Preparation method of barium titanate nanometer powder

A nano-powder, barium titanate technology, applied in titanate, alkaline earth metal titanate, chemical instruments and methods, etc., can solve the problems of unfavorable clean production, strong corrosion, etc., and achieve controllable shape and size , the mild effect of the reaction process

Active Publication Date: 2018-08-28
安徽通湾科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Titanium tetrachloride (TiCl 4 ) is a colorless liquid at normal temperature, but it is very easy to hydrolyze violently with water, even if it encounters a small amount of water in the air, it will hydrolyze violently, releasing toxic corrosive gas Hydrogen chloride (HCl) releases heat when heated or meets water, releasing toxic corrosive gas Strong corrosive fume, which is not conducive to clean production

Method used

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  • Preparation method of barium titanate nanometer powder
  • Preparation method of barium titanate nanometer powder

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Cut about 700g of high-purity titanium plate and divide it into 3 pieces, each piece is connected in parallel with the negative electrode of the pulse power supply, and inserted as an anode into an electrolytic cell filled with 6kg of n-butanol solution, and a graphite electrode is installed at a distance of 30mm from the anode , and connected to the positive pole of the pulse power supply as the cathode. Add 90% lithium chloride to it, raise the temperature of the electrolytic cell to 70°C, turn on the pulse power supply, and adjust the pulse current density to 3000A / m 2 , the pulse time is 30ms, the duty ratio is 0.25 and the reaction is continued until the anode is completely dissolved, and then the solution is distilled at 130°C for 24h to obtain a tetrabutyl titanate solution.

[0033] Take by weighing 3kg tetrabutyl titanate solution and 9kg (25%) n-butanol solution and add it in the high-pressure enamel reaction kettle, then add 1.8kg barium hydroxide and 18g (1%...

Embodiment 2

[0036] Cut and weigh about 300g of titanium sponge, and divide it into 2 pieces. Each piece will be put into a common can-shaped graphite electrode and connected in parallel with the negative electrode of the pulse power supply, and inserted as an anode into an electrolytic cell filled with 4kg of n-butanol solution. Set a graphite electrode at a distance of 10 mm from the anode, and connect it to the positive pole of the pulse power supply as the cathode. Add 4g of ammonium bromide to it again, raise the temperature of the electrolytic cell to 105°C, turn on the pulse power supply, and adjust the pulse current density to 400A / m 2, the pulse time is 150 ms, the duty ratio is 0.5 and the reaction is continued until the anode is completely dissolved, and then the solution is distilled at 130° C. for 24 h to obtain a tetrabutyl titanate solution.

[0037] Weigh 1kg tetrabutyl titanate solution and 19kg (5%) n-butanol solution and add it in the high-pressure enamel reaction kettle...

Embodiment 3

[0040] Cut and weigh about 700g of titanium sponge, and divide it into 3 pieces. Each piece will be put into a common can-shaped graphite electrode and connected in parallel with the negative electrode of the pulse power supply, and inserted as an anode into an electrolytic cell filled with 6kg of n-butanol solution. Set a graphite electrode at a distance of 15 mm from the anode, and connect it to the positive pole of the pulse power supply as the cathode. Add 60g of ammonium chloride to it again, raise the temperature of the electrolytic cell to 95°C, turn on the pulse power supply, and adjust the pulse current density to 1500A / m 2 , the pulse time is 100ms, the duty ratio is 0.25 and the reaction is continued until the anode is completely dissolved, and then the solution is distilled at 130°C for 24h to obtain a tetrabutyl titanate solution.

[0041] Take by weighing 3kg tetrabutyl titanate solution and 17kg (15%) n-butanol solution and add it in the high-pressure enamel rea...

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Abstract

The invention provides a preparation method of barium titanate nanometer powder. According to the preparation method, metallic titanium is used as an anode, and under the action of a pulse power source, dissolving is performed to prepare butyl titanate; under high temperature and high pressure, vapour is inflated into the butyl titanate solution and barium salt for slow control of the hydrolyzingrate, so that the barium titanate powder is prepared. According to the method, a metallic titanium electrolysis method is adopted, preferably, a titanium plate and titanium sponge are adopted, titanium tetrachloride which can be acutely hydrolyzed is not used as a titanium source, the reaction process is mild, reaction products are controllable in shape and size, a reaction by-product namely butanol is used as an electrolytic metallic titanium reactant, and the effects of being recycle, environmentally friendly and economic can be achieved.

Description

technical field [0001] The invention relates to the technical field of raw material preparation of multilayer ceramic capacitors, in particular to a technical method for preparing barium titanate nanopowder. Background technique [0002] Barium titanate (BaTiO 3 ) is a typical ABO 3 Type perovskite ferroelectrics, with high dielectric constant, low dielectric loss and good temperature coefficient, are widely used in monolithic ceramic capacitors, multilayer ceramic capacitors (MLCC) and PTC thermistors. [0003] In recent years, with the miniaturization of electronic devices, the thickness of the dielectric layer of multilayer ceramic capacitors (MLCC) is only about 700-800nm, which requires its raw material barium titanate (BaTiO 3 ) The particle size of the powder particles is 80-200nm, and the particle size distribution is narrow. The barium titanate powder prepared by the solid-phase method using barium carbonate and titanium oxide as raw materials has a coarse particl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G23/00C25B3/12C25B3/13
CPCC01G23/006C01P2002/72C25B3/13
Inventor 周涛
Owner 安徽通湾科技有限公司
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