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Method for preparing nano CaCu3Ti4O12 ceramic material with giant dielectric constant

A technology of giant dielectric constant and ceramic materials, which is applied in the field of electronic ceramic preparation and technical application, can solve the problem of low dielectric constant of nano-copper calcium titanate, and achieve the advantages of promoting and popularizing, overcoming the increase, and shortening the time Effect

Inactive Publication Date: 2016-02-17
胡晓鸿
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the relative dielectric constant of nano-copper calcium titanate produced by existing methods is still low, generally in the range of 5000 to 30000 (under 10KHz conditions)

Method used

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  • Method for preparing nano CaCu3Ti4O12 ceramic material with giant dielectric constant

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] At room temperature as CaCu 3 Ti 4 o 12 The stoichiometric ratio of the substance weighs 48.3gCa(NO 3 ) 2 4H 2 O and 146gCu(NO 3 ) 2 ·3H 2 O is dissolved in a beaker with 210mL of absolute ethanol, stirred evenly (it can be heated until completely dissolved), and made into liquid A; 278.1g of butyl titanate (C 16 h 36 o 4 Ti) was dissolved in a beaker with 300mL of absolute ethanol, stirred evenly to make liquid B; 500mL of ethylene glycol, 110g of citric acid, 6.2g of lithium carbonate, 20mL of oxalic acid aqueous solution (oxalic acid concentration 0.5mol / L) were evenly mixed It is liquid C. Slowly drop solution B into solution A and stir. At the same time, the temperature is raised rapidly and then refluxed for reaction. The reaction temperature is controlled at 80° C., the pH value is adjusted to 5.0-6.0 with acetic acid, and the reaction time is 1 h. Then slowly drop liquid C into the mixed liquid A and B, adjust the pH value to 3.0-4.0 with acetic acid,...

Embodiment 2

[0023] Weigh 48.5g Ca(NO 3 ) 2 4H 2 O and 146gCu(NO 3 ) 2 ·3H 2O was dissolved in a beaker with 220mL of absolute ethanol, stirred evenly to make liquid A; 278.5g of butyl titanate was dissolved in a beaker with 300mL of absolute ethanol, stirred evenly to make liquid B; 520mL Ethylene glycol, 120 g of citric acid, 6.3 g of lithium carbonate, and 22 mL of oxalic acid aqueous solution (0.5 mol / L) were uniformly mixed into liquid C. Slowly drop solution B into solution A and stir, and at the same time rapidly raise the temperature and then reflux reaction, control the reaction temperature to 85°C, adjust the pH value to 5.0-6.0 with acetic acid, and the reaction time is 1h. Then slowly drop liquid C into the mixed liquid A and B, adjust the pH value to 3.0-4.0 with acetic acid, control the temperature at 80°C, and continue stirring for 2 hours after the dropwise addition is completed. Wash the product with water, filter, put it in a drying oven, dry it at 150°C, take it ou...

Embodiment 3

[0025] Weigh 48.7g Ca(NO 3 ) 2 4H 2 O and 146gCu(NO 3 ) 2 ·3H 2 O was dissolved in a beaker with 230mL of absolute ethanol, and stirred evenly to make liquid A; 279.3g of butyl titanate was dissolved in a beaker with 300mL of absolute ethanol, stirred evenly, to make liquid B; 540mL Ethylene glycol, 130 g of citric acid, 6.4 g of lithium carbonate, and 23 mL of oxalic acid aqueous solution (0.5 mol / L) were uniformly mixed into liquid C. Slowly drop solution B into solution A and stir. At the same time, the temperature is raised rapidly and then refluxed for reaction. The reaction temperature range is controlled at 90°C. The pH value is adjusted to 5.0-6.0 with acetic acid, and the reaction time is 1h. Then slowly drop liquid C into the mixed liquid A and B, adjust the pH value to 3.0-4.0 with acetic acid, control the temperature at 80°C, and continue stirring for 2 hours after the dropwise addition is completed. Wash the product with water, filter it, put it in a drying ...

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Abstract

The invention relates to a method for preparing a nano CaCu3Ti4O12 ceramic material with a giant dielectric constant. The method comprises the steps of dissolving Cu(NO3)2.3H2O and Ca(NO3)2.4H2O in absolute ethyl alcohol to prepare a solution A; dissolving butyl titanate into absolute ethyl alcohol to prepare a solution B; mixing glycol, citric acid, lithium carbonate and an oxalic acid aqueous solution to prepare a solution C; dripping the solution B in the solution A and stirring, and controlling the reaction temperature to be 80 to 95 DEG C and the pH (Potential Of Hydrogen) value to be 5.0 to 6.0; then dripping the solution C into the obtained mixed solution of the solution A and the solution B, and controlling the pH value to be 3.0 to 4.0 and the temperature to be 75 to 85 DEG C; obtaining nano CaCu3Ti4O12 by carrying out aftertreatment and calcination on an obtained product, wherein the calcination temperature is 700 to 850 DEG C. According to the method for preparing the nano CaCu3Ti4O12 ceramic material, disclosed by the invention, the nano CaCu3Ti4O12 which is uniform in particle size distribution, high in chemical activity and easy to modify and dope and has a very high dielectric constant and very low dielectric loss is prepared, the reaction period is greatly shortened, the firing temperature is low, and the energy consumption is low.

Description

technical field [0001] The invention belongs to the field of preparation and technical application of electronic ceramics, in particular to a perovskite-type nano calcium copper titanate (CaCu 3 Ti 4 o 12 ) Preparation method of ceramic material. Background technique [0002] In recent years, with the acceleration of miniaturization, integration, and intelligence of electronic products, dielectric materials, as a widely used electronic material, play an increasingly important role in scientific research and practical applications, with large capacity and small size. , The demand for lightweight capacitors makes high dielectric constant materials the hottest research topic in the current electronics industry. [0003] Most of the high dielectric constants are ferroelectric materials. Because of their ferroelectricity, relaxation, and structural transformation behaviors, the dielectric constant is very sensitive to temperature changes, resulting in a decrease in the stabili...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/462C04B35/626B82Y30/00
Inventor 张家松
Owner 胡晓鸿
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