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Method for preparing multi-component trace codoping zirconium barium strontium titanate-based micro powder

A technology of strontium barium zirconate titanate and co-doping, which is applied in the field of powder preparation by wet chemical method, can solve the problems that the uniformity of chemical components of materials is difficult to control, unsuitable, and difficult to distribute uniformly, so as to be beneficial to human health and environmental protection , the uniformity of the composition is improved, and the powder particle size distribution is narrow

Inactive Publication Date: 2012-07-11
SICHUAN UNIV
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Problems solved by technology

The powder of barium titanate has been obtained by solid-phase method, but to prepare multi-component, micro-doped barium titanate-based micropowder, the solid-phase method has many disadvantages: first, other unnecessary impurities are easily introduced during ball milling; second Second, in the solid-phase method synthesis process, for the introduction of trace amounts of doping elements, it is difficult to make them uniformly distributed in the matrix material by ball milling, so the uniformity of the chemical composition of the material is difficult to control; third, the solid-phase method The particle size distribution of the synthetic powder is uneven, and the particle size is large; fourth, multiple ball milling is required, which takes a long time; fifth, the solid-state method synthesizes BaTiO 3 The base powder pre-firing synthesis needs to be at a high temperature of 1300 ° C to meet the requirements, and the solid-state method of firing ceramics must reach above 1400 ° C to obtain excellent ceramics, which is extremely energy-consuming.
Its advantage is that the product system can accommodate insolubles and non-precipitating components at the same time. The disadvantage is that the dissolution and hydrolysis of its salts doped with metal elements are limited by the type of solvent. ZL 011267607 and ZL200410043616.3 respectively disclose the following Method for preparing barium zirconate titanate with zirconium propoxide as zirconium source, ethylene glycol methyl ether and acetylacetone as solvent and zirconium oxynitrate as zirconium source, first synthesize zirconium citrate, then use zirconium citrate and ethylene glycol as solvent Method for preparing barium zirconate titanate
However, for the preparation of multi-component, co-doped barium titanate-based ceramic powders by sol-gel process, since most metal organic salts have different hydrolysis pathways in organic solvents, it is difficult to find a common solvent to achieve hydrolysis, and Organic salts are expensive and should not be used as initial raw materials, and the solubility of nitrates in organic solvents is also very different. Even if citrate solutions are obtained, it is difficult to mix various citrate solutions in the same solution system. Stable sols are obtained, and multi-component, co-doped BaTiO with controllable components cannot be obtained 3 base powder

Method used

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  • Method for preparing multi-component trace codoping zirconium barium strontium titanate-based micro powder
  • Method for preparing multi-component trace codoping zirconium barium strontium titanate-based micro powder
  • Method for preparing multi-component trace codoping zirconium barium strontium titanate-based micro powder

Examples

Experimental program
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Effect test

Embodiment 1

[0037] Example 1: Ba 0.96 Sr 0.04 Ti 0.955 Y 0.005 Zr 0.04 o 2.9975 Preparation of micropowder

[0038] (1) Preparation of a solution containing Ba, Sr ions

[0039] At room temperature and normal pressure, the barium acetate and strontium acetate that meet the stoichiometric ratio of the above chemical formula were dissolved in 120ml deionized water to obtain a clear and transparent solution with a concentration of Ba ions of 0.32M, containing 0.0016mol of Sr ions in the solution;

[0040] (2) Preparation of a solution containing Zr and Y ions

[0041] At room temperature and normal pressure, dissolve yttrium nitrate and zirconium nitrate in accordance with the stoichiometric ratio of the above chemical formula in 20ml of deionized water, and react to form a clear and transparent solution with a zirconium ion concentration of 0.08M and a yttrium ion concentration of 0.01M;

[0042] (3) Preparation of a solution containing Ti ions

[0043] At room temperature and norma...

Embodiment 2

[0051] Example 2: Ba 0.96 Sr 0.04 Ti 0.995 Zr 0.005 o 3 Preparation of micropowder

[0052] (1) Preparation of a solution containing Ba, Sr ions

[0053] At room temperature and normal pressure, the barium acetate and strontium acetate that meet the stoichiometric ratio of the above chemical formula were dissolved in 120ml deionized water to obtain a clear and transparent solution with a concentration of Ba ions of 0.32M, containing 0.0016mol of Sr ions in the solution;

[0054] (2) Preparation of a solution containing Zr ions

[0055] Under room temperature and normal pressure, zirconium nitrate conforming to the stoichiometric ratio of the above chemical formula is dissolved in 20ml of deionized water, and the reaction forms a clear and transparent solution with a zirconium ion concentration of 0.01M;

[0056] (3) Prepare a solution of Ti ions

[0057] At room temperature and normal pressure, dissolve tetrabutyl titanate conforming to the stoichiometric ratio of the a...

Embodiment 3

[0065] Example 3: Ba 0.96 Sr 0.04 Ti 0.895 Dy 0.005 Zr 0.10 o 2.9975 Preparation of micropowder

[0066] (1) Preparation of a solution containing Ba, Sr ions

[0067]At room temperature and normal pressure, the barium acetate and strontium acetate that meet the stoichiometric ratio of the above chemical formula were dissolved in 120ml deionized water to obtain a clear and transparent solution with a concentration of Ba ions of 0.32M, containing 0.0016mol of Sr ions in the solution;

[0068] (2) preparation contains the solution of Zr and Dy nitrate

[0069] At room temperature and normal pressure, dissolve zirconium nitrate and dysprosium nitrate in 20ml of deionized water in accordance with the above stoichiometric ratio, and react to form a clear and transparent solution with a zirconium ion concentration of 0.2M and a dysprosium ion concentration of 0.01M;

[0070] (3) Preparation of a solution containing Ti ions

[0071] At room temperature and normal pressure, dis...

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Abstract

A method for preparing multi-component trace codoping zirconium barium strontium titanate-based micro powder comprises the processing steps of: (1), preparing a solution containing Ba and Sr ions; (2), preparing a solution containing Zr ion or preparing a solution containing Zr ion or codoped with metal ion; (3), preparing a solution containing Ti ion; (4), preparing precursor liquid, mixing and stirring the three solutions prepared in the steps (1), (2) and (3) under ambient temperature and normal pressure, adding glacial acetic acid to enable the concentration of Ba1-x-ySrxMyTi1-zZrzO3+y / 2 or Ba1-xSrxTi1-y-zM' yZrzO3-y / 2 to be 0.1 M, and stirring for at least 10 minutes to ensure that the formed clear and transparent mixed solution is the precursor liquid of the Ba1-x-ySrxMyTi1-zZrzO3+y / 2 or the Ba1-xSrxTi1-y-zM' yZrzO3-y / 2; (5), carrying out polymerization; and (6), drying and roasting gel.

Description

technical field [0001] The invention belongs to the technical field of powder preparation by wet chemical method, in particular to a preparation method of doped strontium barium zirconate titanate-based micropowder. Background technique [0002] It is well known that barium titanate (BaTiO 3 ) Ceramics have a perovskite structure (ABO 3 , Ba occupies the A site, and Ti occupies the B site), which is one of the most widely used dielectric functional materials in electronic ceramics. Since this type of material has a high dielectric constant, scientists have done in-depth research on it since the 1950s. In barium titanate compounds, the contribution of spontaneous polarization mainly comes from the displacement polarization of titanium ions and the electron displacement polarization of a certain oxygen ion in the oxygen octahedron. This bulk effect makes barium titanate ceramic a ferroelectric material. A large number of research works have shown that through doping modifi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/49C04B35/622
Inventor 余萍张小山李军孙晓剑樊明雷
Owner SICHUAN UNIV
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