CN115403068A - Barium titanate nano cube material and preparation method and application thereof - Google Patents
Barium titanate nano cube material and preparation method and application thereof Download PDFInfo
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- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 title claims abstract description 64
- 229910002113 barium titanate Inorganic materials 0.000 title claims abstract description 64
- 239000000463 material Substances 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title abstract description 10
- 239000013078 crystal Substances 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 14
- 238000006243 chemical reaction Methods 0.000 claims abstract description 11
- 238000001354 calcination Methods 0.000 claims abstract description 7
- 230000001699 photocatalysis Effects 0.000 claims abstract description 5
- 230000007613 environmental effect Effects 0.000 claims abstract description 4
- 238000000746 purification Methods 0.000 claims abstract description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- 229910052788 barium Inorganic materials 0.000 claims description 11
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 claims description 11
- 239000010936 titanium Substances 0.000 claims description 11
- 229960000583 acetic acid Drugs 0.000 claims description 10
- 150000001875 compounds Chemical class 0.000 claims description 10
- 239000012362 glacial acetic acid Substances 0.000 claims description 10
- -1 ester compound Chemical class 0.000 claims description 9
- 229910052719 titanium Inorganic materials 0.000 claims description 9
- JMXKSZRRTHPKDL-UHFFFAOYSA-N titanium ethoxide Chemical group [Ti+4].CC[O-].CC[O-].CC[O-].CC[O-] JMXKSZRRTHPKDL-UHFFFAOYSA-N 0.000 claims description 9
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 8
- 239000012046 mixed solvent Substances 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims description 5
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 claims description 5
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 4
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- ITHZDDVSAWDQPZ-UHFFFAOYSA-L barium acetate Chemical compound [Ba+2].CC([O-])=O.CC([O-])=O ITHZDDVSAWDQPZ-UHFFFAOYSA-L 0.000 claims description 3
- WDIHJSXYQDMJHN-UHFFFAOYSA-L barium chloride Chemical compound [Cl-].[Cl-].[Ba+2] WDIHJSXYQDMJHN-UHFFFAOYSA-L 0.000 claims description 3
- 229910001626 barium chloride Inorganic materials 0.000 claims description 3
- RQPZNWPYLFFXCP-UHFFFAOYSA-L barium dihydroxide Chemical compound [OH-].[OH-].[Ba+2] RQPZNWPYLFFXCP-UHFFFAOYSA-L 0.000 claims description 3
- 229910001863 barium hydroxide Inorganic materials 0.000 claims description 3
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims description 3
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 claims description 3
- 238000005286 illumination Methods 0.000 claims description 2
- 239000002243 precursor Substances 0.000 claims description 2
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 2
- 238000000926 separation method Methods 0.000 claims description 2
- 239000002086 nanomaterial Substances 0.000 abstract description 14
- 239000002159 nanocrystal Substances 0.000 abstract description 6
- 238000003980 solgel method Methods 0.000 abstract description 3
- 238000001308 synthesis method Methods 0.000 abstract description 2
- 238000003837 high-temperature calcination Methods 0.000 abstract 1
- 239000012071 phase Substances 0.000 description 11
- 239000002105 nanoparticle Substances 0.000 description 4
- 238000003917 TEM image Methods 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 230000031700 light absorption Effects 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 125000000896 monocarboxylic acid group Chemical group 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 238000010532 solid phase synthesis reaction Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000000862 absorption spectrum Methods 0.000 description 1
- AYJRCSIUFZENHW-DEQYMQKBSA-L barium(2+);oxomethanediolate Chemical compound [Ba+2].[O-][14C]([O-])=O AYJRCSIUFZENHW-DEQYMQKBSA-L 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 1
- 229940043267 rhodamine b Drugs 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
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- C01G23/00—Compounds of titanium
- C01G23/003—Titanates
- C01G23/006—Alkaline earth titanates
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/02—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the alkali- or alkaline earth metals or beryllium
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J35/39—Photocatalytic properties
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Abstract
The invention discloses a barium titanate nano cubic material and a preparation method and application thereof, belonging to the technical field of nano material preparation, solar energy utilization and environmental protection. The invention adopts a sol-gel method, obtains a uniform gel system by reacting under mild acid-base conditions, and combines a calcination process to obtain the pure-phase barium titanate nano material. The invention solves the problems that the barium titanate material prepared by the traditional synthesis method is easy to generate impure phase, the crystal grains are easy to be coarse during high-temperature calcination and the like, the size of the prepared barium titanate nano crystal is less than 1 micron, the barium titanate nano crystal presents cubic morphology, and the barium titanate nano crystal can be used in the fields of photocatalytic purification and gas conversion under the irradiation of sunlight.
Description
Technical Field
The invention relates to the technical field of nano material preparation, solar energy utilization and environmental protection, in particular to a barium titanate nano cubic material and a preparation method and application thereof.
Background
The piezoelectric material can realize the conversion between electric energy and mechanical energy, and has wide application prospect in various fields. Barium titanate with a perovskite phase structure is an ideal material system for researching a piezoelectric effect, but because the barium titanate is composed of metal elements, the barium element and the titanium element have different activities, and meanwhile, high-temperature sintering can bring about change of a stoichiometric ratio, so that the acquisition of a barium titanate material with a fine grain size and a single phase composition is particularly difficult.
The common method for preparing barium titanate is a solid-phase sintering method, wherein oxides are used as raw materials, other fluxing components are used as auxiliary materials, and the barium titanate material can be obtained under the high-temperature sintering condition. In particular, the obtainment of barium titanate materials with regular shapes is often difficult to achieve by solid-phase synthesis. Therefore, the method for preparing the pure-phase barium titanate material with simple process and simple and convenient operation has important scientific significance and practical significance.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a barium titanate nano cubic material and a preparation method and application thereof. The invention solves the problems that the barium titanate material prepared by the traditional synthesis method is easy to generate impure phase, easy to be coarse in crystal grain after being calcined at high temperature and the like, the size of the prepared barium titanate nano crystal is less than 1 micron, the barium titanate nano crystal presents cubic morphology, and the barium titanate nano crystal can be used in the fields of photocatalytic purification and gas conversion under the irradiation of sunlight. The barium titanate nano cubic material not only can be used as a photocatalytic material to be applied to the utilization field of solar energy, but also can be used as a model material to be used for researching the piezoelectric property of barium titanate.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a nano cubic barium titanate material is tetragonal barium titanate crystal with crystal grain size less than 1 micron and cubic morphology.
The forbidden band width of the nano cubic block material is between 2.8 and 3.4 eV.
The preparation method of the barium titanate nano cubic block material comprises the following steps:
(1) Preparing a precursor solution: dissolving an ester compound of titanium in a glacial acetic acid solution to obtain a solution A, and dissolving a barium-containing compound in an alcohol-water mixed solvent to obtain a solution B;
(2) Sol-gel reaction: adding the solution B into the solution A, uniformly stirring, preserving the heat at the temperature of 40-80 ℃ for 0.5-3 hours, and then drying at the temperature of 80-120 ℃ (preferably 85-110 ℃) for 6-24 hours;
(3) Calcining and decomposing: and (3) preserving the heat of the dried product obtained in the step (2) for 2-5 hours at the temperature of 800-1200 ℃, thus obtaining the barium titanate nano cubic material.
In the step (1), the concentration of the ester compound of titanium in the solution a is 0.2-2mol/L, and the ester compound of titanium is tetraethyl titanate (ethyl titanate), isopropyl titanate or butyl titanate (tetrabutyl titanate).
In the step (1), the concentration of the barium-containing compound in the solution B is 0.2-2mol/L, and the barium-containing compound is one or more of barium hydroxide, barium acetate, barium carbonate and barium chloride.
In the step (1), the glacial acetic acid solution is prepared by mixing glacial acetic acid, alcohol and water, wherein the glacial acetic acid accounts for 10-20% by volume, the alcohol accounts for 30-60% by volume, and the balance is water; the alcohol-water mixed solvent is prepared by mixing alcohol and water according to the weight ratio of 1: (0.5-3) by volume ratio; the alcohol is one or more of ethanol, propanol and butanol.
In the sol-gel reaction process in the step (2), the molar ratio of the barium-containing compound in the solution B to the titanium ester compound in the solution A is 1: (0.5-2).
In the step (3), the calcination temperature is preferably 850 to 1100 ℃.
The nano cubic material has high carrier separation efficiency under the illumination condition, and can be used as a photocatalytic material in the fields of environmental purification and gas conversion.
The design idea of the invention is as follows:
pure-phase barium titanate nano materials are difficult to prepare, the product obtained by the solid-phase synthesis method easily contains impurity phases, and the appearance of barium titanate crystals is difficult to control. The invention adopts a mild sol-gel method to limit the crystal grain growth of barium titanate crystals in the calcining process, and simultaneously can accurately control the stoichiometric ratio of elements, thereby obtaining the shape of the crystal inertia growth of the composite barium titanate crystals and synthesizing the pure-phase barium titanate nano material.
The invention has the advantages that:
1. the invention can control the chemical composition of the barium titanate material to a certain extent by blending the element proportion by a mild sol-gel method.
2. According to the invention, the barium titanate crystal can be subjected to inertial growth by accurately controlling the chemical ratio, so that the appearance of the cubic block is obtained. .
3. The invention has simple process flow, simple and convenient operation, low energy consumption and large output, and is suitable for mass production.
4. The barium titanate material has small grain size and can be used as an ideal model for researching piezoelectric and multi-field coupling functional ceramics.
Drawings
FIG. 1 is a characteristic XRD pattern of the crystal structures of nano-sized barium titanate materials prepared in example 1 and example 2;
FIG. 2 is a TEM image of nano-sized barium titanate crystals prepared by the present invention; wherein: (a) example 1; (b) example 2.
FIG. 3 is a UV-VIS absorption curve of the nano-sized barium titanate cubic block material prepared in example 1.
FIG. 4 is a graph showing the relationship between the residual quantity of RhB at different processing times and time under full spectrum excitation for the nano-sized barium titanate cubic material prepared in example 1.
Detailed Description
The invention is described in detail below with reference to the figures and examples.
In the following examples, the ester compound of titanium may be tetraethyl titanate (ethyl titanate), isopropyl titanate, or butyl titanate (tetrabutyl titanate), and the barium-containing compound may be one or more of barium hydroxide, barium acetate, barium carbonate, and barium chloride. The alcohol-water mixed solvent is prepared by mixing ethanol and water according to the weight ratio of 1:2 in a volume ratio. The concentration of the barium-containing compound in the solution B is 1mol/L.
Example 1
The preparation process of the tetragonal barium titanate nano material of the embodiment is as follows:
(1) 5mL of glacial acetic acid (CH) are taken 3 COOH) with 0.01mol of tetrabutyl titanate (C) 16 H 36 O 4 Ti) are mixed homogeneously. 15mL of ethanol (CH) was added 3 CH 2 OH), 10mL of deionized water was added with stirring to obtain solution A, and 0.01mol of Ba (OH) was added 2 Dissolving in an alcohol-water mixed solvent to obtain a solution B;
(2) Sol-gel reaction: adding the solution B into the solution A, uniformly stirring, placing at 55 ℃ for heat preservation for 2 hours, and then placing at 100 ℃ for drying for 15 hours;
(3) Calcining and decomposing: and (3) preserving the product obtained in the step (2) at the temperature of 900 ℃ for 3 hours to obtain the barium titanate nano cubic material (BTO-1).
BTO-1 in FIG. 1 is the XRD pattern of the barium titanate nano material prepared in this example, and it can be seen from BTO-1 that the material is pure tetragonal phase barium titanate crystal without any impurity phase.
Fig. 2 (a) is a TEM image of the barium titanate nanomaterial prepared in this example, and it can be seen from fig. 2 (a) that the prepared barium titanate has uniform crystal size and good dispersibility, and exhibits a cubic morphology.
Fig. 3 is a light absorption spectrum of the barium titanate nanomaterial prepared in this example 1, and it can be seen from fig. 3 that the barium titanate nanomaterial exhibits strong light absorption performance in the ultraviolet light absorption region. The absorption band edge is at 375nm, and the band gap is about 3.31eV.
Fig. 4 shows that the barium titanate nano material prepared in this embodiment can decompose organic rhodamine B under the irradiation condition.
Example 2
The preparation process of the barium titanate nano material of the embodiment is as follows:
(1) 10mL of glacial acetic acid (CH) are taken 3 COOH) with 0.02mol of tetrabutyl titanate (C 16 H 36 O 4 Ti) are mixed homogeneously. 30mL of ethanol (CH) was added 3 CH 2 OH), 20mL of deionized water was added with stirring to obtain solution A, and 0.02mol of Ba (OH) was added 2 Dissolving in an alcohol-water mixed solvent to obtain a solution B;
(2) Sol-gel reaction: adding the solution B into the solution A, uniformly stirring, placing at 60 ℃ for heat preservation for 2 hours, and then placing at 95 ℃ for drying for 20 hours;
(3) Calcining and decomposing: and (3) preserving the heat of the product obtained in the step (2) at the temperature of 1000 ℃ for 3 hours to obtain the barium titanate nano cubic material (BTO-2).
BTO-2 in FIG. 1 is the XRD pattern of the barium titanate nano material prepared in this example, and it can be seen from BTO-2 that the material is pure tetragonal phase barium titanate crystal without any impurity phase.
Fig. 2 (b) is a TEM image of the barium titanate nanomaterial prepared in this example, and it can be seen from fig. 2 (b) that the prepared barium titanate crystal has good dispersibility and a cubic morphology.
Claims (8)
1. A barium titanate nano cube material is characterized in that: the material is tetragonal phase barium titanate crystal, the grain size is less than 1 micron, and the material presents the appearance of cubic blocks.
2. The barium titanate nanocube material of claim 1, wherein: the forbidden band width of the nano cubic block material is between 2.8 and 3.4 eV.
3. The method for preparing a barium titanate nano-cubic material according to claim 1, characterized in that: the method comprises the following steps:
(1) Preparing a precursor solution: dissolving an ester compound of titanium in a glacial acetic acid solution to obtain a solution A, and dissolving a barium-containing compound in an alcohol-water mixed solvent to obtain a solution B;
(2) Sol-gel reaction: adding the solution B into the solution A, uniformly stirring, preserving the heat for 0.5 to 3 hours at the temperature of between 40 and 80 ℃, and then drying for 6 to 24 hours at the temperature of between 80 and 120 ℃;
(3) Calcining and decomposing: and (3) preserving the heat of the dried product obtained in the step (2) at the temperature of 800-1200 ℃ for 2-5 hours to obtain the barium titanate nano cubic material.
4. The method for preparing a barium titanate nano-cubic material according to claim 3, characterized in that: in the step (1), the concentration of the ester compound of titanium in the solution A is 0.2-2mol/L, and the ester compound of titanium is tetraethyl titanate (ethyl titanate), isopropyl titanate or butyl titanate (tetrabutyl titanate).
5. The method for preparing a barium titanate nano-cubic material according to claim 3, characterized in that: in the step (1), the concentration of the barium-containing compound in the solution B is 0.2-2mol/L, and the barium-containing compound is one or more of barium hydroxide, barium acetate, barium carbonate and barium chloride.
6. The method for preparing a barium titanate nano-cubic material according to claim 3, characterized in that: in the step (1), the glacial acetic acid solution is prepared by mixing glacial acetic acid, alcohol and water, wherein the glacial acetic acid accounts for 10-20% by volume, the alcohol accounts for 30-60% by volume, and the balance is water; the alcohol-water mixed solvent is prepared by mixing alcohol and water according to the weight ratio of 1: (0.5-3) by volume ratio; the alcohol is one or more of ethanol, propanol and butanol.
7. The method for preparing a barium titanate nano-cubic material according to claim 3, characterized in that: in the sol-gel reaction process in the step (2), the molar ratio of the barium-containing compound in the solution B to the titanium ester compound in the solution A is 1: (0.5-2).
8. The use of a barium titanate nano-cube material according to claim 1, characterized in that: the nano cubic material has high carrier separation efficiency under the illumination condition, and can be used as a photocatalytic material in the fields of environmental purification and gas conversion.
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Citations (9)
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| CN1472141A (en) * | 2003-06-30 | 2004-02-04 | 山东省国腾功能陶瓷材料有限公司 | Technology for preparing high-purity nano barium titanate powder |
| WO2005061410A1 (en) * | 2003-12-23 | 2005-07-07 | Aalborg Universitet | Method and apparatus for production of a compound having submicron particle size and a compound produced by the method |
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