CN101045554A - Method for preparing uniform dispersion square phase barium titanate nanocrystal - Google Patents
Method for preparing uniform dispersion square phase barium titanate nanocrystal Download PDFInfo
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- CN101045554A CN101045554A CN 200710013368 CN200710013368A CN101045554A CN 101045554 A CN101045554 A CN 101045554A CN 200710013368 CN200710013368 CN 200710013368 CN 200710013368 A CN200710013368 A CN 200710013368A CN 101045554 A CN101045554 A CN 101045554A
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- barium titanate
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- square phase
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- phase barium
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Abstract
A process for preparing the uniformly dispersed square barium sodium titanate nanocrystals by hydrothermal synthesis method includes using inorganic alkali or the combination of organ alkali and inorganic alkali to regulate the pH value of reaction system, respectively preparing the homogeneous solutions of the reactant precursors (TiO2 or tetrabutyl titanate and barium hydroxide) at 80-100 deg.C, and two-stage hydrothermal reaction in high-pressure reactor at 100-200 deg.C while crystallizing.
Description
Technical field
The present invention relates to the preparation of titanate, relate in particular to the hydro-thermal synthetic preparation method of uniform dispersion square phase barium titanate nano material.
Background technology
Barium titanate (BaTiO
3) be a kind of strong dielectric and ferroelectric material of excellent performance, be the special ferroelectric ceramic(s) of found the earliest a kind of performance, still be widely used in making thermistor (PTCR), laminated ceramic capacitor (MLC), electro-optical device etc. so far.It is one of most widely used material of electronic ceramic fields.The development of microelectronics communication has in recent years caused the laminated ceramic capacitor must be microminiaturized to adapt with it, reach the target of electronic ceramics element high precision, microminiaturization and high reliability, that the high quality powder that need prepare single-size is is high-purity, be uniformly dispersed, do not have reunion, superfine four directions phase BaTiO
3The electronic ceramics powder (＜300nm).German Patent 2433279, Japanese Patent 49-69399 and Chinese patent 90109424.2 have proposed liquid phase method respectively and have prepared titanate.Promptly in the aqueous solution of titanium ion that contains mol ratios such as having an appointment and barium ion, add excessive H
2O
2With the aqueous solution of alkali, generate compound superoxide precipitation, will precipitate thermal degradation then and promptly obtain BaTiO
3Product.In above-mentioned patent documentation, what have only relates to the Ba/Ti mol ratio of preparing intermediate product (compound superoxide), and what have relates to a cube phase BaTiO
3The preparation of super-fine powder; Still do not relate to cubic phase BaTiO
3The preparation of super-fine powder does not more have cubic phase BaTiO
3The report that all disperses the nano powder preparation method.Thereby, limited BaTiO to a certain extent
3In industrial application.
Summary of the invention
At the deficiencies in the prior art, the invention provides a kind of method of preparing uniform dispersion square phase barium titanate nanocrystal, to satisfy the needs of making the high quality microdevice on the current electronic industry.
Summary of the invention
The present invention adopts hydro-thermal reaction, pH value technology and control reactant concn by the conditioned reaction system, under proper reaction conditions, make be reflected under the pressurized conditions smooth, realized the separation of nucleation and growth, guaranteed the dispersiveness of product, productive rate reaches more than 90%, and cubic phase content is more than 70%.
Technical scheme of the present invention is, to 10-14, is solvent with the deionized water, with the pH value of alkali conditioned reaction system under hydrothermal condition, with Ba (OH)
28H
2O is the barium source, titanium dioxide (TiO
2) or tetrabutyl titanate (Ti (O
iBu)
4) be the titanium source, a step makes high-purity high-load cubic phase BaTiO
3After reaction is finished, use NH
4The Cl aqueous solution, deionized water, absolute ethanol washing 40 ℃ of down dry a few hours, can obtain product for several times.
Detailed Description Of The Invention
A kind of method of preparing uniform dispersion square phase barium titanate nanocrystal, concrete steps are as follows:
1, under heated and stirred, the titanium source is joined in the reactor, add deionized water dissolving, regulate the pH value to 10-14 with alkali.
2, heating for dissolving Ba (OH)
28H
2O, Ba/Ti=1-2 adds in the aforesaid reaction vessel in molar ratio, heated and stirred 1-3 hour, temperature 80-100 ℃, guarantees that precursor dissolves the formation homogeneous phase solution fully.
Above-mentioned steps 1 and 2 order are not limit.
3, autoclave compactedness 70-80%, sealing autoclave is also put into 100-200 ℃ baking oven and is reacted, and reacts 24-74 hour.
4, take out reactor, filter, solids is neutral to filtrate with ammonium chloride solution, deionized water wash successively for several times, and 40-50 ℃ of oven dry promptly obtains BaTiO
3Powder, productive rate is about 92%.
Alkali in the above-mentioned steps 1 is the mineral alkali combination, also can be the combination of organic and inorganic alkali.
Preferably, above-mentioned organic bases is selected from thanomin, quadrol or polyoxamide.
Preferably, above-mentioned mineral alkali is selected from NaOH or ammoniacal liquor.
Preferably, the titanium source TiO in the above-mentioned steps 1
2Or Ti (O
iBu)
4After the dissolving, Ti (O wherein
iBu)
4Concentration is 0.2-0.5 (volumetric concentration), is preferably between the 0.3-0.4 TiO
2Concentration is 1.0-2.0M, is preferably between the 1.2-1.6M.
Preferably, the Ba (OH) in the above-mentioned steps 2
28H
2O dissolving back concentration is 1.0-4.0M, is preferably between the 2.0-3.5M.
Preferably, the reaction in the above-mentioned steps 3 is a two-stage reaction, reacts 20-26 hour and 28-48 hour at 100 ℃ and 200 ℃ respectively.
Preferably, above-mentioned two-stage reaction, 100 ℃ is hydro-thermal reaction, optimum reacting time 24 hours, 200 ℃ is the hydrothermal crystallizing reaction, optimum reacting time is 48 hours.
Preferably, above-mentioned steps 4 products earlier with 40-50 ℃ hot wash 1-2 time, use ammonium chloride solution, deionized water wash again.
The present invention is to preparing cubic phase BaTiO
3Influence factor test, concrete data declaration is as follows.
Table 1 reaction conditions is to preparation BaTiO
3Influence
| Numbering | n(Ba 2+)∶ n(Ti 4+) | The pH regulator agent | Temperature/℃ | Time/h | Product thing phase |
| 1 | 1.2∶1 | Ammoniacal liquor | 200 | 24 | Anatase octahedrite TiO 211% rutile TiO 2 4％ BaTiO 3 85％ |
| 2 | 1.2∶1 | Ammoniacal liquor | 200 | 24 | Anatase octahedrite TiO 251% rutile TiO 2 15％ BaTiO 3 34％ |
| 3 | 2.0∶1 | Ammoniacal liquor | 200 | 24 | Anatase octahedrite TiO 23% rutile TiO 2 2％ BaTiO 3 85％ |
| 4 | 2.0∶1 | Ammoniacal liquor | 200 | 48 | Four directions phase BaTiO 3 |
| 5 | 2.0∶1 | Ammoniacal liquor | 180 | 72 | Four directions phase BaTiO 3 Ba/Ti＝1.0001 |
| 6 | 2.0∶1 | Ammoniacal liquor NaOH | 200 | 48 | Four directions phase BaTiO 3 Ba/Ti＝0.9995 |
| 7 | 2.0∶1 | Ammoniacal liquor | 150 | 4 days | Four directions phase BaTiO 3Impurity |
| 8 | 2.0∶1 | Hydrated barta | 200 | 48 | Four directions phase BaTiO 3Impurity |
| 9 | 1.6∶1 | Ammoniacal liquor NaOH | 180 | 48 | Four directions phase BaTiO 3 |
Data in the table 1 show:
(1) selection of pH regulator agent influences phase composite of product thing and purity, adopts the combination regulation system pH value gained result of ammoniacal liquor and other alkali more satisfactory.
(2) thing of temperature of reaction and time effects product mutually and purity, comparatively ideal hydrothermal crystallizing condition is 200 ℃, 48-72 hour.
(3) precursor concentration not only influences the thing phase and the purity of product, and has influence on the size and dispersiveness of product.Our experimental result shows: higher precursor concentration has guaranteed the degree of supersaturation that reaction system is higher, and this is the prerequisite of " explosive type nucleation ".Our two sections temperature growing technologies provide advantageous environment for quick nucleation, fast after the nucleation, according to the Lamer growth model of monodisperse particles, after the nucleation, concentration drops to below the minimum concentration rapidly, nucleation no longer then, just growth (after the nucleation, nucleus is evenly grown fast), on the other hand, away from the formed electrostatic double layer of operation under the pH value under the iso-electric point, also can effectively suppress the reunion of nanoparticle.Thereby the equal dispersiveness that has caused product.
Table 2 is BaTiO of the present invention
3The chemical constitution of product
| BaO | TiO 2 | Phase | Ba/Ti | |
| Product content of the present invention (%) | 65.62 | 34.18 | The four directions | 1.0001 |
| CN90109424.2 document product content (%) | 65.62 | 34.18 | Cube | 1.0001 |
| Japan's KYORI company's product content (%) | 65.63 | 34.19 | Cube | 1.0002 |
The cubic phase BaTiO that the present invention obtains
3Product is compared with the product of reporting, has reached high-purity level, especially can obtain equal dispersive four directions phase BaTiO
3Nano-powder.
Technical characterstic of the present invention has been to adopt the method for two sections thermotonus technology and unique regulation system pH value.In addition, method of the present invention adopts higher concentration and the suitable reaction temperature of feeding intake to make reaction to take place in the mode of " explosive type nucleation ", has realized that the nucleation and growth of barium titanate separates, and is beneficial to the generation of uniform dispersion square phase barium titanate; And, can effectively suppress the reunion of nanoparticle away from the formed electrostatic double layer of operation under the pH value of iso-electric point, guaranteed the dispersiveness of product.Operation is simple for the inventive method, and product yield and quality are all higher, and productive rate reaches more than 90%, and cubic phase content has favorable industrial application prospect more than 70%.
Description of drawings
Fig. 1 is cubic phase BaTiO
3The X-ray diffraction spectrogram that all disperses nano-powder.
Fig. 2 is the cubic phase BaTiO of the inventive method preparation
3The transmission electron microscope photo of product.
Embodiment
The present invention will be further described below in conjunction with embodiment, but be not limited thereto.
Embodiment 1:
Take by weighing Ba (OH)
28H
2O 30.9047g adds the 60ml deionized water in the 100ml beaker, change over to after the heating for dissolving in the 160ml stainless steel cauldron.Take by weighing TiO
26.5208g in the 50ml beaker, pour in the reactor.Add each 10ml of water and ammoniacal liquor again, 80 ℃ of Heating temperatures, stirring is dissolved it fully, autoclave compactedness 75%, seal pot is also put in the baking oven, reacts 24 and 48 hours at 100 ℃ and 200 ℃ respectively.Take out reactor, filtration, product 1molL
-1Ammonium chloride solution, deionized water wash to filtrate are neutral, and 45 ℃ of oven dry 14h obtain BaTiO
3White powder.
Embodiment 2:
Pipette 97.16ml tetra-n-butyl titanate (Ti (O
iBu)
4) in 500ml stainless steel cauldron lining; Add 35ml ammoniacal liquor.Take by weighing Ba (OH)
28H
2O 108.1612g adds the deionized water 119ml of heat in 2 100ml plastic beakers, after heating for dissolving is complete, pour the reactor lining into.The envelope still stirs, and reacts 24 and 48 hours at 100 ℃ and 200 ℃ respectively.Product is used 1molL with hot water (50 ℃) washing 2 times
-1Ammonium chloride solution 800ml, deionized water wash to filtrate are neutral, and 45 ℃ of oven dry 14h obtain BaTiO
3Powder.
Embodiment 3:
Take by weighing TiO
222.8228g in the 50ml beaker, pour 500ml stainless steel cauldron lining into, add 35ml ammoniacal liquor; Take by weighing NaOH 1.4000g in the 100ml plastic beaker, use the 13ml deionized water dissolving, pour the reactor lining into; Take by weighing Ba (OH)
28H
2O 180.2686g adds the 50ml hot deionized water respectively in 3 100ml beakers, heating is dissolving fully, pours the reactor lining into after cold slightly, pours in the still with 5ml deionized water wash beaker respectively again.Stirred 2 minutes the envelope still with glass stick.Reacted 26 and 46 hours at 100 ℃ and 200 ℃ respectively.Product is used 1molL with hot water (50 ℃) washing 2 times
-1Ammonium chloride solution, deionized water wash to filtrate are neutral, and 45 ℃ of oven dry 14h obtain BaTiO
3Powder.
According to the X-ray diffraction spectrogram, division has taken place in the diffraction peak between the 40-50 degree (seeing the illustration among Fig. 1), illustrates that product is cubic phase BaTiO
3Simultaneously, can calculate cubic phase content according to diffracted intensity and be about 70%.Rein in formula calculating according to thanking, the product grain-size approximately is 56 nanometers.Transmission electron microscope photo (Fig. 2) illustrates that the product particle diameter is about the 60-80 nanometer, and is approaching with XRD result.
Claims (10)
1. the method for a preparing uniform dispersion square phase barium titanate nanocrystal, step is as follows:
(1) under heated and stirred, the titanium source is joined in the reactor, add deionized water dissolving, regulate the pH value to 10-14 with alkali;
(2) heating for dissolving Ba (OH)
28H
2O, Ba/Ti=1-2 adds in the aforesaid reaction vessel in molar ratio, and heated and stirred 1-3 hour, temperature 80-100 ℃, precursor dissolved the formation homogeneous phase solution fully;
The order of above-mentioned steps (1) and (2) is not limit;
(3) autoclave compactedness 70-80%, sealing autoclave is also put into 100-200 ℃ baking oven and is reacted, and reacts 24-74 hour;
(4) take out reactor, filter, solids is neutral to filtrate with ammonium chloride solution, deionized water wash successively for several times, and 40-50 ℃ of oven dry promptly obtains BaTiO
3Powder.
2. the method for preparing uniform dispersion square phase barium titanate nanocrystal as claimed in claim 1 is characterized in that, the alkali in the described step (1) is the mineral alkali combination, or the combination of organic and inorganic alkali.
3. the method for preparing uniform dispersion square phase barium titanate nanocrystal as claimed in claim 2 is characterized in that, described organic bases is selected from thanomin, quadrol or polyoxamide.
4. the method for preparing uniform dispersion square phase barium titanate nanocrystal as claimed in claim 2 is characterized in that, described mineral alkali is selected from NaOH or ammoniacal liquor.
5. the method for preparing uniform dispersion square phase barium titanate nanocrystal as claimed in claim 1 is characterized in that, the titanium source TiO in the described step (1)
2Or Ti (O
iBu)
4After the dissolving, Ti (O wherein
iBu)
4Volumetric concentration is 0.2-0.5, TiO
2Concentration is 1.0-2.0M.
6. as the method for claim 1 or 5 described preparing uniform dispersion square phase barium titanate nanocrystals, it is characterized in that the titanium source TiO in the described step (1)
2Or Ti (O
iBu)
4After the dissolving, Ti (O wherein
iBu)
4Volumetric concentration is 0.3-0.4, TiO
2Concentration is between the 1.2-1.6M.
7. the method for preparing uniform dispersion square phase barium titanate nanocrystal as claimed in claim 1 is characterized in that, the Ba (OH) in the described step (2)
28H
2O dissolving back concentration is 1.0-4.0M.
8. as the method for claim 1 or 6 described preparing uniform dispersion square phase barium titanate nanocrystals, it is characterized in that the Ba (OH) in the described step (2)
28H
2O dissolving back concentration is 2.0-3.5M.
9. the method for preparing uniform dispersion square phase barium titanate nanocrystal as claimed in claim 1 is characterized in that, the reaction in the described step (3) is a two-stage reaction, reacts 20-26 hour and 28-48 hour at 100 ℃ and 200 ℃ respectively.
10. the method for preparing uniform dispersion square phase barium titanate nanocrystal as claimed in claim 9 is characterized in that, described two-stage reaction, 100 ℃ is hydro-thermal reaction, optimum reacting time 24 hours, 200 ℃ is the hydrothermal crystallizing reaction, optimum reacting time is 48 hours.
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