CN102517637A - Preparation method for lead titanate nanowire - Google Patents

Preparation method for lead titanate nanowire Download PDF

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CN102517637A
CN102517637A CN2011104488608A CN201110448860A CN102517637A CN 102517637 A CN102517637 A CN 102517637A CN 2011104488608 A CN2011104488608 A CN 2011104488608A CN 201110448860 A CN201110448860 A CN 201110448860A CN 102517637 A CN102517637 A CN 102517637A
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reaction kettle
titanium
lead
lead titanate
inner bag
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CN102517637B (en
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王永刚
杨琳琳
王玉江
王晓峰
徐国辉
林海燕
罗伟
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Luoyang Institute of Science and Technology
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Luoyang Institute of Science and Technology
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Abstract

The invention discloses a preparation method for a lead titanate nanowire. The preparation method comprises the following steps of: preparing carbonate precipitation of titanium and lead serving as a reaction material; adding potassium hydroxide with a proper concentration for promoting crystallization; and with water as solvent, carrying out a hydro-thermal reaction at the temperature of 120-200DEG C to obtain the lead titanate nanowire. According to the preparation method disclosed by the invention, a process flow is simple; the size of the nanowire is easy to control; no surfactant is used; no pollution occurs; the cost is low; and the scale production is easily realized. The lead titanate nanowire has broad application prospect in the fields of sensors, capacitors, thermistors, photoelectronic devices, satellite detection systems and the like.

Description

A kind of preparation method of lead titanate nano wire
Technical field
The present invention relates to a kind of preparation method of lead titanate nano wire, belong to field of inorganic nonmetallic material.
Background technology
Lead titanate (PbTiO 3) be a kind of very important perovskite composite oxide, have performances such as excellent piezoelectricity, ferroelectric, pyroelectricity and electric light, be with a wide range of applications in fields such as transmitter, electrical condenser, thermistor, opto-electronic device and satellite detection systems.Lead titanate also is one of important starting material of electronic ceramics simultaneously, is widely used in piezoelectric ceramics and high temperature sensor.
One dimension Nano structure has obtained domestic and international researcher's very big concern with its peculiar physics and chemical property, and the preparation research of one dimension Nano structures such as nano wire, nanometer rod, nanotube has become the research focus of nano material.Lead titanate nano wire tends to show some excellent performances.Therefore, lead titanate nano wire be prepared in theoretical investigation and the practical application aspect all is extremely important.And liquid phase method has demonstrated huge advantage on size and the pattern of control powder, have simple to operate, advantage such as equipment requirements is low, and is pollution-free, 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 technology, the method for preparing lead titanate nano wire with low cost.
The preparation method of lead titanate nano wire of the present invention, employing be hydrothermal synthesis method, concrete steps are following:
1) titanium sulfate is dissolved in the dilute nitric acid solution of 0.3wt%, the Ti in the regulator solution 4+Ionic concn is 0.3 ~ 1.0mol/L;
2) under the whipped state, in the dilute nitric acid solution of the titanium sulfate that step 1) makes, add wet chemical, the pH value that makes solution is 14, with the sedimentation and filtration that obtains, washing, obtains the carbonate deposition of titanium;
3) lead nitrate is dissolved in zero(ppm) water, forms the lead nitrate aqueous solution, the concentration of lead ion is 0.5 ~ 1.0mol/L in the regulator solution;
4) under the whipped state, in the lead nitrate aqueous solution that step 3) makes, add wet chemical, the pH value that makes solution is 14, with the sedimentation and filtration that obtains, washing, obtains plumbous carbonate deposition;
5) titanium and plumbous carbonate deposition, Pottasium Hydroxide are joined in the reaction kettle inner bag; Reaction mass volume with in the zero(ppm) water conditioned reaction still inner bag reaches reaction kettle inner bag volumetrical 70% ~ 90%; Stirred 10 ~ 30 minutes, wherein the volumetric molar concentration number of the carbonate of titanium is 0.1 ~ 0.3mol/L, and plumbous mol ratio with titanium is 1; The volumetric molar concentration number of Pottasium Hydroxide is 4 ~ 8mol/L, and the volume radix of volumetric molar concentration number is introduced the volume of material in the reaction kettle inner bag for all;
6) the reaction kettle inner bag that step 5) is disposed reaction mass places reaction kettle, and sealing is 120 ~ 200 oC down insulation carried out hydrothermal treatment consists in 6 ~ 24 hours, let reaction kettle naturally cool to room temperature then, unload still after, with rare nitric acid and the zero(ppm) water repetitive scrubbing reaction product of 0.3wt%, filtration, dry, obtain lead titanate nano wire.
The present invention prepares in the process, and the reaction kettle of use is a polytetrafluoroethylliner liner, stainless steel external member closed reaction kettle.
The present invention prepares in the process, and the purity of said titanium sulfate, lead nitrate, Pottasium Hydroxide and absolute ethyl alcohol all is not less than CP.
Beneficial effect of the present invention is:
The present invention has adopted simple Hydrothermal Preparation crystallization good stability, the lead titanate nano wire that purity is high, and the size of nano wire can be regulated through changing processing parameter.The hydrothermal synthesis method of lead titanate nano wire of the present invention does not adopt any tensio-active agent, non-environmental-pollution, equipment are simple, easy control of process conditions, preparation with low cost, be easy to suitability for industrialized production.Lead titanate nano wire of the present invention is with a wide range of applications in fields such as transmitter, electrical condenser, thermistor, opto-electronic device and satellite detection systems.
Description of drawings
Fig. 1 is the XRD figure spectrum of the embodiment of the invention 1 synthetic lead titanate nano wire;
Fig. 2 is transmission electron microscope (TEM) photo of the embodiment of the invention 1 synthetic lead titanate nano wire.
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 0.3wt%, the Ti in the regulator solution 4+Ionic concn is 0.3mol/L;
2) under the whipped state, in the dilute nitric acid solution of the titanium sulfate that step 1) makes, add wet chemical, the pH value that makes solution is 14, with the sedimentation and filtration that obtains, washing, obtains the carbonate deposition of titanium;
3) lead nitrate is dissolved in zero(ppm) water, forms the lead nitrate aqueous solution, the concentration of lead ion is 0.5mol/L in the regulator solution;
4) under the whipped state, in the lead nitrate aqueous solution that step 3) makes, add wet chemical, the pH value that makes solution is 14, with the sedimentation and filtration that obtains, washing, obtains plumbous carbonate deposition;
5) titanium and plumbous carbonate deposition, Pottasium Hydroxide are joined in the reaction kettle inner bag; Reaction mass volume with in the zero(ppm) water conditioned reaction still inner bag reaches reaction kettle inner bag volumetrical 70%; Stirred 10 minutes, wherein the volumetric molar concentration number of the carbonate of titanium is 0.1 ~ 0.3mol/L, and plumbous mol ratio with titanium is 1; The volumetric molar concentration number of Pottasium Hydroxide is 4mol/L, and the volume radix of volumetric molar concentration number is introduced the volume of material in the reaction kettle inner bag for all;
The reaction kettle inner bag that 6) will dispose reaction mass places reaction kettle, and sealing is 120 oC down insulation carried out hydrothermal treatment consists in 6 hours, let reaction kettle naturally cool to room temperature then, unload still after; With rare nitric acid and the zero(ppm) water repetitive scrubbing reaction product of 0.3wt%, filter, dry, obtain lead titanate nano wire; Nanowire length is 1-3um, and diameter is 10-20nm.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 0.3wt%, the Ti in the regulator solution 4+Ionic concn is 0.6mol/L;
2) under the whipped state, in the dilute nitric acid solution of the titanium sulfate that step 1) makes, add potassium hydroxide aqueous solution, the pH value that makes solution is 14, with the sedimentation and filtration that obtains, washing, obtains the carbonate deposition of titanium;
3) lead nitrate is dissolved in zero(ppm) water, forms the lead nitrate aqueous solution, the concentration of lead ion is 0.7mol/L in the regulator solution;
4) under the whipped state, in the lead nitrate aqueous solution that step 3) makes, add potassium hydroxide aqueous solution, the pH value that makes solution is 14, with the sedimentation and filtration that obtains, washing, obtains plumbous carbonate deposition;
5) titanium and plumbous carbonate deposition, Pottasium Hydroxide are joined in the reaction kettle inner bag; Reaction mass volume with in the zero(ppm) water conditioned reaction still inner bag reaches reaction kettle inner bag volumetrical 80%; Stirred 18 minutes, wherein the volumetric molar concentration number of the carbonate of titanium is 0.2mol/L, and plumbous mol ratio with titanium is 1; The volumetric molar concentration number of Pottasium Hydroxide is 6mol/L, and the volume radix of volumetric molar concentration number is introduced the volume of material in the reaction kettle inner bag for all;
The reaction kettle inner bag that 6) will dispose reaction mass places reaction kettle, and sealing is 150 oC down insulation carried out hydrothermal treatment consists in 12 hours, let reaction kettle naturally cool to room temperature then, unload still after; With rare nitric acid and the zero(ppm) water repetitive scrubbing reaction product of 0.3wt%, filter, dry, obtain lead titanate nano wire; Nanowire length is 2-3um, and diameter is 20-30nm.
Embodiment 3
1) titanium sulfate is dissolved in the dilute nitric acid solution of 0.3wt%, the Ti in the regulator solution 4+Ionic concn is 0.8mol/L;
2) under the whipped state, in the dilute nitric acid solution of the titanium sulfate that step 1) makes, add potassium hydroxide aqueous solution, the pH value that makes solution is 14, with the sedimentation and filtration that obtains, washing, obtains the carbonate deposition of titanium;
3) lead nitrate is dissolved in zero(ppm) water, forms the lead nitrate aqueous solution, the concentration of lead ion is 0.8mol/L in the regulator solution;
4) under the whipped state, in the lead nitrate aqueous solution that step 3) makes, add potassium hydroxide aqueous solution, the pH value that makes solution is 14, with the sedimentation and filtration that obtains, washing, obtains plumbous carbonate deposition;
5) titanium and plumbous carbonate deposition, Pottasium Hydroxide are joined in the reaction kettle inner bag; Reaction mass volume with in the zero(ppm) water conditioned reaction still inner bag reaches reaction kettle inner bag volumetrical 75%; Stirred 25 minutes, wherein the volumetric molar concentration number of the carbonate of titanium is 0.25mol/L, and plumbous mol ratio with titanium is 1; The volumetric molar concentration number of Pottasium Hydroxide is 7mol/L, and the volume radix of volumetric molar concentration number is introduced the volume of material in the reaction kettle inner bag for all;
The reaction kettle inner bag that 6) will dispose reaction mass places reaction kettle, and sealing is 180 oC down insulation carried out hydrothermal treatment consists in 20 hours, let reaction kettle naturally cool to room temperature then, unload still after; With rare nitric acid and the zero(ppm) water repetitive scrubbing reaction product of 0.3wt%, filter, dry, obtain lead titanate nano wire; Nanowire length is 2-3um, and diameter is 40-50nm.
Embodiment 4
1) titanium sulfate is dissolved in the dilute nitric acid solution of 0.3wt%, the Ti in the regulator solution 4+Ionic concn is 1.0mol/L;
2) under the whipped state, in the dilute nitric acid solution of the titanium sulfate that step 1) makes, add potassium hydroxide aqueous solution, the pH value that makes solution is 14, with the sedimentation and filtration that obtains, washing, obtains the carbonate deposition of titanium;
3) lead nitrate is dissolved in zero(ppm) water, forms the lead nitrate aqueous solution, the concentration of lead ion is 1.0mol/L in the regulator solution;
4) under the whipped state, in the lead nitrate aqueous solution that step 3) makes, add potassium hydroxide aqueous solution, the pH value that makes solution is 14, with the sedimentation and filtration that obtains, washing, obtains plumbous carbonate deposition;
5) titanium and plumbous carbonate deposition, Pottasium Hydroxide are joined in the reaction kettle inner bag; Reaction mass volume with in the zero(ppm) water conditioned reaction still inner bag reaches reaction kettle inner bag volumetrical 90%; Stirred 30 minutes, wherein the volumetric molar concentration number of the carbonate of titanium is 0.3mol/L, and plumbous mol ratio with titanium is 1; The volumetric molar concentration number of Pottasium Hydroxide is 8mol/L, and the volume radix of volumetric molar concentration number is introduced the volume of material in the reaction kettle inner bag for all;
The reaction kettle inner bag that 6) will dispose reaction mass places reaction kettle, and sealing is 200 oC down insulation carried out hydrothermal treatment consists in 24 hours, let reaction kettle naturally cool to room temperature then, unload still after; With rare nitric acid and the zero(ppm) water repetitive scrubbing reaction product of 0.3wt%, filter, dry, obtain lead titanate nano wire; Nanowire length is 2-3um, and diameter is 40-50nm.

Claims (4)

1. the preparation method of a lead titanate nano wire is characterized in that may further comprise the steps:
1) titanium sulfate is dissolved in the dilute nitric acid solution of 0.3wt%, the Ti in the regulator solution 4+Ionic concn is 0.3 ~ 1.0mol/L;
2) under the whipped state, in the dilute nitric acid solution of the titanium sulfate that step 1) makes, add wet chemical, the pH value that makes solution is 14, with the sedimentation and filtration that obtains, washing, obtains the carbonate deposition of titanium;
3) lead nitrate is dissolved in zero(ppm) water, forms the lead nitrate aqueous solution, the concentration of lead ion is 0.5 ~ 1.0mol/L in the regulator solution;
4) under the whipped state, in the lead nitrate aqueous solution that step 3) makes, add wet chemical, the pH value that makes solution is 14, with the sedimentation and filtration that obtains, washing, obtains plumbous carbonate deposition;
5) titanium and plumbous carbonate deposition, Pottasium Hydroxide are joined in the reaction kettle inner bag; Reaction mass volume with in the zero(ppm) water conditioned reaction still inner bag reaches reaction kettle inner bag volumetrical 70% ~ 90%; Stirred 10 ~ 30 minutes, wherein the volumetric molar concentration number of the carbonate of titanium is 0.1 ~ 0.3mol/L, and plumbous mol ratio with titanium is 1; The volumetric molar concentration number of Pottasium Hydroxide is 4 ~ 8mol/L, and the volume radix of volumetric molar concentration number is introduced the volume of material in the reaction kettle inner bag for all;
6) the reaction kettle inner bag that step 5) is disposed reaction mass places reaction kettle, and sealing is 120 ~ 200 oC down insulation carried out hydrothermal treatment consists in 6 ~ 24 hours, let reaction kettle naturally cool to room temperature then, unload still after, with rare nitric acid and the zero(ppm) water repetitive scrubbing reaction product of 0.3wt%, filtration, dry, obtain lead titanate nano wire.
2. the preparation method of lead titanate nano wire according to claim 1 is characterized in that reaction kettle is a polytetrafluoroethylliner liner, stainless steel external member closed reaction kettle.
3. the preparation method of lead titanate nano wire according to claim 1 is characterized in that the purity of said titanium sulfate, lead nitrate, Pottasium Hydroxide and absolute ethyl alcohol all is not less than CP.
4. the preparation method of lead titanate nano wire according to claim 1 does not use any tensio-active agent, and the length of prepared lead titanate nano wire is not less than 1um.
CN201110448860.8A 2011-12-29 2011-12-29 Preparation method for lead titanate nanowire Expired - Fee Related CN102517637B (en)

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Cited By (2)

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CN103877964A (en) * 2014-03-12 2014-06-25 浙江大学 Preparation method of heterojunction between perovskite-phase lead titanate monocrystal nanowire and anatase-phase titanium dioxide
CN111730063A (en) * 2020-06-12 2020-10-02 欧菲微电子技术有限公司 Preparation method of lead nanowire

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103877964A (en) * 2014-03-12 2014-06-25 浙江大学 Preparation method of heterojunction between perovskite-phase lead titanate monocrystal nanowire and anatase-phase titanium dioxide
CN103877964B (en) * 2014-03-12 2016-09-14 浙江大学 A kind of preparation method of the hetero-junctions of Perovskite Phase lead titanate monocrystal nano line and anatase phase titanium dioxide
CN111730063A (en) * 2020-06-12 2020-10-02 欧菲微电子技术有限公司 Preparation method of lead nanowire

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