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Microwave liquid phase compounding process of high-purity barium titanate powder

A pure barium titanate, liquid phase synthesis technology, applied in the preparation of barium titanate powder, microwave liquid phase synthesis, can solve the problem of affecting the performance of barium titanate powder, high Na+ content of barium titanate powder, powder Problems such as washing and purification difficulties, to achieve the effects of short reaction time, high product purity and low reaction temperature

Inactive Publication Date: 2010-02-10
SHANDONG SINOCERA FUNCTIONAL MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the use of NaOH in this method, the Na+ content in the barium titanate powder will be high, and the powder washing and purification will be difficult, thus seriously affecting the performance of the barium titanate powder.

Method used

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  • Microwave liquid phase compounding process of high-purity barium titanate powder
  • Microwave liquid phase compounding process of high-purity barium titanate powder
  • Microwave liquid phase compounding process of high-purity barium titanate powder

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] (1) Weigh 113.68 g of analytically pure tetraisopropyl titanate, and with rapid stirring, hydrolyze it in a beaker filled with 2 L of pure water. After stirring for 10 min, the hydrolyzate is filtered and washed. The hydrolyzate was redispersed and diluted to a volume of 600 ml with pure water in a beaker, 19 g of analytically pure nitric acid with a concentration of 65% was added, and water was replenished to a volume of 1 L. Then, with rapid stirring, the above slurry was heated up and kept at 65° C. for 50 minutes to obtain a transparent sol.

[0029] (2) Add 400ml of pure water to a microwave reactor with a capacity of 2.5L, heat it to 85°C by microwave, weigh 257g of barium hydroxide octahydrate (purity > 98wt%) and add it to the kettle, and start stirring to assist the dissolution of barium hydroxide , and add water to a volume of 1L, and prepare a nearly transparent barium hydroxide solution.

[0030] (3) Under the condition of stirring, the transparent sol obta...

Embodiment 2

[0033] (1) Weigh 284 g of analytically pure tetraisopropyl titanate, and with rapid stirring, hydrolyze it in a beaker filled with 5 L of pure water. After stirring for 10 min, the hydrolyzate is suction-filtered and washed. The hydrolyzate was redispersed and diluted to a volume of 900 ml with pure water in a beaker, 47 g of analytically pure nitric acid with a concentration of 65% was added, and water was replenished to a volume of 1 L. Then with rapid stirring, the above slurry was heated up and kept at 65° C. for 3 hours to obtain a transparent sol.

[0034] (2) Add 700ml of pure water to a microwave reactor with a capacity of 2.5L, heat it to 85°C by microwave, weigh 643g of barium hydroxide octahydrate (purity > 98wt%) and add it to the kettle, and start stirring to assist the dissolution of barium hydroxide , and add water to a volume of 1L, and prepare a nearly transparent barium hydroxide solution.

[0035] (3) Under the condition of stirring, the transparent sol obt...

Embodiment 3

[0038] (1) Weigh 454 g of analytically pure tetraisopropyl titanate, and with rapid stirring, hydrolyze it in a reaction tank filled with 10 L of pure water. After stirring for 10 min, the hydrolyzate is suction-filtered and washed. The hydrolyzate was redispersed and diluted to a volume of 1 L with pure water in a beaker, 76 g of analytically pure nitric acid with a concentration of 65% was added, and water was replenished to a volume of 1.1 L. Then with rapid stirring, the above slurry was heated up and kept at 65° C. for 3 hours to obtain a transparent sol.

[0039] (2) Add 1L of pure water to a microwave reactor with a capacity of 2.5L, heat it to 85°C by microwave, weigh 1029g of octahydrate barium hydroxide (purity > 98wt%) and add it to the kettle, and turn on the stirring auxiliary barium hydroxide Dissolve it, add water to a volume of 1.1L, and prepare a nearly transparent barium hydroxide solution.

[0040] (3) Under the condition of stirring, the transparent sol ob...

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Abstract

The invention relates to a microwave liquid phase compounding process of high-purity barium titanate powder. Main raw materials which are tetraisopropyl titanate or tetrabutyl titanate, barium octahydrate and nitric acid are compounded by microwave auxiliary heating at lower temperature for shorter reaction time to obtain the barium titanate powder in different grain diameter specifications. The process comprises the following concrete steps: (1) hydrolyzing a titanium resource; (2) washing a hydrolyzed product; (3) obtaining the titanium resource; (4) fully dissolving high-purity Ba(OH)2.8H2Oin the pure water in a microwave reaction vessel with a stirring system to obtain barium hydroxide solution; (5) carrying out compounding reaction and obtaining slurry containing barium titanate particles after the reaction; (6) precipitating and washing or filtering the barium titanate slurry obtained in the reaction with high-purity water for many times and then drying to obtain the high-puritycubic phase barium titanate powder. The process has low reaction temperature, short reaction time, controllable particle diameter and high product purity.

Description

technical field [0001] The invention relates to a preparation method of barium titanate powder, in particular to microwave liquid phase synthesis of ultrafine high-purity cubic phase barium titanate powder, belonging to the field of electronic ceramic powder material preparation. technical background [0002] Barium titanate (abbreviated as BT) is an important basic electronic material in the field of electronic ceramics industry. Because of its high dielectric constant, good ferroelectricity, piezoelectricity, withstand voltage and insulation properties, it is widely used in the production of many Multilayer ceramic capacitors (MLCC for short), thermistors, piezoelectric ceramics and optoelectronic devices, etc. With the development of electronic components in the direction of "miniaturization" and "large capacity", high-purity, ultra-fine, uniform particle size barium titanate powder material is the key material to realize this development direction. [0003] Microwave-as...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/626C04B35/468
Inventor 张曦张兵宋锡滨
Owner SHANDONG SINOCERA FUNCTIONAL MATERIAL CO LTD
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