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Process for preparing niobium-doped strontium titanate film

A technology of doping strontium niobate titanate thin film, which is applied in the field of preparation of strontium niobium titanate thin film, can solve the problems of harsh preparation environment, high cost, inconvenient operation, etc. smooth effect

Inactive Publication Date: 2008-12-31
SOUTHWEST JIAOTONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the existing sol-gel method has the following disadvantages: 1. The raw materials used are metal alkoxides, such as niobium ethoxide, niobium butoxide, and strontium ethoxide. These raw materials are expensive and expensive; 2. Metal alkoxides It is easily hydrolyzed in the air, and the preparation process needs to be carried out under a protective atmosphere such as nitrogen, which has strict requirements on the preparation environment and is not easy to operate

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  • Process for preparing niobium-doped strontium titanate film
  • Process for preparing niobium-doped strontium titanate film

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Embodiment 1

[0019] A specific embodiment of the present invention is a method for preparing a strontium niobate-doped titanate thin film, the specific steps of which are:

[0020] a. Preparation of niobium-citrate ethylene glycol solution: place niobium oxide in hydrofluoric acid, stir at 80°C to make it fully dissolve to form a niobium oxide solution, add ammonia water dropwise to the solution to form a white niobium hydroxide precipitate, Aging for 4 hours; after filtration, the precipitate was washed with 3% dilute ammonia water, dehydrated and dried in a vacuum; the dried precipitate was dissolved in citric acid in ethylene glycol solution at 60°C and fully stirred to obtain Niobium-citrate solution in ethylene glycol.

[0021] b. Preparation of strontium niobate titanate precursor solution: molar ratio of Sr 2+ : Ti 4+ : Nb 5+ =1: 0.95: 0.05, respectively measure strontium acetate, butyl titanate and the niobium-citrate ethylene glycol solution prepared in step a; dissolve stronti...

Embodiment 2

[0025] a, niobium-citric acid ethylene glycol solution preparation: niobium oxide Nb 2 o 5 Add it into hydrofluoric acid HF, heat in a water bath at 85°C for 6 hours, and keep stirring, so that the Nb 2 o 5 Fully dissolve. Slowly add ammonia water dropwise to the solution to form white Nb(OH) 5 Precipitate, which was aged at 80°C for 6 hours and then filtered, washed repeatedly with 2% dilute ammonia to remove F - ions, dehydrated and dried in vacuum for 2 minutes. The resulting white precipitate was dissolved in citric acid in ethylene glycol solution at 80° C., and stirred thoroughly to form Nb-citric acid in ethylene glycol solution.

[0026] b. Preparation of strontium niobate titanate precursor solution: molar ratio of Sr 2+ : Ti 4+ : Nb 5+ =1: 0.995: 0.005, respectively measure strontium acetate, butyl titanate and the niobium-citrate ethylene glycol solution prepared in step a; dissolve strontium acetate in acetic acid to form solution A; The molar amount of dr...

Embodiment 3

[0029] a. Preparation of niobium-citrate ethylene glycol solution: place niobium oxide in hydrofluoric acid, stir at 70°C to fully dissolve to form a niobium oxide solution, add ammonia water dropwise to the solution to form a white niobium hydroxide precipitate, Aging for 5 hours; after filtration, the precipitate was washed with 4% dilute ammonia water, dehydrated and dried in vacuum; the dried precipitate was dissolved in citric acid in ethylene glycol solution at 70°C and fully stirred to obtain Niobium-citrate solution in ethylene glycol.

[0030] b. Preparation of strontium niobate titanate precursor solution: molar ratio of Sr 2+ : Ti 4+ : Nb 5+ =1: 0.95: 0.05, respectively measure strontium acetate, butyl titanate and the niobium-citrate ethylene glycol solution prepared in step a; dissolve strontium acetate in acetic acid to form solution A; The molar amount of dropwise addition is Ti 4+ 1.3 times of acetylacetone, then add ethylene glycol methyl ether solvent to ...

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Abstract

A preparation method for niobium-doped strontium titanate thin film comprises the following steps: a)the preparation of niobium-citric acid glycol solution; putting the niobium oxide in hydrofluoric acid to form niobium oxide solution at 70-85 DEG C, then adding ammonia dropwise and aging the solution for 4 to 6 hours; after filtering, taking out the sediment and washing the sediment with dilute ammonia; after drying, the sediment is dissolved into the ethylene glycol solution of the citric acid at 60-80 DEG C. b)the preparation of precursor solution; based on molar ratio, Sr2+: Ti4+: Nb5+ is equal to 1:1-x: x, while x is equal to 0.1- 0.005; measuring and taking strontium acetate, tetrabutyl titanate and the niobium-citric acid glycol solution in the step a; dissolving the strontium acetate into water to get a solution A; adding acetylacetone dropwise into butyl titanate, and then adding ethylene glycol ether solvent to get a solution B; mixing the solution A with the solution B, and then adding the niobium-citric acid glycol solution into the mixed solution, followed by 1-4: 1 of ethylene glycol and glycerol, so that the concentration of the solution can reach Sr2+ ion 0.15-0.40 mol / L. c)thermal decomposition and sintering. The method uses cheap raw materials and has simple production technology and low production costs, which facilitates commercial applications.

Description

technical field [0001] The invention relates to a preparation method of an inorganic material, in particular to a preparation method of a strontium niobate-doped titanate thin film. Background technique [0002] Strontium titanate (SrTiO 3 ) material has a typical perovskite-type structure, the complete stoichiometric ratio of SrTiO 3 As an insulator, its performance will change greatly with the change of doping substance, doping amount and sintering process, such as strontium niobium titanate material, which has superconductivity, semiconductivity, ferroelectricity and pressure sensitivity , heat sensitivity and photosensitivity, low dielectric loss, high dispersion frequency, good thermal stability. It can be used to manufacture grain boundary layer capacitors, varistors, oxygen sensitive elements, PTC thermistors, and is also widely used as electrodes and sensors. It can also be used as a buffer layer for superconducting materials and ferroelectric materials. It is a k...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/47C04B35/622
Inventor 赵立峰黄正银赵勇
Owner SOUTHWEST JIAOTONG UNIV
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