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Preparation of potassium lithium niobate nanometer powder using citric acid gelification method

A technology of potassium lithium niobate and nano powder, applied in chemical instruments and methods, niobium compounds, inorganic chemistry and other directions, can solve the problems of high calcination temperature, poor sintering activity of powder, high price, etc., to overcome the high calcination temperature , the effect of reducing environmental pollution and simplifying the preparation process

Inactive Publication Date: 2005-03-23
HARBIN INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The invention adopts the citric acid gel method to prepare potassium lithium niobate nanopowder, which solves the problems that the metal alkoxide is not easy to obtain, is expensive and easy to hydrolyze in the sol-gel process, and overcomes the high calcining temperature of the solid phase reaction method and the problem of powder The problem of poor sintering activity

Method used

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  • Preparation of potassium lithium niobate nanometer powder using citric acid gelification method
  • Preparation of potassium lithium niobate nanometer powder using citric acid gelification method

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specific Embodiment approach 1

[0005] Specific embodiment one: this embodiment is carried out according to the following steps: 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 + : K + =(5+x): (2-x): 3 ratio Lithium carbonate, Nb-citric acid solution and potassium carbonate are mixed, after fully stirring, add excess citric acid, make metal ion (Nb 5+ , Li + 、K + ) and citric acid in a molar ratio of 1:3, adjust the pH value of the solution to 6 to 7 with ammonia water; c, add ethylene glycol to the mixed solution, and stir evenly to form a potassium lithium niobate precursor solution; d, mix The solution was heated at 60-100°C for 20-30h to obtain a viscous gel-lik...

specific Embodiment approach 2

[0006] Specific embodiment two: this embodiment is carried out according to the following steps: 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 (ICP) 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 dissolve, then the potassium carbonate of 0.15mol is added wherein, after fully stirring, add excessive citric acid, make metal ion (Nb 5+ , Li + 、K + ) and citric acid in a molar ratio of 1:3, the pH value of the solution is adjusted to 6-7 with ammonia water;...

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Abstract

A process for preparing nano-potasium lithium niobate includes such steps as dissolving Nb2O3 in HF, adding ammonium oxalate, dropping ammonia water to form Nb(OH)5, ageing filtering, washing, dissolving it in citric acid to form Nb-citric acid solution, mixing it with lithium carbonate and potassium carbonate, regulating pH value, adding ethanediol to generate precursor solution, heating to become gel solid, and calcining.

Description

Technical field: [0001] The invention relates to a preparation method of an inorganic material, in particular to a preparation method of potassium lithium niobate nanopowder. Background technique: [0002] Potassium lithium niobate has excellent electro-optic properties and nonlinear optical properties. It can realize non-critical matching in a wide range of wavelengths (790-920nm) at room temperature and convert it into blue light. Therefore, KLN is an excellent blue light frequency doubling material. At the same time, KLN is also a photorefractive material. Currently, potassium lithium niobate (K 3 Li 2-x Nb 5+x o 15+2x , 0≤x<0.5, KLN) powders are mostly prepared by sol-gel (sol-gel) method and solid-state reaction method. The above-mentioned methods all have respective limitations, such as the sol-gel method, which has the following disadvantages: (1) The raw materials used are usually metal alkoxides, such as niobium ethoxide, niobium butoxide, potassium butoxid...

Claims

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Application Information

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IPC IPC(8): C01G33/00C04B35/495C04B35/624
Inventor 李垚
Owner HARBIN INST OF TECH
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