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Method for liquid phase synthesis of barium titanate nanopowder

A liquid-phase synthesis, barium titanate technology, applied in chemical instruments and methods, titanium compounds, calcium/strontium/barium compounds, etc., can solve problems such as long sintering time, high post-sintering temperature, difficult to control particle size and shape , to achieve the effects of low cost, lower post-sintering temperature, regular shape and controllable post-sintering temperature

Inactive Publication Date: 2007-08-01
UNIV OF SCI & TECH BEIJING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0015] The object of the present invention is to provide a liquid-phase synthesis method of barium titanate or barium titanate-based doped nano-powder, which solves the problem of agglomeration of barium titanate nano-powder prepared by liquid-phase method, difficult control of particle size and morphology, and The post-sintering temperature of the co-precipitation method is too high and the sintering time is too long.

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  • Method for liquid phase synthesis of barium titanate nanopowder
  • Method for liquid phase synthesis of barium titanate nanopowder
  • Method for liquid phase synthesis of barium titanate nanopowder

Examples

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Effect test

Embodiment 1

[0041] Using n-octane as solvent, Span 80 as active agent, n-hexanol as auxiliary agent and barium acetate solution to form microemulsion, then azeotropic distillation to synthesize nano-barium titanate precursor, and calcining at low temperature 600°C to nano-titanate barium powder. The raw material n-octane 200ml, Span 80 and n-butanol are fully stirred and mixed evenly, the dosage of Span 80 is 20ml, 40ml, 60ml respectively, when the dosage of Span 80 is 40ml, the dosage of n-butanol is 20ml, 40ml respectively . for 1-5. Divide the mixture of n-octane, Span 80 and n-butanol into two parts according to the volume ratio of 3:1 for later use. Then, 20 ml of 1 mol / l barium acetate aqueous solution is added dropwise in a large volume of standby mixed organic solvent to form a microemulsion. Measure 6.8ml of butyl titanate into a small volume of spare mixed organic solvent and stir evenly. Pour the barium acetate microemulsion into the butyl titanate solution, stir well, and ...

Embodiment 2

[0051] Respectively use xylene 200ml, nonane 200ml, n-hexanol 200ml as solvent, form microemulsion with barium acetate solution according to the proportioning of surfactant and auxiliary agent of embodiment 1-5, when using n-hexanol as solvent, do not add auxiliary agent. The dosage and operating steps of other reagents except solvent are the same as in Example 1, but the oil bath temperature is the boiling point of each solvent when the second boiling point is distilled, which are respectively 139°C, 150°C, and 158°C, which are recorded as 2-1, 2- 2, 2-3. The particle size analysis results of the obtained barium titanate powder are shown in Table 2.

[0052] Table 2: Comparison of the specific surface area S and the calculated average particle size d of the powder obtained by forming microemulsions with different types of solvents

Embodiment 3

[0054] According to the reagent consumption provided in embodiment 1-2, use n-octane as solvent, n-hexanol as auxiliary agent, use Tween 60, sodium dodecylsulfonate (SDS), hexadecyltrimethyl bromide respectively Ammonium chloride (CTAB), Triton X-100, etc. indicate that the active agent and barium acetate aqueous solution form a microemulsion, which is recorded as 3-1, 3-2, 3-3, and 3-4. The results of particle size analysis of the finally obtained barium titanate powder are shown in Table 3.

[0055] Table 3: Comparison of specific surface area S and calculated average particle size d of powder obtained from different types of active agents

[0056] sample

[0057] 3-4

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Abstract

This invention provides a method to synthesize nano powder of barium titanate in liquid phase, which belongs to electronic ceramic predecessor powder field, and comprises: with microemulsion azeotropic distillation method, reacting in W / O micro reactor with proper emulsifier; exactly, using Ba and Ti with mole radio as 1~1.5 and oxalic acid or ammonium oxalate with mole radio to Ba as 1~3 to prepare required material; mixing evenly the main organic solvent, surfactant and auxiliary agent to prepare organic solvent; preparing microemulsion, distilling, filtering, drying, calcining, and finally obtaining the objective product. The advantages of this invention cover that the prepared powder has little birdnesting, small particle size, and controllable shape.

Description

technical field [0001] The invention belongs to the technical field of synthesis of electronic ceramic precursor powder, in particular to a liquid-phase synthesis method of barium titanate or barium titanate-based doped nanometer powder. This invention is a project supported by the National Outstanding Youth Fund (No.50325209). Background technique [0002] Barium titanate has excellent electrical properties such as high dielectric constant, ferroelectricity, piezoelectricity and positive temperature coefficient effects, and is widely used in the electronic ceramic industry. With the development of multilayer ceramic capacitors (MLCC) in recent years, the performance requirements for barium titanate powder have increased, and the demand has increased. [0003] Practice has proved that the excellent performance of advanced ceramic materials can be tested through its special chemical composition and microstructure, which in turn requires careful control of each continuous pro...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G23/00C01F11/00C04B35/468C04B35/626
Inventor 张跃李凌峰纪箴
Owner UNIV OF SCI & TECH BEIJING