Process for preparing nano barium titanate and doped solid solution by low temperature solid state reaction

A solid-state reaction, barium titanate technology, applied in self-solid, chemical instruments and methods, crystal growth, etc., can solve the problem of uneven chemical composition distribution of barium titanate powder, easy agglomeration of barium titanate powder, and uneven particle size distribution Uniformity and other issues, to achieve high theoretical and practical value, avoid hard agglomeration, and short reaction time

Inactive Publication Date: 2008-01-16
HEBEI UNIVERSITY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the chemical composition distribution of the barium titanate powder obtained by the solid-state method is uneven; the barium titanate powder formed at high temperature is easy to agglomerate, the particles are relatively coarse (generally > 1m), and the particle size distribution is uneven; it is easy to introduce Impurities, low product purity
Therefore, it cannot meet the requirements of small size and high performance of modern electronic components.

Method used

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  • Process for preparing nano barium titanate and doped solid solution by low temperature solid state reaction
  • Process for preparing nano barium titanate and doped solid solution by low temperature solid state reaction
  • Process for preparing nano barium titanate and doped solid solution by low temperature solid state reaction

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Experimental program
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Effect test

Embodiment 1

[0032] Embodiment 1: Preparation of pure nano barium titanate solid solution

[0033] 1. Formation of metatitanic acid

[0034] 11ml (0.1mol) of TiCl 4 Drop into 100-200ml of deionized water, then adjust the pH to 6-8 with ammonia water, make a slurry, filter under reduced pressure, wash the chloride ions, and then drain to obtain a filter cake that is metatitanic acid (H 2 TiO 3 or TiO 2 ·H 2 O).

[0035] 2. Grinding and drying

[0036] Filter cake according to effective content and solid Ba(OH) 2 ·8H 2 O is mixed at a molar ratio of 1:1, fully ground at room temperature for 30-60 minutes, and then directly dried at 100°C to obtain BaTiO with an average particle size of 50-70nm and a cubic phase. 3 Powder, as shown in Figure 1 and Figure 2. The room temperature dielectric constant of the barium titanate ceramics prepared by the invention can reach more than 4000. However, barium titanate obtained by high-temperature sintering in the prior art has a dielectric constant...

Embodiment 2

[0037] Embodiment 2: to BaTiO 3 (ABO 3 ) solid solution for A-site doping to synthesize Ba 1-x m x TiO 3

[0038] Doped with strontium (Ba 0.9 Sr 0.1 TiO 3 ) as an example: TiCl 4 Hydrolysis process is the same as embodiment 1, and the filter cake that washes off chloride ion is according to effective content and fresh solid Ba(OH) 2 ·8H 2 O and Sr(OH) 2 ·8H 2 O was mixed at a molar ratio of 1:0.9:0.1, fully ground at room temperature for 30-60 minutes, then moved into a crucible, and dried at 120°C to obtain cubic phase Ba with an average particle size of 30-50 nm. 0.9 Sr 0.1 TiO 3 Powder. in Ba 1-x m x TiO 3 In the system, the value of X is between 0, 0.03, 0.05, 0.08, ... until 1.0, and X can take a value continuously or intermittently.

[0039] The pottery test proves that after the method of the present invention is used to dope an appropriate amount of strontium in the barium titanate, the dielectric constant of the material at room temperature can reac...

Embodiment 3

[0040] Example 3. To BaTiO 3 Synthesis of BaTi with B-site Doping in Solid Solution 0.9 N 0.1 o 3

[0041] Doped with tin (BaTi 0.9 sn 0.1 o 3 ) as an example: 9.9mlTiCl 4 , 3.5058g SnCl 4 ·5H 2 After the joint hydrolysis of O, ammonia water was added to make a slurry, the pH was adjusted to 6-8, and the chlorine ions were washed by vacuum filtration, and then the filter cake was mixed with fresh solid Ba(OH) according to the effective content. 2 ·8H 2 O was mixed at a molar ratio of 1:1, fully ground at room temperature for 30-60 minutes, and then placed in an oven at 120°C for direct drying. Nano-BaTi can be prepared 0.9 sn 0.1 o 3 Solid solution powder. BaTi 1-x N x o 3 The value of x in it is: 0.01, 0.02, 0.03, ..., 0.1, 0.15, 0.2, 0.25, 0.3. X can take values ​​continuously or intermittently.

[0042] The pottery test proves that after the method of the present invention is used to add a proper amount of tin to the barium titanate, the dielectric consta...

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Abstract

The invention discloses a nanometer barium titanate preparing method through low-temperature solid-state reaction, which comprises the following steps: A. hydrolyzing TiCl4 at 6-8 pH value to produce H2TiO3 filter cake; B. blending filter cake and Ba(OH)2 .8H2O; grinding under indoor temperature for 30-60 min completely; drying directly at 80-120 deg.c to produce BaTiO3 powder. The preparing method of nanometer barium titanate doping solid solution, which is characterized by the following: doping to synthesize at A and B position of barium titanate; selecting Sr, Ca, Zn and Cu for A position doping material; selecting Zr, Sn, Si and Ce for B position doping material. The method avoids hard birdnesting phenomenon, which improves the dielectric property for doping modified barium titanate solid solution.

Description

technical field [0001] The invention relates to a method for preparing nano barium titanate and a solid solution by a low-temperature solid-state reaction, and belongs to the technical field of chemical synthesis and refining. Background technique [0002] BaTiO 3 As an excellent ferroelectric material, it has an unusually high dielectric constant. In addition to being the basic masterbatch of electronic components such as monolithic ceramic capacitors, laminated ceramic electric heaters, and PTCR thermistors, it is also widely used in dielectric amplifiers, frequency modulation, and storage devices, and has gradually become the most used in the field of electronic ceramics. One of the most widely used materials, known as "the pillar of the electronic ceramic industry". [0003] There are various synthesis methods of nano-barium titanate, among which solid-phase method and liquid-phase method are widely used. The traditional solid phase method refers to the oxides (TiO 2...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C30B29/32C30B29/60C30B1/10C01G23/00
Inventor 丁士文柴佳冯春燕孙会谦刘静培李萧
Owner HEBEI UNIVERSITY
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