CN109399699A - A kind of preparation method of Fe2O3 doping barium titanate nano particle - Google Patents
A kind of preparation method of Fe2O3 doping barium titanate nano particle Download PDFInfo
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- CN109399699A CN109399699A CN201811275843.7A CN201811275843A CN109399699A CN 109399699 A CN109399699 A CN 109399699A CN 201811275843 A CN201811275843 A CN 201811275843A CN 109399699 A CN109399699 A CN 109399699A
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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
- C01G23/006—Alkaline earth titanates
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- 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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/84—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by UV- or VIS- data
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- 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
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Abstract
The invention discloses a kind of preparation methods of Fe2O3 doping barium titanate nano particle.This method is utilized respectively barium hydroxide and two (2 hydroxy propanoic acid) two hydroxide diammoniums close titanium as barium source and titanium source, doping iron ion is provided using soluble ferric iron salt, it is first dissolved in forming mixing precursor solution in deionized water, then with the pH value of 5M sodium hydroxide solution adjustment precursor solution, and using suitable oleic acid and tert-butylamine as surfactant and additive, hydrothermal synthesis goes out BaTi under conditions of 180-220 DEG C1‑XFeXO3(x=0.01-0.15) cubic-phase nano particle.This method energy consumption is lower, easy to operate, the BaTi prepared using this method1‑XFeXO3(x=0.01-0.15) nano particle is characterized as purity is high, the good cubic phase of crystallinity after tested.Compared to undoped barium titanate, due to its lower optical band gap (2.6eV) and there is regular cube pattern and lesser crystallite dimension (20-40nm), so that it is shown preferable photocatalytic activity, has broad application prospects in scientific research and electronics industry.
Description
Technical field
The invention belongs to the preparations of inorganic functional nano material, and in particular to a kind of system of Fe2O3 doping barium titanate nano particle
Preparation Method.
Background technique
Barium titanate (BaTiO3) be a kind of metal oxide with perovskite structure, due to its excellent ferroelectricity, piezoelectricity,
Dielectric, photoelectric properties, in multilayer ceramic capacitor (MLCCs), organic field effect tube, thermistor, pressure sensor etc.
There is huge application prospect in terms of various electronic devices.A large number of studies show that tune can be passed through by being doped modification to barium titanate
Its structure is controlled so as to improve its physical and chemical properties, while barium titanate ABO3The perovskite structure of type for different doping from
The tolerance factor of son is higher, thus becomes an effective way for improving its performance for the doping vario-property of barium titanate.Wherein cross
The doping for crossing element (such as chromium Cr, manganese Mn, cobalt Co, iron Fe) can make barium titanate have room-temperature ferromagnetic and become multiferroic material
Material, ferro element can regulate and control the electronic structure of barium titanate in B doping, its optical band gap be reduced, in visible light catalytic and light
Excellent properties are shown in terms of conductive film, to improve its potential application value.
The preparation method of Fe2O3 doping barium titanate is broadly divided into conventional solid sintering process and wet chemistry method at present.Conventional solid is burnt
Connection generally can cause inevitable crystal grain to be grown up, and have that doping is uneven, calcination temperature is excessively high, technique is cumbersome etc. and lack
Point.Compared with general wet chemistry synthesis barium titanate doping nano particle has hydro-thermal method, sol-gel, coprecipitation etc., this method
Used hydro-thermal method can directly obtain the Fe2O3 doping barium titanate nano particle of crystallite dimension very little, lower with synthesis temperature,
The advantages that purity is high, monodisperse and good crystallinity, while not needing to carry out high-temperature calcination, it avoids in high-temperature process and easily causes
Crystal grain grow up, the introducing of impurity and defect and agglomeration etc..
Summary of the invention
The purpose of the present invention is to provide a kind of preparation methods of Fe2O3 doping barium titanate nano particle.
The present invention adopts the following technical scheme:
A kind of preparation method of Fe2O3 doping barium titanate nano particle.Specifically includes the following steps:
(1) barium hydroxide and soluble ferric iron salt are dissolved in deionized water, dissolved Ba2+Concentration is 0.05mol/
L, Fe3+Concentration is 5 × 10-4-7.5×10-3mol/L.Two (2 hydroxy propanoic acid) two hydroxide diammoniums are added into solution and close titanium,
Make Fe in solution3+And Ti4+The sum of the amount of substance and Ba2+Molar ratio be 1:1.
(2) pH value of the sodium hydroxide solution adjustment solution of 5mol/L is added into solution under magnetic stirring, then to
Oleic acid (OLA) and magnetic agitation 10min are added in solution, wherein OLA:Ti4+Mole the ratio between be 4:1-8:1.
(3) solution after stirring is transferred in autoclave liner, compactedness 70-80% is added into solution
2.10ml tert-butylamine, hydro-thermal reaction 24-72h, naturally cools to room under the conditions of the autoclave being sealed is placed in 180-220 DEG C
Temperature.
(4) sediment is washed with dilute hydrochloric acid first, is then washed for several times and mistake with deionized water, dehydrated alcohol respectively
Filter, 60-80 DEG C dries to get Fe2O3 doping barium titanate nano particle is arrived.
To further realize the purpose of the present invention, preferably 220 DEG C of the hydrothermal temperature.
Barium hydroxide is respectively adopted the present invention is based on hydro-thermal method and two (2 hydroxy propanoic acid) two hydroxide diammoniums close titanium
As barium source and titanium source, the iron ion of doping is provided using soluble ferric iron salt, and make surfactant preparation tapping with oleic acid and mix
Miscellaneous barium titanate cubic nanometer particle.The BaTi that this method is prepared1-XFeXO3(x=0.01-0.15) nano particle has regular
Cube pattern, average crystal grain partial size is 20-40nm, while having extraordinary crystallinity, Fe element is mixed in B differences
Miscellaneous amount may be implemented the regulation to barium titanate electronic structure, the optical band gap of barium titanate from undoped with when 3.2eV or so reduce
2.6eV (doping 10%) has been arrived, has made it that there is stronger absorption in visible light wave range, it means that can using visible light
Effectively to realize the excitation to its valence-band electrons, to improve it in the photocatalytic activity of visible light wave range.Simultaneously because smaller
Particle size and regular cube pattern make it have biggish specific surface area, mentioning for photocatalysis performance can also be promoted
It rises.The BaTi that this method is prepared1-XFeXO3Nano particle urges rhodamine B solution in 30min under the irradiation of visible light
Change efficiency up to 90% or more, while regular cube pattern can be used for self assembly optoelectronic film etc., to show non-
Often good Scientific Research Potential and application value.
Detailed description of the invention
Fig. 1 is the XRD spectrum of barium titanate doping nano particle prepared in 1-4 of the embodiment of the present invention.
Fig. 2 is the TEM figure of barium titanate doping nano particle prepared in the embodiment of the present invention 1.
Fig. 3 is the TEM figure of barium titanate doping nano particle prepared in the embodiment of the present invention 2.
Fig. 4 is the UV-Vis spectrogram of the nano particle for the different dopings level that the method for the present invention is prepared.
Specific embodiment
Below with reference to embodiment, the invention will be further described, but scope of the present invention is not limited to
In this.
Embodiment 1
Weigh Ba (OH) 8H of 0.7887g2Fe (the NO of O and 0.0253g3)·9H2O is dissolved in 50ml deionized water, to
Two (2 hydroxy propanoic acid) the two hydroxide diammoniums that 1.185ml is wherein added close titanium (50wt% aqueous solution), stir.To
The pH value that the 5M NaOH solution adjustment solution of 11.25ml is added in precursor solution is mixed, is then added under magnetic stirring
Above-mentioned solution is transferred in 100ml autoclave liner by 6.35ml oleic acid (OLA) after stirring 10min.It is added at this time into liner
The tert-butylamine of 2.10ml, after the autoclave being sealed is placed in 220 DEG C of reactions for 24 hours, cooled to room temperature.First by sediment
It is washed with dilute hydrochloric acid, is then washed for several times and filtered with deionized water, dehydrated alcohol respectively, in air 60 DEG C of drying to obtain
The barium titanate nano particle of Fe2O3 doping.
The XRD spectrum of product is as shown in fig. 1, all diffraction maximums of sample all with standard cube phase BaTiO3Card
(JCPDS31-0174) in diffraction peak to it is deserved very well, without impurity peaks.From the TEM of Fig. 2 figure it can be seen that size of microcrystal is
20-40nm and have regular cube pattern.
Embodiment 2
Weigh Ba (OH) 8H of 0.7887g2Fe (the NO of O and 0.0505g3)·9H2O is dissolved in 50ml deionized water, to
Two (2 hydroxy propanoic acid) the two hydroxide diammoniums that 1.155ml is wherein added close titanium (50wt% aqueous solution), stir.To
The pH value that the 5M NaOH solution adjustment solution of 11.25ml is added in precursor solution is mixed, is then added under magnetic stirring
Above-mentioned solution is transferred in 100ml autoclave liner by 6.35ml oleic acid (OLA) after stirring 10min.It is added at this time into liner
The tert-butylamine of 2.10ml, after the autoclave being sealed is placed in 220 DEG C of reactions for 24 hours, cooled to room temperature.First by sediment
It is washed with dilute hydrochloric acid, is then washed for several times and filtered with deionized water, dehydrated alcohol respectively, be dried to obtain iron for 60 DEG C in air
Barium titanate doping nano particle.
The XRD spectrum of product is as shown in fig. 1, all diffraction maximums of sample all with standard cube phase BaTiO3Card
(JCPDS31-0174) in diffraction peak to it is deserved very well, without impurity peaks.Its bright size of microcrystal of the TEM chart of Fig. 3 is 20-
40nm and have regular cube pattern.
Embodiment 3
Weigh Ba (OH) 8H of 0.7887g2The FeCl of O and 0.0169g3·6H2O is dissolved in 50ml deionized water, Xiang Qi
Middle two (2 hydroxy propanoic acid) the two hydroxide diammoniums that 1.185ml is added close titanium (50wt% aqueous solution), stir.To mixed
The pH value that the 5M NaOH solution adjustment solution of 11.25ml is added in precursor solution is closed, is then added under magnetic stirring
Above-mentioned solution is transferred in 100ml autoclave liner by 4.76ml oleic acid (OLA) after stirring 10min.It is added into liner
After the autoclave being sealed is placed in 220 DEG C of reactions for 24 hours after the tert-butylamine of 2.10ml, cooled to room temperature.By sediment head
First washed with dilute hydrochloric acid, then washed for several times and filtered with deionized water, dehydrated alcohol respectively, in air 60 DEG C of dryings to
Obtain the barium titanate nano particle of Fe2O3 doping.
The XRD spectrum of product is as shown in fig. 1, all diffraction maximums of sample all with standard cube phase BaTiO3Card
(JCPDS31-0174) in diffraction peak to it is deserved very well, without impurity peaks.Scherrer formula is utilized using (110) crystallographic plane diffraction peak
Calculating sample grain size is about 26.9nm.
Embodiment 4
Weigh Ba (OH) 8H of 0.7887g2The FeCl of O and 0.0338g3·6H2O is dissolved in 50ml deionized water, Xiang Qi
Two (2 hydroxy propanoic acid) two hydroxide diammoniums of middle addition 1.155 close titanium (50wt% aqueous solution), stir.To mixing
The pH value of the 5M NaOH solution adjustment solution of 11.25ml is added in precursor solution, 6.35ml is then added under magnetic stirring
Above-mentioned solution is transferred in 100ml autoclave liner by oleic acid (OLA) after stirring 10min.The uncle of 2.10ml is added into liner
After the autoclave being sealed is placed in 220 DEG C of reaction 48h after butylamine, cooled to room temperature.Sediment is used into dilute hydrochloric acid first
Washing, is then washed for several times and is filtered with deionized water, dehydrated alcohol respectively, and 60 DEG C of dryings are in air to obtain Fe2O3 doping
Barium titanate nano particle.
The XRD spectrum of product is as shown in fig. 1, all diffraction maximums of sample all with standard cube phase BaTiO3Card
(JCPDS31-0174) in diffraction peak to it is deserved very well, without impurity peaks.Scherrer formula is utilized using (110) crystallographic plane diffraction peak
Calculating sample grain size is about 28.7nm.
Claims (6)
1. a kind of preparation method of Fe2O3 doping barium titanate nano particle.Characterized by the following steps:
(1) barium hydroxide and soluble ferric iron salt are dissolved in deionized water, two (2- hydroxyls is added into mixing precursor solution
Base propionic acid) two hydroxide diammoniums conjunction titanium；
(2) pH value of the sodium hydroxide solution adjustment solution of 5mol/L is added into solution under magnetic stirring, then to solution
Middle addition oleic acid (OLA) and magnetic agitation；
(3) solution after stirring is transferred in reaction vessel, vessel filling degree is 70-80%, and 2.10ml is added into solution
The container being sealed is placed in hydro-thermal reaction 24-72h under the conditions of certain temperature, cooled to room temperature by tert-butylamine；
(4) sediment is washed with dilute hydrochloric acid first, is then washed for several times and filtered with deionized water, dehydrated alcohol respectively, 60-
80 DEG C dry to get Fe2O3 doping barium titanate nano particle is arrived.
2. a kind of preparation method of Fe2O3 doping barium titanate nano particle as described in claim 1, which is characterized in that the step
(1) soluble ferric iron salt is nine water ferric nitrates or Iron trichloride hexahydrate in.
3. a kind of preparation method of Fe2O3 doping barium titanate nano particle as described in claim 1, which is characterized in that the step
(1) in barium hydroxide and soluble ferric iron salt mixing precursor solution, Ba2+Concentration is 0.05mol/L, Fe3+Concentration is 5
×10-4-7.5×10-3Mol/L, after two (2 hydroxy propanoic acid) two hydroxide diammoniums conjunction titanium is added, Fe in solution3+And Ti4+Object
The sum of amount of matter and Ba2+Molar ratio be 1:1.
4. a kind of preparation method of Fe2O3 doping barium titanate nano particle as described in claim 1, which is characterized in that the step
(2) amount for the oleic acid (OLA) being added in are as follows: itself and Ba in solution2+The ratio between mole be 4:1-8:1.
5. a kind of preparation method of Fe2O3 doping barium titanate nano particle as described in claim 1, which is characterized in that the hydro-thermal
Reaction is carried out in the autoclave with polytetrafluoroethyllining lining.
6. a kind of preparation method of Fe2O3 doping barium titanate nano particle as described in claim 1, which is characterized in that the hydro-thermal
Reaction temperature is 180-220 DEG C, reaction time 24-72h.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113860390A (en) * | 2020-06-30 | 2021-12-31 | 南京大学 | Co2(OH)3Cl microspheres and Fe2+Doped Co2(OH)3Method for producing Cl |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113860390A (en) * | 2020-06-30 | 2021-12-31 | 南京大学 | Co2(OH)3Cl microspheres and Fe2+Doped Co2(OH)3Method for producing Cl |
| CN113860390B (en) * | 2020-06-30 | 2023-08-25 | 南京大学 | Co 2 (OH) 3 Cl microspheres and Fe 2+ Doped Co 2 (OH) 3 Cl preparation method |
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