CN100391893C - Synthesis of solvent heat method nano strontium titanate powder - Google Patents
Synthesis of solvent heat method nano strontium titanate powder Download PDFInfo
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- CN100391893C CN100391893C CNB2004100813499A CN200410081349A CN100391893C CN 100391893 C CN100391893 C CN 100391893C CN B2004100813499 A CNB2004100813499 A CN B2004100813499A CN 200410081349 A CN200410081349 A CN 200410081349A CN 100391893 C CN100391893 C CN 100391893C
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- suspension liquid
- strontium titanate
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Abstract
The present invention discloses a quick and compact and cheap preparation method of strontium titanate. Under normal pressure, metatitanic acid, soluble strontium salt, alkali and solvent are mixed, the obtained precipitation after reaction for a certain time is processed and dried, namely, the powder of high purity supper fine nanometer strontium titanate is obtained. The obtained powder of strontium titanate has the advantages of high purity, integral development of grain and fine granularity, and the requirement of the electronic ceramic field to the powder of strontium titanate can be satisfied. Compared with other paths, the present invention has the advantages of low price of raw materials, mild reaction condition, low requirement of the device, simple process and convenient operation, and has favorable economical and social benefits.
Description
Technical field
The present invention relates to a kind of method of solvent-thermal method one-step synthesis strontium titanate powder.Say that further relating under the normal pressure with the metatitanic acid is the method for raw material solvent-thermal method one-step synthesis strontium titanate powder.
Background of invention
Strontium titanate has semiconductive, the high withstand voltage of good dielectricity, excellence, and better temperature stability is widely used in the electronic ceramics industrial circle.Along with the develop rapidly of science and technology, electrode component has been proposed high precision, high reliability, multi-functional, microminiaturized requirement, preparing high-purity, superfine Sr titanate powder raw material is the key that reaches above-mentioned requirements.
Suitability for industrialized production strontium titanate method mainly is solid sintering technology and liquid-phase precipitation method at present.Though solid phase method technology is simple, cost is low, the powder purity that makes is low, and particle diameter is big, is difficult to satisfy the requirement of high-performance electronic components and parts.Though but liquid-phase precipitation method has overcome the shortcoming of solid phase method to a certain extent still needed high-temperature calcination, the big and powder of energy consumption is easy to grow up in calcining.Therefore developing preparation method high-purity, ultra-fine Sr titanate powder is subjected to scientific worker's extensive concern.Disclosed a kind of under alkaline condition, among the CN1472169 with TiCl
4For preparing the method for strontium titanate under raw material high temperature (220-270 ℃) high pressure (4-8MP) condition.Yet this method is not only used volatile TiCl
4, human body and environment are all caused an irregular injury, and adopt of the requirement raising of the condition of High Temperature High Pressure equipment.Disclosed among the CN1485276 a kind of in " supergravity reactor ", under the normal pressure alkaline condition, with TiCl
4Method for the feedstock production strontium titanate.Though this method does not adopt high-temperature high-pressure apparatus, still use volatile TiCl
4, human body and environment are had certain injury.Adopting pure oxygen base titanium among CN1039396 and the CN1239076 is the synthetic strontium titanate of raw material.Though wherein on raw material, have some to improve, but pure oxygen base titanium still has certain injury to human body, also pure oxygen base titanium cost an arm and a leg, be difficult to realize industrialization.It is the synthetic strontium titanate of raw material that CN1110598 discloses with water and titanium dioxide.This method has some improvement on raw material, but needs high-temperature calcination (750-1150 ℃), severe reaction conditions.Among above-mentioned several preparation method, there are some defectives at aspects such as raw materials cost, toxicity, reaction process about strontium titanate.Solvent-thermal method can change the thermodynamic property of system and the grain form in the hydrothermal solution system, moreover at present about being raw material with the metatitanic acid, the method for solvent-thermal method one-step synthesis strontium titanate yet there are no report under the normal pressure.
Summary of the invention
The present invention aims to provide a kind of reaction raw materials cheapness, and reaction conditions gentleness, equipment requirements are not high, and environment and human body are not had injury, the method for the synthetic strontium titanate that technology is simple and safe.
For achieving the above object, the method that adopts the normal pressure solvent-thermal method to prepare the strontium titanate nanometer powder according to the present invention may further comprise the steps:
(1) be 20-120 ℃ in temperature, with soluble strontium salt dissolving or be dispersed in the solvent, add alkali while stirring, used alkali is alkali-metal oxyhydroxide or ammoniacal liquor, and adjusting pH is 8-14, obtains suspension liquid A; In temperature is under 20-120 ℃, metatitanic acid is dispersed in forms suspension liquid B in the same solvent; Under violent stirring suspension liquid B is slowly splashed into suspension liquid A, B drips off up to suspension liquid; Perhaps under violent stirring suspension liquid A is slowly splashed into suspension liquid B, A drips off up to suspension liquid, continues then to stir.React under normal pressure, the reaction times is 1-10 hour.
(2) reaction obtains the strontium titanate nanometer powder with reaction solution cooling, washing, filtration, drying after finishing, and the used water of washing suspension liquid is that (specific conductivity is 0.8-1.0*10 to distilled water
-3S/cm); Acid is analytically pure hydrochloric acid or formic acid or acetic acid.
Chemical principle of the present invention:
H
2TiO
3+Sr
2++2HO
- 2→SrTiO
3+2H
2O
The ratio of metatitanic acid, strontium salt and solvent is 1.0 in above-mentioned reaction: 0.8-1.5: 10-200.Used solvent is an at least a mixture in a kind of or water and the above-mentioned finger fat alcohol in water or methyl alcohol, ethanol, propyl alcohol, Virahol, butanols, ethylene glycol, propylene glycol, these Fatty Alcohol(C12-C14 and C12-C18) of glycerol.Used soluble strontium salt is strontium chloride, strontium nitrate, strontium acetate, at least a in the water-soluble strontium salt of strontium bromide.Used alkali is alkali-metal oxyhydroxide or ammoniacal liquor.
The present invention compared with prior art has following advantage:
(1) is reflected under the normal pressure and carries out, do not need autoclave, reduce requirement equipment;
(2) one-step synthesis strontium titanate powder does not need high-temperature calcination, saves energy;
(3) reaction raw materials cheapness, process is simple, and the pure degree of synthetic Sr titanate powder is greater than 98%.
(4) reaction solvent is water or alcohol or alcohol-water mixture, can change the thermodynamic property of system and grain form even the state of aggregation in the hydrothermal solution system.
Description of drawings
Fig. 1 is the IR figure of Sr titanate powder
Fig. 2 is the XRD figure of Sr titanate powder
Embodiment
The present invention will be further described by the following examples.
Embodiment 1
The there-necked flask of 50ml is fixed on the heat collecting type constant temperature blender with magnetic force, prolong, thermometer, constant pressure funnel are housed on there-necked flask.Under the normal pressure, in the time of 60 ℃ 0.08mol strontium chloride and 25ml ethanol are put into mixing stirring in the there-necked flask, ammoniacal liquor is regulated pH to 8, obtain suspension liquid A, the 0.1mol metatitanic acid in the making beating of 15ml ethanol, is obtained suspension liquid B, B is injected constant pressure funnel, slowly splash into suspension liquid A, oil bath heating magnetic agitation.Clock reaction 4h.
After reaction finishes,, handle, obtain product reacting liquid filtering.Titanium strontium ratio through the chemical analysis product is 1.12.The XRD analysis product is a cube phase.According to the Scherrer formula, the primary particle median size that calculates strontium titanate is 15nm.
Embodiment 2
The there-necked flask of 50ml is fixed on the heat collecting type constant temperature blender with magnetic force, prolong, thermometer, constant pressure funnel are housed on there-necked flask.Under the normal pressure, in the time of 90 ℃ 0.1mol strontium chloride and 15ml distilled water are put into mixing stirring in the there-necked flask, potassium hydroxide is regulated pH to 10, obtains suspension liquid A; The 0.1mol metatitanic acid in the making beating of 15ml water, is obtained suspension liquid B; B is injected constant pressure funnel, slowly splash into suspension liquid A, oil bath heating magnetic agitation.Clock reaction 1h.
After reaction finishes,, handle, obtain product reacting liquid filtering.Titanium strontium ratio through the chemical analysis product is 1.03.The XRD analysis product is a cube phase.According to the Scherrer formula, the primary particle median size that calculates strontium titanate is 22nm.
Embodiment 3
The there-necked flask of 100ml is fixed on the heat collecting type constant temperature blender with magnetic force, prolong, thermometer, constant pressure funnel are housed on there-necked flask.Under the normal pressure, in the time of 80 ℃ 0.1mol metatitanic acid and 40ml propyl alcohol put in the there-necked flask and pull an oar, obtain suspension liquid A; 0.12mol strontium nitrate and 15ml distilled water are mixed stirring, and sodium hydroxide is regulated pH to 10, obtains suspension liquid B.B is injected constant pressure funnel, slowly splash into suspension liquid A, oil bath heating magnetic agitation.Clock reaction 6h.
After reaction finishes,, handle obtaining product with reacting liquid filtering.Titanium strontium ratio through the chemical analysis product is 0.98.The XRD analysis product is a cube phase.According to the Scherrer formula, the primary particle median size that calculates strontium titanate is 12nm.
Embodiment 4
The there-necked flask of 100ml is fixed on the heat collecting type constant temperature blender with magnetic force, prolong, thermometer, constant pressure funnel are housed on there-necked flask.Under the normal pressure, in the time of 80 ℃ 0.1mol metatitanic acid and 40ml propyl alcohol put in the there-necked flask and pull an oar, obtain suspension liquid A; 0.12mol strontium chloride and 15ml propyl alcohol are mixed stirring, and sodium hydroxide is regulated pH to 10, obtains suspension liquid B.B is injected constant pressure funnel, slowly splash into suspension liquid A, oil bath heating magnetic agitation.Clock reaction 8h.
After reaction finishes,, handle obtaining product with reacting liquid filtering.Titanium strontium ratio through the chemical analysis product is 0.93.The XRD analysis product is a cube phase.According to the Scherrer formula, the primary particle median size that calculates strontium titanate is 10nm.
Embodiment 5
The there-necked flask of 100ml is fixed on the heat collecting type constant temperature blender with magnetic force, prolong, thermometer, constant pressure funnel are housed on there-necked flask.Under the normal pressure, in the time of 115 ℃ 0.1mol metatitanic acid and 40ml butanols put in the there-necked flask and pull an oar, obtain suspension liquid A; 0.15mol strontium acetate and 35ml butanols are mixed stirring, and sodium hydroxide is regulated pH to 12, obtains suspension liquid B.B is injected constant pressure funnel, slowly splash into suspension liquid A, oil bath heating magnetic agitation.Clock reaction 10h.
After reaction finishes,, handle obtaining product with reacting liquid filtering.Titanium strontium ratio through the chemical analysis product is 0.85.The XRD analysis product is a cube phase.According to the Scherrer formula, the primary particle median size that calculates strontium titanate is 8nm.
Claims (5)
1. one kind prepares method high-purity, the nano strontium titanate powder, it is characterized in that may further comprise the steps:
(1) be 20-120 ℃ in temperature, with soluble strontium salt dissolving or be dispersed in the solvent, add alkali while stirring, adjusting pH is 8-14, obtains suspension liquid A; In temperature is under 20-120 ℃, metatitanic acid is dispersed in forms suspension liquid B in the same solvent; Under violent stirring suspension liquid B is slowly splashed into suspension liquid A, B drips off up to suspension liquid; Perhaps under violent stirring suspension liquid A is slowly splashed into suspension liquid B, A drips off up to suspension liquid, continues then to stir, and reacts under normal pressure, and the reaction times is 1-10 hour;
(2) reaction obtains the strontium titanate nanometer powder with reaction solution cooling, washing, filtration, drying after finishing.
2. by the described method of claim 1, it is characterized in that: used solvent is an at least a mixture in a kind of or water and the above-mentioned Fatty Alcohol(C12-C14 and C12-C18) in water or methyl alcohol, ethanol, propyl alcohol, Virahol, butanols, ethylene glycol, propylene glycol, these Fatty Alcohol(C12-C14 and C12-C18) of glycerol.
3. by the described method of claim 1, it is characterized in that: used soluble strontium salt is strontium chloride, strontium nitrate, strontium acetate, at least a in the water-soluble strontium salt of strontium bromide.
4. by the described method of claim 1, it is characterized in that: the ratio of used metatitanic acid, strontium salt and solvent is 1.0: 0.8-1.5: 10-200.
5. by the described method of claim 1, it is characterized in that: used alkali is alkali-metal oxyhydroxide or ammoniacal liquor.
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|---|---|---|---|---|
| CN101723441B (en) * | 2008-10-22 | 2012-03-07 | 湖南人文科技学院 | Method for preparing strontium titanate superfine powder |
| CN111204798B (en) * | 2020-03-05 | 2022-03-25 | 福州大学 | High-sensitivity two-dimensional nano strontium titanate gas-sensitive material with low working temperature and preparation method and application thereof |
| CN113797910B (en) * | 2020-06-16 | 2023-06-16 | 中国科学院化学研究所 | Defect-containing nano microspherical perovskite catalyst and preparation method and application thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS4866600A (en) * | 1971-12-17 | 1973-09-12 | ||
| CN1171369A (en) * | 1997-06-26 | 1998-01-28 | 中国科学院固体物理研究所 | Process for preparing nm-class bismuth titanate and its sosoloid |
| CN1082491C (en) * | 1998-06-12 | 2002-04-10 | 中国科学院青海盐湖研究所 | Process for preparing nm-class strontium titanate |
| CN1472169A (en) * | 2003-06-30 | 2004-02-04 | 山东省国腾功能陶瓷材料有限公司 | Technology for preparing high-purity nanometer strontium titanate powder |
| CN1485276A (en) * | 2002-09-24 | 2004-03-31 | �Ϻ���ͨ��ѧ | method for preparation of Sr titanate powder |
-
2004
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS4866600A (en) * | 1971-12-17 | 1973-09-12 | ||
| CN1171369A (en) * | 1997-06-26 | 1998-01-28 | 中国科学院固体物理研究所 | Process for preparing nm-class bismuth titanate and its sosoloid |
| CN1082491C (en) * | 1998-06-12 | 2002-04-10 | 中国科学院青海盐湖研究所 | Process for preparing nm-class strontium titanate |
| CN1485276A (en) * | 2002-09-24 | 2004-03-31 | �Ϻ���ͨ��ѧ | method for preparation of Sr titanate powder |
| CN1472169A (en) * | 2003-06-30 | 2004-02-04 | 山东省国腾功能陶瓷材料有限公司 | Technology for preparing high-purity nanometer strontium titanate powder |
Non-Patent Citations (2)
| Title |
|---|
| 水热法制备表面修饰的钛酸锶纳米微粉. 徐存英，张鹏翔，洪品杰.化学物理学报，第13卷第2期. 2004 |
| 水热法制备表面修饰的钛酸锶纳米微粉. 徐存英，张鹏翔，洪品杰.化学物理学报，第13卷第2期. 2004 * |
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