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Method for preparing barium-strontium niobate powder and barium-strontium niobate film by organic gel method

A technology of barium strontium niobate and organogel, which is applied in chemical instruments and methods, calcium/strontium/barium compounds, inorganic chemistry, etc., can solve the problems of easy hydrolysis, high price, and difficulty in obtaining metal alkoxides.

Inactive Publication Date: 2005-01-26
HARBIN INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] In order to solve the problems that metal alkoxides are difficult to obtain, expensive and easily hydrolyzed in the sol-gel process, the present invention provides a method for preparing barium strontium niobate powder and barium strontium niobate film by organogel method, which has The advantages of simple process, low cost and little environmental pollution

Method used

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  • Method for preparing barium-strontium niobate powder and barium-strontium niobate film by organic gel method
  • Method for preparing barium-strontium niobate powder and barium-strontium niobate film by organic gel method
  • Method for preparing barium-strontium niobate powder and barium-strontium niobate film by organic gel method

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specific Embodiment approach 1

[0005] Specific embodiment one: this embodiment is prepared according to the following steps: a, preparation of Nb-citric acid complex: Nb 2 o 5 Dissolve in HF at 70-90°C, then add ammonium oxalate solution to it, after mixing thoroughly, add ammonia water to the solution to form white Nb(OH) 5 Precipitate, which is aged at 70-90°C for 10-14 hours, filtered and washed, dissolved in citric acid aqueous solution to form a light yellow Nb-citric acid solution; b, water-soluble Ba-EDTA and Preparation of Sr-EDTA complex: equimolar Ba(NO 3 ) 2 and EDTA were dissolved in deionized water, and the pH was adjusted to be alkaline with ammonia water to obtain a transparent Ba-EDTA solution, and finally HNO 3 Adjust pH=7, prepare Sr-EDTA solution in the same way; c, preparation of barium strontium niobate nanopowder: measure Sr-EDTA, Ba-EDTA and Nb-citric acid solution respectively, control molar ratio as Sr 2+ : Ba 2+ : Nb 5+ =x: (1-x): 2, wherein x=0~1, add citric acid after the t...

specific Embodiment approach 2

[0006] Specific implementation mode two: see figure 1 , this embodiment is prepared according to the following steps: a, 0.1molNb 2 o 5 Add it into 1.4mol of HF, heat in a water bath at 80°C for 48-50h, and keep stirring to make Nb 2 o 5 Dissolved in HF to form NbOF 5 2- or NbF 7 2- complex ion; then add the newly prepared ammonium oxalate aqueous solution, and keep C 2 o 4 2- Ion excess; add ammonia dropwise to solution to form white Nb(OH) 5 precipitate, the precipitate was aged at 80 °C for 12 h, filtered, and washed with 5 wt% ammonia to remove F - ion; finally the Nb(OH) 5 Precipitation is dissolved in the citric acid aqueous solution, forms light yellow Nb-citric acid solution, adopts inductively coupled plasma emission spectrometry (ICP) to measure the concentration of metal ion; b, 0.1molBa (NO 3 ) 2 After mixing with 0.1mol EDTA, add deionized water, adjust the pH with ammonia water to make it alkaline, and keep stirring to obtain a transparent Ba-EDTA so...

specific Embodiment approach 3

[0007] Specific embodiment three: this embodiment is prepared according to the following steps: a, preparation of Nb-citric acid complex: Nb 2 o 5 Dissolve in HF at 70-90°C, then add ammonium oxalate solution to it, after mixing thoroughly, add ammonia water to the solution to form white Nb(OH) 5 Precipitate, which is aged at 70-90°C for 10-14 hours, filtered and washed, dissolved in citric acid aqueous solution to form a light yellow Nb-citric acid solution; b, water-soluble Ba-EDTA and Preparation of Sr-EDTA complex: equimolar Ba(NO 3 ) 2 and EDTA were dissolved in deionized water, and the pH was adjusted to be alkaline with ammonia water to obtain a transparent Ba-EDTA solution, and finally HNO 3 Adjust pH=7, prepare Sr-EDTA solution in the same way; c, the preparation of SBN film: Measure Sr-EDTA, Ba-EDTA and Nb-citric acid solution respectively, control molar ratio as Sr 2+ : Ba 2+ : Nb 5+ =x: (1-x): 2, wherein x=0~1, after mixing the three solutions evenly, add cit...

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Abstract

The invention discloses a method for preparing barium-strontium niobate powder and barium-strontium niobate film by organic gel method which comprises the steps of, (1) dissolving Nb2O5 into HF, charging ammonium oxalate and mixing, dropping ammoniacal liquor to form Nb(OH)5, dissolving the deposit into aqueous solution of citric acid, forming Nb-citric acid solution, (2) dissolving Ba(NO3)2 and EDTA into deionized water, adjusting pH to alkaline with ammoniacal liquor, so as to obtain Ba-EDTA solution, adjusting pH=7 with HNO3, preparing Sr-EDTA solution by the same process, (3) mixing Sr-EDTA, Ba-EDTA and Nb-citric acid solutions, charging citric acid, adjusting pH=8 with ammonia, obtaining light yellow sol, drying the sol to obtain gel form solid, calcining to obtain the end product.

Description

Technical field: [0001] The invention relates to the preparation process of inorganic materials, in particular to the preparation process of barium strontium niobate powder and barium strontium niobate film. Background technique: [0002] At present, strontium barium niobate SBN powder and ferroelectric thin film are mostly prepared by sol-gel (sol-gel) method, which has the following disadvantages: (1) The raw materials used are usually metal alkoxides, such as niobium ethoxide and butanol Niobium, strontium butoxide, barium butoxide, etc. There are no domestic products for these raw materials, and the imported reagents are expensive. For example, the price of niobium pentaethoxide produced by Inorgtech, a famous British company that produces metal alkoxides, is 1300 pounds / L; (2) raw materials Metal alkoxides are easily hydrolyzed in the air, so the conditions required in the preparation process are very harsh. In addition to requiring the preparation of films in non-aqueo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01F11/00C01G33/00
Inventor 赵九蓬李垚
Owner HARBIN INST OF TECH
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