CN102531045B - Preparation method of barium titanate nano-rings - Google Patents
Preparation method of barium titanate nano-rings Download PDFInfo
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- CN102531045B CN102531045B CN2011104489013A CN201110448901A CN102531045B CN 102531045 B CN102531045 B CN 102531045B CN 2011104489013 A CN2011104489013 A CN 2011104489013A CN 201110448901 A CN201110448901 A CN 201110448901A CN 102531045 B CN102531045 B CN 102531045B
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Abstract
The invention relates to a preparation method of barium titanate nano-rings, which comprises the steps of preparing titanium hydroxide and barium hydroxide which are used as reaction materials, adding potassium hydroxide with proper concentration to promote crystallization, and under 120-200 DEG C, taking ethanol as solvent and conducting ethanol thermal reaction to obtain the barium titanate nano-rings. The preparation method firstly realizes the synthesis of the barium titanate nano-rings, the process is simple, the size of the nano-rings is apt to be controlled, the cost is low, the pollution is not caused and the scale production can be easily realized; the product crystallization quality is stable and the powder particle dispersibility is good; and the application prospect in the fields of thermistor, semiconductor materials, sensitive elements, multilayer ceramic capacitors, dielectric amplifiers, dynamic random access memories and the like is wide.
Description
Technical field
The present invention relates to a kind of preparation method of barium titanate nano-rings, belong to field of inorganic nonmetallic material.
Background technology
Barium titanate (BaTiO
3) be a kind of very important ABO
3The type perovskite composite oxides, as a kind of typical ferroelectric and dielectric materials, barium titanate is having a wide range of applications aspect making dielectric amplifier, thermistor, nonlinear circuit component, laminated ceramic capacitor, dynamic RAM and other photoelectric device.
The performance of nano material depends on pattern and the size of nanocrystal, and the nano material with special appearance tends to show some excellent performances.Therefore, the resonable opinion research of the barium titanate nano crystal of research and development pattern novelty and practical application aspect all are extremely important.And liquid phase method has demonstrated huge advantage at size and the pattern of control powder, have simple to operate, the advantage such as equipment requirements is low, and is with low cost.
Summary of the invention
It is simple, easy to operate to the purpose of this invention is to provide a kind of technique, the method for preparing barium titanate nano-rings with low cost.
The preparation method of barium titanate nano-rings of the present invention, employing be the ethanol thermal synthesis method, concrete steps are as follows:
1) titanium sulfate is dissolved in the dilute nitric acid solution of 0.5wt%, the Ti in the regulator solution
4+Ionic concn is 0.5 ~ 1.0mol/L;
2) under the whipped state, to step 1) add potassium hydroxide aqueous solution in the dilute nitric acid solution of the titanium sulfate that makes, the pH value that makes solution is 14, with sedimentation and filtration, the washing that obtains, obtains the oxyhydroxide precipitation of titanium;
3) nitrate of baryta is dissolved in distilled water, forms barium nitrate aqueous solution, the concentration of barium ion is 0.5 ~ 1.0mol/L in the regulator solution;
4) under the whipped state, to step 3) add potassium hydroxide aqueous solution in the barium nitrate aqueous solution that makes, the pH value that makes solution is 14, with sedimentation and filtration, the washing that obtains, obtains the oxyhydroxide precipitation of barium;
5) oxyhydroxide precipitation, the potassium hydroxide with titanium and barium joins in the reactor inner bag, reach 70% ~ 90% of reactor inner bag volume with the reaction mass volume in the dehydrated alcohol conditioned reaction still inner bag, stirred at least 10 minutes, wherein the volumetric molar concentration of the oxyhydroxide of titanium is 0.1 ~ 0.2mol/L, the mol ratio of barium and titanium is 1, the volumetric molar concentration of potassium hydroxide is 0.1 ~ 1mol/L, and the volume radix of volumetric molar concentration is the volume of material in all introducing reactor inner bags;
6) with step 5) the reactor inner bag that disposes reaction mass places reactor, and sealing is 120 ~ 200
oBe incubated 6 ~ 24 hours under the C and carry out ethanol thermal treatment, then allow reactor naturally cool to room temperature, unload still after, with rare nitric acid and the distilled water repetitive scrubbing reaction product of 0.5wt%, filter, oven dry, obtain barium titanate nano-rings.
In the preparation process of the present invention, the reactor of use is polytetrafluoroethylliner liner, the reactor that the stainless steel external member is airtight.
In the preparation process of the present invention, the purity of said titanium sulfate, nitrate of baryta, potassium hydroxide and dehydrated alcohol all is not less than chemical pure.
Beneficial effect of the present invention is:
The present invention adopt the hot legal system of simple ethanol standby crystallization good stability, barium titanate nano-rings that purity is high, and the size of nano-rings can be regulated by changing processing parameter.The ethanol process for thermosynthesizing equipment of barium titanate nano-rings of the present invention is simple, easy control of process conditions, and preparation with low cost is easy to suitability for industrialized production.Barium titanate nano-rings of the present invention has broad application prospects in fields such as thermistor, semiconductor material, sensor, laminated ceramic capacitor, dielectric amplifier, dynamic RAM.
Description of drawings
Fig. 1 is the XRD figure spectrum of the synthetic barium titanate nano-rings of the embodiment of the invention 1;
Fig. 2 is transmission electron microscope (TEM) photo of the synthetic barium titanate nano-rings of the embodiment of the invention 1.
Embodiment
Further specify the present invention below in conjunction with embodiment.
Embodiment 1
1) titanium sulfate is dissolved in the dilute nitric acid solution of 0.5wt%, the Ti in the regulator solution
4+Ionic concn is 0.5mol/L;
2) under the whipped state, to step 1) add potassium hydroxide aqueous solution in the dilute nitric acid solution of the titanium sulfate that makes, the pH value that makes solution is 14, with sedimentation and filtration, the washing that obtains, obtains the oxyhydroxide precipitation of titanium;
3) nitrate of baryta is dissolved in distilled water, forms barium nitrate aqueous solution, the concentration of barium ion is 0.5mol/L in the regulator solution;
4) under the whipped state, to step 3) add potassium hydroxide aqueous solution in the barium nitrate aqueous solution that makes, the pH value that makes solution is 14, with sedimentation and filtration, the washing that obtains, obtains the oxyhydroxide precipitation of barium;
5) oxyhydroxide precipitation, the potassium hydroxide with titanium and barium joins in the reactor inner bag, reach 70% of reactor inner bag volume with the reaction mass volume in the dehydrated alcohol conditioned reaction still inner bag, stirred 10 minutes, wherein the volumetric molar concentration of the oxyhydroxide of titanium is 0.1mol/L, the mol ratio of barium and titanium is 1, the volumetric molar concentration of potassium hydroxide is 0.1mol/L, and the volume radix of volumetric molar concentration is the volume of material in all introducing reactor inner bags;
The reactor inner bag that 6) will dispose reaction mass places reactor, and sealing is 120
oInsulation was carried out ethanol thermal treatment in 6 hours under the C, then allowed reactor naturally cool to room temperature, unload still after, with rare nitric acid and the distilled water repetitive scrubbing reaction product of 0.5wt%, filter, dry, obtain barium titanate nano-rings, the external diameter of nano-rings is 100-120nm, and internal diameter is 50-60nm.Its XRD figure spectrum is seen Fig. 1, and transmission electron microscope (TEM) photo is seen Fig. 2.
Embodiment 2
1) titanium sulfate is dissolved in the dilute nitric acid solution of 0.5wt%, the Ti in the regulator solution
4+Ionic concn is 0.75mol/L;
2) under the whipped state, to step 1) add potassium hydroxide aqueous solution in the dilute nitric acid solution of the titanium sulfate that makes, the pH value that makes solution is 14, with sedimentation and filtration, the washing that obtains, obtains the oxyhydroxide precipitation of titanium;
3) nitrate of baryta is dissolved in distilled water, forms barium nitrate aqueous solution, the concentration of barium ion is 0.8mol/L in the regulator solution;
4) under the whipped state, to step 3) add potassium hydroxide aqueous solution in the barium nitrate aqueous solution that makes, the pH value that makes solution is 14, with sedimentation and filtration, the washing that obtains, obtains the oxyhydroxide precipitation of barium;
5) oxyhydroxide precipitation, the potassium hydroxide with titanium and barium joins in the reactor inner bag, reach 80% of reactor inner bag volume with the reaction mass volume in the dehydrated alcohol conditioned reaction still inner bag, stirred 15 minutes, wherein the volumetric molar concentration of the oxyhydroxide of titanium is 0.15mol/L, the mol ratio of barium and titanium is 1, the volumetric molar concentration of potassium hydroxide is 0.6mol/L, and the volume radix of volumetric molar concentration is the volume of material in all introducing reactor inner bags;
The reactor inner bag that 6) will dispose reaction mass places reactor, and sealing is 160
oInsulation was carried out ethanol thermal treatment in 13 hours under the C, then allowed reactor naturally cool to room temperature, unload still after, with rare nitric acid and the distilled water repetitive scrubbing reaction product of 0.5wt%, filter, dry, obtain barium titanate nano-rings, the external diameter of nano-rings is 110-130nm, and internal diameter is 55-65nm.
Embodiment 3
1) titanium sulfate is dissolved in the dilute nitric acid solution of 0.5wt%, the Ti in the regulator solution
4+Ionic concn is 0.6mol/L;
2) under the whipped state, to step 1) add potassium hydroxide aqueous solution in the dilute nitric acid solution of the titanium sulfate that makes, the pH value that makes solution is 14, with sedimentation and filtration, the washing that obtains, obtains the oxyhydroxide precipitation of titanium;
3) nitrate of baryta is dissolved in distilled water, forms barium nitrate aqueous solution, the concentration of barium ion is 0.3mol/L in the regulator solution;
4) under the whipped state, to step 3) add potassium hydroxide aqueous solution in the barium nitrate aqueous solution that makes, the pH value that makes solution is 14, with sedimentation and filtration, the washing that obtains, obtains the oxyhydroxide precipitation of barium;
5) oxyhydroxide precipitation, the potassium hydroxide with titanium and barium joins in the reactor inner bag, reach 82% of reactor inner bag volume with the reaction mass volume in the dehydrated alcohol conditioned reaction still inner bag, stirred 30 minutes, wherein the volumetric molar concentration of the oxyhydroxide of titanium is 0.4mol/L, the mol ratio of barium and titanium is 1, the volumetric molar concentration of potassium hydroxide is 0.8mol/L, and the volume radix of volumetric molar concentration is the volume of material in all introducing reactor inner bags;
The reactor inner bag that 6) will dispose reaction mass places reactor, and sealing is 140
oInsulation was carried out ethanol thermal treatment in 18 hours under the C, then allowed reactor naturally cool to room temperature, unload still after, with rare nitric acid and the distilled water repetitive scrubbing reaction product of 0.5wt%, filter, dry, obtain barium titanate nano-rings, the external diameter of nano-rings is 120-140nm, and internal diameter is 60-70nm.
Embodiment 4
1) titanium sulfate is dissolved in the dilute nitric acid solution of 0.5wt%, the Ti in the regulator solution
4+Ionic concn is 1.0mol/L;
2) under the whipped state, to step 1) add potassium hydroxide aqueous solution in the dilute nitric acid solution of the titanium sulfate that makes, the pH value that makes solution is 14, with sedimentation and filtration, the washing that obtains, obtains the oxyhydroxide precipitation of titanium;
3) nitrate of baryta is dissolved in distilled water, forms barium nitrate aqueous solution, the concentration of barium ion is 1.0mol/L in the regulator solution;
4) under the whipped state, to step 3) add potassium hydroxide aqueous solution in the barium nitrate aqueous solution that makes, the pH value that makes solution is 14, with sedimentation and filtration, the washing that obtains, obtains the oxyhydroxide precipitation of barium;
5) oxyhydroxide precipitation, the potassium hydroxide with titanium and barium joins in the reactor inner bag, reach 90% of reactor inner bag volume with the reaction mass volume in the dehydrated alcohol conditioned reaction still inner bag, stirred 20 minutes, wherein the volumetric molar concentration of the oxyhydroxide of titanium is 0.2mol/L, the mol ratio of barium and titanium is 1, the volumetric molar concentration of potassium hydroxide is 1mol/L, and the volume radix of volumetric molar concentration is the volume of material in all introducing reactor inner bags;
The reactor inner bag that 6) will dispose reaction mass places reactor, and sealing is 200
oInsulation was carried out ethanol thermal treatment in 24 hours under the C, then allowed reactor naturally cool to room temperature, unload still after, with rare nitric acid and the distilled water repetitive scrubbing reaction product of 0.5wt%, filter, dry, obtain barium titanate nano-rings, the external diameter of nano-rings is 130-150nm, and internal diameter is 65-75nm.
Claims (3)
1. the preparation method of a barium titanate nano-rings is characterized in that may further comprise the steps:
1) titanium sulfate is dissolved in the dilute nitric acid solution of 0.5wt%, the Ti in the regulator solution
4+Ionic concn is 0.5 ~ 1.0mol/L;
2) under the whipped state, to step 1) add potassium hydroxide aqueous solution in the dilute nitric acid solution of the titanium sulfate that makes, the pH value that makes solution is 14, with sedimentation and filtration, the washing that obtains, obtains the oxyhydroxide precipitation of titanium;
3) nitrate of baryta is dissolved in distilled water, forms barium nitrate aqueous solution, the concentration of barium ion is 0.5 ~ 1.0mol/L in the regulator solution;
4) under the whipped state, to step 3) add potassium hydroxide aqueous solution in the barium nitrate aqueous solution that makes, the pH value that makes solution is 14, with sedimentation and filtration, the washing that obtains, obtains the oxyhydroxide precipitation of barium;
5) oxyhydroxide precipitation, the potassium hydroxide with titanium and barium joins in the reactor inner bag, reach 70% ~ 90% of reactor inner bag volume with the reaction mass volume in the dehydrated alcohol conditioned reaction still inner bag, stirred at least 10 minutes, wherein the volumetric molar concentration of the oxyhydroxide of titanium is 0.1 ~ 0.2mol/L, the mol ratio of barium and titanium is 1, the volumetric molar concentration of potassium hydroxide is 0.1 ~ 1mol/L, and the volume radix of volumetric molar concentration is the volume of material in all introducing reactor inner bags;
6) with step 5) the reactor inner bag that disposes reaction mass places reactor, and sealing is 120 ~ 200
oBe incubated 6 ~ 24 hours under the C and carry out ethanol thermal treatment, then allow reactor naturally cool to room temperature, unload still after, with rare nitric acid and the distilled water repetitive scrubbing reaction product of 0.5wt%, filter, oven dry, obtain barium titanate nano-rings.
2. the preparation method of barium titanate nano-rings according to claim 1 is characterized in that reactor is polytetrafluoroethylliner liner, the reactor that the stainless steel external member is airtight.
3. the preparation method of barium titanate nano-rings according to claim 1 is characterized in that the purity of said titanium sulfate, nitrate of baryta, potassium hydroxide and dehydrated alcohol all is not less than chemical pure.
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