CN100462332C - Method for preparing nano strontium titanate by lactic acid adjuvant process - Google Patents
Method for preparing nano strontium titanate by lactic acid adjuvant process Download PDFInfo
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- CN100462332C CN100462332C CNB2007100184325A CN200710018432A CN100462332C CN 100462332 C CN100462332 C CN 100462332C CN B2007100184325 A CNB2007100184325 A CN B2007100184325A CN 200710018432 A CN200710018432 A CN 200710018432A CN 100462332 C CN100462332 C CN 100462332C
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Abstract
The invention relates to a preparation method of nanometer strontium titanate with lactic acid aid. The invention takes strontium salt and butyl titanate as materials, lactic acid as solvent and inhibitor, and takes a small amount of water to promote hydrolyzing. The procedures of the invention are as follows: Firstly, strontium titanate is dissolved in the lactic acid, and then is added with the solvent of the butyl titanate slowly with violent stirring, and is kept still, thus homogeneous and transparent gel is obtained. The gel is calcineed at a high temperature, thus nanometer strontium titanate power is obtained. The composition components of the invention are less, can be got easily and are environment friendly without pollution. The lactic acid acts as the solvent of the strontium salt and as the inhibitor of the butyl titanate, and can well control the sol-gel process; therefore, the productive rate of the nanometer strontium titanate power prepared by the method is increased. The invention needs only 80 ml of gel for to make 0.1 mol of SrTiO3r. The proposal has a wide application and is suitable for the preparations of nanometer barium titanate and nanometer barium strontium titanate, etc.
Description
Technical field
The present invention relates to a kind of preparation method of nano strontium titanate powder.Specifically be to be the colloidal sol-gel process for preparing of solvent and inhibitor with lactic acid.
Background technology
Strontium titanate (SrTiO
3) have a typical A BO
3Uhligite (ABO
3) structure, be a kind of important electron ceramic material, have high specific inductivity, low dielectric loss, advantage such as temperature stability is good.Be widely used in fields such as high voltage capacitor, grain-boundary layer capacitor, voltage-sensitive ceramic, thermal sensing element.Prospect is boundless.At present, also more and more stricter along with the raising of electron trade to the requirement of strontium titanate powder characteristic to meticulous functional material performance requriements, require the fine size of Sr titanate powder, evenly, purity is high, component is controlled etc.The research of nano strontium titanate material is very active, and many researchists successfully prepare nano strontium titanate powder or film in the laboratory with wet chemistry method, and has carried out the work of relevant doping vario-property aspect.But the ubiquity problem is that wet chemical method synthetic productive rate is low, pollutes greatly, and cost is high.
The preparation technology of Sr titanate powder is the emphasis that the scientific research personnel studies always.The method for preparing nano strontium titanate mainly contains gas phase synthesis method, hydrothermal method, and sol-gel processing etc., the principal feature of sol-gel processing is to make multicomponent mixture system starting material thorough mixing in the molecular level scope.The preparation process temperature is low, and firing temperature is than low 400～500 ℃ approximately of traditional methods, because the part formation before burning till of required resultant.Chinese patent, 1239076, " preparation method of nano strontium titanate " announces that on December 22nd, 1999 this patent has adopted strontium acetate-butyl (tetra) titanate-Virahol system, utilizes sol-gel processing to prepare the processing method of nano strontium titanate.The report strontium acetate is dissolved in the deionized water in this patent, but does not have report how to solve the little problem of solubleness, and bigger as the dispersant dosage of butyl (tetra) titanate with Virahol, this patent prepares 0.1mol and needs the 800ml dispersion agent.In the China YouSe Acta Metallurgica Sinicas in 2005 " sol-gel processing prepares the perovskite typed nano strontium titanate " (author Zhang Wenkui etc.) civilian play-by-play prepare the technology of nano strontium titanate with strontium nitrate-butyl (tetra) titanate-dehydrated alcohol-Glacial acetic acid system, and studied the some factors that influence gelation process.But its preparation process still need add a large amount of acetic acid and ethanol, and this can be in follow-up drying and heat treatment process discharges a large amount of irritating smells, and experimental situation is caused certain pollution, and influences experimental installation work-ing life.According to document report preparation 0.1mol SrTiO
3Need about 700ml colloidal sol.And the strontium nitrate raw material has the danger of burning and blast, and can produce NO, NO in follow-up sintering
2Deng obnoxious flavour.
The external relevant method for preparing strontium titanate seldom, the processing method of utilizing sol-gel processing to prepare nano strontium titanate does not also have at present.
Summary of the invention
The objective of the invention is to overcome above-mentioned prior art deficiency, a kind of method with preparing nano strontium titanate by lactic acid adjuvant process is provided, this method reaction raw materials easily obtains, and reaction conditions is easily controlled, and conversion unit is simple.
Technical scheme of the present invention is achieved in that and may further comprise the steps:
1) strontium salt is dissolved in the lactic acid solution, lactic acid and strontium salt mol ratio are 6～12:1, add deionized water while stirring, and the strontium salt of 1mol needs the deionized water of 100ml～300ml, 60 ℃～90 ℃ down heating, be stirred well to transparent, solution A;
2) under 200～350 rev/mins rotating speed stirs, butyl (tetra) titanate is slowly joined in the solution A, butyl (tetra) titanate and strontium salt mol ratio are 1:1, add afterwards restir 30～50 minutes, leave standstill the colloidal sol of transparent homogeneous;
3) add nitric acid and ammoniacal liquor and regulate colloidal sol pH=4～5;
4) colloidal sol leaves standstill aging 23h～25h and gets the transparent gel of homogeneous under 50 ℃～70 ℃;
5) gel dry 10h～12h in 120 ℃～140 ℃ vacuum gets xerogel;
6) xerogel after will wearing out places retort furnace 600 ℃～800 ℃ temperature ranges, and calcining 1h～3h can obtain the nano strontium titanate powder.
Strontium salt is Strontium carbonate powder in the described raw material, strontium lactate, any in strontium acetate or the strontium nitrate.
In the described raw material, Strontium carbonate powder is partly replaced with barium carbonate, can prepare Ba
xSr
1-xTiO
3(0≤x≤1) nano-powder.
The present invention adopts the sol-gel processing synthesis technique, selected suitable inhibitor, controlled the hydrolysis of butyl (tetra) titanate well, reduced the consumption of dispersion agents such as dehydrated alcohol, and abandon pungency solvents such as acetate, improve the productive rate that sol-gel processing prepares the nano strontium titanate powder, also improved experimental situation simultaneously greatly.After tested, the nano strontium titanate powder of the present invention's preparation belongs to perovskite structure, and degree of crystallinity is good, and diameter of particle is in 30nm～80nm scope.The characteristics of maximum of the present invention are, reaction raw materials is simple, and reaction conditions more easily obtains, and experimentation is environmentally friendly, the nano strontium titanate productive rate height of preparation.The present invention prepares 0.1mol SrTiO
3Only need 80ml colloidal sol.
The present invention has the following advantages:
(1) reaction is synthetic at normal temperatures and pressures, and reaction conditions more easily obtains.
(2) reaction raw materials is simple, and need not to add ethanol, acetate equal solvent, has reduced production cost.
(3) reaction as the solvent of strontium salt and the inhibitor of butyl (tetra) titanate, has obtained good result with lactic acid. the present invention prepares 0.1mol SrTiO
3Only need 80ml colloidal sol.
Description of drawings
Fig. 1 is the X ray diffracting spectrum of the strontium titanate powder crossed of treatment of different temperature of the present invention;
Fig. 2 is SrTiO
3Powder is at 700 ℃ of transmission electron microscope photos after 2h thermal treatment;
Below in conjunction with accompanying drawing content of the present invention is described in further detail.
Embodiment
With reference to shown in Figure 1, when heat treated temperature is 500 ℃, has in the diffraction spectra part SrCO is only arranged
3Diffraction peak exists, and shows SrCO
3Do not decompose fully as yet.Simultaneously, SrTiO
3Diffraction three strongest ones peak is apparent in view, and this shows SrTiO under this temperature
3Structure begins to generate.After thermal treatment temp surpasses 600 ℃, SrCO
3Diffraction peak weakens gradually, disappears substantially when temperature is higher than 700 ℃, and this shows SrCO
3Decompose fully.While SrTiO
3Diffraction peak intensity constantly strengthen along with temperature raises, the peak width at half height of diffraction peak narrows down, and shows SrTiO
3Crystallinity improve, the pairing diffraction angle of three strongest ones' line is: 32.54,46.60,57.90.The crystal indices are respectively (110), (200), (211), this and standard SrTiO
3The X diffracting spectrum is very identical.In view of the above, we can think that gel is synthetic after the powder after 600 ℃ of thermal treatment is pure SrTiO
3Composition.
With reference to shown in Figure 2, the strontium titanate gel is after 700 ℃ of thermal treatment, and ultra-sonic dispersion in dehydrated alcohol is done TEM (transmission electron microscope) analysis.Particle among the figure is similar to ball-type, and grain diameter branch broad, part grain diameter are about 30nm～50nm, and most of particle diameter is about 50nm～80nm.
Embodiment 1
The Strontium carbonate powder that takes by weighing 0.1mol is dissolved in the 0.8mol lactic acid, adds the deionized water of 10ml, and 80 ℃ are stirred 3h to homogeneous transparent on magnetic force constant temperature stirrer, get solution A.Take by weighing the 0.1mol butyl (tetra) titanate then, slowly be added drop-wise in the solution A, and, mixed the back and continued to stir the colloidal sol that can obtain homogeneous transparent in 30 minutes with 200 rev/mins of stirrings of rotating speed.Add nitric acid and ammoniacal liquor and regulate colloidal sol pH=5.Colloidal sol in baking oven 50 ℃ place the gel that 23h just can obtain homogeneous transparent.Gel gets xerogel at 120 ℃ of vacuum-drying 11h, and xerogel is ground, and grinds after 600 ℃ of thermal treatment then and can obtain the strontium titanate nano-powder.
Embodiment 2
The Strontium carbonate powder that takes by weighing 0.15mol is dissolved in the 1.2mol lactic acid, adds the deionized water of 30ml, and 90 ℃ are stirred 3h to homogeneous transparent on magnetic force constant temperature stirrer, get solution A.Take by weighing the 0.15mol butyl (tetra) titanate then, slowly be added drop-wise in the solution A, and, mixed the back and continued to stir the colloidal sol that can obtain homogeneous transparent in 45 minutes with 250 rev/mins of stirrings of rotating speed.Add nitric acid and ammoniacal liquor and regulate colloidal sol pH=4.Colloidal sol in baking oven 70 ℃ place the gel that 24h just can obtain homogeneous transparent.Gel gets xerogel at 130 ℃ of vacuum-drying 10h, and xerogel is ground, and grinds after 700 ℃ of thermal treatment then and can obtain the strontium titanate nano-powder.
Embodiment 3
The Strontium carbonate powder that takes by weighing 0.2mol is dissolved in the 1.4mol lactic acid, adds the deionized water of 50ml, and 70 ℃ are stirred 3h to homogeneous transparent on magnetic force constant temperature stirrer, get solution A.Take by weighing the 0.2mol butyl (tetra) titanate then, slowly be added drop-wise in the solution A, and, mixed the back and continued to stir the colloidal sol that can obtain homogeneous transparent in 30 minutes with 300 rev/mins of stirrings of rotating speed.Add nitric acid and ammoniacal liquor and regulate colloidal sol pH=4.Colloidal sol in baking oven 60 ℃ place the gel that 23h just can obtain homogeneous transparent.Gel gets xerogel at 120 ℃ of vacuum-drying 11h, and xerogel is ground, and grinds after 600 ℃ of thermal treatment then and can obtain the strontium titanate nano-powder.
Embodiment 4
The Strontium carbonate powder that takes by weighing 0.3mol is dissolved in the 3mol lactic acid, adds the deionized water of 70ml, and 60 ℃ are stirred 3h to homogeneous transparent on magnetic force constant temperature stirrer, get solution A.Take by weighing the 0.3mol butyl (tetra) titanate then, slowly be added drop-wise in the solution A, and, mixed the back and continued to stir the colloidal sol that can obtain homogeneous transparent in 50 minutes with 350 rev/mins of stirrings of rotating speed.Add nitric acid and ammoniacal liquor and regulate colloidal sol pH=5.Colloidal sol in baking oven 60 ℃ place the gel that 25h just can obtain homogeneous transparent.Gel gets xerogel at 120 ℃ of vacuum-drying 12h, and xerogel is ground, and grinds after 800 ℃ of thermal treatment then and can obtain the strontium titanate nano-powder.
Embodiment 5
The strontium lactate that takes by weighing 0.1mol is dissolved in the 0.8mol lactic acid, adds the deionized water of 10ml, and 80 ℃ are stirred 3h to homogeneous transparent on magnetic force constant temperature stirrer, get solution A.Take by weighing the 0.1mol butyl (tetra) titanate then, slowly be added drop-wise in the solution A, and, mixed the back and continued to stir the colloidal sol that can obtain homogeneous transparent in 30 minutes with 200 rev/mins of stirrings of rotating speed.Add nitric acid and ammoniacal liquor and regulate colloidal sol pH=5.Colloidal sol in baking oven 65 ℃ place the gel that 24h just can obtain homogeneous transparent.Gel gets xerogel at 120 ℃ of vacuum-drying 11h, and xerogel is ground, and grinds after 500 ℃ of thermal treatment then and can obtain the strontium titanate nano-powder.
Embodiment 6
The strontium lactate that takes by weighing 0.2mol is dissolved in the 1.4mol lactic acid, adds the deionized water of 50ml, and 70 ℃ are stirred 3h to homogeneous transparent on magnetic force constant temperature stirrer, get solution A.Take by weighing the 0.2mol butyl (tetra) titanate then, slowly be added drop-wise in the solution A, and, mixed the back and continued to stir the colloidal sol that can obtain homogeneous transparent in 40 minutes with 250 rev/mins of stirrings of rotating speed.Add nitric acid and ammoniacal liquor and regulate colloidal sol pH=4.Colloidal sol in baking oven 60 ℃ place the gel that 23h just can obtain homogeneous transparent.Gel gets xerogel at 130 ℃ of vacuum-drying 11h, and xerogel is ground, and grinds after 600 ℃ of thermal treatment then and can obtain the strontium titanate nano-powder.
Embodiment 7
The strontium lactate that takes by weighing 0.3mol is dissolved in the 3mol lactic acid, adds the deionized water of 70ml, and 90 ℃ are stirred 3h to homogeneous transparent on magnetic force constant temperature stirrer, get solution A.Take by weighing the 0.3mol butyl (tetra) titanate then, slowly be added drop-wise in the solution A, and, mixed the back and continued to stir the colloidal sol that can obtain homogeneous transparent in 45 minutes with 300 rev/mins of stirrings of rotating speed.Add nitric acid and ammoniacal liquor and regulate colloidal sol pH=5.Colloidal sol in baking oven 70 ℃ place the gel that 25h just can obtain homogeneous transparent.Gel gets xerogel at 130 ℃ of vacuum-drying 12h, and xerogel is ground, and grinds after 700 ℃ of thermal treatment then and can obtain the strontium titanate nano-powder.
Embodiment 8
The strontium lactate that takes by weighing 0.5mol is dissolved in the 4mol lactic acid, adds the deionized water of 75ml, and 90 ℃ are stirred 3h to homogeneous transparent on magnetic force constant temperature stirrer, get solution A.Take by weighing the 0.5mol butyl (tetra) titanate then, slowly be added drop-wise in the solution A, and, mixed the back and continued to stir the colloidal sol that can obtain homogeneous transparent in 45 minutes with 350 rev/mins of stirrings of rotating speed.Add nitric acid and ammoniacal liquor and regulate colloidal sol pH=5.Colloidal sol in baking oven 70 ℃ place the gel that 25h just can obtain homogeneous transparent.Gel gets xerogel at 140 ℃ of vacuum-drying 12h, and xerogel is ground, and grinds after 800 ℃ of thermal treatment then and can obtain the strontium titanate nano-powder.
Embodiment 9
The strontium acetate that takes by weighing 0.1mol is dissolved in the 0.6mol lactic acid, adds the deionized water of 15ml, and 70 ℃ are stirred 3h to homogeneous transparent on magnetic force constant temperature stirrer, get solution A.Take by weighing the 0.1mol butyl (tetra) titanate then, slowly be added drop-wise in the solution A, and, mixed the back and continued to stir the colloidal sol that can obtain homogeneous transparent in 40 minutes with 200 rev/mins of stirrings of rotating speed.Add nitric acid and ammoniacal liquor and regulate colloidal sol pH=5.Colloidal sol in baking oven 60 ℃ place the gel that 24h just can obtain homogeneous transparent.Gel gets xerogel at 120 ℃ of vacuum-drying 10h, and xerogel is ground, and grinds after 700 ℃ of thermal treatment then and can obtain the strontium titanate nano-powder.
Embodiment 10
The strontium acetate that takes by weighing 0.2mol is dissolved in the 1.4mol lactic acid, adds the deionized water of 50ml, and 70 ℃ are stirred 3h to homogeneous transparent on magnetic force constant temperature stirrer, get solution A.Take by weighing the 0.2mol butyl (tetra) titanate then, slowly be added drop-wise in the solution A, and, mixed the back and continued to stir the colloidal sol that can obtain homogeneous transparent in 40 minutes with 300 rev/mins of stirrings of rotating speed.Add nitric acid and ammoniacal liquor and regulate colloidal sol pH=4.Colloidal sol in baking oven 60 ℃ place the gel that 23h just can obtain homogeneous transparent.Gel gets xerogel at 130 ℃ of vacuum-drying 11h, and xerogel is ground, and grinds after 600 ℃ of thermal treatment then and can obtain the strontium titanate nano-powder.
Embodiment 11
The strontium acetate that takes by weighing 0.3mol is dissolved in the 3mol lactic acid, adds the deionized water of 70ml, and 90 ℃ are stirred 3h to homogeneous transparent on magnetic force constant temperature stirrer, get solution A.Take by weighing the 0.3mol butyl (tetra) titanate then, slowly be added drop-wise in the solution A, and, mixed the back and continued to stir the colloidal sol that can obtain homogeneous transparent in 45 minutes with 300 rev/mins of stirrings of rotating speed.Add nitric acid and ammoniacal liquor and regulate colloidal sol pH=5.Colloidal sol in baking oven 70 ℃ place the gel that 25h just can obtain homogeneous transparent.Gel gets xerogel at 130 ℃ of vacuum-drying 12h, and xerogel is ground, and grinds after 700 ℃ of thermal treatment then and can obtain the strontium titanate nano-powder.
Embodiment 12
The strontium lactate that takes by weighing 0.4mol is dissolved in the 3.5mol lactic acid, adds the deionized water of 75ml, and 90 ℃ are stirred 3h to homogeneous transparent on magnetic force constant temperature stirrer, get solution A.Take by weighing the 0.4mol butyl (tetra) titanate then, slowly be added drop-wise in the solution A, and, mixed the back and continued to stir the colloidal sol that can obtain homogeneous transparent in 45 minutes with 350 rev/mins of stirrings of rotating speed.Add nitric acid and ammoniacal liquor and regulate colloidal sol pH=5.Colloidal sol in baking oven 70 ℃ place the gel that 25h just can obtain homogeneous transparent.Gel gets xerogel at 140 ℃ of vacuum-drying 12h, and xerogel is ground, and grinds after 800 ℃ of thermal treatment then and can obtain the strontium titanate nano-powder.
Embodiment 13
The strontium nitrate that takes by weighing 0.1mol is dissolved in the 1mol lactic acid, adds the deionized water of 20ml, and 60 ℃ are stirred 3h to homogeneous transparent on magnetic force constant temperature stirrer, get solution A.Take by weighing the 0.1mol butyl (tetra) titanate then, slowly be added drop-wise in the solution A, and, mixed the back and continued to stir the colloidal sol that can obtain homogeneous transparent in 35 minutes with 200 rev/mins of stirrings of rotating speed.Add nitric acid and ammoniacal liquor and regulate colloidal sol pH=5.Colloidal sol in baking oven 50 ℃ place the gel that 23h just can obtain homogeneous transparent.Gel gets xerogel at 140 ℃ of vacuum-drying 12h, and xerogel is ground, and grinds after 800 ℃ of thermal treatment then and can obtain the strontium titanate nano-powder.
Embodiment 14
The strontium nitrate that takes by weighing 0.2mol is dissolved in the 1.4mol lactic acid, adds the deionized water of 50ml, and 70 ℃ are stirred 3h to homogeneous transparent on magnetic force constant temperature stirrer, get solution A.Take by weighing the 0.2mol butyl (tetra) titanate then, slowly be added drop-wise in the solution A, and, mixed the back and continued to stir the colloidal sol that can obtain homogeneous transparent in 40 minutes with 250 rev/mins of stirrings of rotating speed.Add nitric acid and ammoniacal liquor and regulate colloidal sol pH=4.Colloidal sol in baking oven 60 ℃ place the gel that 23h just can obtain homogeneous transparent.Gel gets xerogel at 130 ℃ of vacuum-drying 11h, and xerogel is ground, and grinds after 600 ℃ of thermal treatment then and can obtain the strontium titanate nano-powder.
Embodiment 15
The strontium nitrate that takes by weighing 0.4mol is dissolved in the 3.5mol lactic acid, adds the deionized water of 75ml, and 90 ℃ are stirred 3h to homogeneous transparent on magnetic force constant temperature stirrer, get solution A.Take by weighing the 0.4mol butyl (tetra) titanate then, slowly be added drop-wise in the solution A, and, mixed the back and continued to stir the colloidal sol that can obtain homogeneous transparent in 45 minutes with 300 rev/mins of stirrings of rotating speed.Add nitric acid and ammoniacal liquor and regulate colloidal sol pH=5.Colloidal sol in baking oven 65 ℃ place the gel that 24h just can obtain homogeneous transparent.Gel gets xerogel at 140 ℃ of vacuum-drying 12h, and xerogel is ground, and grinds after 700 ℃ of thermal treatment then and can obtain the strontium titanate nano-powder.
Embodiment 16
The strontium nitrate that takes by weighing 0.5mol is dissolved in the 4mol lactic acid, adds the deionized water of 75ml, and 90 ℃ are stirred 3h to homogeneous transparent on magnetic force constant temperature stirrer, get solution A.Take by weighing the 0.5mol butyl (tetra) titanate then, slowly be added drop-wise in the solution A, and, mixed the back and continued to stir the colloidal sol that can obtain homogeneous transparent in 50 minutes with 350 rev/mins of stirrings of rotating speed.Add nitric acid and ammoniacal liquor and regulate colloidal sol pH=5.Colloidal sol in baking oven 70 ℃ place the gel that 25h just can obtain homogeneous transparent.Gel gets xerogel at 140 ℃ of vacuum-drying 12h, and xerogel is ground, and grinds after 800 ℃ of thermal treatment then and can obtain the strontium titanate nano-powder.
Embodiment 17
The barium carbonate that takes by weighing 0.1mol is dissolved in the 0.8mol lactic acid, adds the deionized water of 15ml, and 80 ℃ are stirred 3h to homogeneous transparent on magnetic force constant temperature stirrer, get solution A.Take by weighing the 0.1mol butyl (tetra) titanate then, slowly be added drop-wise in the solution A, and, mixed the back and continued to stir the colloidal sol that can obtain homogeneous transparent in 30 minutes with 200 rev/mins of stirrings of rotating speed.Add nitric acid and ammoniacal liquor and regulate colloidal sol pH=5.Colloidal sol in baking oven 60 ℃ place the gel that 23h just can obtain homogeneous transparent.Gel gets xerogel at 120 ℃ of vacuum-drying 10h, and xerogel is ground, and grinds after 700 ℃ of thermal treatment then and can obtain Barium Titanate nano-powder.
Embodiment 18
The barium carbonate that takes by weighing 0.15mol is dissolved in the 1.2mol lactic acid, adds the deionized water of 30ml, and 90 ℃ are stirred 3h to homogeneous transparent on magnetic force constant temperature stirrer, get solution A.Take by weighing the 0.15mol butyl (tetra) titanate then, slowly be added drop-wise in the solution A, and, mixed the back and continued to stir the colloidal sol that can obtain homogeneous transparent in 45 minutes with 250 rev/mins of stirrings of rotating speed.Add nitric acid and ammoniacal liquor and regulate colloidal sol pH=4.Colloidal sol in baking oven 70 ℃ place the gel that 24h just can obtain homogeneous transparent.Gel gets xerogel at 130 ℃ of vacuum-drying 10h, and xerogel is ground, and grinds after 800 ℃ of thermal treatment then and can obtain the strontium titanate nano-powder.
Embodiment 19
The barium carbonate that takes by weighing 0.2mol is dissolved in the 1.4mol lactic acid, adds the deionized water of 50ml, and 70 ℃ are stirred 3h to homogeneous transparent on magnetic force constant temperature stirrer, get solution A.Take by weighing the 0.2mol butyl (tetra) titanate then, slowly be added drop-wise in the solution A, and, mixed the back and continued to stir the colloidal sol that can obtain homogeneous transparent in 40 minutes with 300 rev/mins of stirrings of rotating speed.Add nitric acid and ammoniacal liquor and regulate colloidal sol pH=4.Colloidal sol in baking oven 60 ℃ place the gel that 23h just can obtain homogeneous transparent.Gel gets xerogel at 130 ℃ of vacuum-drying 11h, and xerogel is ground, and grinds after 600 ℃ of thermal treatment then and can obtain the strontium titanate nano-powder.
The barium carbonate that takes by weighing 0.4mol is dissolved in the 3.5mol lactic acid, adds the deionized water of 75ml, and 90 ℃ are stirred 3h to homogeneous transparent on magnetic force constant temperature stirrer, get solution A.Take by weighing the 0.4mol butyl (tetra) titanate then, slowly be added drop-wise in the solution A, and, mixed the back and continued to stir the colloidal sol that can obtain homogeneous transparent in 50 minutes with 350 rev/mins of stirrings of rotating speed.Add nitric acid and ammoniacal liquor and regulate colloidal sol pH=5.Colloidal sol in baking oven 70 ℃ place the gel that 25h just can obtain homogeneous transparent.Gel gets xerogel at 140 ℃ of vacuum-drying 12h, and xerogel is ground, and grinds after 800 ℃ of thermal treatment then and can obtain the strontium titanate nano-powder.
Claims (2)
1. the method with preparing nano strontium titanate by lactic acid adjuvant process is characterized in that, may further comprise the steps:
1) strontium salt is dissolved in the lactic acid solution, lactic acid and strontium salt mol ratio are 6～12:1, add deionized water while stirring, and the strontium salt of 1mol needs the deionized water of 100ml～300ml, 60 ℃～90 ℃ down heating, be stirred well to transparent, solution A;
2) under 200～350 rev/mins rotating speed stirs, butyl (tetra) titanate is slowly joined in the solution A, butyl (tetra) titanate and strontium salt mol ratio are 1:1, add afterwards restir 30～50 minutes, leave standstill the colloidal sol of transparent homogeneous;
3) add nitric acid and ammoniacal liquor and regulate colloidal sol pH=4～5;
4) colloidal sol leaves standstill aging 23h～25h and gets the transparent gel of homogeneous under 50 ℃～70 ℃;
5) gel dry 10h～12h in 120 ℃～140 ℃ vacuum gets xerogel;
6) the xerogel grinding is placed on retort furnace,, the xerogel after the calcining is ground, obtain the nano strontium titanate powder at 600 ℃～800 ℃ temperature ranges calcining 1h～3h.
2. the method with preparing nano strontium titanate by lactic acid adjuvant process according to claim 1 is characterized in that strontium salt is Strontium carbonate powder in the described raw material, strontium lactate, any in strontium acetate or the strontium nitrate.
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| CN102898147A (en) * | 2012-11-05 | 2013-01-30 | 西华师范大学 | Environment-coordinating method for preparing titanate piezoelectric ceramic powder |
| WO2018084959A2 (en) * | 2016-09-30 | 2018-05-11 | Nelson Deanna J | Pharmaceutical quality strontium l-lactate |
| CN107033708A (en) * | 2017-04-25 | 2017-08-11 | 安徽博硕科技有限公司 | A kind of preparation method of attapulgite/nano strontium titanate/nano tin dioxide photocatalysis silicon-acrylic coatings |
| CN113697852B (en) * | 2021-08-26 | 2023-03-14 | 陕西君普新航科技有限公司 | Preparation method of coralline semiconductive strontium titanate powder |
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|---|---|---|---|---|
| CN1239076A (en) * | 1998-06-12 | 1999-12-22 | 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 |
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2007
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1239076A (en) * | 1998-06-12 | 1999-12-22 | 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 |
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