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Preparation method of temperature stability type capacitor ceramic powder with high dielectric constant

A temperature-stable, high-dielectric-constant technology, applied in the direction of fixed capacitor dielectrics, fixed-capacitance parts, laminated capacitors, etc., can solve the problem of size reduction, ball milling can't completely destroy particle agglomeration, material dielectric constant drop, etc. question

Inactive Publication Date: 2013-07-31
HEBEI UNIVERSITY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] (1) The preparation method is still limited to the traditional solid-phase method, which is easy to bring in impurities and consumes a lot of energy. Ball milling itself cannot completely destroy the agglomeration between particles, and in the drying process after ball milling, the dispersed particles will be reunited and sintered The higher the temperature, the coarser the particles
At present, the specifications of MLCC are rapidly reduced, and large particle powder cannot meet the increasingly miniaturized MLCC production needs.
At present, although some research groups at home and abroad use methods such as microemulsion method, sol-gel method and liquid phase precipitation method to prepare barium titanate porcelain, but in the preparation process, organic solvents are used, which not only has high toxicity, but also increases the production efficiency. cost, and the process is complicated, which is not conducive to industrial production
[0006] (2) Since the dielectric constant of barium titanate will drop sharply after exceeding the Curie point, in order to improve the temperature stability, a large amount of paraelectric phase is added to the medium, which greatly suppresses the dielectric peak of barium titanate, although The temperature stability of the material is improved, but the dielectric constant of the material is greatly reduced
[0012] Although the above method can produce barium titanate-based ceramic powders with core-shell structure and certain temperature stability, the powders often have coarse particle size and wide size distribution, and due to the existence of paraelectric phase oxides The dielectric constant of the material is low, which cannot meet the high-capacity development requirements of new electronic components

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  • Preparation method of temperature stability type capacitor ceramic powder with high dielectric constant
  • Preparation method of temperature stability type capacitor ceramic powder with high dielectric constant
  • Preparation method of temperature stability type capacitor ceramic powder with high dielectric constant

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Embodiment 1

[0073] A method for preparing high dielectric constant temperature-stable capacitor porcelain powder, and a subsequent method for preparing ceramic materials, the steps of which include:

[0074] A. Preparation of powder particle inner layer material Ba by reflux method 0.985 Bi 0.01 TiO 3 :

[0075] A-1, 3.9499g Bi(NO 3 ) 3 Dissolved in 200ml of distilled water to make a solution, 11mL of analytical pure TiCl 4 Slowly drop into the solution, then slowly add 1:1 concentrated ammonia water dropwise to the solution, adjust the pH value to 7, make TiO 2+ Precipitation, and then vacuum filtration to obtain TiO 2 Filter cake (which is doped with Bi element), add 250ml of distilled water to make a slurry;

[0076] A-2, 31.5462g Ba(OH) 2 ·8H 2 O was dissolved in boiled 200ml distilled water, and after it was completely dissolved, it was mixed with the obtained TiO 2 Mix the slurry, control the reaction temperature at 95°C to 100°C, react under stirring for 3 hours, wash and...

Embodiment 2

[0084] A method for preparing high dielectric constant temperature-stable capacitor porcelain powder, and a subsequent method for preparing ceramic materials, the steps of which include:

[0085] A. Preparation of powder particle inner layer material Ba by reflux method 0.985 Bi 0.01 TiO 3 :

[0086] A-1, 3.9499g Bi(NO 3 ) 3 Dissolved in 200ml of distilled water to make a solution, 11mL of analytical pure TiCl 4 Slowly drop into the solution, then slowly add 1:1 concentrated ammonia water dropwise to the solution, adjust the pH value to 7, make TiO 2+ Precipitation, and then vacuum filtration to obtain TiO 2 Filter cake (which is doped with Bi element), add 240ml of distilled water to make a slurry;

[0087] A-2, 31.5462g Ba(OH) 2 ·8H 2 O was dissolved in boiled 200ml distilled water, and after it was completely dissolved, it was mixed with the obtained TiO 2 Mix the slurry, control the reaction temperature at 95°C to 100°C, react under stirring for 3 hours, wash and...

Embodiment 3

[0095] A method for preparing high dielectric constant temperature-stable capacitor porcelain powder, and a subsequent method for preparing ceramic materials, the steps of which include:

[0096] A. Preparation of powder particle inner layer material Ba by reflux method 0.97 Bi 0.02 TiO 3 :

[0097] A-1, the 7.8998gBi (NO 3 ) 3 Dissolved in 200ml of distilled water to make a solution, 11mL of analytical pure TiCl 4 Slowly drop into the solution, then slowly add 1:1 concentrated ammonia water dropwise to the solution, adjust the pH value to 7, make TiO 2+ Precipitation, and then vacuum filtration to obtain TiO 2 Filter cake (which is doped with Bi element), add 220ml of distilled water to make a slurry;

[0098] A-2, 31.0658g Ba(OH) 2 ·8H 2 O was dissolved in boiled 200ml distilled water, and after it was completely dissolved, it was mixed with the obtained TiO 2 Mix the slurry, control the reaction temperature at 95°C to 100°C, react under stirring for 3 hours, wash ...

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Abstract

The invention discloses a preparation method of temperature stability type capacitor ceramic powder with high dielectric constant. The preparation method comprises the steps of A. preparing inner-layer material (Ba, Bi) TiO of powder particles by a reflux method: A-1. dissolving Bi(NO3)3, dropping TiC14 into solution to obtain a mixture, then dropping stronger ammonia water into the mixture so asto precipitate TiO2+ to obtain a TiO2 filter cake, and A-2. dissolving Ba(OH)2 / 8H2O into boiled distilled water and mixing with TiO2 obtained from the step A-1, controlling the reaction temperature to be 95 DEG C-100 DEG C, reacting for 2-4h while stirring, washing and drying to obtain the inner-layer material; and B. preparing graded hierarchical structure powders by a wet solid phase method: B-1. dissolving ZrOCl2, SnCl4 or La2O3 into distilled water, dropping TiCl4 into solution, then dropping stronger ammonia water, adjusting a pH value to be 7 and precipitating TiO2+, and B-2. uniformly mixing Ba(OH)2 / 8H2O and the TiO2 filter cake obtained from the step B-1 to obtain a mixture, and pouring the (Ba, Bi) TiO3 power obtained in the step A into the mixture, grinding for 1h, and then drying to obtain the graded hierarchical structure powders. According to the preparation method disclosed by the invention, the dielectric constant of the material is increased and the temperature property is improved.

Description

technical field [0001] The invention relates to a method for preparing temperature-stable capacitor porcelain powder, in particular to a method for preparing nanometer or micron powder with a multilayer structure. Background technique [0002] Multilayer ceramic capacitors (MLCC) are widely used in broadcasting and television, communications, household appliances, measuring instruments, medical equipment, military electronic equipment and other fields. MLCC is constantly developing towards the direction of high capacity, miniaturization and low cost, which requires the thickness of a single layer of MLCC to be less than 1 μm, and its microstructure is easy to precisely control. For this reason, the main raw material of MLCC - BaTiO 3 The size of the powder should be controlled below 200nm [1] . In addition, the development of the automobile industry in recent years has put forward higher requirements for MLCC capacitors in terms of high temperature resistance, such as eng...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C04B35/626C04B35/468H01G4/30H01G4/12
Inventor 王静姜胜林丁士文张光祖
Owner HEBEI UNIVERSITY