Preparation method for tetragonal phase nano barium titanate

A technology of barium titanate and tetragonal phase, which is applied in the field of preparation of tetragonal phase nano barium titanate, can solve the problems of complex process, cumbersome operation, large particle size, etc., achieve simple and easy process, avoid particle growth, and average particle size small diameter effect

Inactive Publication Date: 2013-03-20
XIANGTAN UNIV
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  • Abstract
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  • Application Information

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Problems solved by technology

[0005] Chinese patent CN1323759 discloses a preparation method of nano-scale tetragonal phase barium titanate powder, but the preparation method is a hydrothermal method, which requires high temperature and high pressure reaction conditions, which requires too high equipment, and the process is complicated and difficult to achieve continuous production
[0006] Chinese patent CN101746814A discloses a production process for preparing tetragonal phase barium titanate, but the preparation method is a hydrothermal method, which requires too much equipment, the process is complicated, and the produced product particles are relatively large, so it is impossible to produce titanium smaller than 100nm Barium Oxide Powder
[0007] Chinese patent CN102060325A discloses a preparation method of a tetragonal barium titanate nanorod array, but the obtained product is not a tetragonal barium titanate powder, and requires two-step hydrothermal reaction, the reaction conditions are complex, and the operation is cumbersome
[0008] Chinese patent CN102584215A

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  • Preparation method for tetragonal phase nano barium titanate
  • Preparation method for tetragonal phase nano barium titanate
  • Preparation method for tetragonal phase nano barium titanate

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[0043] Example 1

[0044] Weigh BaCl accurately respectively 2 ·2H 2 O27.48g, H 2 C 2 O 4 ·2H 2 O30.88g, Ti(OC 4 H 9 ) 4 39.2ml, prepare barium chloride and oxalic acid into an aqueous solution, dissolve butyl titanate in an appropriate amount of ethanol solution, then add the butyl titanate alcohol solution to the oxalic acid solution, stir to form a transparent light yellow solution, adjust the pH range with ammonia 2.5-3.0, ultrasonic vibration for 10 minutes, the total amount of solution is 2.0L. Use spiral channel type rotating bed supergravity reactor to generate supergravity field and supergravity field level, that is, control the rotation speed of supergravity reactor rotor at 700 rpm, react and circulate in the supergravity field, and drop into the supergravity field reactor Add BaCl 2 ·2H 2 O solution, the liquid volume is 0.5L, the reaction produces a white precipitate. The resulting precipitation suspension was allowed to stand in a water bath at 80°C for 2 hours and...

Example Embodiment

[0045] Example 2

[0046] Weigh BaCl accurately respectively 2 ·2H 2 O27.48g, H 2 C 2 O 4 ·2H 2 O30.88g, Ti(OC 4 H 9 ) 4 39.2ml, prepare barium chloride and oxalic acid into an aqueous solution, dissolve butyl titanate in an appropriate amount of ethanol solution, then add the butyl titanate alcohol solution to the oxalic acid solution, stir to form a transparent light yellow solution, adjust the pH range with ammonia 2.5-3.0, ultrasonic vibration for 10 minutes, the total amount of solution is 2.0L. Use spiral channel type rotating bed supergravity reactor to generate supergravity field and supergravity field level, that is, control the rotation speed of supergravity reactor rotor at 800 rpm, react and circulate in the supergravity field, and drop into the supergravity field reactor Add BaCl 2 ·2H 2 O solution, the liquid volume is 0.5L, the reaction produces a white precipitate. The resulting precipitation suspension was allowed to stand in a water bath at 80°C for 2 hours and...

Example Embodiment

[0047] Example 3

[0048] Weigh BaCl accurately respectively 2 ·2H 2 O142.8g, H 2 C 2 O 4 ·2H 2 O162g, Ti(OC 4 H 9 ) 4 200ml, prepare barium chloride and oxalic acid into an aqueous solution, dissolve butyl titanate in an appropriate amount of ethanol solution, then add the butyl titanate alcohol solution to the oxalic acid solution, stir to form a transparent light yellow solution, adjust the pH range with ammonia 2.5-3.0, ultrasonic vibration for 10min, the total amount of solution is 2.0L. Use the spiral channel type rotating bed supergravity reactor to generate the supergravity field. The supergravity field level is to control the rotation speed of the supergravity reactor rotor at 800 rpm, and react and circulate in the supergravity field to the supergravity field reactor. Add BaCl dropwise 2 ·2H 2 O solution, the liquid volume is 0.5L, the reaction produces a white precipitate. The resulting precipitation suspension was allowed to stand in a water bath at 80°C for 2 hours ...

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Abstract

The invention provides a preparation method for tetragonal phase nano barium titanate. The preparation method comprises the steps as follows: i), preparing water solutions of barium chloride and oxalic acid respectively, and mixing alcoholic solution of butyl titanate and oxalic acid solution uniformly to obtain titanium oxyoxalate complex ion solution; ii), adding titanium oxyoxalate complex ion solution obtained in the step i) into a supergravity reactor as a circulating flowing phase to control the supergravity level; and meanwhile, dropping barium chloride solution to obtain white barium titanyl oxalate precipitation suspension as a precursor of barium titanate, and keeping the pH value of the whole system at 2.5-3.5 during reaction; and iii),ageing the precipitation suspension obtained in the step ii), leaching, washing and drying to obtain white barium titanyl oxalate power. The preparation method provided by the invention has the advantages that tetragonal phase nano barium titanate can be prepared; and the particle size of the prepared power can be controlled to be within the range of 30-90 nm; the average particle size is small, and the particle size is narrow in distribution; and the degree of crystallinity is high, and the crystal formation is intact.

Description

technical field [0001] The invention relates to the field of inorganic nanometer materials, in particular to a preparation method of tetragonal nano barium titanate. Background technique [0002] In recent years, nanomaterials have become a research hotspot in current materials science due to their unique interface effects. Among them, barium titanate is a typical ferroelectric and dielectric material in the manufacture of nonlinear components such as dielectric amplifiers, ceramics Electronic components such as capacitors and ferroelectric devices have a wide range of important applications. The development of barium titanate powder began in the 1940s. At present, my country has introduced a number of multilayer ceramic capacitor (MLCC) production lines, and its dielectric material is mainly barium titanate. Since the thickness of each layer of a multilayer ceramic capacitor has reached about 3 μm, and each layer requires more than 5 layers of effective grain boundary laye...

Claims

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Application Information

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IPC IPC(8): C01G23/00B82Y30/00
Inventor 周继承廖晶晶黄新武
Owner XIANGTAN UNIV
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