CN102249669A - Preparation method of nanometer high-purity barium titanate - Google Patents
Preparation method of nanometer high-purity barium titanate Download PDFInfo
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- CN102249669A CN102249669A CN2010105310186A CN201010531018A CN102249669A CN 102249669 A CN102249669 A CN 102249669A CN 2010105310186 A CN2010105310186 A CN 2010105310186A CN 201010531018 A CN201010531018 A CN 201010531018A CN 102249669 A CN102249669 A CN 102249669A
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Abstract
The invention provides a preparation method of nanometer high-purity barium titanate, which comprises the following steps: mixing nanometer titanium tetrachloride, nanometer barium chloride, and oxalic acid according to a molar ratio of 1:1-1.15:2-2.3, reacting, washing and filtering the reaction precipitates, performing spin-drying and calcination, performing pulverization and nanometer grinding to prepare the nanometer high-purity barium titanate. The nanometer high-purity barium titanate prepared by the invention has high purity, good dispersibility, single morphology of powder particles, and reasonable granularity, and can be used as a dielectric of a laminated ceramic capacitor.
Description
Technical field
The present invention relates to a kind of preparation method of barium titanate, relate in particular to a kind of preparation method of nano high purity barium titanate.
Background technology
Barium titanate claims barium metatitanate again, and chemical formula is BaTiO
3, because of it has good ferroelectric, piezoelectricity, withstand voltage and insulating property are widely used in every field such as electronics, calorifics, acoustics and optics, are a kind of good electron pottery functional materialss.In recent years, the application of barium titanate is developed rapidly, and the application of high-quality barium titanate aspect semiconductive ceramic, PTC themistor and other sensors is increasingly extensive.
The main manufacture methods of barium carbonate has solid phase method and liquid method.In the solid phase method, barium titanate prepares by at high temperature making the mixture of barium titanate and titanium dioxide that substantial reaction take place with thermal treatment.The barium titanate particle diameter that adopts this method to make is big, and size distribution is wide, and particle shape is inhomogeneous, and needs higher relatively sintering temperature, can not be used to prepare have a heavy body comprise the multiwalled ceramic condenser.Liquid method comprises hydrothermal synthesis method, hydroxide process and sol-gel method, aspect crystallinity, size-grade distribution and the particle shape of powder more excellent character is being arranged all.Wherein hydro-thermal is synthetic is a kind of exemplary process in these methods, and suitable preparation has the multiwalled high capacity capacitor.
Among the patent CN01143432.5 " barium titanate powder and preparation method thereof ", it is characterized in that: will generate barytic barium compound by thermal degradation and mix with titanium dioxide, be 1X10 in total pressure preferably
3Calcine under the pressure of ambient gas below the Pa, obtain the high barium titanate powder of square crystallinity.Thereby realize that the micronize of agglomerating barium titanate powder is improved crystal formation simultaneously in order to obtain the dielectric medium in the laminated ceramic compacitor, make the temperature profile of electrostatic capacitance of laminated ceramic compacitor better.
Summary of the invention
The objective of the invention is, a kind of preparation method of nano high purity barium titanate is provided, with the better dielectric medium of obtained performance.
For achieving the above object, the preparation method of a kind of nano high purity barium titanate provided by the invention, it is characterized in that, this nano high purity barium titanate is by nanometer titanium tetrachloride, nanometer bariumchloride and oxalic acid in molar ratio 1: 1-1.15: 2-2.3 mixes, after the hybrid reaction,, calcine again after the drying throw out washing, the filtration of reaction, pulverize then with nano-milled, make the nano high purity barium titanate.
The preparation method of aforesaid a kind of nano high purity barium titanate the steps include:
1) the nanometer titanium tetrachloride is dissolved in the deionized water, is mixed with the solution of 1mol/L;
2) the nanometer bariumchloride is dissolved in the deionized water, is mixed with the solution of 1-1.15mol/L;
3) oxalic acid is dissolved in the deionized water, is mixed with the solution of 2-2.3mol/L;
4) isopyknic nanometer titanium tetrachloride solution, nanometer barium chloride solution and oxalic acid solution are put into reactor simultaneously, controlled temperature 50-60 ℃, form the titanium oxyoxalate precipitated barium, through washing, filtration, obtain the barium titanium oxalate solid after the drying again;
5) the barium titanium oxalate solid is put into high-temperature vacuum furnace, control vacuum tightness 10
-5-10
-3Pa, per hour 100 ℃ of heat-up rates of control are warming up to 800-1300 ℃, this temperature lower calcination 5-20 hour, take out and carry out comminution by gas stream and nano-milled, make the nano high purity barium titanate.
The invention has the advantages that, the nano high purity barium titanate purity height of this method preparation, good dispersity, the powder granule pattern is single, and reasonable particle size can be used as the dielectric medium of laminated ceramic compacitor.
Specific embodiment
Embodiment one:
1) the nanometer titanium tetrachloride is dissolved in the deionized water, is mixed with the solution of 1mol/L;
2) the nanometer bariumchloride is dissolved in the deionized water, is mixed with the solution of 1mol/L;
3) oxalic acid is dissolved in the deionized water, is mixed with the solution of 2mol/L;
4) isopyknic nanometer titanium tetrachloride solution, nanometer barium chloride solution and oxalic acid solution are put into reactor simultaneously, 60 ℃ of controlled temperature form the titanium oxyoxalate precipitated barium, through washing, filtration, obtain the barium titanium oxalate solid after the drying again.
5) the barium titanium oxalate solid is put into high-temperature vacuum furnace, control vacuum tightness 10
-5-10
-3Pa, per hour 100 ℃ of heat-up rates of control are warming up to 1000 ℃, this temperature lower calcination 10 hours, take out and carry out comminution by gas stream and nano-milled, make the nano high purity barium titanate, and particle diameter is 0.3-0.4um.
Embodiment two:
1) the nanometer titanium tetrachloride is dissolved in the deionized water, is mixed with the solution of 1mol/L;
2) the nanometer bariumchloride is dissolved in the deionized water, is mixed with the solution of 1.05mol/L;
3) oxalic acid is dissolved in the deionized water, is mixed with the solution of 2mol/L;
4) isopyknic nanometer titanium tetrachloride solution, nanometer barium chloride solution and oxalic acid solution are put into reactor simultaneously, 60 ℃ of controlled temperature form the titanium oxyoxalate precipitated barium, through washing, filtration, obtain the barium titanium oxalate solid after the drying again;
5) the barium titanium oxalate solid is put into high-temperature vacuum furnace, control vacuum tightness 10
-5-10
-3Pa, per hour 100 ℃ of heat-up rates of control are warming up to 1200 ℃, this temperature lower calcination 10 hours, take out and carry out comminution by gas stream and nano-milled, make the nano high purity barium titanate, and particle diameter is 0.2-0.3um.
Embodiment three:
1) the nanometer titanium tetrachloride is dissolved in the deionized water, is mixed with the solution of 1mol/L;
2) the nanometer bariumchloride is dissolved in the deionized water, is mixed with the solution of 1.15mol/L;
3) oxalic acid is dissolved in the deionized water, is mixed with the solution of 2.3mol/L;
4) isopyknic nanometer titanium tetrachloride solution, nanometer barium chloride solution and oxalic acid solution are put into reactor simultaneously, 50 ℃ of controlled temperature form the titanium oxyoxalate precipitated barium, through washing, filtration, obtain the barium titanium oxalate solid after the drying again;
5) the barium titanium oxalate solid is put into high-temperature vacuum furnace, control vacuum tightness 10
-5-10
-3Pa, per hour 100 ℃ of heat-up rates of control are warming up to 900 ℃, this temperature lower calcination 8 hours, take out and carry out comminution by gas stream and nano-milled, make the nano high purity barium titanate, and particle diameter is 0.5-0.6um.
Claims (2)
1. the preparation method of a nano high purity barium titanate, it is characterized in that: this nano high purity barium titanate is by nanometer titanium tetrachloride, nanometer bariumchloride and oxalic acid in molar ratio 1: 1-1.15: 2-2.3 mixes, after the hybrid reaction, throw out washing, filtration with reaction, calcine again after the drying, pulverize then with nano-milled, make the nano high purity barium titanate.
2. the preparation method of a kind of nano high purity barium titanate as claimed in claim 1 the steps include:
1) the nanometer titanium tetrachloride is dissolved in the deionized water, is mixed with the solution of 1mol/L;
2) the nanometer bariumchloride is dissolved in the deionized water, is mixed with the solution of 1-1.15mol/L;
3) oxalic acid is dissolved in the deionized water, is mixed with the solution of 2-2.3mol/L;
4) isopyknic nanometer titanium tetrachloride solution, nanometer barium chloride solution and oxalic acid solution are put into reactor simultaneously, controlled temperature 50-60 ℃, form the titanium oxyoxalate precipitated barium, through washing, filtration, obtain the barium titanium oxalate solid after the drying again;
5) the barium titanium oxalate solid is put into high-temperature vacuum furnace, control vacuum tightness 10
-5-10
-3Pa, per hour 100 ℃ of heat-up rates of control are warming up to 800-1300 ℃, this temperature lower calcination 5-20 hour, take out and carry out comminution by gas stream and nano-milled, make the nano high purity barium titanate.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102887705A (en) * | 2012-10-24 | 2013-01-23 | 浙江大学 | Preparation method of tetragonal-phase barium titanate (BaTiO3) hollow nanocrystal |
| CN102976400A (en) * | 2012-12-28 | 2013-03-20 | 湘潭大学 | Preparation method for tetragonal phase nano barium titanate |
| WO2015080303A1 (en) * | 2013-11-26 | 2015-06-04 | 삼성전기 주식회사 | Method for preparing barium titanyl oxalate and method for preparing barium titanate |
| CN104797543A (en) * | 2012-11-30 | 2015-07-22 | 三星电机株式会社 | Method for preparing barium titanate, and barium titanate prepared by same |
| CN116253564A (en) * | 2023-03-03 | 2023-06-13 | 重庆新申世纪新材料科技有限公司 | Preparation process of nanoscale tetragonal phase barium titanate powder |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1417162A (en) * | 2001-11-09 | 2003-05-14 | 刘胜绪 | Wet process of preparing high-purity barium titanate superfine powder as electronic functional material |
-
2010
- 2010-11-04 CN CN2010105310186A patent/CN102249669A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1417162A (en) * | 2001-11-09 | 2003-05-14 | 刘胜绪 | Wet process of preparing high-purity barium titanate superfine powder as electronic functional material |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102887705A (en) * | 2012-10-24 | 2013-01-23 | 浙江大学 | Preparation method of tetragonal-phase barium titanate (BaTiO3) hollow nanocrystal |
| CN102887705B (en) * | 2012-10-24 | 2013-12-25 | 浙江大学 | Preparation method of tetragonal-phase barium titanate (BaTiO3) hollow nanocrystal |
| CN104797543A (en) * | 2012-11-30 | 2015-07-22 | 三星电机株式会社 | Method for preparing barium titanate, and barium titanate prepared by same |
| CN102976400A (en) * | 2012-12-28 | 2013-03-20 | 湘潭大学 | Preparation method for tetragonal phase nano barium titanate |
| WO2015080303A1 (en) * | 2013-11-26 | 2015-06-04 | 삼성전기 주식회사 | Method for preparing barium titanyl oxalate and method for preparing barium titanate |
| CN116253564A (en) * | 2023-03-03 | 2023-06-13 | 重庆新申世纪新材料科技有限公司 | Preparation process of nanoscale tetragonal phase barium titanate powder |
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Application publication date: 20111123 |