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Compound perovskite oxide and preparation method thereof

A composite perovskite and oxide technology, applied in the field of electronic ceramics, can solve the problems of large lattice stress and failure to synthesize, and achieve the effect of suppressing lattice strain

Inactive Publication Date: 2014-04-16
GUILIN UNIVERSITY OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the high temperature during the calcination process, CaCu 3 Ni 4 o 12 The lattice stress of is too high to be synthesized

Method used

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  • Compound perovskite oxide and preparation method thereof
  • Compound perovskite oxide and preparation method thereof
  • Compound perovskite oxide and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Composite perovskite oxide: CaCu 3 Ni 4 o 12 .

[0020] The preparation steps are:

[0021] (1) Using calcium oxide, copper oxide and nickel monoxide as raw materials, according to the general formula CaCu 3 Ni 4 o 12 The stoichiometric ratio for batching.

[0022] (2) Put the raw materials prepared in step (1) into a ball mill jar, add zirconia balls and absolute ethanol as the ball milling medium, the mass of the added zirconia balls is twice the mass of the raw materials, and the added absolute ethanol The mass is 0.5 times that of the raw material, and the wet milling method is used for ball milling and mixing for 4 hours at a speed of 450 rpm, and the mixed slurry is taken out and dried at 140°C.

[0023] (3) Put the powder dried in step (2) into a niobium crucible, and then press the powder together with the niobium crucible under a one-way pressure of 200MPa.

[0024] (4) Place the block formed in step (3) in a high-pressure sintering furnace, first apply...

Embodiment 2

[0027] Composite perovskite oxide CaCu 3 Sb 4 o 12 .

[0028] The preparation steps are:

[0029] (1) Using calcium oxide, copper oxide and antimony pentoxide as raw materials, according to the general formula CaCu 3 Sb 4 o 12 The stoichiometric ratio for batching.

[0030] (2) Put the raw materials prepared in step (1) into a ball mill jar, add zirconia balls and absolute ethanol as the ball milling medium, the mass of the added zirconia balls is 6 times the mass of the raw materials, and the added absolute ethanol The mass is 1 times that of the raw material, and the wet milling method is used for ball milling and mixing for 12 hours at a speed of 350 rpm, and the mixed slurry is taken out and dried at 100°C.

[0031] (3) Put the powder dried in step (2) into a molybdenum crucible, and then press the powder together with the molybdenum crucible under a one-way pressure of 300MPa.

[0032] (4) Place the block formed in step (3) in a high-pressure sintering furnace, fi...

Embodiment 3

[0036] Composite perovskite oxide: CaCu 3 Bi 4 o 12 .

[0037] The preparation steps are:

[0038] (1) Using calcium oxide, copper oxide and bismuth trioxide as raw materials, according to the general formula CaCu 3 Bi 4 o 12 The stoichiometric ratio of

[0039] material.

[0040] (2) Put the raw materials prepared in step (1) into a ball mill jar, add zirconia balls and absolute ethanol as the ball milling medium, the mass of the added zirconia balls is 8 times the mass of the raw materials, and the added absolute ethanol The mass is twice that of the raw material, and the wet milling method is used for ball milling and mixing for 24 hours at a speed of 200 rpm, and the mixed slurry is taken out and dried at 80°C.

[0041] (3) Put the powder dried in step (2) into a titanium crucible, and then press the powder together with the titanium crucible under a one-way pressure of 400MPa.

[0042] (4) Place the block formed in step (3) in a high-pressure sintering furnace, fir...

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Abstract

The invention discloses a compound perovskite oxide and a preparation method thereof. A general formula of the compound perovskite oxide is CaCu3Me4O12, wherein Me is one of Ni, Sb and Bi. The preparation method comprises the steps of taking calcium oxide, cupric oxide, nickel oxide, antimony pentoxide and bismuth trioxide as raw materials, mixing and ballmilling for 4-24h at the ballmilling rate of 200-450rpm, conducting pressure molding on ballmilled powder under 200-400MPa unidirectional pressure, sintering under high pressure, boosting 3-5GPa high pressure, heating to 1000-1200 DEG C with a heating rate of 30-50 DEG C / min, sintering for 30-120min, cooling to the room temperature at a rate of 20-50 DEG C / min, and removing the high pressure. Under the extra high pressure, the metastable compound perovskite oxide CaCu3Me4O12 can be kept stable; related compounds remain extra high pressure states in a whole high-temperature synthetic process; and a second phase due to lattice strain and the like is inhibited, so that the pure compound perovskite oxide can be obtained.

Description

technical field [0001] The invention relates to a composite perovskite oxide and a preparation method thereof, belonging to the field of electronic ceramics. Background technique [0002] With the rapid development of science and technology, multilayer ceramic capacitors are increasingly developing in the direction of miniaturization, low cost, and large capacity, and correspondingly require materials with higher dielectric constants. According to literature reports, Subramanian discovered CaCu in 2000 3 Ti 4 o 12 The high dielectric properties of [Subramanian M. A et al, High dielectric constant in ACu 3 Ti 4 o 12 and ACu 3 Ti 3 FeO 12 phase, Journal of Solid State Chemistry, 2000, 151, 323-325], the material has a very high dielectric constant at room temperature, about 10000, in a wide frequency range, and in a wide temperature range Exhibits high temperature stability with dielectric response. Most scholars believe that CaCu 3 Ti 4 o 12 The high dielectric...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C04B35/45C04B35/453C04B35/622
Inventor 刘来君黄延民史丹平郑少英方亮
Owner GUILIN UNIVERSITY OF TECHNOLOGY
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