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Wet chemical method for preparing lead-based relaxor ceramics with perovskite structure or their solid solutions

A technology of perovskite structure and wet chemical method, which is applied in the field of ceramic preparation, can solve the problems of difficult removal of impurities, toxic substances, and high price, and achieve the effects of short mixing time, low cost, and easy production control and application

Inactive Publication Date: 2011-12-14
INST OF METAL RESEARCH - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The purpose of the present invention is to provide a new wet chemical method for preparing lead-based relaxation ceramics and its solid solution system, which solves the problems in the prior art that the price is expensive, most of them are toxic substances, and impurities are difficult to remove.

Method used

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  • Wet chemical method for preparing lead-based relaxor ceramics with perovskite structure or their solid solutions
  • Wet chemical method for preparing lead-based relaxor ceramics with perovskite structure or their solid solutions
  • Wet chemical method for preparing lead-based relaxor ceramics with perovskite structure or their solid solutions

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Experimental program
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Effect test

Embodiment 1

[0060] Weigh lead acetate, ferric nitrate and ammonium tungstate according to the molar ratio of Pb:Fe:W 3:2:1, and weigh citric acid and ethylene glycol respectively according to the molar ratio of complexing agent and metal ion of 2:1. Aminetetraacetic acid, citric acid and ethylenediaminetetraacetic acid were dissolved in deionized water respectively, the concentration of citric acid was 1.0Mol / L, the concentration of ethylenediaminetetraacetic acid was 1.0Mol / L, and then according to figure 1 The process flow diagram shown is synthesized and prepared as figure 2 Pure Pb(Fe 2 / 3 W 1 / 3 )O 3 , the crystal grains of the product present a cubic shape, with an average size of about 250nm, and the X-ray diffraction spectrum is shown in image 3 . Among them, the optimum sintering temperature is 725°C, and the purity is as high as 99wt%.

Embodiment 2

[0062] According to the molar ratio of Pb:Fe:W:Bi 3:4:1:2, weigh appropriate weights of lead acetate, iron nitrate, ammonium tungstate and bismuth nitrate, respectively according to the molar ratio of complexing agent and metal ion of 2:1 Weigh citric acid and ethylenediaminetetraacetic acid, citric acid and ethylenediaminetetraacetic acid are dissolved in deionized water respectively, the concentration of citric acid is 1.5Mol / L, and the concentration of ethylenediaminetetraacetic acid is 1.5Mol / L, then according to figure 1 The process flow diagram shown synthesizes and prepares 0.6Pb(Fe 2 / 3 W 1 / 3 )O 3 -0.4BiFeO 3 Single-phase solid solution, the average size of cubic crystal grains is about 100nm, and its morphology is as follows Figure 4 Shown, the X-ray diffraction spectrum is shown in Figure 5 . Among them, the optimum sintering temperature is 700°C, and the purity of the obtained bismuth-doped iron lead tungstate is as high as 99wt%.

Embodiment 3

[0064] Weigh appropriate weights of lead acetate, iron nitrate, ammonium tungstate and magnesium nitrate according to the molar ratio of Pb:Fe:W:Mg 5:2:2:1, and weigh according to the molar ratio of complexing agent to metal ion of 2:1 Get citric acid and ethylenediaminetetraacetic acid, citric acid and ethylenediaminetetraacetic acid are dissolved in deionized water respectively, the concentration of citric acid is 2.0Mol / L, the concentration of ethylenediaminetetraacetic acid is 2.0Mol / L, and then according to figure 1 0.6Pb(Fe 2 / 3 W 1 / 3 )O 3 -0.4Pb(Mg 1 / 2 W 1 / 2 )O 3 Single-phase solid solution, its X-ray diffraction spectrum is as follows Figure 6 shown. Among them, the optimum sintering temperature is 700°C, and the purity of the obtained magnesium-doped iron lead tungstate is as high as 99wt%.

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Abstract

The invention relates to a wet chemical method for preparing lead-based relaxation ceramics with a pure perovskite structure and its solid solution, belonging to the technical field of ceramic preparation. The method uses metal inorganic salts lead acetate, iron nitrate, ammonium tungstate, bismuth nitrate, magnesium nitrate and cobalt nitrate as precursors, and forms a sol through the complexation of ethylenediaminetetraacetic acid and citric acid. The sol is dried to obtain a xerogel, and the xerogel is calcined at a temperature not lower than 400°C to obtain a powder, which can be pressed into tablets to obtain a green magnetic sheet. Finally, the powder or raw magnetic sheet is sintered at 600-800° C. to obtain a lead-based relaxation ceramic with a pure perovskite structure or a solid solution thereof. The present invention avoids the use of expensive metal alkoxides in the traditional wet chemical method, effectively suppresses the formation of the pyrochlore phase with evil dielectric properties, greatly reduces the sintering temperature, and provides high-performance lead-based relaxation ceramics or its Solid solutions offer a practical approach.

Description

technical field [0001] The invention relates to a wet chemical method for preparing lead-based relaxation ceramics with a pure perovskite structure and its solid solution, belonging to the technical field of ceramic preparation. Background technique [0002] Composite Perovskite Ferroelectric A(B′B″)O 3 The dielectric relaxation phenomenon was first discovered by the former Soviet scientist G.A.Smolensky and others. As one of the most common and important members, lead-based relaxor ceramics have high dielectric constant, low capacity temperature change rate, high electromechanical coupling coefficient, large saturation strain, small strain hysteresis, and fast response. , good return to zero, and low driving power, it is an ideal material for manufacturing functional original devices such as multilayer ceramic capacitors, transducers and actuators, among which Pb(Zr x Ti 1-x )O 3 It is one of the lead-based relaxation ceramics widely used in actual production. At the s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/497C04B35/26C04B35/622
Inventor 刘志权姚春发李财富
Owner INST OF METAL RESEARCH - CHINESE ACAD OF SCI
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