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Preparation method of Barium Titanate nano-powder

A technology of nanopowder and barium titanate, which is applied in nanostructure manufacturing, nanotechnology, nanotechnology, etc., can solve the problems of large product particle size, high production pressure of hydrothermal method, strict operating conditions, etc., and achieve particle size distribution Uniformity, high relative permittivity, and safe production process

Inactive Publication Date: 2011-05-25
XIANGTAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the main methods for preparing barium titanate powder include high-temperature solid-phase method, sol-gel method, chemical co-precipitation method and hydrothermal method, etc., but each of these methods has some disadvantages: the high-temperature solid-phase method has a high synthesis temperature, and the obtained The powder has severe hard agglomeration, large particle size, and wide particle size distribution. Due to uneven mixing, the chemical composition of the product is uneven and the purity is low; the raw materials of the sol-gel method are expensive, and the organic solvent used is toxic. The powder is quickly agglomerated, the operating conditions are strict and difficult to control; the chemical co-precipitation method has improved the uniformity of the reaction compared with the high-temperature solid-phase method, but the calcination temperature is still high, and the product particle size is large and the particle size distribution is wide; hydrothermal method production High pressure, high requirements for production equipment, also has the disadvantages of serious particle agglomeration and uneven particle size distribution
The above methods may have the defects of low product purity, difficult to remove impurities, complex process and difficult control, or serious product particle agglomeration, large particles and wide particle size distribution.

Method used

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  • Preparation method of Barium Titanate nano-powder
  • Preparation method of Barium Titanate nano-powder
  • Preparation method of Barium Titanate nano-powder

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] (1) Weigh 1.22g BaCl 2 2H 2 O was added to 20 mL of 3% H 2 o 2 In solution, BaCl 2 2H 2 O and H 2 o 2 The ratio of the amount of the substances is 1:3.9, and constantly stirred. Then, add an appropriate amount of ammonia water to adjust the pH of the solution to 8.5, and let it stand for 30 minutes to obtain a yellow precipitate. Filtrate, wash the precipitate alternately with dilute ammonia water and absolute ethanol, and dry it in a vacuum oven at room temperature to obtain light yellow precursor powder BaO 2 ·H 2 o 2 . to BaO 2 ·H 2 o 2 Carry out X-ray diffraction (XRD) analysis to know that the prepared BaO 2 ·H 2 o 2 It is a monoclinic crystal system without impurity peaks, indicating that BaO 2 ·H 2 o 2 High purity, such as figure 1 shown.

[0020] (2) Weigh 2.03g BaO 2 ·H 2 o 2 and 0.59g H2 TiO 3 Put it in a mortar, mix and grind evenly, then add 1.69g KOH, 10.00g KNO 3 and 10 mL absolute ethanol (BaO 2 ·H 2 o 2 with H 2 TiO 3 The r...

Embodiment 2

[0023] (1) Weigh 2.42g Ba(NO 3 ) 3 ·5H 2 O was added to 8 mL of 9% H 2 o 2 In solution, Ba(NO 3 ) 3 ·5H 2 O and H 2 o 2 The ratio of the amount of the substances is 1:4.7, and keep stirring. Then, add an appropriate amount of ammonia water to adjust the pH of the solution to 10, and let it stand for 20 minutes to obtain a yellow precipitate. Filtrate, wash the precipitate alternately with dilute ammonia water and absolute ethanol, and dry it in a vacuum oven at room temperature to obtain light yellow precursor powder BaO 2 ·H 2 o 2 . to BaO 2 ·H 2 o 2 Carry out X-ray diffraction (XRD) analysis to know that the prepared BaO 2 ·H 2 o 2 It is a monoclinic crystal system without impurity peaks, indicating that BaO 2 ·H 2 o 2 High purity.

[0024] (2) Weigh 2.03g BaO 2 ·H 2 o 2 and 0.39g H 2 TiO 3 Put it in a mortar, mix and grind evenly, then add 1.12g KOH, 8.29g KNO 3 and 8 mL absolute ethanol, BaO 2 ·H 2 o 2 with H 2 TiO 3 The ratio of the amount...

Embodiment 3

[0027] (1) Weigh 1.37g Ba(CH 3 COO) 3 ·H 2 O was added to 10 mL of 5% H 2 o 2 In solution, Ba(CH 3 COO) 3 ·H 2 O and H 2 o 2 The ratio of the amount of the substances is 1: 3.2, and constantly stirred. Then, add an appropriate amount of ammonia water to adjust the pH of the solution to 9, and let it stand for 25 minutes to obtain a yellow precipitate. Filtrate, wash the precipitate alternately with dilute ammonia water and absolute ethanol, and dry it in a vacuum oven at room temperature to obtain light yellow precursor powder BaO 2 ·H 2 o 2 . to BaO 2 ·H 2 o 2 Carry out X-ray diffraction (XRD) analysis to know that the prepared BaO 2 ·H 2 o 2 It is a monoclinic crystal system without impurity peaks, indicating that BaO 2 ·H 2 o 2 High purity.

[0028] (2) Weigh 3.05g BaO 2 ·H 2 o 2 and 0.73g H 2 TiO 3 Put it in a mortar, mix and grind evenly, then add 2.19g KOH, 13.6g KNO 3 and 12mL absolute ethanol (BaO 2 ·H 2 o 2 with H 2 TiO 3 The ratio of ...

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Abstract

The invention provides a preparation method of Barium Titanate nano-powder, which comprises the following steps that: soluble barium salt is added into H2O2 solution to be mixed continuously, the pH value of the solution is adjusted with ammonia water, and the mixed solution is held statically, filtered, washed and vacuum-dried to obtain a precursor BaO2. H2O2 powder; then the BaO2.H2O2 and H2TiO3 are mixed and ground, KOH and KNO3 are added to be used as a flux, then absolute ethyl alcohol is added for grinding, the ultrasonic treatment on the mixed ground powder is undertaken, and after being dried and removed ethanol, the mixture is dissolved with deionized water, centrifugally separated and washed with deionized water after being roasted and cooled; and finally the sample is put into thin HNO3 solution to be immersed so as to remove the foreign matters, and the sample is centrifugally separated, washed and dried to obtain the barium titanate powder with the granularity of about 15to 40 nm. The barium titanate powder prepared with the method has the advantages of small power granularity, uniform particles, low roasting temperature, simple production process, safe production process, difficult accumulation of the product particles, high purity of the product, high production efficiency and low implementation cost, and can be widely used for the preparation of different inorganic nano functional materials.

Description

technical field [0001] The invention relates to a preparation method of an inorganic functional nanometer material. Background technique [0002] Barium titanate is an important electronic ceramic material with perovskite structure, which has high relative permittivity, low dielectric loss and excellent piezoelectric, ferroelectric, withstand voltage and insulating properties. It can be widely used in electro-optic devices, ferroelectric detectors, capacitors and other electronic components as heat-sensitive materials, ferroelectric materials and capacitor materials. Therefore, the preparation of ultrafine barium titanate powder has aroused great interest. focus on. At present, the main methods for preparing barium titanate powder include high-temperature solid-phase method, sol-gel method, chemical co-precipitation method and hydrothermal method, etc., but each of these methods has some disadvantages: the high-temperature solid-phase method has a high synthesis temperature...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G23/00B82B3/00
Inventor 朱启安项尚雍高兵陈利霞徐军古谭志刚
Owner XIANGTAN UNIV
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