CN103882525A - Preparation method of regular and square perovskite-structured lead titanate mono-crystal nano-particles - Google Patents
Preparation method of regular and square perovskite-structured lead titanate mono-crystal nano-particles Download PDFInfo
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- CN103882525A CN103882525A CN201410101655.8A CN201410101655A CN103882525A CN 103882525 A CN103882525 A CN 103882525A CN 201410101655 A CN201410101655 A CN 201410101655A CN 103882525 A CN103882525 A CN 103882525A
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Abstract
The invention relates to a preparation method of regular and square perovskite-structured lead titanate mono-crystal nano-particles. The preparation method comprises the following steps: by adopting a polymer auxiliary hydro-thermal process, adding KOH (potassium hydroxide) used as a mineralizer and PVP (polyvinylpyrrolidone) used as a surface modifier into a reaction kettle, and performing a hydrothermal reaction at a temperature of 180-200 DEG C; filtering, cleaning and drying a reaction product to obtain the regular and square perovskite-structured lead titanate mono-crystal nano-particles. The preparation method disclosed by the invention is simple in technical process, easy in control, pollution-free, low in cost and easy in large-scale production; the prepared regular and square perovskite-structured lead titanate mono-crystal nano-particles are high in purity, regular in shape and appearance, and uniform in size.
Description
Technical field
The preparation method who the present invention relates to a kind of perovskite structure lead titanate monocrystal nano particle, belongs to field of inorganic nonmetallic material.
Background technology
The development of IT industry and scientific and technological progress make the miniaturization of electron device become the powerful trend of hyundai electronics industry development, and electron device has proposed increasing requirement to the nanometer of material thus.Especially about the research of the aspects such as Ferroelectic Nanomaterials, under the demand driving of nanometer engine, ferroelectric non-volatile storer etc., more and more receive people's concern.Therefore, the synthetic and performance of nano structural material becomes the study hotspot of many Research Teams.Traditional perovskite structure lead titanate (PbTiO
3) be a kind of typical ferroelectric oxide, its ABO
3type simple in structure, has high ferroelectric phase transition Curie temperature (490
oand high spontaneous polarization C).Lead titanate has abundant physicals, such as ferroelectric, the piezoelectric & dielectric properties of excellence, therefore has a wide range of applications in field of electronic devices such as non-volatility ferroelectric storer, piezoelectric transducer, pyroelectricity sensor and high dielectric capacitor.
Macromolecular surface modification agent such as PVAC polyvinylalcohol, polyoxyethylene glycol PEG, POLYPROPYLENE GLYCOL PAA and polyvinylpyrrolidone PVP etc., is played very important effect in the process of hydro-thermal reaction.Particularly PVP, can play the effect of structure directing agent and dispersion agent.Therefore utilize PVP as coating materials, can prepare the square perovskite structure lead titanate monocrystal nano particle with regular facet.
Summary of the invention
The object of the present invention is to provide a kind of technique simple, process is easy to the preparation method of the perovskite structure lead titanate monocrystal nano particle of the regular square of controlling.
The preparation method of the perovskite structure lead titanate monocrystal nano particle of regular square, comprises following processing step:
1) tetrabutyl titanate is dissolved in ethylene glycol monomethyl ether, being made into concentration is the tetrabutyl titanate solution of 0.51mol/L, under whipped state, be 30% ammonia soln to splashing into massfraction in tetrabutyl titanate solution, make tetrabutyl titanate hydrolysis precipitation, filter, washing, obtains titanium precipitation;
2) lead nitrate, potassium hydroxide and polyvinylpyrrolidone are dissolved in respectively to deionized water, the polyvinylpyrrolidone aqueous solution that the lead nitrate aqueous solution that configuration concentration is 0.55mol/L, the potassium hydroxide aqueous solution that concentration is 0.5mol/L and concentration are 2g/L;
3) by the lead nitrate aqueous solution making above, potassium hydroxide aqueous solution and the polyvinylpyrrolidone aqueous solution by volume 1:1:0.05 ~ 1 and titanium precipitation join in the reactor inner bag of tetrafluoroethylene, regulate its volume to reach 80% of reactor inner bag volume with deionized water, stir at least 10-30min, obtain suspension liquid;
4) the reactor inner bag that step 3) is disposed to reaction mass is placed in reactor, and sealing, at 180-200
oat C temperature, carry out, after hydro-thermal reaction 3-48h, being placed in air and being naturally cooled to room temperature;
5) reaction product in step 4) reactor is taken out, filter, with deionized water and dehydrated alcohol cleaning, dry, obtain the perovskite structure lead titanate monocrystal nano particle of regular square.
The purity of the chemical reagent such as the tetrabutyl titanate, lead nitrate, potassium hydroxide and the polyvinylpyrrolidone that adopt in the present invention is all not less than chemical pure.
The present invention adopts polymer assisting alcohol-hydrothermal method, utilize mineralizer potassium hydroxide to promote product crystallization, utilize coating materials polyvinylpyrrolidone to make structure directing agent and dispersion agent, at 180-200 DEG C of temperature, carry out hydro-thermal reaction, reaction product after filtration, clean, dry, obtain the perovskite structure lead titanate monocrystal nano particle of regular square.Technological process of the present invention is simple, is easy to control, and pollution-free, cost is low, is easy to scale operation; The perovskite structure lead titanate monocrystal nano particle purity of the regular square making is high, pattern rule, size homogeneous.
Brief description of the drawings
Fig. 1 is the XRD figure spectrum of the perovskite structure lead titanate monocrystal nano particle of regular square;
Fig. 2 is the SEM picture of the perovskite structure lead titanate monocrystal nano particle of regular square;
Fig. 3 is the high-resolution-ration transmission electric-lens figure of the perovskite structure lead titanate monocrystal nano particle of regular square.
Embodiment
Below in conjunction with embodiment, the inventive method is described in further detail.
1) tetrabutyl titanate is dissolved in ethylene glycol monomethyl ether, being made into concentration is the tetrabutyl titanate solution of 0.51mol/L, under whipped state, be 30% ammonia soln to splashing into massfraction in tetrabutyl titanate solution, make tetrabutyl titanate hydrolysis precipitation, filter, washing, obtains titanium precipitation;
2) lead nitrate, potassium hydroxide and polyvinylpyrrolidone are dissolved in respectively to deionized water, the polyvinylpyrrolidone aqueous solution that the lead nitrate aqueous solution that configuration concentration is 0.55mol/L, the potassium hydroxide aqueous solution that concentration is 0.5mol/L and concentration are 2g/L;
3) by the lead nitrate aqueous solution making above, potassium hydroxide aqueous solution and the polyvinylpyrrolidone aqueous solution by volume 1:1:0.8 and titanium precipitation join in the reactor inner bag of tetrafluoroethylene, regulate its volume to reach 80% of reactor inner bag volume with deionized water, stir 20min, obtain suspension liquid;
4) the reactor inner bag that step 3) is disposed to reaction mass is placed in reactor, and sealing, 200
oat C temperature, carry out, after hydro-thermal reaction 10h, being placed in air and being naturally cooled to room temperature;
5) reaction product in step 4) reactor is taken out, filter, with deionized water and dehydrated alcohol cleaning, dry, obtain the perovskite structure lead titanate monocrystal nano particle of regular square.
The XRD figure of the perovskite structure lead titanate monocrystal nano particle of regular square is composed as shown in Figure 1, and its diffraction peak corresponds to pure Tetragonal lead titanate.As shown in Figure 2, nano particle is regular square to the shape appearance figure of product, and size is about 200nm.Nano particle purity is high, pattern rule, size homogeneous.Fig. 3 is the high-resolution-ration transmission electric-lens figure of product, can show that by figure the perovskite structure lead titanate nano particle making is single crystal structure.Spacing 0.227nm and 0.391nm, respectively corresponding (111) and (100) crystal face.
Embodiment 2
1) tetrabutyl titanate is dissolved in ethylene glycol monomethyl ether, being made into concentration is the tetrabutyl titanate solution of 0.51mol/L, under whipped state, be 30% ammonia soln to splashing into massfraction in tetrabutyl titanate solution, make tetrabutyl titanate hydrolysis precipitation, filter, washing, obtains titanium precipitation;
2) lead nitrate, potassium hydroxide and polyvinylpyrrolidone are dissolved in respectively to deionized water, the polyvinylpyrrolidone aqueous solution that the lead nitrate aqueous solution that configuration concentration is 0.55mol/L, the potassium hydroxide aqueous solution that concentration is 0.5mol/L and concentration are 2g/L;
3) by the lead nitrate aqueous solution making above, potassium hydroxide aqueous solution and the polyvinylpyrrolidone aqueous solution by volume 1:1:0.05 and titanium precipitation join in the reactor inner bag of tetrafluoroethylene, regulate its volume to reach 80% of reactor inner bag volume with deionized water, stir 10min, obtain suspension liquid;
4) the reactor inner bag that step 3) is disposed to reaction mass is placed in reactor, and sealing, 180
oat C temperature, carry out, after hydro-thermal reaction 48h, being placed in air and being naturally cooled to room temperature;
5) reaction product in step 4) reactor is taken out, filter, with deionized water and dehydrated alcohol cleaning, dry, obtain the perovskite structure lead titanate monocrystal nano particle of regular square.
Embodiment 3
1) tetrabutyl titanate is dissolved in ethylene glycol monomethyl ether, being made into concentration is the tetrabutyl titanate solution of 0.51mol/L, under whipped state, be 30% ammonia soln to splashing into massfraction in tetrabutyl titanate solution, make tetrabutyl titanate hydrolysis precipitation, filter, washing, obtains titanium precipitation;
2) lead nitrate, potassium hydroxide and polyvinylpyrrolidone are dissolved in respectively to deionized water, the polyvinylpyrrolidone aqueous solution that the lead nitrate aqueous solution that configuration concentration is 0.55mol/L, the potassium hydroxide aqueous solution that concentration is 0.5mol/L and concentration are 2g/L;
3) by the lead nitrate aqueous solution making above, potassium hydroxide aqueous solution and the polyvinylpyrrolidone aqueous solution by volume 1:1:1 and titanium precipitation join in the reactor inner bag of tetrafluoroethylene, regulate its volume to reach 80% of reactor inner bag volume with deionized water, stir 30min, obtain suspension liquid;
4) the reactor inner bag that step 3) is disposed to reaction mass is placed in reactor, and sealing, 200
oat C temperature, carry out, after hydro-thermal reaction 3h, being placed in air and being naturally cooled to room temperature;
5) reaction product in step 4) reactor is taken out, filter, with deionized water and dehydrated alcohol cleaning, dry, obtain the perovskite structure lead titanate monocrystal nano particle of regular square.
Embodiment 4
1) tetrabutyl titanate is dissolved in ethylene glycol monomethyl ether, being made into concentration is the tetrabutyl titanate solution of 0.51mol/L, under whipped state, be 30% ammonia soln to splashing into massfraction in tetrabutyl titanate solution, make tetrabutyl titanate hydrolysis precipitation, filter, washing, obtains titanium precipitation;
2) lead nitrate, potassium hydroxide and polyvinylpyrrolidone are dissolved in respectively to deionized water, the polyvinylpyrrolidone aqueous solution that the lead nitrate aqueous solution that configuration concentration is 0.55mol/L, the potassium hydroxide aqueous solution that concentration is 0.5mol/L and concentration are 2g/L;
3) by the lead nitrate aqueous solution making above, potassium hydroxide aqueous solution and the polyvinylpyrrolidone aqueous solution by volume 1:1:0.5 and titanium precipitation join in the reactor inner bag of tetrafluoroethylene, regulate its volume to reach 80% of reactor inner bag volume with deionized water, stir 20min, obtain suspension liquid;
4) the reactor inner bag that step 3) is disposed to reaction mass is placed in reactor, and sealing, 180
oat C temperature, carry out, after hydro-thermal reaction 8h, being placed in air and being naturally cooled to room temperature;
5) reaction product in step 4) reactor is taken out, filter, with deionized water and dehydrated alcohol cleaning, dry, obtain the perovskite structure lead titanate monocrystal nano particle of regular square.
Claims (2)
1. a preparation method for the perovskite structure lead titanate monocrystal nano particle of regular square, is characterized in that comprising the following steps:
1) tetrabutyl titanate is dissolved in ethylene glycol monomethyl ether, being made into concentration is the tetrabutyl titanate solution of 0.51mol/L, under whipped state, be 30% ammonia soln to splashing into massfraction in tetrabutyl titanate solution, make tetrabutyl titanate hydrolysis precipitation, filter, washing, obtains titanium precipitation;
2) lead nitrate, potassium hydroxide and polyvinylpyrrolidone are dissolved in respectively to deionized water, the polyvinylpyrrolidone aqueous solution that the lead nitrate aqueous solution that configuration concentration is 0.55mol/L, the potassium hydroxide aqueous solution that concentration is 0.5mol/L and concentration are 2g/L;
3) by the lead nitrate aqueous solution making above, potassium hydroxide aqueous solution and the polyvinylpyrrolidone aqueous solution by volume 1:1:0.05 ~ 1 and titanium precipitation join in the reactor inner bag of tetrafluoroethylene, regulate its volume to reach 80% of reactor inner bag volume with deionized water, stir at least 10-30min, obtain suspension liquid;
4) the reactor inner bag that step 3) is disposed to reaction mass is placed in reactor, and sealing, at 180-200
oat C temperature, carry out, after hydro-thermal reaction 3-48h, being placed in air and being naturally cooled to room temperature;
5) reaction product in step 4) reactor is taken out, filter, with deionized water and dehydrated alcohol cleaning, dry, obtain the perovskite structure lead titanate monocrystal nano particle of regular square.
2. the preparation method of the perovskite structure lead titanate monocrystal nano particle of regular square according to claim 1, is characterized in that the purity of described tetrabutyl titanate, lead nitrate, potassium hydroxide and polyvinylpyrrolidone is all not less than chemical pure.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106701072A (en) * | 2016-12-22 | 2017-05-24 | 中国科学院合肥物质科学研究院 | Europium-doped calcium titanate nano cube fluorescent powder and preparation method thereof |
| CN108328650A (en) * | 2018-03-20 | 2018-07-27 | 浙江理工大学 | One one-step hydro-thermal synthesis method of one-dimensional Perovskite Phase lead titanates nanofiber |
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| CN102139913A (en) * | 2011-04-20 | 2011-08-03 | 浙江大学 | Method for preparing lead titanate nanoparticles |
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Patent Citations (4)
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| JP2008230872A (en) * | 2007-03-19 | 2008-10-02 | Tokyo Institute Of Technology | Cube-shaped nanoparticle and its manufacturing method |
| CN102139913A (en) * | 2011-04-20 | 2011-08-03 | 浙江大学 | Method for preparing lead titanate nanoparticles |
| CN102925979A (en) * | 2012-11-08 | 2013-02-13 | 浙江大学 | Method for preparing perovskite lead titanate crystal nanosheet |
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Cited By (3)
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| CN106701072A (en) * | 2016-12-22 | 2017-05-24 | 中国科学院合肥物质科学研究院 | Europium-doped calcium titanate nano cube fluorescent powder and preparation method thereof |
| CN106701072B (en) * | 2016-12-22 | 2019-02-19 | 中国科学院合肥物质科学研究院 | Europium-doped calcium titanate nano square fluorescent powder and preparation method thereof |
| CN108328650A (en) * | 2018-03-20 | 2018-07-27 | 浙江理工大学 | One one-step hydro-thermal synthesis method of one-dimensional Perovskite Phase lead titanates nanofiber |
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Application publication date: 20140625 |