uniform suspension of Y(OH) 3 Particle colloid; then add tungsten salt solution to Y(OH) 3 In the colloid, slowly add oxalic acid with a concentration of 10wt% dropwise, adjust the pH to 6.5, and add 2g PEG...

Embodiment 2

[0029] The preparation composition is W-0.3wt% La 2 o 3 Take the dispersion strengthened fine-grained tungsten material as an example.

[0030] (1) First, according to the mass fraction of the rare earth oxide to be prepared, weigh the soluble rare earth salt and tungstate according to the mass ratio, that is, weigh 1.53g of lanthanum oxalate and 410.45g of ammonium paratungstate, and prepare 60g / L rare earth salt solution respectively And 200g / L tungsten salt solution.

[0031] (2) First, slowly drop NaOH with a concentration of 10wt% in the lanthanum oxalate solution, adjust the pH to 7.3, and add 0.3g N, N-dimethylformamide as a reaction dispersant, under the action of ultrasonic vibration and electric mixer stirring , the rare earth salt reacts with alkali to form a uniform suspension of La(OH) 3 particle colloid; then the tungsten salt solution was added to the La(OH) 3 In the colloid, slowly add HCl with a concentration of 10wt%, adjust the pH to 6.8, and add 1.5g PE...

Embodiment 3

[0036] The preparation composition is W-0.5wt% CeO 2 Take the dispersion strengthened fine-grained tungsten material as an example.

[0037] (1) First, according to the final mass fraction of the rare earth oxide to be prepared, take the soluble rare earth salt and tungstate according to the mass ratio, that is, 2.10g of cerium carbonate, 409.6g of ammonium tungstate, and prepare a 70g / L rare earth salt solution respectively And 220g / L tungsten salt solution.

[0038] (2) First slowly add KOH with a concentration of 10wt% in the cerium carbonate solution, adjust the pH to 7.5, and add 0.3g stearic acid as a reaction dispersant, under the action of ultrasonic vibration and electric mixer stirring, make the rare earth salt React with alkali to form a homogeneous suspension of Ce(OH) 3 particle colloid; then the tungsten salt solution was added to the Ce(OH) 3 In the colloid, slowly dropwise add HNO with a concentration of 10wt% 3 , adjust the pH to 6.5, and add 2.5g stearic ...

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Abstract

A method for preparing a rare-earth oxide dispersion strengthened fine-grained tungsten material, comprising: according to a condition that a mass percentage of rare-earth oxide is 0.1-2%, and the remaining composition is W, weighing soluble rare-earth salt and tungstic acid salt, and respectively preparing 50-100 g / L of rare-earth saline solution and 150-300 g / L of tungstic acid saline solution; adding a minor amount of alkali into the rare-earth salt to control the pH to be 7-8, adding an organic dispersing agent, and stirring to enable the rare-earth salt to form uniformly suspending R(OH)3 colloidal particles (R represents a rare-earth element); adding the tungstic acid saline solution into the R(OH)3 colloidal particles, adding a minor amount of acid to control the pH to be 6-7, adding the organic dispersing agent, stirring to enable the tungstic acid salt to form tungstic acid micro-particles, precipitating and coating the R(OH)3 colloidal particles with the R(OH)3 colloidal particles as a core, and forming coprecipitated coated colloidal particles; conducting spray drying on the coprecipitated coated colloidal particles to obtain a composite precursor powder of tungsten and rare-earth oxide; calcining, conducting thermal reduction via hydrogen, and preparing superfine nanometer tungsten powder having a particle size of 50-500 nm; and conducting normal high-temperature sintering after a general pressing forming. The high-performance fine-grained tungsten material dispersed and strengthened by a minor amount of rare-earth oxide prepared by the above method has a density approximate to full density (>=98.5%), and uniform and small tungsten grains having an average size of 5-10 [mu]m; in addition, rare-earth oxide particles having a particle size of 100 nm - 500 nm are uniformly distributed in a tungsten crystal or a crystal boundary.

Description

Technical field: [0001] The invention relates to the fields of nanomaterials and powder metallurgy, in particular to a method for preparing rare earth oxide dispersion-strengthened fine-grained tungsten materials prepared by nanocomposite technology. Background technique: [0002] Tungsten has high melting point, high hardness, good high temperature strength, thermal conductivity, electrical conductivity, low thermal expansion coefficient, low sputtering when interacting with plasma, no chemical reaction with H, H + With low retention characteristics, it is a very important high-temperature structural material and functional material, and is widely used as a plasma-facing material and divertor component material in the field of nuclear fusion. [0003] Among the tungsten materials that have been applied, pure tungsten materials are typical high-temperature materials that are widely used at present. At present, sintered pure tungsten materials are prepared by means of high p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22C27/04C22C1/05B22F9/22B22F1/00B22F1/054
CPCB22F9/22C22C1/05C22C27/04C22C32/0031B22F2998/10B22F1/054B22F1/00B22F3/02B22F3/10C22C1/1026B22F9/24B22F1/16B22F9/026B22F1/142B22F1/145B22F3/04B22F2999/00B22F2201/013C22C1/045C22C2200/04B22F3/16B22F9/30B22F2301/20B22F2302/25
Inventor 范景莲韩勇李鹏飞刘涛成会朝田家敏
Owner 长沙微纳坤宸新材料有限公司
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