Method of synthesizing nano grade calcium titanium ceramic powder

A technology of ceramic powder and perovskite, applied in the field of ultra-fine nano powder preparation, can solve the problems of difficulty in getting out of the limitation of hydrothermal synthesis method, increasing the difficulty of process and operation, and difficulty in guaranteeing the purity of powder. Narrow distribution range, avoid grain growth and agglomeration, and stabilize the ratio of barium to titanium

Inactive Publication Date: 2005-02-16
TSINGHUA UNIV
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Problems solved by technology

[0005] Chinese patent CN1101634A proposes to co-precipitate an aqueous solution of two or more metal ions (Ba, Ti, Sr, Zr, etc.) in an alkaline environment (aqueous solution) with pH = 14 (not lower than 13.6), and the temperature range is 70~ The particle size of the powder obtained after washing and drying the precipitate at 100°C is 70-400nm, but due to the use of strong alkali such as NaOH, KOH, etc. The purity of the body is difficult to guarantee, and in order to obtain a smaller particle size, it is necessary to add BETA-cyclodextrin as a dispersant, which increases the difficulty of the process and operation, and increases the cost of the product
S.Urek of Slovenia etc. have reported a kind of low-temperature hydrothermal method (J.Euro.Ceram.Soc., 18 (1997): 279-286), the aqueous solution of barium ion and the alcoholic solution of titanium ion are under strong alkaline environment Mixing to form a prepolymer, and then a perovskite micropowder precipitation (~20nm) was obtained at a lower temperature of 150°C, but the temperature of this method has exceeded the boiling point of water, and it must be in a high-pressure chamber to reach a supercritical state. In fact, it belongs to the hydrothermal synthesis method at a lower temperature, and it is difficult to get rid of the limitations of the hydrothermal synthesis method

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  • Method of synthesizing nano grade calcium titanium ceramic powder
  • Method of synthesizing nano grade calcium titanium ceramic powder
  • Method of synthesizing nano grade calcium titanium ceramic powder

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] 631 g of Ba(OH) 2 ·8H 2 O was dissolved in 5 liters of water and heated to 70°C as bottom solution A. Dissolve 680 g of tetrabutyl titanate in 5 liters of absolute ethanol as liquid B. Slowly add liquid B to bottom liquid A. During this period, when there is 1 / 5 of liquid B left, add 100 ml of concentrated ammonia water to bottom liquid A, and continue to add the remaining liquid B. During the whole process, the temperature of the bottom liquid must be kept roughly constant, and at the same time, vigorously stirred to facilitate the control of powder properties. After the reaction was finished, filter with suction. Dry the solid part at 60-100 ° C to obtain BaTiO with a particle size of ~ 30 nanometers 3 Powder. The XRD results show that the obtained powder is a fine powder of perovskite structure. From the TEM photos, the finished product belongs to nearly spherical crystalline particles.

Embodiment 2

[0024] Change the temperature of the bottom liquid in Example 1 to 60°C, and keep the other conditions constant, to obtain BaTiO with a particle size of ~30 nanometers. 3 Powder.

Embodiment 3

[0026] Change the temperature of the bottom liquid in Example 1 to 45°C, and keep the other conditions constant, to obtain BaTiO with a particle size of ~100 nanometers 3 Powder.

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Abstract

A process for synthesizing the nanometre-class perovskite ceramic powder under the conditions of temp. lower than boiling point of substrate liquid and normal pressure includes such steps as directly mixing the substrate liquid which is the aqueous solution of barium hydroxide, strontium hydroxide, calcium hydroxide and lead hydroxide with the solution of metallic alkoxide in organic solvent, adding precipitant and disperser, and drying the deposit. Its advantages are high sintering activity, uniformity and stability of Ba / Ti rate, and cubic perovskite structure.

Description

technical field [0001] The invention relates to the preparation technology of ultrafine nanometer powder, in particular to a synthesis method of nanoscale perovskite ceramic powder. Background technique [0002] A class of ceramic materials with a perovskite structure represented by barium titanate is widely used in various electronic components due to its excellent ferroelectric and piezoelectric properties, such as multilayer ceramic capacitors (MLCC), positive Temperature coefficient thermistor (PTCR), piezoelectric motor, ceramic filter, etc. The purity and fineness of perovskite ceramic powder have a decisive influence on the performance and quality of electronic ceramic components. With the rapid development of electronic components in the direction of high integration, high precision, high reliability, multi-function and miniaturization, the electronics industry is concerned about the purity, particle size, and molding of barium titanate and other powders with perovs...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C04B35/462C04B35/465C04B35/622
Inventor 齐建全李龙土王永力桂治轮
Owner TSINGHUA UNIV
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