Method for preparing doped barium titanate powder through wet process

A barium titanate powder, barium titanate technology, applied in chemical instruments and methods, titanium compounds, inorganic chemistry, etc., can solve the problems such as gel precipitate drying and anti-hard agglomeration that are not proposed.

Inactive Publication Date: 2011-05-18
刘秦
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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  • Method for preparing doped barium titanate powder through wet process
  • Method for preparing doped barium titanate powder through wet process
  • Method for preparing doped barium titanate powder through wet process

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Embodiment 1

[0086] The doped barium titanate of the present embodiment is (Ba 0.9575 Gd 0.0025 Ca 0.04 )[Ti 0.815 mn 0.0025 Y 0.0025 Zr 0.18 ] 0.997 o 3 . First deionized water was boiled for 20 minutes, and cooled for later use; 61.1788 grams of titanium isopropoxide (98%) were weighed in a nitrogen protection box, then 58 milliliters of lactic acid (85%) was added, and an appropriate amount of deionized water was added after fully stirring. React at 60°C for 4 hours; dissolve 10.7729 g of zirconyl nitrate in 40 ml of deionized water at 50°C, add 9 ml of lactic acid (85%), stir well, and then pour the formed white suspension into titanium isopropoxide and the reaction solution of lactic acid, stir and mix evenly; add 80.0185 grams of Ba(OH) 2 ·8H 2 O (98%) and 0.8099 g Ca(OH) 2 (95%), reacted for 8 hours at 50°C; then added 0.1586 gram of Mn(CH 3 COO) 2 4H 2 O, 0.2478 g Y (NO 3 ) 3 ·6H 2 O and .0.2929 g Gd(NO 3) 3 ·6H 2 0, add water and dilute to 300 milliliters, stir...

Embodiment 2

[0088] Compared with embodiment 1, the differences of this embodiment are:

[0089] Weigh 42 grams (NH 4 ) 2 C 2 o 4 ·H 2 O, make an ammonium oxalate solution with a temperature of 80°C and a mass concentration of 18.2%, then add 0.110 grams of nonionic surfactant APG; while stirring, slowly pour the metal ion precursor solution A2 whose temperature is raised to 80°C Oxalic acid solution to form a precipitate; vacuum filter, wash 4 times with deionized water containing 0.05% polyethylene glycol, and wash 3 times with absolute ethanol; put the precipitated filter cake in an ordinary drying oven, bake at 85°C for 20 hours; place in Incubate in a muffle furnace at 350°C for 120 minutes and at 550°C for 4 hours, take out the powder and grind it, then heat at 800°C for 180 minutes to obtain doped barium titanate powder.

Embodiment 3

[0091] The doped barium titanate of the present embodiment is (Ba 0.9575 Nd 0.0025 Ca 0.04 )[Ti 0.815 mn 0.0025 Er 0.0025 Zr 0.18 ] 0.997 o 3 . First deionized water was boiled for 20 minutes, cooled for later use; 44 milliliters of lactic acid (85%) was added to 80.2520 grams of tetrabutyl titanate (99%), after fully stirring, deionized water was added to adjust the total volume of the solution to 200 milliliters, React at 50°C for 6 hours; dissolve 11.9210 g of zirconyl nitrate in 40 ml of deionized water at 50°C, add 10 ml of lactic acid (85%), stir well and then pour the formed white suspension into tetrabutyl titanate The reaction solution of ester and lactic acid, stirring and mixing; add 88.5464 grams of Ba (OH) 2 ·8H 2 O (98%) and 0.8962 g Ca(OH) 2 (95%), reacted for 3 hours at 90°C; then added 0.1754 gram of Mn(CH 3 COO) 2 4H 2 O, 0.3174 grams of Er(NO 3 ) 3 ·5H 2 O and 0.3266 g Nd(NO 3 ) 3 ·nH 2 O(37%Nd 2 o 3 ), diluted with water to 400 ml, sti...

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Abstract

The invention discloses a method for preparing doped barium titanate powder with superhigh dielectric constant, high insulation resistance, long circulation service life and stable temperature, and belongs to the technical field of electronic ceramic precursor power synthesis. The method comprises the following steps of: directly preparing hydrolytic stable solution through complex reaction of tetra-alkoxy titanium, barium hydroxide, calcium hydroxide and alpha-hydroxy acid; adding soluble nitrate and acetate of other doped components, mixing uniformly, ageing, mixing with a precipitator in oxalic acid, ammonium oxalate and tetramethylammonium hydroxide, and a surfactant to generate precipitates, wherein alkaline precipitates are subjected to deflocculation treatment of water-organic reagent azeotropic dehydration and reflux ageing; and separating, drying and calcining to obtain the powder. The method has the advantages of simple process, low cost, low powder agglomeration, low calcining temperature, and small secondary granularity, and can be applied to the fields such as multilayer ceramic capacitors, electric energy storage capacitors and the like.

Description

technical field [0001] The invention belongs to the technical field of synthesis of electronic ceramic precursor powder, and relates to a wet preparation method of doped barium titanate powder with ultra-high dielectric constant, high insulation resistance, long cycle service life and temperature stability. Background technique [0002] The dielectric material is the basic material of ceramic capacitors. The capacitance value of a flat panel capacitor is proportional to the dielectric constant of the dielectric material and inversely proportional to its thickness. Usually, the thickness of the dielectric is at least 10 times the grain size. Using fine-grained powder materials with ultra-high dielectric constant, long cycle life, low dissipation factor, high insulation resistance and temperature stability to manufacture multi-layer ceramic capacitors (MLCC), can achieve smaller volume and larger capacity , higher precision and reliability. In addition, dielectric materials w...

Claims

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Application Information

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IPC IPC(8): C01G23/00
Inventor 刘秦
Owner 刘秦
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