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Improved sol-gel method for preparing nano-powder

A technology of nano-powder and gel method, which is applied in the field of nano-powder, submicron, and micron by sol-gel method, which can solve the problems that a large number of solvents cannot be recovered, unfavorable powder preparation, and long preparation cycle, etc., to achieve The effect of eliminating the step of adding water, uniform distribution of components, and simple and easy preparation process

Inactive Publication Date: 2005-05-25
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The technical problem to be solved in the present invention is to disclose a method for preparing nano-powders by an improved sol-gel method, so as to overcome the long preparation period in the prior art, the large amount of solvent used cannot be recovered, the preparation cost is high, and it is not conducive to a large amount of powder. defects in body preparation

Method used

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Embodiment 1

[0020] With 0.105mol strontium acetate Sr (CH 3 COO) 2 · 1 / 2 h 2 O (analytically pure), 0.195mol barium acetate Ba(CH 3 COO) 2 (analytically pure), 0.300mol n-butyl titanate Ti(n-C 4 h 9 O) 4 (chemically pure) as the starting compound, add 450ml of glacial acetic acid to prepare light yellow transparent sol A, after heating to 120°C, gel B will be formed rapidly within 2 minutes, change the distillation device, and collect about 200ml of fractions at 120°C , the residue is a semi-dried concentrated gel C, transferred to a watch glass, heat-treated in a horse-boiler furnace for 0.5 hours at 400°C, and then raised to 700°C, after 2.0 hours of calcination, it was taken out from the furnace, and a white powder was obtained after natural cooling Body Ba 0.65 Sr 0.35 TiO 3 Product 64.0 g, yield 98.9%. The mass of the target product is 64.0, accounting for 23.3% of the total mass of 259.4g of the input material. The traditional process of gel preparation is treated by a...

Embodiment 2

[0023] With 0.061mol lead acetate Pb(CH 3 COO) 2 ·3H 2 O (analytically pure), 0.058mol zirconium nitrate Zr (NO 3 ) 4 ·5H 2 O, 0.003mol n-butyl titanate Ti(n-C 4 h 9 O) 4 (chemically pure) is the starting compound, and 200ml of ethylene glycol monomethyl ether CH 3 OCH 2 CH 2 OH (chemically pure) solvent was prepared to obtain Sol A. After heating sol A to 125°C, gel B is rapidly formed within 2 minutes, refluxed for 10 minutes, and the distillation device is changed to collect solvent D at 120°C, the residue is concentrated gel E, which is transferred to a porcelain watch glass at 400°C Heat treatment in a horse boiling furnace for 0.5 hours, then heated to 750 ° C, and roasted for 2 hours to obtain a light yellow powder product PbZr 0.95 Ti 0.05 o 3 (PZT) 19.8 g, yield 94.3%.

[0024] PbZr x Ti 1-x o 3 The product is analyzed by XRD, which is the same as the standard pattern, and is a pure perovskite structure. TEM analysis shows that the particles are round...

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Abstract

A process for preparing the nano-powder by improved sol-gel method features that a temp variation method is used to quickly convert sol to gel, a distilling concentration method is used for recovering a great deal of solvent, and the concentrated gel is segmentally heated and calcined for shortening period. Its advantages are high purity of product, low cost and less pollution.

Description

technical field [0001] The invention relates to a preparation method of nanometer powder, in particular to a method for preparing micron, submicron and nanometer powder by using a sol-gel method. Background technique [0002] The sol-gel method is one of the commonly used methods for preparing micron, submicron and nanometer powders. This method has the advantages of accurate stoichiometry, easy addition of active ingredients, fine powder particles, good surface activity of particle materials, and low industrialization cost. Especially in the preparation of composite oxide nano-powder material has great advantages. [0003] The common preparation process of the sol-gel method includes steps such as sol, gel preparation, gel drying and grinding, and xerogel roasting. It is required that the content of metal alkoxide in the sol is greater than 0.3, and the gel drying method is adopted, either naturally air-dried or dried in an oven. The gel time can range from a few days to a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/462C04B35/622C04B35/624
Inventor 谢湘华董亚明林琳
Owner EAST CHINA UNIV OF SCI & TECH