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A method for preparing perovskite-type composite oxide high-entropy ceramic powder by co-precipitation of ion compensation mixture

A composite oxide and perovskite type technology, applied in the field of lead-free dielectric ceramic materials, can solve the problems of final product deviation from stoichiometric ratio, composition segregation, etc.

Active Publication Date: 2021-09-28
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] However, due to the differences in the concentration, speed and pH range of the precipitation of each cation in the multi-principal oxide, and with the change of pH, the change of the precipitant is also different, resulting in component segregation and making the final product deviate from the stoichiometric ratio.

Method used

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  • A method for preparing perovskite-type composite oxide high-entropy ceramic powder by co-precipitation of ion compensation mixture
  • A method for preparing perovskite-type composite oxide high-entropy ceramic powder by co-precipitation of ion compensation mixture
  • A method for preparing perovskite-type composite oxide high-entropy ceramic powder by co-precipitation of ion compensation mixture

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] (1) with analytically pure BaCl 2 ·H 2 O, ZrCl 4 、TiCl 4 , SnCl 2 , niobium oxalate and high-purity YCl 3 ·6H 2 O, CeCl 3 ·7H 2 O or ErCl 3 ·6H 2 O is raw material, according to the molar ratio of Zr, Sn, Ti, Nb, M is 1:1.1:1.05:1:1, Ba:(Zr 0.2 sn 0.2 Ti 0.2 Nb 0.2 m 0.2) in a molar ratio of 1.05:1, wherein M is one of Y, Ce or Er.

[0025] (2) Dissolve analytically pure concentrated hydrochloric acid in deionized water to prepare a 0.1mol / L hydrochloric acid solution; 4 and SnCl 2 respectively added to hydrochloric acid solution to prepare TiCl 4 and SnCl 2 hydrochloric acid solution, hydrochloric acid is added dropwise to the solution, and the pH value is adjusted to 2-4; the BaCl 2 ·H 2 O, ZrCl 4 , niobium oxalate and MCl 3 Dissolve in deionized water, stir for 60 minutes and slowly add TiCl 4 and SnCl 2 hydrochloric acid solution, continue stirring for 30 minutes to obtain a mixed salt solution with a concentration of 0.5 mol / L, add hydrochlor...

Embodiment 2

[0031] (1) with analytically pure SrCl 2 ·6H 2 O, ZrCl 4 , SnCl 2 、TiCl 4 , HfCl 4 High purity YCl 3 ·6H 2 O or MnCl 2 ·6H 2 O is raw material, according to the molar ratio of Zr, Sn, Ti, Hf, M is 1:1.1:1.05:1.10:1, Sr:(Zr 0.2 sn 0.2 Ti 0.2 f 0.2 m 0.2 ) in a molar ratio of 1.05:1, where M is Mn or Y.

[0032] (2) Dissolve analytically pure concentrated hydrochloric acid in deionized water to prepare a 0.1mol / L hydrochloric acid solution; 4 , SnCl 2 and HfCl 4 respectively added to hydrochloric acid solution to prepare TiCl 4 , SnCl 2 and HfCl 4 hydrochloric acid solution, hydrochloric acid is added dropwise to the solution, and the pH value is adjusted to 2-4; the BaCl 2 ·H 2 O, ZrCl 4 , and MCl 3 Dissolve in deionized water, stir for 60 minutes and slowly add TiCl 4 , SnCl 2 and HfCl 4 hydrochloric acid solution, and continue to stir for 30 minutes to obtain a mixed salt solution with a concentration of 0.5 mol / L. Hydrochloric acid is added dropwise ...

Embodiment 3

[0038] (1) with analytically pure SrCl 2 ·6H 2 O, BaCl 2 , ZrCl 4 、TiCl 4 , SnCl 2 , niobium oxalate, high-purity YCl 3 ·6H 2 O is the raw material, according to the chemical formula Ba of the target product 0.5 Sr 0.5 (Zr 0.2 sn 0.2 Ti 0.2 Nb 0.2 Y 0.2 )O 3 , according to the molar ratio of Zr, Sn, Ti, Nb, Y is 1:1.1:1.05:1:1, (Ba 0.5 Sr 0.5 ): (Zr 0.2 sn 0.2 Ti 0.2 Nb 0.2 Y 0.2 ) in a mol ratio of 1.02:1 for proportioning.

[0039] (2) Dissolve analytically pure concentrated hydrochloric acid in deionized water to prepare a 0.1mol / L hydrochloric acid solution; 4 and SnCl 2 respectively added to hydrochloric acid solution to prepare TiCl 4 and SnCl 2 hydrochloric acid solution, hydrochloric acid is added dropwise to the solution, and the pH value is adjusted to 2-4; the SrCl 2 ·6H 2 O, BaCl 2 ·H 2 O, ZrCl 4 , niobium oxalate and YCl 3 ·6H 2 O was dissolved in deionized water, and TiCl was slowly added to it after stirring for 60 min 4 and SnCl ...

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Abstract

The invention discloses a method for preparing perovskite type composite oxide high-entropy ceramic powder by co-precipitation method of ion compensation mixture, which belongs to the field of lead-free dielectric ceramic materials. The method comprises the following steps: dissolving and mixing the chlorides of Ba and Sr or their mixture, and the chlorides and oxalates of Zr, Sn, Ti, Nb(Hf), Y or Ce, Er(Mn) into a mixed salt solution, in which the concentration of easily lost components Ba, Sn, Ti and Hf is compensated; the aqueous ammonia solution is used as the precipitant or the mixed aqueous solution of sodium carbonate and ammonia is used as the precipitant; the mixed salt solution and the precipitant solution are violently A reaction occurs under stirring to form a precipitate; the ammonium bicarbonate solution is used as a buffer solution to repeatedly clean and filter the precipitate; and a high-entropy ceramic powder is obtained after vacuum azeotropic distillation and roasting.

Description

technical field [0001] The invention belongs to the field of lead-free dielectric ceramic materials, and in particular relates to a method for preparing perovskite-type composite oxide high-entropy ceramic powder by co-precipitation of an ion compensation mixture. Background technique [0002] Lead-based perovskite dielectric ceramic materials are crucial basic materials in electronic devices and communications. However, with the enhancement of people's awareness of environmental protection, lead-containing ceramic materials will eventually be replaced by lead-free ceramics. At present, simple perovskite ceramic materials such as BaTiO 3 , CaTiO 3 , SrTiO 3 and SrZrO 3 can not meet the application requirements. Forming composite perovskite compounds by solid solution or doping, changing the element combination of A and B sites in the perovskite structure, and improving ceramic preparation methods are important means to improve the dielectric properties of lead-free perov...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C04B35/01C04B35/626
CPCC04B35/01C04B35/62605C04B2235/3215C04B2235/3224C04B2235/3225C04B2235/3229C04B2235/3249C04B2235/3251C04B2235/3293
Inventor 仲晓羽陈智慧邱建华任玉荣朱媛媛
Owner CHANGZHOU UNIV
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