CN102140694A - Preparation method of barium-doped lead titanate monocrystal nano fiber with one-dimensional column structure - Google Patents
Preparation method of barium-doped lead titanate monocrystal nano fiber with one-dimensional column structure Download PDFInfo
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- CN102140694A CN102140694A CN 201110066126 CN201110066126A CN102140694A CN 102140694 A CN102140694 A CN 102140694A CN 201110066126 CN201110066126 CN 201110066126 CN 201110066126 A CN201110066126 A CN 201110066126A CN 102140694 A CN102140694 A CN 102140694A
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- barium
- columnar structure
- titanium
- potassium hydroxide
- polyvinyl alcohol
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Abstract
The invention relates to a preparation method of a barium-doped lead titanate monocrystal nano fiber with a one-dimensional column structure, which adopts a hydro-thermal reaction method comprising the steps of: with ethylene glycol monomethyl ether as a solvent for dissolving titanium ions, precipitating titanium ions by using aqueous ammonia as a precipitator; controlling the growing direction by utilizing polyving akohol as a surface modifier; and finally promoting crystallization by utilizing potassium hydroxide as a mineralizer to synthesize the barium-doped lead titanate monocrystal nano fiber with the one-dimensional column structure. The preparation method of the barium-doped lead titanate monocrystal nano fiber with the one-dimensional column structure has a simple technical process and low cost, is easy to control and produce in batch, and does not cause pollution; and the prepared barium-doped lead titanate monocrystal nano fiber with the one-dimensional column structure has high purity and good dispersibility.
Description
Technical field
The present invention relates to a kind of one dimension columnar structure barium Doped with Titanium lead plumbate nanometer monocrystalline fiber preparation method, belong to field of inorganic nonmetallic material.
Background technology
The lead titanate of tradition perovskite structure is one of the most representative ferroelectric oxide material, has important theory and is worth for the ferroelectricity origin of understanding and cognition perovskite oxide material, the novel ferroelectric material of synthetic design.Lead titanate has excellent ferroelectric, piezoelectricity, dielectric properties, therefore has a wide range of applications at electronic applications such as non-volatility ferroelectric storer, piezoelectric transducer, pyroelectricity sensor and high dielectric capacitor.Barium titanate is the ABO that finds the earliest
3The typical ferroelectric material of type perovskite crystal structure owing to have high-k, low-dielectric loss, is widely used in electronic components such as laminated ceramic capacitor, thermistor, photoelectric device.The formed sosoloid of lead titanate and barium titanate also becomes scientist's research emphasis.
Zhejiang University uses the polymer assisting alcohol-hydrothermal method to make lead titanate monocrystal nano fiber (Zhaohui Ren, Gang Xu, the Yong Liu of one dimension columnar structure first, Xiao Wei, Yihan Zhu, Xiaobin Zhang, Guanglie Lv, Youwen Wang, Yuewu Zeng, Piyi Du, Wenjian Weng, Ge Shen, J. Z. Jiang and Gaorong Han, PbTiO
3Nanofibers with Edge-Shared TiO
6Octahedra, 2010,132 (16), 5572-5573.).The lead titanate crystal of this structure, its titanyl octahedral body are to be connected to form the one dimension columnar structure by being total to the limit.And the barium doping enters one dimension columnar structure lead titanate, obtains the nanometer monocrystalline fiber of one dimension columnar structure barium Doped with Titanium lead plumbate, there is no relevant preparation method and technology report both at home and abroad.One dimension columnar structure barium Doped with Titanium lead plumbate nanofiber is showing very excellent performance aspect optical property and the piezoelectric property, and can bending phenomenon occurs under electric field action, be the very excellent material of a kind of performance, have very big researching value and application potential.
Summary of the invention
The object of the present invention is to provide a kind of technology simple, the one dimension columnar structure barium Doped with Titanium lead plumbate nanometer monocrystalline fiber preparation method that process is easy to control.
One dimension columnar structure barium Doped with Titanium lead plumbate nanometer monocrystalline fiber preparation method of the present invention comprises following processing step:
1) by the chemical formula Pb that desires synthetic one dimension columnar structure barium Doped with Titanium lead plumbate nanometer monocrystalline fiber
1-xBa
xTiO
3Metering, 0.001≤X≤0.15 takes by weighing plumbic acetate and barium acetate and is dissolved in the deionized water jointly; Regulate Pb
2+Ionic concn is 0.4995-0.425 mol/L; Ba
2+Ionic concn is 0.0005-0.075mol/L;
2) butyl (tetra) titanate is dissolved in ethylene glycol monomethyl ether, the Ti in the regulator solution
4+Ionic concn is 0.25-1mol/L, under the whipped state, splashes into the ammonia soln of mass concentration 30%, makes the butyl (tetra) titanate hydrolytic precipitation, filter, and washing, the oxyhydroxide that obtains titanium precipitates;
3) potassium hydroxide and polyvinyl alcohol are dissolved in deionized water respectively, configuration concentration is that potassium hydroxide aqueous solution and the concentration of 0.5-5mol/L is the polyvinyl alcohol water solution of 2-8g/L;
4) oxyhydroxide precipitation, potassium hydroxide aqueous solution and the polyvinyl alcohol water solution of the plumbic acetate that makes more than the general and the barium acetate aqueous solution, titanium join in the reactor inner bag of tetrafluoroethylene, regulating its volume with deionized water is 2/3 ~ 4/5 of reactor volume, stirring is no less than 5 minutes, obtains suspension;
5) the reactor inner bag that step 4) is disposed reaction mass places reactor, and is airtight, places 190-200
oBe incubated in the stove of C, react after 8-12 hour, place air to be cooled to room temperature naturally, take out reaction product, filter, use washed with de-ionized water, oven dry obtains one dimension columnar structure barium Doped with Titanium lead plumbate nanometer monocrystalline fiber.
Plumbic acetate of the present invention, barium acetate, butyl (tetra) titanate, potassium hydroxide and polyvinyl alcohol purity all are not less than chemical pure.
The present invention adopts hydro-thermal reaction, with the solvent of ethylene glycol monomethyl ether as the dissolving titanium ion, utilizes ammoniacal liquor as precipitation agent precipitated titanium ion; Utilize the coating materials polyvinyl alcohol to realize the regulation and control of the direction of growth; Utilize mineralizer potassium hydroxide to promote crystallization at last, realize the synthetic of one dimension columnar structure barium Doped with Titanium lead plumbate nanometer monocrystalline fiber.Technological process of the present invention is simple, is easy to control, and pollution-free, cost is low, is easy to scale operation; The one dimension columnar structure barium Doped with Titanium lead plumbate nanometer monocrystalline fiber that makes, purity height, good dispersity.
Description of drawings
Fig. 1 is one dimension columnar structure Pb
0.9Ba
0.1TiO
3The XRD figure spectrum of nanofiber.
Fig. 2 is one dimension columnar structure Pb
0.9Ba
0.1TiO
3The scanning electron microscope picture of nanofiber.
Fig. 3 is one dimension columnar structure Pb
0.85Ba
0.15TiO
3The energy spectrogram of nanofiber.
Embodiment
Below in conjunction with embodiment the inventive method is described in further detail.
Embodiment 1
1) by the chemical formula Pb that desires synthetic one dimension columnar structure barium Doped with Titanium lead plumbate nanometer monocrystalline fiber
1-xBa
xTiO
3(X=0.001) metering takes by weighing plumbic acetate and barium acetate and is dissolved in jointly in the deionized water, obtains transparent liquid; Regulate Pb
2+Ionic concn is 0.4995mol/L, Ba
2+Ionic concn is 0.0005 mol/L;
2) butyl (tetra) titanate is dissolved in ethylene glycol monomethyl ether, the Ti in the regulator solution
4+Ionic concn is 0.25mol/L.Under the whipped state, splash into the ammonia soln of 2ml mass concentration 30% in the butyl (tetra) titanate light yellow transparent liquid that makes, make the butyl (tetra) titanate hydrolytic precipitation, filter, ammonia radical ion is removed in washing, obtains the oxyhydroxide precipitation of titanium;
3) potassium hydroxide and polyvinyl alcohol are dissolved in deionized water respectively, configuration concentration is that potassium hydroxide aqueous solution and the concentration of 0.5mol/L is the polyvinyl alcohol water solution of 8g/L;
4) oxyhydroxide precipitation, potassium hydroxide aqueous solution and the polyvinyl alcohol water solution of the plumbic acetate that makes more than the general and the barium acetate aqueous solution, titanium join in the reactor inner bag of tetrafluoroethylene, regulating its volume with deionized water is 2/3 of reactor volume, magnetic stirrer 5 minutes obtains suspension;
5) the reactor inner bag that step 4) is disposed reaction mass places reactor, and is airtight, places 200
oBe incubated in the stove of C, react after 12 hours, place air to be cooled to room temperature naturally, take out reaction product, filter, use washed with de-ionized water, potassium hydroxide is fully separated with synthetic one dimension columnar structure barium Doped with Titanium lead plumbate nanometer monocrystalline fiber with polyvinyl alcohol, and oven dry obtains one dimension columnar structure Pb
0.999Ba
0.001TiO
3The nanometer monocrystalline fiber.
1) by the chemical formula Pb that desires synthetic one dimension columnar structure barium Doped with Titanium lead plumbate nanometer monocrystalline fiber
1-xBa
xTiO
3(X=0.1) metering takes by weighing plumbic acetate and barium acetate and is dissolved in jointly in the deionized water, obtains transparent liquid; Regulate Pb
2+Ionic concn is 0.45mol/L; Ba
2+Ionic concn is 0.05mol/L;
2) butyl (tetra) titanate is dissolved in ethylene glycol monomethyl ether, the Ti in the regulator solution
4+Ionic concn is 0.5mol/L.Under the whipped state, splash into the ammonia soln of 2ml mass concentration 30% in the butyl (tetra) titanate light yellow transparent liquid that makes, make the butyl (tetra) titanate hydrolytic precipitation, filter, ammonia radical ion is removed in washing, obtains the oxyhydroxide precipitation of titanium;
3) potassium hydroxide and polyvinyl alcohol are dissolved in deionized water respectively, configuration concentration is that potassium hydroxide aqueous solution and the concentration of 1mol/L is the polyvinyl alcohol water solution of 6g/L;
4) oxyhydroxide precipitation, potassium hydroxide aqueous solution and the polyvinyl alcohol water solution of the plumbic acetate that makes more than the general and the barium acetate aqueous solution, titanium join in the reactor inner bag of tetrafluoroethylene, regulating its volume with deionized water is 3/4 of reactor volume, magnetic stirrer 5 minutes obtains suspension;
5) the reactor inner bag that step 4) is disposed reaction mass places reactor, and is airtight, places 200
oBe incubated in the stove of C, react after 8 hours, place air to be cooled to room temperature naturally, take out reaction product, filter, use washed with de-ionized water, potassium hydroxide is fully separated with synthetic one dimension columnar structure barium Doped with Titanium lead plumbate nanometer monocrystalline fiber with polyvinyl alcohol, and oven dry obtains one dimension columnar structure Pb
0.9Ba
0.1TiO
3The nanometer monocrystalline fiber, its XRD figure spectrum is seen Fig. 1, the nanofiber that is obtained is pure one dimension columnar structure as seen from the figure, and the nanofiber shape appearance figure that is obtained is seen Fig. 2, consistent with the XRD figure spectrum that is obtained, be single nanofiber, Fig. 1 and Fig. 2 are in conjunction with showing the one dimension columnar structure barium Doped with Titanium lead plumbate nanometer monocrystalline fiber fineness height that this method is prepared, good dispersity.
Embodiment 3
1) by the chemical formula Pb that desires synthetic one dimension columnar structure lead barium titanate nanometer monocrystalline pipe
1-xBa
xTiO
3(X=0.15) metering takes by weighing plumbic acetate and barium acetate and is dissolved in jointly in the deionized water, obtains transparent liquid; Regulate Pb
2+Ionic concn is 0.425mol/L; Ba
2+Ionic concn is 0.075mol/L;
2) butyl (tetra) titanate is dissolved in ethylene glycol monomethyl ether, the Ti in the regulator solution
4+Ionic concn is 1mol/L.Under the whipped state, splash into the ammonia soln of 2ml mass concentration 30% in the butyl (tetra) titanate light yellow transparent liquid that makes, make the butyl (tetra) titanate hydrolytic precipitation, filter, ammonia radical ion is removed in washing, obtains the oxyhydroxide precipitation of titanium;
3) potassium hydroxide and polyvinyl alcohol are dissolved in deionized water respectively, configuration concentration is that potassium hydroxide aqueous solution and the concentration of 2mol/L is the polyvinyl alcohol water solution of 2g/L;
4) oxyhydroxide white precipitate, potassium hydroxide aqueous solution and the polyvinyl alcohol water solution of the plumbic acetate that makes more than the general and the barium acetate aqueous solution, titanium join in the reactor inner bag of tetrafluoroethylene, regulating its volume with deionized water is 4/5 of reactor volume, magnetic stirrer 5 minutes obtains suspension;
5) the reactor inner bag that step 4) is disposed reaction mass places reactor, and is airtight, places 190
oBe incubated in the stove of C, react after 10 hours, place air to be cooled to room temperature naturally, take out reaction product, filter, use washed with de-ionized water, potassium hydroxide is fully separated with synthetic one dimension columnar structure barium Doped with Titanium lead plumbate nanometer monocrystalline fiber with polyvinyl alcohol, and oven dry obtains one dimension columnar structure Pb
0.85Ba
0.15TiO
3The nanometer monocrystalline fiber.Prepared nanofiber can be seen Fig. 3 by spectrogram, and the composition of nanofiber is Pb as seen from the figure, Ba, and Ti, four kinds of elements of O prove absolutely that the Ba ion doping has entered one dimension columnar structure PbTiO
3Lattice.
Claims (2)
1. one dimension columnar structure barium Doped with Titanium lead plumbate nanometer monocrystalline fiber preparation method is characterized in that comprising following processing step:
1) by the chemical formula Pb that desires synthetic one dimension columnar structure barium Doped with Titanium lead plumbate nanometer monocrystalline fiber
1-xBa
xTiO
3Metering, 0.001≤X≤0.15 takes by weighing plumbic acetate and barium acetate and is dissolved in the deionized water jointly; Regulate Pb
2+Ionic concn is 0.4995-0.425 mol/L; Ba
2+Ionic concn is 0.0005-0.075mol/L;
2) butyl (tetra) titanate is dissolved in ethylene glycol monomethyl ether, the Ti in the regulator solution
4+Ionic concn is 0.25-1mol/L, under the whipped state, splashes into the ammonia soln of mass concentration 30%, makes the butyl (tetra) titanate hydrolytic precipitation, filter, and washing, the oxyhydroxide that obtains titanium precipitates;
3) potassium hydroxide and polyvinyl alcohol are dissolved in deionized water respectively, configuration concentration is that potassium hydroxide aqueous solution and the concentration of 0.5-5mol/L is the polyvinyl alcohol water solution of 2-8g/L;
4) oxyhydroxide precipitation, potassium hydroxide aqueous solution and the polyvinyl alcohol water solution of the plumbic acetate that makes more than the general and the barium acetate aqueous solution, titanium join in the reactor inner bag of tetrafluoroethylene, regulating its volume with deionized water is 2/3 ~ 4/5 of reactor volume, stirring is no less than 5 minutes, obtains suspension;
5) the reactor inner bag that step 4) is disposed reaction mass places reactor, and is airtight, places 190-200
oBe incubated in the stove of C, react after 8-12 hour, place air to be cooled to room temperature naturally, take out reaction product, filter, use washed with de-ionized water, oven dry obtains one dimension columnar structure barium Doped with Titanium lead plumbate nanometer monocrystalline fiber.
2. according to claims 1 described one dimension columnar structure barium Doped with Titanium lead plumbate nanometer monocrystalline fiber preparation method, it is characterized in that described plumbic acetate, barium acetate, butyl (tetra) titanate, potassium hydroxide and polyvinyl alcohol purity all are not less than chemical pure.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN113279062A (en) * | 2021-05-17 | 2021-08-20 | 浙江大学 | Nickel-doped lead titanate single crystal film and preparation and application thereof |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2005069858A2 (en) * | 2004-01-16 | 2005-08-04 | Northern Illinois University | Nano-composite piezoelectric material |
| CN1818150A (en) * | 2005-12-21 | 2006-08-16 | 浙江大学 | Production of single-crystal nano meter four-phase rod with lead zirconate titanate and perof skite |
| CN1935659A (en) * | 2006-10-23 | 2007-03-28 | 浙江大学 | Method for preparing lead zirconatetianate nano powder |
| KR20090126455A (en) * | 2008-06-04 | 2009-12-09 | 한양대학교 산학협력단 | Manufacturing method of pblatio3 nano powder |
| CN101618889A (en) * | 2009-08-03 | 2010-01-06 | 浙江大学 | Method for preparing lead titanate nano column automatically assembled by perovskite structure nano pieces |
| CN101619494A (en) * | 2009-08-03 | 2010-01-06 | 浙江大学 | Method for preparing perovskite structure lead titanate monocrystal nano rod |
| CN101831710A (en) * | 2010-05-28 | 2010-09-15 | 浙江大学 | Method for preparing lead titanate monocrystal nanometer branch crystal with perovskite structure |
| CN101830499A (en) * | 2010-05-21 | 2010-09-15 | 浙江大学 | Lead titanate nanotube with one-dimensional crystal structure and preparation method thereof |
-
2011
- 2011-03-18 CN CN 201110066126 patent/CN102140694A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2005069858A2 (en) * | 2004-01-16 | 2005-08-04 | Northern Illinois University | Nano-composite piezoelectric material |
| CN1818150A (en) * | 2005-12-21 | 2006-08-16 | 浙江大学 | Production of single-crystal nano meter four-phase rod with lead zirconate titanate and perof skite |
| CN1935659A (en) * | 2006-10-23 | 2007-03-28 | 浙江大学 | Method for preparing lead zirconatetianate nano powder |
| KR20090126455A (en) * | 2008-06-04 | 2009-12-09 | 한양대학교 산학협력단 | Manufacturing method of pblatio3 nano powder |
| CN101618889A (en) * | 2009-08-03 | 2010-01-06 | 浙江大学 | Method for preparing lead titanate nano column automatically assembled by perovskite structure nano pieces |
| CN101619494A (en) * | 2009-08-03 | 2010-01-06 | 浙江大学 | Method for preparing perovskite structure lead titanate monocrystal nano rod |
| CN101830499A (en) * | 2010-05-21 | 2010-09-15 | 浙江大学 | Lead titanate nanotube with one-dimensional crystal structure and preparation method thereof |
| CN101831710A (en) * | 2010-05-28 | 2010-09-15 | 浙江大学 | Method for preparing lead titanate monocrystal nanometer branch crystal with perovskite structure |
Non-Patent Citations (2)
| Title |
|---|
| 《四川大学学报》 20051031 郑凯泓等 水热合成PbTiO3纳米线 217-219 1-2 第42卷, 第2期 * |
| 《无机化学学报》 20061231 杨小勤等 聚合物对锆钛酸铅纳米晶须形貌的影响 2193-2196 1-2 第22卷, 第12期 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN113279062A (en) * | 2021-05-17 | 2021-08-20 | 浙江大学 | Nickel-doped lead titanate single crystal film and preparation and application thereof |
| CN113279062B (en) * | 2021-05-17 | 2022-07-08 | 浙江大学 | Nickel-doped lead titanate single crystal film and preparation and application thereof |
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Application publication date: 20110803 |