Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

A preparation method of rare earth oxide dispersion strengthened fine grain tungsten materials

a technology of rare earth oxide and fine grain tungsten, which is applied in the field of rare earth oxide dispersion strengthening fine grain tungsten materials, can solve the problems of high dbtt, material defects, coarse grain,

Inactive Publication Date: 2017-08-10
CENT SOUTH UNIV
View PDF1 Cites 27 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

The present invention relates to a new technology for preparing high performance rare-earth oxide dispersion strengthened fine grain tungsten materials. This technology involves the use of rare earth oxides particles that are evenly distributed throughout the tungsten material, resulting in a uniform and fine grain size. The method uses a combination of rare earth oxide addition through a heterogeneous precipitation process, spray drying, calcination, and thermal reduction, followed by conventional sintering, to achieve high density and good performance at room temperature and high temperature. The ultrafine tungsten composite powder prepared by this method has high sintering activity and excellent toughness at room temperature and high temperature.

Problems solved by technology

However, this material exists defects such as coarse grain, fiber microstructure, high DBTT, low recrystallization temperature, high brittleness.
But there exist some problems in the preparation of above: using high-energy ball milling or mechanical alloying preparation powder is easy to produce heterogeneous component distribution and impurities, and SPS, hot-pressing sintering method is not suitable for the engineering of large scale preparation.
And although Guo's method improve the oxide dispersion distribution uniformity in tungsten matrix, but Ni must be added as sinter activator, and Ni element in many fields, such as nuclear fusion, nuclear fission is forbidden to use, this will be greatly limit the application scope.
But due to poor compatibility of tungsten and rare earth oxide on the surface of the particles, if sol spray drying method is directly used to prepare tungsten materials containing trace rare earth oxide, rare earth oxide particle dispersion strengthening effect for tungsten is very limited, leading to poor performance, so it is difficult to meet the application requirement of nuclear fusion.

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Examples

Experimental program
Comparison scheme
Effect test

implementation example 2

[0029]In the preparation of W-0.3 wt % La2O3 of La2O3 dispersion strengthening fine grain tungsten materials, for example.

[0030](1) First of all, according to the mass fraction of rare earth oxides, weigh and soluble rare earth salt and tungstate by quality proportion, namely take 1.53 g lanthanum oxalate hydrate, 411.27 g ammonium tungstate, respectively made into 60 g / L of rare earth salt solution and 200 g / L of tungsten salt solution.

[0031](2) Slowly drop NaOH with 10 wt % concentration into lanthanum oxalate hydrate solution, adjusting the pH to 7.3, and add 0.3 g N,N-dimethyl formamide as dispersant, under the action of ultrasonic vibration and electric blender mixing, the rare earth salt and alkali reaction to form homogeneous suspension La(OH)3 particle colloid; Then adding tungsten salt solution into the La(OH)3 gel slowly drop HCl with 10 wt % concentration, adjusting the pH to 6.8, and add 1.5 g PEG400 as dispersant, under the action of ultrasonic vibration and electric bl...

implementation example 3

[0035]In the preparation of W-0.5 wt % CeO2 of CeO2 dispersion strengthening fine grain tungsten-materials, for example.

[0036](1) First of all according to the mass fraction of rare earth oxides, weigh and soluble rare earth salt and tungstate by quality proportion, namely take 2.1 g cerium carbonate, 409.6 g ammonium tungstate, respectively made into 70 g / L of rare earth salt solution and 220 g / L of tungsten salt solution.

[0037](3) Slowly drop KOH with 10 wt % concentration into cerium carbonate solution, adjusting the pH to 7.5, and add 0.3 g PEG400 as dispersant, under the action of ultrasonic vibration and electric blender mixing, the rare earth salt and alkali reaction to form homogeneous suspension Ce(OH)3 particle colloid: Then adding tungsten salt solution into the Ce(OH)3 gel, slowly drop HNO3 with 10 wt % concentration, adjusting the pH to 6.5, and add 2.3 g PEG400 as dispersant, under the action of ultrasonic vibration and electric blender mixing to form tungstate micro p...

implementation example 4

[0041]In the preparation of W-0.3 wt %Y2O3-0.3 wt % La2O3 dispersion strengthening fine grain tungsten materials, for example.

[0042](1) First of all, according to the mass fraction of rare earth oxides, weigh, and soluble rare earth salt and tungstate by quality proportion, namely take 1.52 g yttrium nitrate, 2.18 g lanthanum chloride, 409.2 g ammonium tungstate, respectively made into 80 g / L of mixed rare earth salt solution and 250 g / L of tungsten salt solution.

[0043](2) Slowly drop ammonia with 10 wt % concentration into yttrium nitrate and lanthanum chloride solution, adjusting the pH to 7.8, and add 0.4 g sodium dodecyl sulfate as dispersant, under the action of ultrasonic vibration and electric blender mixing, the rare earth salt, and alkali reaction to form homogeneous suspension Y(OH)3+ La(OH)3particle colloid: Then adding tungsten salt solution into the Y(OH)3+ La(OH)3 gel, slowly drop oxalic acid with 10 wt % concentration, adjusting the pH to 6.2, and add 3.0 g sodium dod...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

PropertyMeasurementUnit
particle sizeaaaaaaaaaa
tensile strengthaaaaaaaaaa
tensile strengthaaaaaaaaaa
Login to View More

Abstract

This invention relates to a preparation method of rare earth oxide dispersion strengthened fee grain tungsten materials, the mass percent of the rare earth oxide is of 0.1-2%, and the rest ingredient is W. Weigh soluble rare earth salt and tungstate, dissolve into water to made into 50-100 g / L of rare earth salt solution and 150-300 g / L of tungstate solution, respectively. Firstly, add trace alkali in rare earth salt solution to control pH in 7-8, then add organic dispersant and stir to form evenly suspended R(OH)3 particle colloid (R refers to rare earth element). Secondly pour the tungstate solution into the R(OH)3colloid, add trace acid to control pH in 6-7, then add organic dispersant and stir to form tungstic acid micro particles, which wrap around the colloidal particles, forming coprecipitation coating particle colloid. Thirdly, the coprecipitation coating particle colloidal is spray-dried, forming tungsten and rare earth oxide compound precursor powder. Alter that, ultrafine or nanoscale tungsten powder with particle size of 50˜500 nm is obtained through a process of calcination subsequent with hydrogen thermal reduction. Finally, the tungsten powder is subjected to ordinary compression molding and then conventional high temperature sintering. The trace rare earth oxide dispersion strengthened high performance fine grain tungsten materials prepared by this invention, its density is close to full density (98.5% or higher), its grain size is uniform and very fine (average in 5˜10 microns), and the rare earth oxides particles evenly distribute in tungsten intracrystalline or grain, boundary with particle size of 100˜500 nm.

Description

CROSS-REFERENCE TO RELATED APPLICATIONS[0001]The present application claims priority to the PCT application Ser. No. PCT / CN2014 / 088882, filed on Oct. 20, 2014, the disclosure of which is expressly incorporated by reference herein in its entirety.TECHNICAL FIELD[0002]The invention relates to field of nanomaterials and powder metallurgy field, especially a preparation method of rare earth oxide dispersion strengthened fine grain tungsten materials by nano-composite technology.TECHNICAL BACKGROUND[0003]Tungsten has characteristics such as high melting point, high hardness, good high temperature strength, thermal conductivity, electrical conductivity, low thermal expansion coefficient low sputtering and plasma effect, does not react with H, low H+ retention, is a very important high temperature structural materials and functional materials and is widely used as a plasma facing material and divertor component material in the nuclear fusion field.[0004]Among the tungsten materials which h...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Applications(United States)
IPC IPC(8): B22F9/30B22F1/00B22F9/22B22F3/16B22F3/04B22F1/054
CPCB22F9/30B22F3/16B22F3/04B22F2302/25B22F1/0003B22F2301/20B22F2998/10B22F9/22C22C1/05C22C27/04C22C32/0031B22F1/054B22F1/00B22F3/02B22F3/10C22C1/1026B22F9/24B22F1/16B22F9/026B22F1/142B22F1/145B22F2999/00B22F2201/013C22C1/045C22C2200/04
Inventor FAN, JINGLIANHAN, YONG
Owner CENT SOUTH UNIV
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products