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A kind of preparation method of cacu3ti4o12

A powder and crystal technology, which is applied in the field of electronic ceramics preparation and application, can solve the problems of obtaining CCTO crystal powder, unfavorable CCTO crystal dynamic characteristics, cumbersome preparation process, etc., and achieve narrow particle size distribution range, sintering process optimization, process simple effect

Active Publication Date: 2019-04-16
SHANGQIU NORMAL UNIVERSITY
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Problems solved by technology

[0003] CCTO ceramics mainly adopt the traditional high-temperature solid-state method to form CuO, TiO 2 and CaCO 3 It is obtained by high-temperature sintering of raw materials, and its grain size, purity, degree of agglomeration and other factors will affect the grain size and shape of CCTO ceramics, and have a greater impact on the dielectric properties of the product. Since the sintering temperature is generally above 1000 ° C, It is difficult to obtain CCTO crystal powder at low temperature, which is not conducive to the study of the kinetic properties of CCTO crystals
The preparation of CCTO by sol-gel method and liquid phase synthesis method is simpler than the solid phase synthesis method, but the preparation process is more cumbersome, and high temperature (>800°C) sintering process is still required to obtain CCTO ceramics

Method used

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Embodiment 1

[0032] The preparation method of the present embodiment CCTO crystal powder is based on calcium acetylacetonate Ca (acac) 2 , Copper acetylacetonate Cu(acac) 2 and titanyl acetylacetonate TiO(acac) 2 As a raw material, using absolute ethanol as a solvent and anhydrous citric acid as a stabilizer, the CCTO crystal powder is obtained by low-temperature calcination, which specifically includes the following steps:

[0033] (1) Weigh 0.01mol of Ca(acac) 2 , 0.03mol of Cu(acac) 2 and 0.04mol of TiO(acac) 2 , add 20ml of absolute ethanol, and stir vigorously with a magnetic stirrer to obtain a mixed solution;

[0034] (2) Add anhydrous citric acid to the mixed solution to adjust the pH value to 1.5 to obtain a light blue solution, and continue to stir for 1 hour;

[0035] (3) drying the solution in step (2) at 80° C. for 12 hours to obtain light blue needle-like crystals;

[0036] (4) Fully grind the light blue needle-shaped crystals, then raise the temperature to 450°C at a r...

Embodiment 2

[0045] The preparation method of the present embodiment CCTO crystal powder is based on calcium acetylacetonate Ca (acac) 2 , Copper acetylacetonate Cu(acac) 2 and titanyl acetylacetonate TiO(acac) 2 As a raw material, using absolute ethanol as a solvent and anhydrous citric acid as a stabilizer, the CCTO crystal powder is obtained by low-temperature calcination, which specifically includes the following steps:

[0046] (1) Weigh 0.01mol of Ca(acac) 2 , 0.033mol of Cu(acac) 2 and 0.04mol of TiO(acac) 2 , add 20ml of absolute ethanol, and stir vigorously with a magnetic stirrer to obtain a mixed solution;

[0047] (2) Add anhydrous citric acid to the mixed solution to adjust the pH value to 1.8 to obtain a light blue solution, and continue to stir for 0.5 h;

[0048] (3) drying the solution in step (2) at 85° C. for 15 hours to obtain light blue needle-like crystals;

[0049] (4) Fully grind the light blue needle-shaped crystals, then raise the temperature to 500°C at a r...

Embodiment 3

[0052] The preparation method of the present embodiment CCTO crystal powder is based on calcium acetylacetonate Ca (acac) 2 , Copper acetylacetonate Cu(acac) 2 and titanyl acetylacetonate TiO(acac) 2 As a raw material, using absolute ethanol as a solvent and anhydrous citric acid as a stabilizer, the CCTO crystal powder is obtained by low-temperature calcination, which specifically includes the following steps:

[0053] (1) Weigh 0.01mol of Ca(acac) 2 , 0.035mol of Cu(acac) 2 and 0.04mol of TiO(acac) 2 , add 20ml of absolute ethanol, and stir vigorously with a magnetic stirrer to obtain a mixed solution;

[0054] (2) Add anhydrous citric acid to the mixed solution to adjust the pH value to 1.2 to obtain a light blue solution, and continue to stir for 1 hour;

[0055] (3) drying the solution in step (2) at 90° C. for 10 h to obtain light blue needle-like crystals;

[0056] (4) Fully grind the light blue needle-shaped crystals, then raise the temperature to 600° C. at a ra...

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Abstract

The invention discloses a preparation method of CaCu3Ti4O12. The method comprises a preparation method of CaCu3Ti4O12 crystal powder and a preparation method of CaCu3Ti4O12 ceramic. The preparation method of the CaCu3Ti4O12 crystal powder includes: adopting calcium acetylacetonate Ca(acac)2, copper acetylacetonate Cu(acac)2 and titanium oxide acetylacetonate TiO(acac)2 as the raw materials, using anhydrous ethanol as the solvent, taking anhydrous citric acid as the stabilizer, and conducting low temperature calcination to obtain CaCu3Ti4O12 crystal powder; the preparation method of the CaCu3Ti4O12 ceramic includes: conducting tabletting on the CaCu3Ti4O12 crystal powder, and then performing high temperature sintering to obtain CaCu3Ti4O12 ceramic. The method provided by the invention for the first time takes the organic metal compound calcium acetylacetonate, copper acetylacetone and titanium oxide acetylacetonate as the precursor raw materials, adopts anhydrous ethanol as the solvent, employs anhydrous citric acid as the stabilizer, and carries out simple mixing, drying and low temperature calcination to obtain high purity and good crystal form CaCu3Ti4O12 crystal powder. The method solves the technical problem that with a necessary high temperature sintering process, the solid phase oxide method, sol-gel method and liquid phase synthesis method cannot acquire high purity CaCu3Ti4O12 crystal powder at low temperature.

Description

technical field [0001] The present invention relates to a kind of CaCu 3 Ti 4 o 12 The preparation method of (CCTO), in particular relates to a preparation method of CCTO crystal powder and CCTO ceramics, and belongs to the technical field of electronic ceramics preparation and application. Background technique [0002] ACu 3 Ti 4 o 12 The (A=Ca, Ba, Sr) series of materials was discovered in 1967, and its precise structure was determined in 1979. It was not until 2000 that Subramanian and others first discovered the dielectric properties of CCTO. ACu 3 Ti 4 o 12 Type oxides have a relatively complex perovskite structure and a huge dielectric constant related to their perovskite structure, so they have extremely high potential application value in different fields. Currently widely used BaTiO 3 and non-environmentally friendly Pb(Mg 1 / 3 Nb 2 / 3 )O 3 (PMN) and other types of materials have a high dielectric constant. BaTiO 3 It is a ferroelectric perovskite mater...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C04B35/462C04B35/626C04B35/632C04B35/622C04B35/64
CPCC04B35/462C04B35/622C04B35/626C04B35/62675C04B35/632C04B35/64C04B2235/3208C04B2235/3281C04B2235/96
Inventor 张文星李立强程文静梁果
Owner SHANGQIU NORMAL UNIVERSITY
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