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Method of preparing lithium niobate nanometer powder at low-temp by citric acid gel method

A nano-powder and citric acid technology, applied in chemical instruments and methods, niobium compounds, inorganic chemistry, etc., can solve the problems of difficult acquisition of metal alkoxide, poor sintering activity of powder, high calcination temperature, etc., to overcome high calcination temperature , low calcination temperature and simplified preparation process

Inactive Publication Date: 2006-05-24
HARBIN INST OF TECH
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Problems solved by technology

[0003] The invention uses the citric acid gel method to prepare lithium niobate nanopowder at low temperature, which solves the problems that metal alkoxides are not easy to obtain, expensive and easily hydrolyzed in the sol-gel process, and the method can also overcome the solid-phase reaction method Problems of high calcination temperature and poor sintering activity of powder

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  • Method of preparing lithium niobate nanometer powder at low-temp by citric acid gel method
  • Method of preparing lithium niobate nanometer powder at low-temp by citric acid gel method

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specific Embodiment approach 1

[0005] Specific embodiment one: present embodiment is realized in this way: a, Nb 2 o 5 Dissolve in HF at 70-90°C, then add excess ammonium oxalate solution to it, after mixing thoroughly, add ammonia water dropwise 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, according to the molar ratio of Nb 5+ : Li + =1:1 ratio Lithium carbonate is joined in the Nb-citric acid solution, stirs and it is fully dissolved; c, add excessive citric acid solution in the solution, make the mol ratio of metal ion and citric acid be 1:(1.5 ~3); d, then ethylene glycol is added in the above-mentioned solution, and the mol ratio of ethylene glycol and citric acid is (1~2): 1, forms lithium niobate precursor solution after stirring; E, this solution is in Heating at 60-100°C for 20-30 hours to obtain a viscous gel-like solid; f, finally ca...

specific Embodiment approach 2

[0006] Specific embodiment two: present embodiment is realized in this way: a, Nb 2 o 5 Dissolve in HF at 80°C, then add excess ammonium oxalate solution to it, after mixing well, add ammonia water dropwise to the solution to form white Nb(OH) 5 Precipitate, the precipitate was aged at 80°C for 12 hours, filtered and washed, dissolved in citric acid aqueous solution to form a light yellow Nb-citric acid solution, and the solution was measured by inductively coupled plasma emission spectrometry (IP) method The concentration of metal Nb in the medium; b, get Nb-citric acid solution (containing Nb 5+ 0.5mol), the lithium carbonate of 0.1mol is added in the Nb-citric acid solution, stirring makes it fully dissolved; c, in the solution, add excessive citric acid solution, make the mol ratio of metal ion and citric acid be 1: 3; d, then ethylene glycol is added to the above solution, the molar ratio of ethylene glycol and citric acid is 1.8: 1, after stirring evenly, a lithium nio...

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Abstract

The invention discloses a method for preparing lithium niobate nanometer powder at low temperature by using a citric acid gel method, which relates to a preparation method of lithium niobate. The present invention is carried out according to the following steps: a, Nb 2 o 5 Dissolve in HF, then add excess ammonium oxalate solution to it, after mixing well, add ammonia water dropwise to the solution to form white Nb(OH) 5 Precipitate, the precipitate is aged, filtered and washed, dissolved in citric acid aqueous solution to form a light yellow Nb-citric acid solution; b, lithium carbonate is added to the Nb-citric acid solution, stirred to fully dissolve ; c, adding excess citric acid solution to the solution; d, then adding ethylene glycol to the above solution, stirring evenly to form a lithium niobate precursor solution; e, heating the solution to obtain a viscous gel Solid; f, finally calcining the gel to obtain nanometer LiNbO 3 Powder. The invention has the advantages of low cost, little environmental pollution and simple process.

Description

technical field [0001] The invention relates to a preparation method of lithium niobate nanometer powder. Background technique [0002] Lithium niobate is an important ferroelectric material. It has a series of special properties such as piezoelectricity, electro-optic, acousto-optic, thermoelectric, photorefractive and nonlinear optical properties. Due to these characteristics, lithium niobate has been Widely used in light guides, optical modulators, optical switches, non-volatile memory, surface acoustic wave and second harmonic generators and other devices. For LiNbO 3 Polycrystalline ceramic powder is mostly prepared by sol-gel process and solid-state reaction method, but the above-mentioned methods have their own limitations. For example, the sol-gel method has the following disadvantages: (1) The raw materials used are usually metal alkoxides , such as niobium ethoxide, niobium butoxide, lithium butoxide, etc. There are no domestic products for these raw materials, a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C04B35/495C04B35/624C01G33/00
Inventor 赵九蓬强亮生张蕾
Owner HARBIN INST OF TECH
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