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Process for preparing superfine powder of lead magnesium niobate-lead titanate solid solution

A technology of ultra-fine powder and lead magnesium niobate, which is applied in the field of ferroelectric material preparation, can solve the problems of affecting the dispersion of powder, poor particle uniformity, and inability to separate grains, achieving good stability and easy control , the effect of doping convenience

Inactive Publication Date: 2006-01-18
INST OF ELECTRICAL ENG CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But because the difference of material system, prepare PMNT superfine powder with the procedure of this patent, following problem can occur: 1, because adopted the method that sol is added in the acetone rapidly in this method, although adding while carrying out strong Stirring, but due to the simultaneous entry of a large number of sols, it is difficult to avoid the growth of grains, and the formation and growth of grains cannot be completely separated, which creates conditions for the growth of particles, and at the same time causes the generation of large particles. Make the generated particle uniformity worse
2. Use the method of drying the precipitate in an oven at 60°C to 80°C to dry the powder quickly, which will cause some powders to agglomerate and affect the dispersibility of the final powder

Method used

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  • Process for preparing superfine powder of lead magnesium niobate-lead titanate solid solution
  • Process for preparing superfine powder of lead magnesium niobate-lead titanate solid solution

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] The first step: the synthesis of PMNT sol.

[0031] With the molecular formula 0.9Pb(Mg 1 / 3 Nb 2 / 3 )O 3 -0.1PbO 3 The molar ratio of each component (5mol% excess of Mg substance, 10mol% excess of Pb substance amount) was used as a measurement standard, and a PMNT precursor solution of 0.2mol / l was prepared. Weigh 1.672g of lead acetate (Pb(CH 3 COO) 2 ·3H 2 O), 0.270g of magnesium acetate (Mg(CH 3 COO) 2 4H 2 O), 0.7632g of niobium ethoxide (Ni(OC 2 h 5 )) and 0.136g of tetrabutyl titanate (Ti(OC 4 h 9 ) 4 ). Lead acetate (Pb(CH 3 COO) 2 ·3H 2 O) and magnesium acetate (Mg(CH 3 COO) 2 4H 2 O) Incubate in a drying oven at 120° C. for 30 minutes, then dissolve them in 7 ml of ethylene glycol methyl ether, and stir for 1 hour to fully dissolve them. Dissolve niobium ethoxide and tetrabutyl titanate in 3ml of ethylene glycol monomethyl ether, stir for 0.5 hours, then add 2ml of acetylacetone to the solution of niobium ethoxide and tetrabutyl titanate res...

Embodiment 2

[0041] The first step: the synthesis of PMNT sol.

[0042] With the molecular formula 0.9Pb(Mg 1 / 3 Nb 2 / 3 )O 3 -0.1PbO 3 The molar ratio of each component (3mol% excess of Mg substance, 10mol% excess Pb substance amount) was used as a measurement standard, and a PMNT precursor solution of 0.2mol / l was prepared. Weigh 1.672g of lead acetate (Pb(CH 3 COO) 2 ·3H 2 O), 0.1893g of magnesium acetate (Mg(CH 3 COO) 2 4H 2 O), 0.7632g of niobium ethoxide (Ni(OC 2 h 5 )) and 0.136g of tetrabutyl titanate (Ti(OC 4 h 9 ) 4 ). Lead acetate (Pb(CH 3 COO) 2 ·3H 2 O) and magnesium acetate (Mg(CH 3 COO) 2 4H 2 O) heat preservation in a drying oven at a temperature of 120° C. for 60 minutes, then dissolve in 7 ml of ethylene glycol methyl ether, and stir for 1 hour to fully dissolve. Dissolve niobium ethoxide and tetrabutyl titanate in 5ml of ethylene glycol monomethyl ether, stir for 0.5 hours, then add 1ml of acetylacetone to the solution of niobium ethoxide and tetrabuty...

Embodiment 3

[0052] The first step: the synthesis of PMNT sol.

[0053] With the molecular formula 0.9Pb(Mg 1 / 3 Nb 2 / 3 )O 3 -0.1PbO 3 The molar ratio of each component (5 mol% excess of Mg and 5 mol% of Pb excess) was used as a measurement standard, and a PMNT precursor solution of 0.2 mol / l was prepared. Weigh 1.596g of lead acetate (Pb(CH 3 COO) 2 ·3H 2 O), 0.2696g of magnesium acetate (Mg(CH 3 COO) 2 4H 2 O), 0.7632g of niobium ethoxide (Ni(OC 2 h 5 )) and 0.136g of tetrabutyl titanate (Ti(OC 4 h 9 ) 4 ). Lead acetate (Pb(CH 3 COO) 2 ·3H 2 O) and magnesium acetate (Mg(CH 3 COO) 2 4H 2 O) Insulate in a drying oven at a temperature of 120° C. for 40 minutes, then dissolve in 7 ml of ethylene glycol methyl ether, and stir for 1 hour to fully dissolve. Dissolve niobium ethoxide and tetrabutyl titanate in 3ml of ethylene glycol monomethyl ether, stir for 0.5 hours, then add 1ml of acetylacetone to the solution of niobium ethoxide and tetrabutyl titanate respectively, the...

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Abstract

The preparation process of superfine lead magnesate niobate-lead titanate solid solution powder, unlike conventional superfine powder preparing process, adopts capillary with peristaltic pump to add sol slowly into alkali solution for controlling the powder producing condition and thus has short powder preparing period and lowered sintering temperature. During the powder drying stage, the cleaning with organic solvent and the vacuum freeze drying are combined to raise the dispersivity of prepared powder. The powder of the present invention has the feature of low sintering temperature, and, TEM, EDS and XRD test and analysis shows, has precise components, fine and homogeneous granularity, high dispersivity and complete perovskite phase structure.

Description

technical field [0001] The invention relates to a method for preparing a ferroelectric material, in particular to a method for preparing ultrafine powder of lead magnesium niobate-lead titanate (PMN-PT) solid solution. Background technique [0002] Lead magnesium niobate-lead titanate solid solution (Pb(Mg 1 / 3 Nb 2 / 3 )O 3 -PbTiO 3 , abbreviated as PMN-PT), is a kind of relaxor ferroelectric with perovskite phase structure, which is widely used in the preparation of multilayer thin films due to its high dielectric constant and large field stretching coefficient Capacitors and electromechanical conversion transducers and other microelectronics fields. PMN-PT also has the characteristics of large pyroelectric coefficient, which is suitable for use as a working medium in refrigerators and infrared detectors. [0003] With the development of electronic technology, thick-film materials and thick-film devices have become research hotspots at home and abroad. Thick-film materia...

Claims

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Application Information

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IPC IPC(8): C04B35/462C04B35/499C04B35/624
Inventor 张清涛李艳秋刘少波
Owner INST OF ELECTRICAL ENG CHINESE ACAD OF SCI
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