CN106892450A - One kind synthesizes PbTiO by La ion dopings3The method of disk - Google Patents

One kind synthesizes PbTiO by La ion dopings3The method of disk Download PDF

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CN106892450A
CN106892450A CN201710121644.XA CN201710121644A CN106892450A CN 106892450 A CN106892450 A CN 106892450A CN 201710121644 A CN201710121644 A CN 201710121644A CN 106892450 A CN106892450 A CN 106892450A
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pbtio
disk
deionized water
synthesized
ion
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CN106892450B (en
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肖珍
张嘉玮
徐时清
雷磊
王焕平
张军杰
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China Jiliang University
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G23/00—Compounds of titanium
    • C01G23/003—Titanates
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/80—Particles consisting of a mixture of two or more inorganic phases

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Inorganic Chemistry (AREA)
  • Compositions Of Oxide Ceramics (AREA)

Abstract

PbTiO is synthesized by La ion dopings the present invention relates to one kind3The method of disk.Using the aqueous solution of the aqueous solution of Ti and Pb/La as reaction mass, crystallization is promoted using mineralizer potassium hydroxide, introduce rare earth La ion to regulate and control pattern, the disc-shaped PbTiO of polymolecularity is synthesized using hydro-thermal method3, its diameter/thickness ratio is up to 20 ~ 50.Preparation process is simple of the present invention, it is easy to control, and it is pollution-free, it is with low cost, it is easy to accomplish large-scale production.

Description

One kind synthesizes PbTiO by La ion dopings3The method of disk
Technical field
PbTiO is synthesized by La ion dopings the present invention relates to one kind3The method of disk, belongs to Inorganic Non-metallic Materials neck Domain.
Background technology
Perovskite ferroelectric oxide has the performances such as excellent piezoelectricity, ferroelectricity and pyroelectric property, in scientific research and work There is important researching value in the fields such as Cheng Yingyong.PbTiO3, a kind of typical perovskite structure ferroelectric oxide, its Curie's temperature Degree about 490oC.When less than Curie point, PbTiO3With excellent ferroelectricity, piezoelectric and dielectric properties, spontaneous polarization is strong Degree is big, therefore always as piezoelectricity and the leiomyoma cells in ferroelectric material field, in non-volatility ferroelectric memory, piezoelectric sensing Had a wide range of applications in the preparations of microelectronic component such as device, pyroelectricity sensor and dielectric capacitor high.
With the miniaturization of electronic device, monocrystalline two dimension ferroelectric oxide turns into study hotspot.Research shows, ultra-thin list Brilliant BaTiO3So that the thickness of monocrystalline capacitor is reduced to 65 nm；Additionally, theoretical research shows, the ferroelectricity of ferroelectric nano disk is deposited Storage density reaches every square feet 60 × 1012 bits.However, PbTiO3Crystal structure be Tetragonal, the easy cubic particle of generation Shape.Prepared on a large scale using chemical method diameter/thickness high than ferroelectric nano disk it is still less at home and abroad.
The content of the invention
It is an object of the invention to provide a kind of process is simple, it is easy to control by La ion dopings synthesize PbTiO3Circle The method of piece.
It is of the invention that PbTiO is synthesized by La ion dopings3The method of disk, comprises the following steps：
1) by the La to be synthesized doping PbTiO3The molecular formula Pb of disk1-xLaxTiO3Metering, X=0.001-0.2 weigh Pb sources It is dissolved in deionized water jointly with La sources, forms the aqueous solution of Pb/La ions, regulation（Pb2++La3+)/Ti4+Ion concentration is 1~1.5；
2) P25 is dissolved in deionized water, adjusts Ti4+Ion concentration is 0.2 ~ 0.4 mol/L；Under stirring, hydrogen is added Potassium oxide, makes potassium hydroxide concentration in the solution be 5 ~ 8 mol/L；
3) under stirring, by step 1) Pb/La deionized water solutions drop to step 2) solution in, persistently stir 4-6 it is small When, form the oxyhydroxide mixing suspension of Ti and Pb/La；
4) by step 3) obtained in mixing suspension be added in hydrothermal reaction kettle inner bag, and with deionized water instrumentality material body Product is the 1/3 ~ 4/5 of reactor inner bag volume, and stirring makes it be sufficiently mixed uniformly；
5）By through step 4) the reactor inner bag equipped with precursor pulp be placed in reactor, seal, at 170 ~ 210 DEG C protect Temperature carries out hydro-thermal process in 10 ~ 20 hours, then allows reactor to naturally cool to room temperature, takes out reactant, filtering, spend successively from Sub- water, ethanol cyclic washing product, filtering, drying.
In the present invention, described La sources can be lanthanum nitrate or lanthanum acetate.
In the present invention, described Pb sources can be plumbi nitras or lead acetate.
The present invention promotes crystalline substance using the aqueous solution of Ti and the aqueous solution of Pb/La as reaction mass using mineralizer potassium hydroxide Change, PbTiO is regulated and controled by introducing rare earth La ion3Pattern, form it into the two-dimentional ferroelectricity disk with high storage density, Diameter/thickness ratio is up to 20 ~ 50.Preparation process is simple of the present invention, process is easily controllable, and pollution-free, with low cost, it is easy to real Existing large-scale production.
Brief description of the drawings
Fig. 1 is the La doping PbTiO prepared by embodiment 13The XRD of disk.
Fig. 2 is the La doping PbTiO prepared by embodiment 23The SEM figures of disk.
Specific implementation method
Embodiment 1
1) by the La to be synthesized doping PbTiO3The molecular formula Pb of disk1-xLaxTiO3（X=0.05）Metering, weigh plumbi nitras and Lanthanum nitrate is dissolved in deionized water jointly, forms the aqueous solution of Pb/La ions, regulation（Pb2++La3+)/Ti4+Ion concentration is 1.2；
2) P25 is dissolved in deionized water, adjusts Ti4+Ion concentration is 0.25mol/L；Under stirring, hydroxide is added Potassium, makes potassium hydroxide concentration in the solution be 6 mol/L；
3) under stirring, by step 1) Pb/La deionized water solutions drop to step 2) solution in, persistently stir 5 small When, form the oxyhydroxide mixing suspension of Ti and Pb/La；
4) by step 3) obtained in mixing suspension be added in hydrothermal reaction kettle inner bag, and with deionized water instrumentality material body Product is the 4/5 of reactor inner bag volume, and stirring makes it be sufficiently mixed uniformly；
5）The reactor inner bag that will be equipped with precursor pulp is placed in reactor, sealing, and insulation enters water-filling in 12 hours at 200 DEG C Heat treatment, then allows reactor to naturally cool to room temperature, takes out reactant, filtering, successively with deionized water, ethanol cyclic washing Product, filtering, drying.Its product X RD figures are shown in Fig. 1.
Embodiment 2
1) by the La to be synthesized doping PbTiO3The molecular formula Pb of disk1-xLaxTiO3（X=0.001）Metering, weigh plumbi nitras and Lanthanum acetate is dissolved in deionized water jointly, forms the aqueous solution of Pb/La ions, regulation（Pb2++La3+)/Ti4+Ion concentration is 1；
2) P25 is dissolved in deionized water, adjusts Ti4+Ion concentration is 0.25 mol/L；Under stirring, hydroxide is added Potassium, makes potassium hydroxide concentration in the solution be 7 mol/L；
3) under stirring, by step 1) Pb/La deionized water solutions drop to step 2) solution in, persistently stir 4 small When, form the oxyhydroxide mixing suspension of Ti and Pb/La；
4) by step 3) obtained in mixing suspension be added in hydrothermal reaction kettle inner bag, and with deionized water instrumentality material body Product is the 4/5 of reactor inner bag volume, and stirring makes it be sufficiently mixed uniformly；
5）The reactor inner bag that will be equipped with precursor pulp is placed in reactor, sealing, and insulation enters water-filling in 10 hours at 210 DEG C Heat treatment, then allows reactor to naturally cool to room temperature, takes out reactant, filtering, successively with deionized water, ethanol cyclic washing Product, filtering, drying.Its product SEM figures are shown in Fig. 2.
Embodiment 3
1) by the La to be synthesized doping PbTiO3The molecular formula Pb of disk1-xLaxTiO3（X=0.2）Metering, weighs lead acetate and nitre Sour lanthanum is dissolved in deionized water jointly, forms the aqueous solution of Pb/La ions, regulation（Pb2++La3+)/Ti4+Ion concentration is 1.5；
2) P25 is dissolved in deionized water, adjusts Ti4+Ion concentration is 0.4 mol/L；Under stirring, hydroxide is added Potassium, makes potassium hydroxide concentration in the solution be 8 mol/L；
3) under stirring, by step 1) Pb/La deionized water solutions drop to step 2) solution in, persistently stir 6 small When, form the oxyhydroxide mixing suspension of Ti and Pb/La；
4) by step 3) obtained in mixing suspension be added in hydrothermal reaction kettle inner bag, and with deionized water instrumentality material body Product is the 2/3 of reactor inner bag volume, and stirring makes it be sufficiently mixed uniformly；
5）The reactor inner bag that will be equipped with precursor pulp is placed in reactor, sealing, and insulation enters water-filling in 16 hours at 190 DEG C Heat treatment, then allows reactor to naturally cool to room temperature, takes out reactant, filtering, successively with deionized water, ethanol cyclic washing Product, filtering, drying.

Claims (3)

1. it is a kind of that PbTiO is synthesized by La ion dopings3The method of disk, it is characterised in that comprise the following steps：
1) by the La to be synthesized doping PbTiO3The molecular formula Pb of disk1-xLaxTiO3Metering, X=0.001-0.2 weigh Pb sources It is dissolved in deionized water jointly with La sources, forms the aqueous solution of Pb/La ions, regulation（Pb2++La3+)/Ti4+Ion concentration is 1~1.5；
2) P25 is dissolved in deionized water, adjusts Ti4+Ion concentration is 0.2 ~ 0.4 mol/L；Under stirring, hydrogen is added Potassium oxide, makes potassium hydroxide concentration in the solution be 5 ~ 8 mol/L；
3) under stirring, by step 1) Pb/La deionized water solutions drop to step 2) solution in, persistently stir 4-6 it is small When, form the oxyhydroxide mixing suspension of Ti and Pb/La；
4) by step 3) obtained in mixing suspension be added in hydrothermal reaction kettle inner bag, and with deionized water instrumentality material body Product is the 1/3 ~ 4/5 of reactor inner bag volume, and stirring makes it be sufficiently mixed uniformly；
5）By through step 4) the reactor inner bag equipped with precursor pulp be placed in reactor, seal, at 170 ~ 210 DEG C Insulation carries out hydro-thermal process in 10 ~ 20 hours, then allows reactor to naturally cool to room temperature, takes out reactant, and filtering spends successively Ionized water, ethanol cyclic washing product, filtering, drying.
2. it is according to claim 1 that PbTiO is synthesized by La ion dopings3The method of disk, it is characterised in that described La Source is lanthanum nitrate or lanthanum acetate.
3. it is according to claim 1 that PbTiO is synthesized by La ion dopings3The method of disk, it is characterised in that described Pb Source is plumbi nitras or lead acetate.
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107999053A (en) * 2017-11-06 2018-05-08 哈尔滨理工大学 A kind of lanthanium titanate lead/pucherite and preparation method
CN109351357A (en) * 2018-10-16 2019-02-19 华中科技大学 A kind of effective universal method for promoting perovskite catalyst catalytic performance

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1850616A (en) * 2006-05-19 2006-10-25 西北工业大学 Method for preparing lanthanum-zirconium-doped lead titanate film

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1850616A (en) * 2006-05-19 2006-10-25 西北工业大学 Method for preparing lanthanum-zirconium-doped lead titanate film

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
YIN SI-MIN等: "Highly oriented growth of PbTiO3 ferroelectric nanostructure directed by organic molecules under hydrothermal condition", 《电子显微学报》 *
张衡: "稀土掺杂钛酸铅系电子陶瓷的制备与表征", 《中优秀硕士学位论文全文数据库 工程科技I辑》 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107999053A (en) * 2017-11-06 2018-05-08 哈尔滨理工大学 A kind of lanthanium titanate lead/pucherite and preparation method
CN107999053B (en) * 2017-11-06 2020-06-16 哈尔滨理工大学 Lead lanthanum titanate/bismuth vanadate and preparation method thereof
CN109351357A (en) * 2018-10-16 2019-02-19 华中科技大学 A kind of effective universal method for promoting perovskite catalyst catalytic performance

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