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Preparation method of CaCu3Ti4O12 ceramic

A technology of ceramics and cuo, applied in the field of preparation of CaCu3Ti4O12 ceramics, can solve the problems of secondary growth of crystal grains, ceramic properties, influence of ceramic structure, densification, deterioration, etc., to reduce high temperature and low frequency dissipation, uniform particle size, structure dense effect

Inactive Publication Date: 2011-09-07
NORTHWESTERN POLYTECHNICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The selection of sintering temperature, holding time and heating rate all directly affect the structure and densification of ceramics, especially the secondary growth of grains that tends to occur in the later stage of sintering often leads to deterioration of ceramic performance

Method used

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  • Preparation method of CaCu3Ti4O12 ceramic
  • Preparation method of CaCu3Ti4O12 ceramic
  • Preparation method of CaCu3Ti4O12 ceramic

Examples

Experimental program
Comparison scheme
Effect test

Embodiment l

[0019] Embodiment 1: with high-purity 3.0414g CaCO 3 (>99%), 7.2514g CuO (>99%), 9.7074gTiO 2 (>99%) powder as the raw material, according to the CCTO stoichiometric ratio, mix 20g of material, ball mill in distilled water medium for 12h; dry and sieve the powder and pre-calcine at 960°C for 2h. Add 15.4ml ethanol, 0.25ml n-butanol and 0.36ml trioleic acid glyceride to the powder after pre-burning, then put into the nylon ball mill jar, and use ZrO 2 The ball is used as the grinding medium, and it is put into a planetary ball mill with a speed of 400rad / min for wet grinding for 23 hours; 0.9592g of polyethylene glycol, 1.0ml of dioctyl phthalate, and 1.3174g of polyethylene are added to the wet material that has been ground for 23 hours. Alcohol butyral and 0.24ml cyclohexane, and then ball milled for 20h at a speed of 350rad / min; pour the slurry into a small beaker and take out all the ZrO 2 Then pour the slurry into a casting machine with a clean and smooth glass plate, so...

Embodiment 2

[0020] Embodiment 2: with high-purity 3.344g CaCO 3 (>99%), 7.9765g CuO (>99%), 10.6788gTiO 2 (>99%) powder as the raw material, according to the CCTO stoichiometric ratio of 22g material, ball milled in distilled water medium for 12h; the dried and sieved powder was pre-fired at 960°C for 2h. Add 15.48ml ethanol, 0.3ml n-butanol and 0.4ml triolein to the powder after pre-burning, then put it into a nylon ball mill jar, and use ZrO 2 The ball is used as the grinding medium, and it is put into a planetary ball mill with a speed of 400rad / min for wet grinding for 20 hours; 0.960g of polyethylene glycol, 0.997ml of dioctyl phthalate, and 1.321g of polyethylene are added to the wet material that has been ground for 20 hours. Alcohol butyral and 0.28ml cyclohexane, and then ball milled for 20h at a speed of 400rad / min; pour the slurry into a small beaker and take out all the ZrO 2Then pour the slurry into a casting machine with a clean and smooth glass plate, so that it moves at ...

Embodiment 3

[0021] Embodiment 3: with high-purity 3.7561g CaCO 3 (>99%), 8.9555g CuO (>99%), 11.9886gTiO 2 (>99%) powder as the raw material, according to the CCTO stoichiometric ratio of 24.7g material, ball milled in distilled water medium for 10h; the dried and sieved powder was pre-fired at 960°C for 2h. ; Add 15.5ml ethanol, 0.4ml n-butanol and 0.4ml trioleic acid glyceride to the powder after pre-burning, then put into the nylon ball mill jar, and use ZrO 2 The ball is used as the grinding medium, put it into a planetary ball mill with a rotation speed of 400rad / min for 24 hours; add 0.9663g of polyethylene glycol, 0.99ml of dioctyl phthalate, and 1.34g of polyethylene to the wet material that has been ground for 24 hours Alcohol butyral and 0.3ml cyclohexane, and then ball milled for 20h at a speed of 400rad / min; pour the slurry into a small beaker and take out all the ZrO 2 Then pour the slurry into a casting machine with a clean and smooth glass plate, so that it moves at a con...

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Abstract

The invention discloses a preparation method of CaCu3Ti4O12 (CCTO) ceramic, and the method can be used for solving the technical problem of high dielectric loss caused by the existing preparation method of the CaCu3Ti4O12 ceramic. The technical scheme of the invention is as follows: a casting technology is adopted to prepare a CCTO ceramic wafer, then a two-step sintering technology is adopted to obtain a ceramic material with dense structure and uniform particle size; and according to the changes of the dielectric constant epsilon r and dielectric loss tan delta of the CCTO ceramic along with the testing frequency and the temperature, CCTO crystalline integrity, grain boundary, defect and other aspects can directly influence the high dielectric constant. In addition, at the room temperature and 1KHz, when the sintering temperature is 1025-1100 DEG C and heat preservation is performed for 10 hours, the epsilon r of the CCTO ceramic prepared through two-step sintering is 104, which is more or less the same with the value reported in literatures; and the dielectric loss is reduced from 0.3-0.6 reported in the background art to 0.03, which shows that the concentration of oxygen vacancies can be reduced by adopting the two-step sintering method. Therefore, the high-temperature low-frequency dissipation of the ceramic can be significantly reduced; and the lattice distortions can be reduced along with the increase of the heat preservation time.

Description

technical field [0001] The present invention relates to a preparation method of ceramics, in particular to a CaCu 3 Ti 4 o 12 Methods of preparation of ceramics. Background technique [0002] Ceramic dielectric capacitors are widely used electronic components, and their dielectric materials are expected to have a high dielectric constant in order to achieve miniaturization. CaCu 3 Ti 4 o 12 (CCTO) is a high dielectric constant material discovered in recent years. It does not undergo structural phase transition in the range of 100-600K and has good temperature stability. Therefore, the possibility of using it as a high dielectric constant material in high-density information storage, thin film devices and high dielectric capacitors has attracted widespread attention. [0003] For the CCTO research, there are orders of magnitude differences in εr reported by different scholars, ranging from 478 to 300,000. Document 1 "Giant dielectric constant response in a copper-tita...

Claims

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Application Information

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IPC IPC(8): C04B35/462C04B35/622
Inventor 郑茜樊慧庆
Owner NORTHWESTERN POLYTECHNICAL UNIV
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