Nanometer grade tetragonal-phase barium titanate powder and its prepn.

A phase barium titanate, nano-scale technology, applied in the field of nano-ceramics, can solve the problems of not effectively improving the electrical properties of MLCc, poor electrical properties of cubic phase barium titanate, reducing the volume of MLCc, etc. The effect of low cost and simple process

Inactive Publication Date: 2001-11-28
SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, the submicron and micron-scale barium titanate of the tetragonal phase exhibits excellent electrical properties, while the electrical properties of the cubic phase barium titan...

Method used

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  • Nanometer grade tetragonal-phase barium titanate powder and its prepn.
  • Nanometer grade tetragonal-phase barium titanate powder and its prepn.
  • Nanometer grade tetragonal-phase barium titanate powder and its prepn.

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Prepare a high-concentration aqueous solution of barium chloride and titanium tetrachloride, then prepare 200 mL of a mixed solution of 0.625 M titanium tetrachloride and 1.0 M barium chloride, add 36 g of sodium hydroxide, stir well, and transfer to a container with a tetrafluoroethylene liner. In the autoclave, the temperature was raised at an average rate of 3°C / min to 240°C, and the hydrothermal reaction was carried out for 12 hours. After cooling to room temperature with the furnace, the autoclave was unloaded, and the reaction product was washed and repeated several times. After the solution was neutral, it was filtered and dried. The resulting reaction product was dried as a white powder. The crystal form of the sample was analyzed by a Rigaku powder diffractometer using CuKα radiation. The instrument model was Geigerflex D / Max 2200, and the analysis was carried out at 10-80°2θ. The particle size of the samples was measured using a SEM electron microscope. Such ...

Embodiment 2

[0029] Prepare a high-concentration aqueous solution of barium chloride and titanium tetrachloride, then prepare 200mL of a mixed solution of 0.625M titanium tetrachloride and 0.90M barium chloride, add 36g of sodium hydroxide, stir evenly, and transfer it to a tank with polytetrafluoroethylene In a lined autoclave, raise the temperature at an average rate of 3°C / min to 240°C, conduct a hydrothermal reaction for 18 hours, cool down to room temperature with the furnace, unload the autoclave, wash the reaction product and repeat it several times until the solution is neutral. The reaction product obtained by drying is a white powder. The crystal form of the sample was analyzed by a Rigaku powder diffractometer using CuKα radiation. The instrument model was Geigerflex D / Max 2200, and the analysis was carried out at 10-80°2θ. The particle size of the samples was measured using a SEM electron microscope. The sample has an average particle size of 75nm, a crystal phase of tetragona...

Embodiment 3

[0031] Prepare a high-concentration aqueous solution of barium chloride and titanium tetrachloride, then prepare 200mL of a mixed solution of 1.0M titanium tetrachloride and 1.2M barium chloride, add 56g of sodium hydroxide, stir evenly, and transfer to a container with a tetrafluoroethylene liner. In the autoclave, the temperature was raised at an average speed of 3°C / min to 230°C, and the hydrothermal reaction was carried out for 12 hours. After cooling to room temperature with the furnace, the autoclave was unloaded, and the reaction product was washed and repeated several times. After the solution was neutral, it was filtered and dried. The resulting reaction product was dried as a white powder. The crystal form of the sample was analyzed by a Rigaku powder diffractometer using CuKα radiation, the instrument model is Geigerflex D / Max2200, and the analysis was carried out at 10-80°2θ. The particle size of the samples was measured using a SEM electron microscope. The sample...

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Abstract

The present invention relates to method of preparing nanometer grade tetragonal phase barium titanate powder. Said method uses low price barium chloride, titanium tetrachloride as barium, titanium source for hydrothermal reaction and uses sodium hydroxide as mineralization agent. Prepare high concentration barium chloride solution and titanium tetrachloride solution respectively then mix together, add in sodium hydroxide to form colloidal sol with very good fluidity as hydrothermal reaction mixture which is put in high pressure anticorrosion reactor and raise temperature to 240 deg.C, maintain this temperature for 12hr., filter, wash with deionized water., dry to obtain monodispersional nanometer grade tetragonal phase barium titanate powder with average size smaller than 100 nm.

Description

technical field [0001] The invention relates to a preparation method of nano-scale tetragonal phase barium titanate powder, and in more detail relates to the preparation of nano-scale tetragonal phase barium titanate powder by a hydrothermal method. It belongs to the field of nano ceramics. Background technique [0002] Barium titanate, especially tetragonal barium titanate, has a high dielectric constant, which makes it a preferred material in the fabrication of capacitors. With the rapid development of the electronics industry, multi-layer ceramic capacitors (“MLCc”) are gradually gaining attention. MLCc includes alternating dielectric and conductive materials. In order to obtain MLCc with better performance, the number of layers should be as many as possible, so the grain size of the dielectric material barium titanate should be as small as possible. The use of traditional submicron or even micron barium titanate is limited and will Gradually replaced by nano-scale bar...

Claims

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Application Information

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IPC IPC(8): C01G23/00C04B35/468
Inventor 高濂徐华蕊刘会冲
Owner SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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