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Preparation method of single-phase pyrochlore-type La2Zr2O7 nano-powder

A technology of nano-powder and pyrochlore, which is applied in the field of preparing single-phase pyrochlore-type La2Zr2O7 nano-powder, which can solve the problems of easy sintering, high crystallinity, and good dispersion, and achieve no corrosion of equipment and good crystallinity , The effect of simple process

Active Publication Date: 2013-11-20
NAT UNIV OF DEFENSE TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the invention is to overcome the deficiencies in the prior art, solve the existing sol-gel method to prepare La 2 Zr 2 o 7 Insufficient high-temperature stability of the powder, easy sintering, and low mechanical strength, etc., provide a single crystal phase, high crystallinity, good dispersion, and small particle size La 2 Zr 2 o 7 Powder preparation method

Method used

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  • Preparation method of single-phase pyrochlore-type La2Zr2O7 nano-powder
  • Preparation method of single-phase pyrochlore-type La2Zr2O7 nano-powder

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Experimental program
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Effect test

Embodiment 1

[0028] A kind of single-phase pyrochlore type La prepared by the present invention 2 Zr 2 o 7 Nano powder mainly has the following steps:

[0029] (1) Molar ratio of ZrOCl 2 ·8H 2 O:H 2 O:CH 3 OH=1:5:10, 5.00g ZrOCl 2 ·8H 2 O was slowly added to the mixed solution of 1.40g water and 4.97g methanol, and kept stirring to obtain a transparent solution A liquid; at the same time, by molar ratio La(NO 3 ) 3 ·6H 2 O:H 2 O:CH 3 OH=1:0.5:10, 6.66g La(NO 3 ) 3 ·6H 2 O slowly add 0.14g of water and 4.97g of methanol in the mixed solution, stirring constantly, to obtain a transparent solution B liquid;

[0030] (2) Mix liquid A and liquid B to obtain a transparent mixed solution, and stir evenly;

[0031] (3) Under the condition of continuous stirring, add molar ratio: citric acid: Zr to the mixed solution in sequence 4+ =0.1:1 Add 0.33g of citric acid, polyethylene glycol by mass ratio: Zr 4+ =1:1 Add polyethylene glycol 1.41g, wherein, the number average molecular wei...

Embodiment 2

[0036] A kind of single-phase pyrochlore type La prepared by the present invention 2 Zr 2 o 7 Nano powder mainly has the following steps:

[0037] (1) Molar ratio of ZrOCl 2 ·8H 2 O:H 2 O:C 3 h 7 OH=1:8:10, 5.00g ZrOCl 2 ·8H 2 O was slowly added to the mixed solution of 2.24g water and 9.31g propanol, and kept stirring to obtain a transparent solution A; meanwhile, La(NO 3 ) 3 ·6H 2 O:H 2 O:C 3 h 7 OH=1:2:10, 6.66g La(NO 3 ) 3 ·6H 2 O slowly add 0.56g water and 9.31g propanol in the mixed solution, stir constantly, obtain transparent solution B liquid;

[0038] (2) Mix liquid A and liquid B to obtain a transparent mixed solution, and stir evenly;

[0039] (3) Under the condition of continuous stirring, add molar ratio: citric acid: Zr to the mixed solution in sequence 4+ =0.4:1 Add 1.32g of citric acid, polyethylene glycol by mass ratio: Zr 4+ =1:7.5 adds Polyethylene Glycol 0.19g, wherein, the number average molecular weight of Polyethylene Glycol is 20000...

Embodiment 3

[0044] A kind of single-phase pyrochlore type La prepared by the present invention 2 Zr 2 o 7 Nano powder mainly has the following steps:

[0045] (1) Molar ratio of ZrOCl 2 ·8H 2 O: H 2 O: C 2 h 5 OH=1:6:10, 5.00g ZrOCl 2 ·8H 2 O was slowly added to the mixed solution of 1.68g water and 7.14g ethanol, and kept stirring to obtain a transparent solution A; meanwhile, La(NO 3 ) 3 ·6H 2 O: H 2 O: C 2 h 5 OH=1:1:10, 6.66g La(NO 3 ) 3 ·6H 2 O slowly add 0.28g water and 7.14g ethanol in the mixed solution, stir constantly, obtain transparent solution B liquid;

[0046] (2) Mix liquid A and liquid B to obtain a transparent mixed solution, and stir evenly;

[0047] (3) Under the condition of continuous stirring, add molar ratio: citric acid: Zr to the mixed solution in sequence 4+ =0.2:1 Add citric acid 0.65g, polyethylene glycol by mass ratio: Zr 4+ =1:5 adds polyethylene glycol 0.28g, wherein, the number average molecular weight of polyethylene glycol is 20000, b...

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Abstract

The invention relates to a preparation method of single-phase pyrochlore-type La2Zr2O7 nano-powder. The preparation method is characterized in that the La2Zr2O7 nano-powder is obtained by ageing, drying and high-temperature roasting by using Zr<4+> and La<3+> hydration inorganic salt as a precursor, citric acid as a complexing agent, an amide organic matter as a gel accelerant and polyethylene glycol as a dispersing agent. The single-phase pyrochlore-type La2Zr2O7 nano-powder has the advantages that the particle size of the obtained La2Zr2O7 nano-powder is 20-100nm, the molar ratio of Zr to La is approximate to 1:1, the crystal structure of the La2Zr2O7 nano-powder is single-phase pyrochlore-type, and the La2Zr2O7 nano-powder has high degree of crystallinity and excellent performances such as low heat conduction, sintering resistance, good high-temperature stability and the like and is applied to the field of thermal barrier coatings of aviation turbine engines and protective coatings in high-temperature wet-oxygen environments.

Description

technical field [0001] The invention relates to a preparation method of a single-phase rare earth oxide ceramic ultrafine powder, in particular to the preparation of single-phase pyrochlore-type La by a sol-gel method. 2 Zr 2 o 7 Nano powder. Background technique [0002] As the gas temperature and pressure of aero turbine engines continue to increase, traditional high-temperature structural alloys can no longer meet the demand. Improving the stability and service life of materials at higher temperatures is an urgent problem to be solved. At present, thermal barrier coatings (TBCs) technology has become a current research hotspot by reducing the surface temperature of bulk materials to improve engine service life. The usual methods for preparing TBCs include plasma spraying, electron beam physical vapor deposition, chemical vapor deposition, and laser melting. Among them, the plasma spraying method is relatively mature and widely used, and its raw material is powder mater...

Claims

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Application Information

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IPC IPC(8): C04B35/48C04B35/50C04B35/626
Inventor 李伟王生学王松祝玉林陈朝辉
Owner NAT UNIV OF DEFENSE TECH
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