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Preparation method of size-controllable nanoscale cubic-phase super-fine barium titanate powder

A fine barium titanate, nano-scale technology, applied in the direction of nanotechnology, nanotechnology, chemical instruments and methods, etc., can solve the problem of difficulty in obtaining dispersed ultrafine barium titanate powder, lengthy preparation process, non-concentrated particle size distribution, etc. problems, to achieve the effect of improving reactivity and reaction rate, reducing powder agglomeration, and narrow distribution range

Inactive Publication Date: 2016-02-17
安徽凯盛应用材料有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] Therefore, if the traditional method, such as the oxalic acid precipitation method in the patent CN1417162A, can meet the needs and purity requirements of common capacitor materials, but each purification process is time-consuming and increases production costs, and because the abrasive particles are very large, The shape is poor, the particle size distribution is not concentrated, and the energy consumption is large
Another example is the patent CN101428850A of TDK Corporation of Japan, which solves the problem of lengthy preparation process time by means of direct calcination by solid phase sintering method, but it still takes a lot of energy to achieve the above points and good condition control
[0011] Under normal circumstances, the oxalate co-precipitation method can obtain sub-micron ultrafine barium titanate powder, and some companies use this method, but there are many production processes, resulting in larger particles after the powder is agglomerated
At the same time, solid-phase sintering method, another method of severe powder agglomeration, is more difficult to obtain well-dispersed ultra-fine barium titanate powder
Relatively speaking, the sol-gel method can obtain powders with high nano-scale purity, but it is difficult to promote and adopt it in the large-scale production process due to its long growth cycle and high cost.

Method used

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  • Preparation method of size-controllable nanoscale cubic-phase super-fine barium titanate powder
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  • Preparation method of size-controllable nanoscale cubic-phase super-fine barium titanate powder

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Embodiment approach 1

[0035] Weigh 2.0KgTiCl 4 , under the condition that the reaction temperature is lower than 30°C, slowly add it dropwise to the mixed solution containing 4.0Kg deionized water and 40g dispersant ethanol in the reaction kettle under constant stirring to obtain light yellow viscous TiOCl 2 Aqueous solution, the HCl gas generated during the process is absorbed by NaOH lye, and the solution after the exhaust gas is concentrated and crystallized to obtain industrial-grade NaCl crystals. Then the reaction temperature is less than 30 ℃ and the TiOCl 2 Add 6.0Kg of mineralizer ammonia water to the aqueous solution to make it NH 3 ·H 2 O: TiCl 4 The mass ratio is between 3.0:1.0, and the final pH of the reaction system is between 8-12, during which a white colloidal precipitate is formed. The precipitate was centrifuged and washed with deionized water until the chloride ion content was less than 100ppm. The washed white precipitate was then mixed with Ba(OH) 2 ·8H 2 O solid and w...

Embodiment approach 2

[0037]Weigh 2.0KgTiCl 4 , under the condition that the reaction temperature is lower than 30°C, slowly add it dropwise to the mixed solution containing 4.0kg deionized water and 200g ethanol under continuous stirring in the reactor to prepare light yellow viscous TiOCl 2 Aqueous solution, the HCl gas generated during the process is absorbed by NaOH lye, and the solution after the exhaust gas is concentrated and crystallized to obtain industrial-grade NaCl crystals. Then the reaction temperature is less than 30 ℃ and the TiOCl 2 Add 2.0Kg of ammonia water to the aqueous solution to make NH 3 ·H 2 O: TiCl 4 The mass ratio is 1.0:1.0, and the final pH of the reaction system is between 8-12, during which a white colloidal precipitate is formed. The precipitate was centrifuged and washed with deionized water until the chloride ion content was less than 100ppm. The washed white precipitate was then mixed with Ba(OH) 2 ·8H 2 O solid and water 15.0Kg, control the molar ratio of...

Embodiment approach 3

[0039] Weigh 2.0KgTiCl 4 , under the condition that the reaction temperature is lower than 30°C, slowly add it dropwise into 3.0Kg of deionized water under constant stirring in the reactor to obtain light yellow viscous TiOCl 2 Aqueous solution, the HCl gas generated during the process is absorbed by NaOH lye, and the solution after the exhaust gas is concentrated and crystallized to obtain industrial-grade NaCl crystals. Then the reaction temperature is less than 30 ℃ and the TiOCl 2 Add 4.0Kg of ammonia water to the aqueous solution to make NH 3 ·H 2 O: TiCl 4 The mass ratio is between 2.5:1.0, and the final pH of the reaction system is between 8-14, during which a white colloidal precipitate is formed. The precipitate was centrifuged and washed with deionized water until the chloride ion content was less than 50 ppm. The washed white precipitate was then mixed with Ba(NO 3 ) 2 Solid and water 20.0Kg, control the molar ratio of barium source and titanium source at 1.1...

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Abstract

The invention discloses a preparation method of size-controllable nanoscale cubic-phase super-fine barium titanate powder. Relatively cheap titanium tetrachloride is used for preparing a titanium precursor solution TiClO2 through hydrolysis, the precursor solution is dropwise added into a mineralizing agent and dispersant solution, and continuous stirring is performed to obtain a titanium precursor gel solution; then centrifugal gel washing is performed to remove chloride ions, the prepared H4TiO4 gel and barium hydroxide or barium nitrate are grinded and dispersed with water and a dispersant according to a certain proportion to prepare mixed dispersed slurry, the mixed dispersed slurry is put into a reaction kettle for hydrothermal reaction, and then washing and drying are performed to obtain the nanoscale cubic-phase super-fine barium titanate powder good in dispersion and centralized in particle size, the average particle size of the power is smaller than 100 nm, and the specific surface area is within the range of 12.5-15.0 m<2> / g.

Description

technical field [0001] The invention relates to the technical field of preparation of ultrafine powder of functional ceramic raw materials, in particular to a preparation technology of nanoscale barium titanate powder ultrafine particles. Background technique [0002] Barium titanate powder material is widely used in heat-sensitive components, ferroelectric components, multilayer ceramic capacitors, etc. as dielectric materials. [0003] With the rapid development of electronic information technology, there is a demand for miniaturization, light weight, high performance and stabilization of various electronic equipment accessories. The demand for nano-scale barium titanate functional ceramic powder materials with high dielectric constant is also in short supply, and it is even known as the pillar of electronic functional ceramic materials. Development hotspots and key development directions. [0004] Barium titanate powder has been paid attention to by the electronics indu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G23/00B82Y30/00
Inventor 彭寿王永和刘强严回王利胡石磊
Owner 安徽凯盛应用材料有限公司
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