CN111470529A - Preparation method of strontium titanate nano material with adjustable morphology - Google Patents
Preparation method of strontium titanate nano material with adjustable morphology Download PDFInfo
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- CN111470529A CN111470529A CN201910061471.6A CN201910061471A CN111470529A CN 111470529 A CN111470529 A CN 111470529A CN 201910061471 A CN201910061471 A CN 201910061471A CN 111470529 A CN111470529 A CN 111470529A
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- oleic acid
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- 239000002086 nanomaterial Substances 0.000 title claims abstract description 21
- VEALVRVVWBQVSL-UHFFFAOYSA-N strontium titanate Chemical compound [Sr+2].[O-][Ti]([O-])=O VEALVRVVWBQVSL-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- DHEQXMRUPNDRPG-UHFFFAOYSA-N strontium nitrate Chemical compound [Sr+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O DHEQXMRUPNDRPG-UHFFFAOYSA-N 0.000 claims abstract description 34
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims abstract description 30
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims abstract description 30
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims abstract description 30
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims abstract description 30
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000005642 Oleic acid Substances 0.000 claims abstract description 30
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims abstract description 30
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims abstract description 30
- 238000000034 method Methods 0.000 claims abstract description 24
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 15
- 125000004108 n-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 claims abstract description 7
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims abstract description 3
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 238000004140 cleaning Methods 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims 2
- 238000005119 centrifugation Methods 0.000 claims 1
- 229910002367 SrTiO Inorganic materials 0.000 abstract description 21
- 230000001699 photocatalysis Effects 0.000 abstract description 9
- 229910002370 SrTiO3 Inorganic materials 0.000 abstract description 8
- 239000000693 micelle Substances 0.000 abstract description 6
- 238000001338 self-assembly Methods 0.000 abstract description 6
- 239000013081 microcrystal Substances 0.000 abstract description 5
- 238000001179 sorption measurement Methods 0.000 abstract description 5
- 238000007146 photocatalysis Methods 0.000 abstract description 4
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 16
- 239000002105 nanoparticle Substances 0.000 description 14
- 230000000052 comparative effect Effects 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- 238000004627 transmission electron microscopy Methods 0.000 description 6
- 239000002245 particle Substances 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 239000004530 micro-emulsion Substances 0.000 description 3
- 239000002159 nanocrystal Substances 0.000 description 3
- 239000011858 nanopowder Substances 0.000 description 3
- 239000002244 precipitate Substances 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 239000002135 nanosheet Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 239000004809 Teflon Substances 0.000 description 1
- 229920006362 Teflon® Polymers 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- MCPLVIGCWWTHFH-UHFFFAOYSA-L methyl blue Chemical compound [Na+].[Na+].C1=CC(S(=O)(=O)[O-])=CC=C1NC1=CC=C(C(=C2C=CC(C=C2)=[NH+]C=2C=CC(=CC=2)S([O-])(=O)=O)C=2C=CC(NC=3C=CC(=CC=3)S([O-])(=O)=O)=CC=2)C=C1 MCPLVIGCWWTHFH-UHFFFAOYSA-L 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000005232 molecular self-assembly Methods 0.000 description 1
- 239000007908 nanoemulsion Substances 0.000 description 1
- 239000002060 nanoflake Substances 0.000 description 1
- 239000002064 nanoplatelet Substances 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 239000004417 polycarbonate Substances 0.000 description 1
- 229920000515 polycarbonate Polymers 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000004506 ultrasonic cleaning Methods 0.000 description 1
Images
Classifications
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- 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
-
- B01J35/39—
-
- 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
-
- 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
- C01P2004/24—Nanoplates, i.e. plate-like particles with a thickness from 1-100 nanometer
Abstract
The invention discloses a preparation method of a strontium titanate nano material with adjustable morphology. The method comprises the steps of uniformly mixing a strontium nitrate solution, a sodium hydroxide solution, a butanol solution of n-butyl titanate and a butanol solution of oleic acid, and then carrying out hydrothermal reaction for 6-24 hours at 100-200 ℃ to obtain the strontium titanate nano material. The micelle pair SrTiO formed by self-assembly of oleic acid molecules3The influence of the dynamic behavior of the directional adsorption of the nano-microcrystal finally realizes the regulation and control of the product morphology, and the prepared SrTiO3The nano material has good dispersibility and high photocatalysis efficiency, and is beneficial to the application of a later-stage photocatalysis device.
Description
Technical Field
The invention relates to a preparation method of a strontium titanate nano material with adjustable morphology, belonging to the technical field of nano material preparation
Background
Strontium titanate (SrTiO)3) As a typical perovskite metal oxide, the perovskite metal oxide is an electronic functional ceramic material with wide application, has the characteristics of good thermal stability, low dielectric loss, high dielectric constant and the like, and plays an important role in the application of catalytic, ferroelectric, piezoelectric and dielectric materials. SrTiO3Has good photocatalytic activity and proper forbidden band width (3.2-3.8 eV), and can be used in photochemical cell, photocatalytic hydrolysis and photocatalysisHas wide application prospect in the fields of degrading organic pollutants and the like. SrTiO3The growth process and morphology control of the crystal have important effects on its physicochemical properties, since its structural dependence can be adjusted by controlling the growth parameters and processes.
One of the main synthetic strategies in nanoparticle growth is the use of a suitable reaction template. The template may provide a confined environment for the nanoparticles during growth to tailor the final shape of the particles by the morphology of the template. In a limited space with a certain shape provided by the template, the nano-crystallites can form a larger nano-material in a directional adsorption mode, and the process completely imitates the classical crystal growth mechanism in textbooks except that ions and molecules are replaced by the nano-crystallites. The literature is that the nano material with special appearance is constructed by a template method. Banfield et al first reported a method for the preparation of nanomaterials by directed adsorption of nanocrystallites in the presence of surfactants (Science,1998,281,969), the TiO prepared by this method2The nanoparticles have problems of poor crystallinity and non-uniform particle size. Zhan et al (J.Phys.chem.C,2015,119,3530) prepared SrTiO with mesoporous structure by hydrothermal method in the presence of polyethylene glycol self-assembled molecular template3Evolution of the size and morphology of the nanoparticles, SrTiO obtained by this process3Nanoparticles also suffer from non-uniform product size. Therefore, the selection of a proper molecular self-assembly template and the guidance of the directional adsorption process of the nano-crystallites determine key parameters of the final product such as crystallinity, morphology, uniformity and the like. Common templates include porous alumina, polycarbonate membranes, carbon nanotubes and micro-nano emulsions. However, SrTiO is prepared by a templating method3The nano particles have the problems of single appearance and relatively narrow size regulation range. The above problems severely limit SrTiO3The application range of the nano material hinders the great improvement of the photocatalytic performance.
Disclosure of Invention
To solve the problem of SrTiO of the prior art3The nanometer material has uncontrollable appearance and grain sizeThe problems of narrow range, low orientation, poor stability and deteriorated performance in the application of the strontium titanate nano material caused by overlarge adjustable range and relatively narrow adjustable range are solved.
The technical scheme of the invention is as follows:
the preparation method of the strontium titanate nano material with adjustable morphology comprises the following steps:
uniformly mixing a strontium nitrate solution, a sodium hydroxide solution, a butanol solution of n-butyl titanate and a butanol solution of oleic acid, performing hydrothermal reaction at 100-200 ℃ for 6-24 h, cooling to room temperature after the reaction is finished, centrifuging, cleaning and drying to obtain the strontium titanate nano material.
Preferably, the concentration of the butanol solution of the oleic acid is 0.1-0.6 mol/L.
Preferably, the molar ratio of the strontium nitrate to the oleic acid is 2: 1-1: 3.
Preferably, the molar ratio of the strontium nitrate to the n-butyl titanate is 1: 1.
Preferably, the cooling is natural cooling.
Preferably, the centrifugal rotating speed is 3000-5000 rpm, and the centrifugal time is 5-10 minutes.
Preferably, the drying temperature is 50-70 ℃, and the drying time is 24-36 hours.
Preferably, the cleaning is ultrasonic cleaning in acetone, alcohol and water in sequence.
The SrTiO with adjustable form is synthesized by a hydrothermal method with the assistance of oleic acid molecules with self-assembly capacity3And (3) nano materials. The structure of the microemulsion formed by the self-assembly of the oleic acid molecules can be changed from spherical micelles to lamellar micelles in the water-oil mixture. The micelle pair SrTiO formed by self-assembly of oleic acid molecules3The influence of the dynamic behavior of the directional adsorption of the nano-microcrystals finally realizes the regulation and control of the appearance of the product.
Compared with the prior art, the invention has the following advantages:
1) the invention adjusts the concentration of the oleic acid in the reaction systemThe shape of the oleic acid microemulsion in the solution was changed. In the limited space provided by microemulsion formed by oleic acid molecule self-assembly, SrTiO3The diffusion of the nano-crystallites is limited so that SrTiO3Directionally attaching the nanocrystals to form nanoparticles and nanosheets;
2) the method has the advantages of simple raw materials, low cost and simple preparation process, and the prepared SrTiO is3The nano material has good dispersion and high photocatalysis efficiency, and is beneficial to the application of a later photocatalysis device.
Drawings
FIG. 1 is SrTiO prepared in example 13Transmission electron microscopy of the nanocrystals.
FIG. 2 is SrTiO prepared in example 23Transmission electron microscopy of nanoparticles.
FIG. 3 is SrTiO prepared in example 33Transmission electron microscopy of nanoplatelets.
FIG. 4 shows SrTiO compounds prepared in examples 1 to 33Nanomaterial and commercial SrTiO3The photocatalytic performance of the nano powder is compared with that of the nano powder.
FIG. 5 shows SrTiO prepared in comparative example 13Transmission electron microscopy of the nanocrystals.
FIG. 6 is SrTiO prepared in comparative example 23Transmission electron microscopy of nanoparticles.
Detailed Description
The present invention will be described in further detail with reference to the following examples and the accompanying drawings.
Example 1
1) In the process of synthesizing the strontium titanate nanoparticles, 1mmol of strontium nitrate is dissolved in 5m L deionized water, 12.5mmol of sodium hydroxide is dissolved in 5m L deionized water, 1mmol of n-butyl titanate is dissolved in 5m L anhydrous butanol, 1.5mmol of oleic acid is dissolved in 5m L anhydrous butanol, and a strontium nitrate aqueous solution, a sodium hydroxide aqueous solution, an n-butyl titanate anhydrous butanol solution and an oleic acid anhydrous butanol solution are prepared;
2) the prepared solutions were mixed together and the resulting solution was then transferred to a 50m L teflon lined stainless steel autoclave;
3) sealing the autoclave, heating at 200 ℃ for 24h, and naturally cooling to room temperature after the reaction is finished;
4) centrifuging the obtained product for 5 minutes at 3000round/min, pouring out supernatant, taking precipitate, ultrasonically cleaning the precipitate in acetone, alcohol and deionized water in sequence, and drying the precipitate for 24 hours at 50 ℃ to obtain SrTiO3And (4) nano-microcrystal.
Example 2
The same procedure as in example 1 was followed, except that the amount of oleic acid added in step 1) of example 1 was changed to 0.5mmol, and the other conditions were kept the same.
Example 3
The same procedure as in example 1 was followed, except that the amount of oleic acid added in step 1) of example 1 was changed to 3mmol, and the other conditions were kept the same.
The shape of micelle formed by oleic acid molecules in a reaction system through self-assembly can be changed by adjusting the oleic acid content, and SrTiO formed at the initial stage of the reaction3Directionally assembling the nano-microcrystal in the micelles with different shapes so as to obtain SrTiO with different appearances3And (3) nano materials.
SrTiO prepared in examples 1 to 3 were tested separately3For comparison, the common dye of methyl blue was also degraded by strontium titanate nanopowder (Aldrich, 30nm) commercially available under the same conditions. The degradation effect is shown in FIG. 4, from which it can be seen that SrTiO synthesized by the present invention3The catalytic activity of the nano material is higher than that of commercial strontium titanate powder. The strontium titanate nano-crystallite synthesized in the embodiment 1 has the best photocatalytic performance which is 2 times that of commercial strontium titanate powder.
The concentration of a butanol solution of oleic acid is 0.3 mol/L, the concentration of a strontium nitrate solution is 0.2 mol/L, when the molar ratio of strontium nitrate to oleic acid is 2:3, strontium titanate nano-crystallites with the particle size of 20nm are obtained, the concentration of a butanol solution of oleic acid is 0.6 mol/L, the concentration of a strontium nitrate solution is 0.2 mol/L, when the molar ratio of strontium nitrate to oleic acid is 3:1, strontium titanate nano-sheets with the length of 200nm and the thickness of 20nm are obtained, the concentration of a butanol solution of oleic acid is 0.1 mol/L, the concentration of a strontium nitrate solution is 0.2 mol/L, and when the molar ratio of strontium nitrate to oleic acid is 1:2, strontium titanate nano-particles with the particle size of 100nm are obtained.
Comparative example 1
The same procedure as in example 1 was used except that the amount of oleic acid added in step 1) of example 1 was changed to 0.05mmol, and the other conditions were kept the same. FIG. 5 shows SrTiO prepared in comparative example 13In a transmission electron microscope image of the nano-microcrystal, when the molar ratio of strontium nitrate to oleic acid is 2:3, the obtained product is in a nano-particle shape, but the problems of more surface defects and nonuniform size exist.
Comparative example 2
The same procedure as in example 1 was used except that the amount of oleic acid added in step 1) of example 1 was changed to 4mmol, and the other conditions were kept the same. FIG. 6 is SrTiO prepared in comparative example 23Transmission electron microscopy of nanoparticles. It can be seen from the figure that when the molar ratio of strontium nitrate to oleic acid is 1:4, the obtained product has non-uniform morphology and is a mixed product of strontium titanate nano-flakes and nano-particles.
Claims (10)
1. The preparation method of the strontium titanate nano material with adjustable morphology is characterized by comprising the following steps:
uniformly mixing a strontium nitrate solution, a sodium hydroxide solution, a butanol solution of n-butyl titanate and a butanol solution of oleic acid, performing hydrothermal reaction at 100-200 ℃ for 6-24 h, cooling to room temperature after the reaction is finished, centrifuging, cleaning and drying to obtain the strontium titanate nano material.
2. The method according to claim 1, wherein the concentration of the butanol solution of oleic acid is 0.1 to 0.6 mol/L.
3. The preparation method according to claim 1, wherein the molar ratio of strontium nitrate to oleic acid is 2:1 to 1: 3.
4. The method according to claim 1, wherein the molar ratio of strontium nitrate to n-butyl titanate is 1: 1.
5. The method of claim 1, wherein the cooling is natural cooling.
6. The method according to claim 1, wherein the centrifugal speed is 3000 to 5000 rpm.
7. The method according to claim 6, wherein the centrifugation time is 5 to 10 minutes.
8. The method according to claim 1, wherein the drying temperature is 50 to 70 ℃.
9. The method according to claim 8, wherein the drying time is 24 to 36 hours.
10. The method of claim 1, wherein the washing is ultrasonic washing in acetone, alcohol, and water in this order.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112760711A (en) * | 2020-12-14 | 2021-05-07 | 中国科学院过程工程研究所 | Strontium titanate single crystal particle and preparation method and application thereof |
| CN114618537A (en) * | 2022-04-10 | 2022-06-14 | 贵州大学 | Red phosphorus/strontium titanate heterojunction photocatalyst and preparation method and application thereof |
-
2019
- 2019-01-23 CN CN201910061471.6A patent/CN111470529A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| ZHENHUA CONG ET AL: ""Tunable Morphology of SrTiO3 Nanomaterials Controlled by Surfactant Concentration"", 《JOURNAL OF NANOSCIENCE AND NANOTECHNOLOGY》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112760711A (en) * | 2020-12-14 | 2021-05-07 | 中国科学院过程工程研究所 | Strontium titanate single crystal particle and preparation method and application thereof |
| CN114618537A (en) * | 2022-04-10 | 2022-06-14 | 贵州大学 | Red phosphorus/strontium titanate heterojunction photocatalyst and preparation method and application thereof |
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Application publication date: 20200731 |