Hydrothermal preparation method of ultrafine yttrium oxide doped tungsten composite powder

A composite powder, yttrium oxide technology, applied in the field of powder preparation engineering, can solve problems such as grain growth and agglomeration, and achieve the effect of reducing waste, shortening calcination and reduction time

Active Publication Date: 2018-11-13
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The hydrothermal method does not introduce impurities, and the grains are relatively small, but the metal oxides precipitated later in the hydrothermal process will deposit on the metal oxide grains precipitated earlier, causing the grains to grow and agglomerate

Method used

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  • Hydrothermal preparation method of ultrafine yttrium oxide doped tungsten composite powder
  • Hydrothermal preparation method of ultrafine yttrium oxide doped tungsten composite powder
  • Hydrothermal preparation method of ultrafine yttrium oxide doped tungsten composite powder

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] (1) Dissolve 2g of AMT and 0.1332g of yttrium nitrate hexahydrate in 25mL of deionized water, then add 0.1g of PVP, and add the mixture to 50mL with deionized water (the concentration of AMT is 0.04g / mL, and the concentration of yttrium nitrate hexahydrate The quality of PVP is 6.66% of the quality of ammonium metatungstate, the quality of PVP is 5% of the quality of ammonium metatungstate), adjust the pH to 3 with nitric acid, and then use ultrasonic treatment (ultrasonic treatment power is 100W, ultrasonic time 1h) to fully dissolve After dispersion, a mixed solution is obtained.

[0032] (2) Put the mixed solution in a reaction kettle with a filling capacity of 70%, conduct a hydrothermal reaction at 240° C., and keep it warm for 12 hours.

[0033] (3) After the reaction, the obtained suspension was filtered and washed twice, and then vacuum-dried at 60° C. for 8 h.

[0034] (4) Calcining the powder in air flow at 500° C. for 0.5 h to remove residual dispersant to o...

Embodiment 2

[0037] (1) Dissolve 1.0g of AMT and 0.067g of yttrium nitrate hexahydrate in 25mL of deionized water, then add 0.15g of SDS, and add the mixture to 50mL with deionized water (the concentration of AMT is 0.02g / mL, and the concentration of yttrium nitrate hexahydrate The mass of the hydrate is 6.66% of the mass of ammonium metatungstate, the mass of SDS is 15% of the mass of ammonium metatungstate), the pH is adjusted to 1 with nitric acid, and then ultrasonic treatment (ultrasonic treatment power is 60W, ultrasonic time 2h) After fully dissolving and dispersing, a mixed liquid is obtained.

[0038] (2) Put the mixed solution in a reaction kettle with a filling capacity of 80%, conduct a hydrothermal reaction at 180° C., and keep it warm for 18 hours.

[0039] (3) After the reaction, the obtained suspension was filtered and washed three times, and then vacuum-dried at 60° C. for 8 h.

[0040] (4) Calcining the powder in air flow at 450° C. for 1 h to remove residual dispersant ...

Embodiment 3

[0043] (1) Dissolve 5g of AMT and 0.533g of yttrium nitrate hexahydrate in 25mL of deionized water, then add 0.25g of CTAB, and add the mixture to 50mL with deionized water (the concentration of AMT is 0.1g / mL, and the concentration of yttrium nitrate hexahydrate The quality of the substance is 2.65% of the quality of ammonium metatungstate, the quality of CTAB is 5% of the quality of ammonium metatungstate), the pH is adjusted to 0.1 with nitric acid, and then ultrasonic treatment (ultrasonic treatment power is 300W, ultrasonic time 0.5h) After fully dissolving and dispersing, a mixed liquid is obtained.

[0044] (2) Put the mixed solution in a reaction kettle with a filling capacity of 90%, conduct a hydrothermal reaction at 180° C., and keep it warm for 20 hours.

[0045] (3) After the reaction, the obtained suspension was filtered and washed four times, and then vacuum-dried at 60° C. for 8 h.

[0046] (4) Calcining the powder in air flow at 400° C. for 0.75 h to remove r...

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Abstract

The invention provides a hydrothermal preparation method of ultrafine yttrium oxide doped tungsten composite powder. The hydrothermal preparation method comprises the steps of dissolving one of polyvinylpyrrolidone (PVP), sodium dodecyl sulfate (SDS) or cetyl trimethyl ammonium bromide (CTAB) as dispersant in water together with ammonium metatungstate and yttrium nitrate hexahydrate, regulating pHwith nitric acid or hydrochloric acid, and fully dispersing and dissolving by ultrasonic treatment so as to prepare a solution or a suspension; putting the solution or the suspension in a reaction kettle for hydrothermal reaction; filtering, washing and drying the suspension after the reaction is completed; and calcining composite powder in air flow so as to remove residual dispersant, and performing two-step reduction with hydrogen so as to prepare the ultrafine yttrium oxide doped tungsten composite powder. Compared with a mechanical alloying method, a vacuum drying method, a sol-gel method, a wet chemical precipitation method, a spray drying method and the like, the powder prepared by adopting the hydrothermal preparation method adding the dispersant has the advantages of small grainsand less aggregation, the average grain size can reach about 10 nm, and the grain size distribution is narrow. The method has obvious advantages.

Description

technical field [0001] The invention proposes an ultrafine yttrium oxide doped tungsten W-Y 2 o 3 The technology of the hydrothermal preparation method of composite powder belongs to the technical field of powder preparation engineering. Background technique [0002] Tungsten-based alloy materials play an important role in national defense, aerospace and other fields, and are also widely used in electronic information, environment, energy and power machinery. With the rapid development of industries such as information, energy, environment, and national defense, higher requirements are placed on the performance of tungsten-based alloy materials. Because plasma-oriented materials PFM must have high thermal conductivity, high melting point, high thermal shock resistance and other properties, tungsten is considered to be the most likely candidate material for future fusion reactor PFM. However, tungsten-based materials also have many problems that need to be solved urgently,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B22F9/22
CPCB22F9/22
Inventor 马宗青扈伟强董智柳楠刘永长王祖敏余黎明李冲刘晨曦
Owner TIANJIN UNIV
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