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Method for producing barium titanate powder

A manufacturing method, barium titanate technology, applied in titanate, alkaline earth metal titanate, chemical instruments and methods, etc., can solve problems such as difficult adjustment of mixed aqueous solution, low solubility, agglutination, etc.

Inactive Publication Date: 2000-11-15
TOHO TITANIUM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In addition, for the production method of the above-mentioned Japanese Patent Publication No. 6-649, after the chloride of titanium or zirconium is hydrolyzed in an aqueous solution, a step of returning to alkalinity is required, so there are complicated steps and a long time. the problem of
[0012] In addition, barium salts such as barium chloride have very low solubility in an acidic state, and in the production method of the above-mentioned Japanese Patent Application Laid-Open No. 7-232923, a mixed aqueous solution of an acidic titanium compound and a barium salt is used as a starting material. Therefore, the adjustment of this mixed aqueous solution is difficult, especially the concentrations of titanium compounds and barium salts in the mixed aqueous solution have certain limits
Specifically, when preparing a mixed aqueous solution of titanium tetrachloride and barium chloride, the total concentration of metal ions is limited to about 1.2 mol / liter, so the productivity is not high
In addition, when carbonate is mixed into the starting raw material liquid, it is difficult to control the atomic ratio of Ba / Ti, resulting in the mixing of carbonate in the reaction product powder, which lowers the quality of the product. As a result, it cannot be obtained without sintering. raises its dielectric constant, so there are also problems with
[0013] In addition, although the barium titanate obtained according to the above-mentioned prior art has fine particles, it has poor dispersibility when slurrying, and as a result, aggregation phenomenon occurs, so that it is difficult to achieve thinning of the ceramic dielectric layer. question

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1A

[0057] The present invention is further explained below by specific examples. Embodiment 1A, the manufacture of barium titanate powder

[0058] A 2000 cc stainless steel flask equipped with a stirring device was used as a reaction vessel, and a NaOH aqueous solution having a concentration of 0.92N was previously injected into the reaction vessel, and the NaOH aqueous solution was maintained at about 90°C.

[0059] Then, use a water pump to keep the TiCl at 40°C 4 Aqueous solution (using ion-exchanged water, TiCl 4 Concentration is 0.472mol / L) and BaCl which has previously removed undissolved components and heated at about 95°C 2 / NaOH aqueous solution (using ion-exchanged water, BaCl 2 Concentration is 0.258mol / liter, NaOH concentration is 2.73mol / liter) according to TiCl 4 Aqueous solution 77cc / min, BaCl 2 A flow rate of 151 cc / min of NaOH aqueous solution was continuously supplied into the reaction vessel. At this time, TiCl 4 / BaCl 2 The molar ratio is 1.07. In add...

Embodiment 2

[0064] A 2000 cc stainless steel flask equipped with a stirring device was used as a reaction vessel, and a NaOH aqueous solution having a concentration of 0.77N was injected into the reactor in advance, and the NaOH aqueous solution was maintained at about 90°C.

[0065] Then, use a water pump to keep the TiCl at 40°C 4 Aqueous solution (using ion-exchanged water, TiCl concentration of 0.466 mol / liter) and Ba(OH) that has previously removed undissolved components and kept heated at about 95°C 2 / NaOH aqueous solution (using ion-exchanged water, Ba(OH) 2 Concentration is 0.264mol / liter, NaOH concentration is 2.09mol / liter) according to TiCl 4 Aqueous solution 80cc / min, Ba(OH) 2 A flow rate of 158 cc / min of NaOH aqueous solution was continuously supplied into the reaction vessel. At this time, TiCl 4 / Ba(OH) 2 The molar ratio of is 1.11. In addition, the mixed aqueous solution in the reaction vessel was stirred for 2 minutes while keeping the temperature of the mixed aque...

Embodiment 3

[0067] except TiCl 4 TiCl at a concentration of 2.25 mol / liter 4 Aqueous solution according to 100cc / min and BaCl 2 BaCl with a concentration of 1.25 mol / liter and a NaOH concentration of 8.3 mol / liter 2 / NaOH aqueous solution was fed at a rate of 200 cc / min, and the rest were the same as in Example 1, and Example 3 barium titanate powder was obtained. The physical properties of the obtained barium titanate powder were analyzed in the same manner as in Example 1, and the obtained results are listed in Table 1 together. Comparative example 1

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Abstract

A method for producing a barium titanate powder with improved productivity, which is composed of fine particles and has a narrow particle diameter distribution, has good dispersibility and has an excellent Ba / Ti atomic ratio. An aqueous solution of a titanium compound such as titanium tetrachloride is contacted under agitation with an alkaline aqueous solution of a barium compound such as the barium chloride which has been subjected to filtration treatment, while adjusting a chemical equivalent ratio of titanium compound / barium compound in 0.8 to 1.2, to thereby produce a barium titanate powder.

Description

technical field [0001] The present invention relates to a method for producing barium titanate powder composed of primary spherical particles with a particle diameter of 1 μm or less and having a crystalline perovskite structure. Background technique [0002] Barium titanate powder is widely used as a dielectric material in electronic components such as piezoelectric elements and PTC thermistor thermometers, and is especially suitable as a substrate for multilayer ceramic capacitors. Such multilayer ceramic capacitors are generally produced by laminating and pressing ceramic dielectric layers and internal electrode layers in alternate layers, and then sintering them to form a whole. The preparation method of the ceramic dielectric layer is firstly to prepare the barium titanate powder and the binder together into a slurry, and then sintering it to form the ceramic dielectric layer. Especially recently, there is a demand for miniaturization and increase...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G23/00
CPCC01P2002/34C01P2004/32C01P2004/52C01P2004/62C01G23/006C01G23/00C01F11/00
Inventor 堀川松秀堺英树笼桥亘
Owner TOHO TITANIUM CO LTD
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