Preparation method for CaCu3Ti4-xZrxO12 ceramic with high dielectric constant and low dielectric loss

A high dielectric constant, low dielectric technology, applied in the field of dielectric ceramic synthesis, to achieve the effect of good grain uniformity, good temperature stability, and reduced dielectric loss

A high dielectric constant, low dielectric technology, applied in the field of dielectric ceramic synthesis, to achieve the effect of good grain uniformity, good temperature stability, and reduced dielectric loss

CN104909747AActive Publication Date: 2015-09-16TAIYUAN UNIV OF TECH
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  • Preparation method for CaCu3Ti4-xZrxO12 ceramic with high dielectric constant and low dielectric loss
  • Preparation method for CaCu3Ti4-xZrxO12 ceramic with high dielectric constant and low dielectric loss
  • Preparation method for CaCu3Ti4-xZrxO12 ceramic with high dielectric constant and low dielectric loss

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] (1) Weigh 8.349 g of calcium nitrate, 25.624 g of copper nitrate, 0.407 g of zirconium oxynitrate and 64.876 g of citric acid, use absolute ethanol as the solvent, completely dissolve the four raw materials, and then use nitric acid to adjust the pH value to 2- 3. Finally, a blue transparent mixed solution A (x=0.05) was obtained;

[0029] (2) Measure 47.771 mL of butyl titanate, add an equal amount of absolute ethanol, stir until completely mixed, and obtain a light yellow mixed solution B;

[0030] (3) Put solution A in a magnetic stirrer and keep stirring, then slowly add solution B into solution A (to prevent hydrolysis of butyl titanate) until a transparent mixed solution is formed, then add 2 g of polyethylene glycol to promote into glue;

[0031](4) Place the mixed solution finally obtained in the above step (3) in a water bath, adjust the temperature to 80°C, and stir at 200 rpm until a blue xerogel is formed;

[0032] (5) Put the obtained blue x...

Embodiment 2

[0039] The difference between this embodiment and embodiment 1 is that the doping amount of Zr is different (CaCu 3 Ti 4-x Zr x o 12 , x=0.1), after the dielectric performance test, it was found that compared with Example 1, the grain size of the sample was reduced, and ε' was greatly reduced; the tanδ was higher than that of Example 1 as a whole, and the lowest tanδ was 0.039, which appeared in around 10 kHz.

Embodiment 3

[0041] The difference between this embodiment and embodiment 1 is that the doping amount of Zr is different (CaCu 3 Ti 4-x Zr x o 12 , x=0.2), after the dielectric performance test, it was found that compared with Examples 1 and 2, the grain size of the sample was further reduced, and ε' continued to decrease as a whole; tanδ was higher than that of Examples 1 and 2, and the lowest value was 0.058. Also occurs around 10 kHz.

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Abstract

The invention discloses a preparation method for a Zr-doping CaCu3Ti4O12 ceramic material with a high dielectric constant and low dielectric loss by utilization of a sol-gel method, and belongs to the dielectric material synthesis technology field. The concrete method is as follows: a sol-gel method is employed, calcium nitrate, cupric nitrate, zirconium oxynitrate and butyl titanate are employed as raw materials, absolute ethyl alcohol is employed as a solvent, nitric acid is employed to adjust the pH of a solution, the raw materials are weighed according to chemical element mol ratios, sol is prepared and placed in a water-bath kettle, stirring is carried out continuously until xerogel is formed, organic matters are removed, CaCu3Ti4-xZrxO12 precursor powder is obtained, then calcining, crushing, grinding, sieving and granulation are carried out, then a ceramic body with a thickness of 1mm and with a diameter of 12mm is prepared, then the ceramic body is placed in a sintering furnace, sintering and thermal insulation are carried out, and finally a CaCu3Ti4-xZrxO12 ceramic sample can be obtained. The method is simple in technology and is easy for industrial production. The prepared ceramic sample has a high density, good particle uniformity and has an enough high dielectric constant and low dielectric loss.

Description

technical field [0001] The invention belongs to the technical field of dielectric ceramic synthesis, in particular to a high dielectric constant, low dielectric loss CaCu 3 Ti 4-x Zr x o 12 Methods of preparation of ceramics. Background technique [0002] The research and development of high dielectric constant ceramic materials (ε’ > 1000) has led to the rapid development of the application of large-capacity capacitors and the integration and miniaturization of electronic components. Calcium copper titanate (CaCu 3 Ti 4 o 12 , CCTO) is the most typical and representative new type of high dielectric material discovered so far in the 21st century. In the temperature range from 100 K to 400 K, the dielectric constant fluctuates little, and the low-frequency dielectric constant of the single crystal sample can even reach more than 100 k. In addition, CCTO does not contain lead, the preparation process is simple, and the required preparation conditions are relat...

Claims

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Application Information

Patent Timeline
16 Sep 2015
Publication
CN104909747A
IPC
C04B35/49; C04B35/622
Inventors
孙礼; 郝文涛