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Preparation method of negative thermal expansion material ZrW2O8 thin film

A negative thermal expansion material and negative thermal expansion technology, applied in metal material coating process, ion implantation plating, coating, etc., can solve the problems of no preparation, easy volatilization, and film content, and achieve high deposition rate and high film quality , good reproducible effect

Inactive Publication Date: 2010-08-04
JIANGSU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Electron Beam Evaporation of ZrW 2 o 8 Preparation of ZrW by powder method 2 o 8 thin film, due to the difficult control of the evaporation process and the WO 3 Due to high temperature and volatile reasons, the composition of the prepared film deviates from the ZrW 2 o 8 stoichiometric ratio; ZrW prepared by sol-gel coating method 2 o 8 The preparation parameters of the film are difficult to quantify, and the reaction between the film and the substrate occurs during the high temperature heat treatment at 1150 ° C, and no pure ZrW 2 o 8 Thin films; ZrW prepared by radio frequency magnetron sputtering 2 o 8 Thin films, due to the presence of preferential sputtering of the target part of the substance and WO during heat treatment 3 Volatile, resulting in some impurities in the film
So far, no pulsed laser deposition method has been used to prepare ZrW 2 o 8 film reports

Method used

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  • Preparation method of negative thermal expansion material ZrW2O8 thin film
  • Preparation method of negative thermal expansion material ZrW2O8 thin film

Examples

Experimental program
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Effect test

Embodiment 1

[0024] 1. Target preparation:

[0025] To analyze pure zirconyl nitrate ZrO(NO 3 ) 2 ·5H 2 O and ammonium tungstate N 5 h 37 W 6 o 24 ·H 2 O is the raw material, and the two are dissolved in deionized water to make a solution, which is added dropwise and mixed with stirring, wherein Zr 4+ :W 6+ The molar ratio of the solution is 1:2. After the dropwise addition, the pH value of the solution is adjusted to 3.5 with nitric acid and ammonia water, and the stirring is continued for 2 hours. The ZrW is separated by centrifugation and dried at 60°C to obtain ZrW 2 o 8 Precursor. Heat-treat the precursor at 600°C for 8 hours, take it out and cool it in air, then add 2% PVA to the total mass of the precursor, grind to make the mixture uniform, and then cold press at 80MPa. After debinding at 500°C for 0.5h, sintering at 1150°C for 6h, quenching and drying to obtain pure ZrW 2 o 8 target.

[0026] 2. The quartz substrate is cleaned and activated by the conventional proces...

Embodiment 2

[0032] l. Target preparation:

[0033] To analyze pure zirconyl nitrate ZrO(NO 3 ) 2 ·5H 2 O and ammonium tungstate [N 5 h 37 W 6 o 24 ·H 2 O] as raw material, the two were dissolved in deionized water to make a solution, added dropwise and mixed with stirring, wherein Zr 4+ :W 6+ The molar ratio of the solution is 1:2. After the dropwise addition, the pH value of the solution is adjusted to 4 with nitric acid and ammonia water, and the stirring is continued for 4 hours. The ZrW is separated by centrifugation and dried at 80°C to obtain ZrW 2 o 8 Precursor. Heat-treat the precursor at 650°C for 6 hours, take it out and cool it in air, then add 4% of the total mass of the precursor to PVA, grind to make the mixture uniform, and then cold press at 100MPa. After debinding at 500°C for 0.7h, sintering at 1180°C for 4h, quenching and drying to obtain pure ZrW 2 o 8 target.

[0034] 2. The quartz substrate is cleaned and activated by the conventional process, and the q...

Embodiment 3

[0040] 1. Target preparation:

[0041] To analyze pure zirconyl nitrate ZrO(NO 3 ) 2 ·5H 2 O and ammonium tungstate N 5 h 37 W 6 o 24 ·H 2 O is the raw material, and the two are dissolved in deionized water to make a solution, which is added dropwise and mixed with stirring, wherein Zr 4+ :W 6+ The molar ratio of the solution is 1:2. After the dropwise addition, adjust the pH value of the solution to 4 with nitric acid and ammonia water, continue to stir for 4 hours, centrifuge with a centrifuge, and dry at 100°C to obtain ZrW 2 o 8 Precursor. Heat-treat the precursor at 700°C for 4 hours, take it out and cool it in air, then add 5% PVA to the total mass of the precursor, grind to make the mixture uniform, and then cold-press at 110MPa. After debinding at 500°C for 1h, sintering at 1200°C for 2h, quenching and drying to obtain pure ZrW 2 o 8 target.

[0042] 2. The quartz substrate is cleaned and activated by the conventional process, and the quartz substrate is ...

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Abstract

The invention relates to a preparation method of a film of negative thermal expansion material ZrW2O8, which belongs to the technical field of preparing inorganic functional film material. The preparation method is characterized in that a pulse laser method is adopted to prepare the film of the negative thermal expansion material ZrW2O8. The preparation method has the advantage of utilizing a pulse laser depositing method to prepare the film of ZrW2O8, thus leading the chemical components of the deposited film and target materials to maintain excellent consistency and avoiding the problem of preferential depositing of a certain component; simultaneously the escape grains have larger energies, thus facilitating to the growth of the film, having a high quality for preparing the film and having excellent repeatability and high depositing speed during the preparation process.

Description

technical field [0001] The invention belongs to the technical field of preparation of inorganic functional film materials, in particular to a negative thermal expansion ZrW 2 o 8 The method of film preparation. Background technique [0002] wxya 2 o 8 It is an excellent isotropic negative thermal expansion compound, and its negative thermal expansion coefficient is as high as -8.7×10 in the temperature range of 0.5-1050K -6 K -1 . This excellent property enables the negative thermal expansion material to be used alone or to prepare composite materials, thereby precisely controlling the expansion coefficient of the material. Its potential applications include electronics, optics, optical communication systems and daily life. At present, the material scientists in the world regard ZrW as 2 o 8 Powder, ceramics and related composite materials are used as research objects, focusing on revealing their related preparation methods, the mechanism of negative thermal expansio...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C23C14/54C23C14/28C23C14/58C23C14/08
Inventor 刘红飞程晓农张志萍杨娟
Owner JIANGSU UNIV
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