CN101311376A - Method for preparing strontium titanate nanometer powder of one-dimensional structure - Google Patents
Method for preparing strontium titanate nanometer powder of one-dimensional structure Download PDFInfo
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- CN101311376A CN101311376A CNA2008100598838A CN200810059883A CN101311376A CN 101311376 A CN101311376 A CN 101311376A CN A2008100598838 A CNA2008100598838 A CN A2008100598838A CN 200810059883 A CN200810059883 A CN 200810059883A CN 101311376 A CN101311376 A CN 101311376A
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Abstract
The invention discloses a method for preparing strontium titanate nanometer powder with one-dimension structure, which consists of procedures of preparing the oxyhydroxide precipitate of titanium and the deionized aqueous solution of barium acetate as reaction materials, adding a feasible quantity of potassium hydroxide to promote crystallization, and appending a suitable viscosity of patterned vertical alignment polymer surfactant to control the feature; under the temperature of 100-150 DEG C, strontium titanate nanowire and a branched crystal structure are obtained after a hydrothermal reaction. The craftwork of the invention is simple; the micro feature of the product is easy to control, the pollution is free; the cost is low; a large-scale production is suitable. The quality of the crystallization of the prepared product is stable; the specific surface is big. A broad application prospect is possessed in fields of micro electronic devices, EO devices, storage devices, oxygen sensors, photocatalyst, and solar battery, etc.
Description
Technical field
The present invention relates to a kind of preparation method of strontium titanate nanometer powder of one-dimensional structure, belong to field of inorganic nonmetallic material.
Background technology
Owing to exist quantum size effect, nano material to have the physicochemical property more excellent than block materials, its preparation also is the focus of Materials science concern in recent years and research.Simultaneously, the same performance that is determining material of the microscopic appearance of material with size, for example, nanotube, nano wire, nanometer rod and nano belt with one-dimentional structure have shown performances such as excellent electricity, optics and magnetics, and more and more researchers has concentrated on attention in the control of material microscopic appearance.
Strontium titanate is a kind of important ABO
3The type perovskite oxide because it has high-k, high voltage withstanding property and temperature stability, is widely used in the electronic ceramics industrial circle.By stress induced or doping, strontium titanate can also have ferroelectricity.In addition, strontium titanate also has good semiconduction, has similar energy gap (3.2eV) with titanium dioxide, in recent years, has caused extensive studies interest in fields such as photochemical catalysis, electrode of solar battery, oxygen sensor, luminous and storages.The strontium titanate nano material of one-dimentional structure is expected to improve the performance of related fields owing to having big length-to-diameter ratio and specific surface area, high chemically reactive.
The traditional preparation method of Sr titanate powder is a solid reaction process, though this method technology is simple, the product purity of preparation is low.Owing to there is the high-temperature calcination process, particle agglomeration is very serious, and particulate size and pattern also are difficult to control.In order to overcome the shortcoming of solid phase method, liquid phase method has caused investigators' extensive interest.Wherein, the auxiliary hydrothermal method of tensio-active agent has all shown huge advantage at aspects such as control powder size, pattern and dispersivenesses, and this method is simple to operate, and is low for equipment requirements, with low cost.
Summary of the invention
The objective of the invention is provides a kind of preparation method of strontium titanate nanometer powder of one-dimensional structure for overcoming the problem that prior art exists.
The preparation method of strontium titanate nanometer powder of one-dimensional structure of the present invention, employing be hydrothermal synthesis method, concrete steps are as follows:
1) tetrabutyl titanate is dissolved in dehydrated alcohol, the Ti in the regulator solution
4+Ionic concn is 0.1～0.5mol/L;
2) under the whipped state, add the ammonia soln of the mass concentration 30% of 1～2ml in the ethanolic soln of the tetrabutyl titanate that step 1) prepares, precipitation is filtered, washing, and the oxyhydroxide that obtains titanium precipitates;
3) strontium nitrate is dissolved in deionized water, forms the aqueous solution of strontium nitrate, Sr in the regulator solution
2+Ionic concentration is 0.05～0.5mol/L;
4) polyvinyl alcohol is dissolved in deionized water, configuration concentration is the aqueous solution of the polyvinyl alcohol of 4～32g/L;
5) oxyhydroxide with titanium precipitates, the strontium nitrate aqueous solution, polyvinyl alcohol water solution and potassium hydroxide solid join in the reactor inner bag, reach reactor inner bag volumetrical 70%～90% with the volume of material in the deionized water conditioned reaction still inner bag, stir 10min at least, obtain the precursor slurry, wherein the molecular volume mark of titanium is 0.02～0.1mol/L, the molecular volume mark of strontium is 0.01～0.1mol/L, the mol ratio of strontium and titanium is 0.5～1.0, the molecular volume mark of potassium hydroxide is 0.2～1mol/L, the quality volume fraction of polyvinyl alcohol is 1～8g/L, and molecular volume fractional volume radix is the cumulative volume of precursor slurry;
6) the reactor inner bag that the precursor slurry will be housed places reactor, sealing, be incubated 48～96 hours down at 100～150 ℃ and carry out hydrothermal treatment consists, allow reactor naturally cool to room temperature then, after unloading still, with deionized water repetitive scrubbing reaction product, filter, dry, obtain the strontium titanate nano-powder of one-dimentional structure.
The strontium titanate nanometer powder of one-dimensional structure that the present invention makes comprises strontium titanate nano wire and the branch crystal structure that is made of nano wire.
In the preparation process of the present invention, the reactor of use is a polytetrafluoroethylliner liner, stainless steel external member closed reaction kettle.
In the preparation process of the present invention, the purity of said tetrabutyl titanate, strontium nitrate, potassium hydroxide, dehydrated alcohol and polyvinyl alcohol all is not less than chemical pure.
Beneficial effect of the present invention is:
The present invention has adopted the auxiliary Hydrothermal Preparation of tensio-active agent strontium titanate nano wire and strontium titanate branch crystal.The method for preparing the strontium titanate branch crystal particularly is provided for the first time.Hydrothermal synthesis method equipment of the present invention is simple, and easy control of process conditions is with low cost, is easy to suitability for industrialized production.The strontium titanate nanometer powder of one-dimensional structure of the present invention's preparation has broad application prospects in fields such as microelectronic device, electro-optical device, memory device, oxygen sensor, photocatalyst, solar cells.
Description of drawings
Fig. 1 is X-ray diffraction (XRD) collection of illustrative plates of the strontium titanate nano wire for preparing of the present invention;
Fig. 2 is transmission electron microscope (TEM) photo of the strontium titanate nano wire for preparing of the present invention;
Fig. 3 is X-ray diffraction (XRD) collection of illustrative plates of the strontium titanate branch crystal for preparing of the present invention;
Fig. 4 is transmission electron microscope (TEM) photo of the strontium titanate branch crystal for preparing of the present invention.
Embodiment
Further specify the present invention below in conjunction with embodiment.
Embodiment 1
1) take by weighing the 1.702g tetrabutyl titanate, join in the 10ml dehydrated alcohol, magnetic agitation is to dissolving;
2) under the whipped state, adding 1ml mass concentration is 30% ammonia soln in the ethanolic soln of the tetrabutyl titanate that step 1) prepares, and precipitation is filtered, washing, and the oxyhydroxide that obtains titanium precipitates;
3) take by weighing the 0.529g strontium nitrate, join in the 10ml deionized water, magnetic agitation is to dissolving;
4) take by weighing the 0.016g polyvinyl alcohol, join in the 10ml deionized water, heating, magnetic agitation is to dissolving;
5) the hydroxyl hydrogen oxide precipitation of titanium, the aqueous solution of strontium nitrate, the aqueous solution and the 1.710g potassium hydroxide solid of polyvinyl alcohol are added in the reactor inner bag of volume 60ml, the volume of regulating the precursor slurry with deionized water is a reactor inner bag volumetrical 80%, stirred at least 10 minutes, and obtained the precursor slurry;
6) the reactor inner bag that the precursor slurry will be housed places reactor, sealing, be incubated 48 hours down at 150 ℃ and carry out hydrothermal treatment consists, allow reactor naturally cool to room temperature then, after unloading still, with deionized water repetitive scrubbing reaction product, filter, oven dry, obtain length-to-diameter ratio greater than 20 strontium titanate nano wire.Its X-ray diffraction (XRD) collection of illustrative plates is seen Fig. 1, and transmission electron microscope (TEM) photo is seen Fig. 2.
Embodiment 2
1) take by weighing the 1.702g tetrabutyl titanate, join in the 10ml dehydrated alcohol, magnetic agitation is to dissolving;
2) under the whipped state, adding 1ml mass concentration is 30% ammonia soln in the ethanolic soln of the tetrabutyl titanate that step 1) prepares, and precipitation is filtered, washing, and the oxyhydroxide that obtains titanium precipitates;
3) take by weighing the 1.058g strontium nitrate, join in the 10ml deionized water, magnetic agitation is to dissolving;
4) take by weighing the 0.016g polyvinyl alcohol, join in the 10ml deionized water, heating, magnetic agitation is to dissolving;
5) the hydroxyl hydrogen oxide precipitation of titanium, the aqueous solution of strontium nitrate, the aqueous solution and the 1.710g potassium hydroxide solid of polyvinyl alcohol are added in the reactor inner bag of volume 60ml, the volume of regulating the precursor slurry with deionized water is a reactor inner bag volumetrical 80%, stirred at least 10 minutes, and obtained the precursor slurry;
6) the reactor inner bag that the precursor slurry will be housed places reactor, sealing, 150 ℃ down insulation carried out hydrothermal treatment consists in 48 hours, allow reactor naturally cool to room temperature then, unload still after, with deionized water repetitive scrubbing reaction product, filter, dry, obtain the strontium titanate branch crystal.Its X-ray diffraction (XRD) collection of illustrative plates is seen Fig. 3, and transmission electron microscope (TEM) photo is seen Fig. 4.
1) take by weighing the 0.340g tetrabutyl titanate, join in the 10ml dehydrated alcohol, magnetic agitation is to dissolving;
2) under the whipped state, adding 1ml mass concentration is 30% ammonia soln in the ethanolic soln of the tetrabutyl titanate that step 1) prepares, and precipitation is filtered, washing, and the oxyhydroxide that obtains titanium precipitates;
3) take by weighing the 0.106g strontium nitrate, join in the 10ml deionized water, magnetic agitation is to dissolving;
4) take by weighing the 0.016g polyvinyl alcohol, join in the 10ml deionized water, heating, magnetic agitation is to dissolving;
5) the hydroxyl hydrogen oxide precipitation of titanium, the aqueous solution of strontium nitrate, the aqueous solution and the 1.710g potassium hydroxide solid of polyvinyl alcohol are added in the reactor inner bag of volume 60ml, the volume of regulating the precursor slurry with deionized water is a reactor inner bag volumetrical 80%, stirred at least 10 minutes, and obtained the precursor slurry;
6) the reactor inner bag that the precursor slurry will be housed places reactor, sealing, 150 ℃ down insulation carried out hydrothermal treatment consists in 96 hours, allow reactor naturally cool to room temperature then, unload still after, with deionized water repetitive scrubbing reaction product, filter, dry, obtain the strontium titanate nano wire.
Embodiment 4
1) take by weighing the 1.702g tetrabutyl titanate, join in the 10ml dehydrated alcohol, magnetic agitation is to dissolving;
2) under the whipped state, adding 1ml mass concentration is 30% ammonia soln in the ethanolic soln of the tetrabutyl titanate that step 1) prepares, and precipitation is filtered, washing, and the oxyhydroxide that obtains titanium precipitates;
3) take by weighing the 1.058g strontium nitrate, join in the 10ml deionized water, magnetic agitation is to dissolving;
4) take by weighing the 0.032g polyvinyl alcohol, join in the 10ml deionized water, heating, magnetic agitation is to dissolving;
5) the hydroxyl hydrogen oxide precipitation of titanium, the aqueous solution of strontium nitrate, the aqueous solution and the 0.684g potassium hydroxide solid of polyvinyl alcohol are added in the reactor inner bag of volume 60ml, the volume of regulating the precursor slurry with deionized water is a reactor inner bag volumetrical 70%, stirred at least 10 minutes, and obtained the precursor slurry;
6) the reactor inner bag that the precursor slurry will be housed places reactor, sealing, 150 ℃ down insulation carried out hydrothermal treatment consists in 72 hours, allow reactor naturally cool to room temperature then, unload still after, with deionized water repetitive scrubbing reaction product, filter, dry, obtain the strontium titanate branch crystal.
Embodiment 5
1) take by weighing the 1.702g tetrabutyl titanate, join in the 10ml dehydrated alcohol, magnetic agitation is to dissolving;
2) under the whipped state, adding 1ml mass concentration is 30% ammonia soln in the ethanolic soln of the tetrabutyl titanate that step 1) prepares, and precipitation is filtered, washing, and the oxyhydroxide that obtains titanium precipitates;
3) take by weighing the 1.058g strontium nitrate, join in the 10ml deionized water, magnetic agitation is to dissolving;
4) take by weighing the 0.008g polyvinyl alcohol, join in the 10ml deionized water, heating, magnetic agitation is to dissolving;
5) the hydroxyl hydrogen oxide precipitation of titanium, the aqueous solution of strontium nitrate, the aqueous solution and the 1.710g potassium hydroxide solid of polyvinyl alcohol are added in the reactor inner bag of volume 60ml, the volume of regulating the precursor slurry with deionized water is a reactor inner bag volumetrical 80%, stirred at least 10 minutes, and obtained the precursor slurry;
6) the reactor inner bag that the precursor slurry will be housed places reactor, sealing, 100 ℃ down insulation carried out hydrothermal treatment consists in 96 hours, allow reactor naturally cool to room temperature then, unload still after, with deionized water repetitive scrubbing reaction product, filter, dry, obtain the strontium titanate branch crystal.
Claims (4)
1. the preparation method of a strontium titanate nanometer powder of one-dimensional structure is characterized in that may further comprise the steps:
1) tetrabutyl titanate is dissolved in dehydrated alcohol, the Ti in the regulator solution
4+Ionic concn is 0.1～0.5mol/L;
2) under the whipped state, add the ammonia soln of the mass concentration 30% of 1～2ml in the ethanolic soln of the tetrabutyl titanate that step 1) prepares, precipitation is filtered, washing, and the oxyhydroxide that obtains titanium precipitates;
3) strontium nitrate is dissolved in deionized water, forms the aqueous solution of strontium nitrate, Sr in the regulator solution
2+Ionic concentration is 0.05～0.5mol/L;
4) polyvinyl alcohol is dissolved in deionized water, configuration concentration is the aqueous solution of the polyvinyl alcohol of 4～32g/L;
5) oxyhydroxide with titanium precipitates, the strontium nitrate aqueous solution, polyvinyl alcohol water solution and potassium hydroxide solid join in the reactor inner bag, reach reactor inner bag volumetrical 70%～90% with the volume of material in the deionized water conditioned reaction still inner bag, stir 10min at least, obtain the precursor slurry, wherein the molecular volume mark of titanium is 0.02～0.1mol/L, the molecular volume mark of strontium is 0.01～0.1mol/L, the mol ratio of strontium and titanium is 0.5～1.0, the molecular volume mark of potassium hydroxide is 0.2～1mol/L, the quality volume fraction of polyvinyl alcohol is 1～8g/L, and molecular volume fractional volume radix is the cumulative volume of precursor slurry;
6) the reactor inner bag that the precursor slurry will be housed places reactor, sealing, be incubated 48～96 hours down at 100～150 ℃ and carry out hydrothermal treatment consists, allow reactor naturally cool to room temperature then, after unloading still, with deionized water repetitive scrubbing reaction product, filter, dry, obtain the Sr titanate powder of one dimension Nano structure.
2. the preparation method of strontium titanate nanometer powder of one-dimensional structure according to claim 1 is characterized in that said one-dimentional structure comprises strontium titanate nano wire and the branch crystal structure that is made of nano wire.
3. the preparation method of strontium titanate nanometer powder of one-dimensional structure according to claim 1 is characterized in that said reactor is a polytetrafluoroethylliner liner, stainless steel external member closed reaction kettle.
4. the preparation method of strontium titanate nanometer powder of one-dimensional structure according to claim 1 is characterized in that the purity of said tetrabutyl titanate, strontium nitrate, potassium hydroxide, dehydrated alcohol and polyvinyl alcohol all is not less than chemical pure.
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