CN108722384B - Oxygen-enriched vacancy titanium dioxide nanoflower and preparation method thereof - Google Patents
Oxygen-enriched vacancy titanium dioxide nanoflower and preparation method thereof Download PDFInfo
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 161
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 77
- 239000002057 nanoflower Substances 0.000 title claims abstract description 61
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 47
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 47
- 239000001301 oxygen Substances 0.000 title claims abstract description 47
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000000463 material Substances 0.000 claims abstract description 18
- 238000006243 chemical reaction Methods 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 12
- 239000002135 nanosheet Substances 0.000 claims abstract description 12
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 25
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 claims description 12
- POILWHVDKZOXJZ-ARJAWSKDSA-M (z)-4-oxopent-2-en-2-olate Chemical compound C\C([O-])=C\C(C)=O POILWHVDKZOXJZ-ARJAWSKDSA-M 0.000 claims description 10
- ZFFMLCVRJBZUDZ-UHFFFAOYSA-N 2,3-dimethylbutane Chemical group CC(C)C(C)C ZFFMLCVRJBZUDZ-UHFFFAOYSA-N 0.000 claims description 10
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 8
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- 238000009776 industrial production Methods 0.000 abstract description 2
- 238000004729 solvothermal method Methods 0.000 abstract description 2
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- 230000001699 photocatalysis Effects 0.000 description 10
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- 239000000243 solution Substances 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 5
- 229910052739 hydrogen Inorganic materials 0.000 description 5
- 239000001257 hydrogen Substances 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 238000004435 EPR spectroscopy Methods 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
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- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
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- 238000005086 pumping Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
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- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
- B01J21/063—Titanium; Oxides or hydroxides thereof
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Abstract
The invention discloses a preparation method of oxygen-enriched vacancy titanium dioxide nanoflowers. The method comprises the following steps: the oxygen-rich vacancy titanium dioxide nanoflower prepared by the method is self-assembled by ultrathin anatase nanosheets and is rich in a large number of oxygen vacancies. The oxygen-enriched vacancy titanium dioxide nanoflower material is an efficient and stable photoelectric conversion material, is prepared by a solvothermal method, is simple in preparation process, easy to control reaction conditions, and suitable for large-scale preparation and industrial production.
Description
Technical Field
The invention relates to an oxygen-rich vacancy titanium dioxide nanoflower and a preparation method thereof, belonging to the technical field of nano materials, semiconductor oxide materials and photocatalysis.
Background
In recent years, titanium dioxide nanoflowers have been widely used in the field of photocatalysis because of their large specific surface area, good crystal orientation and good separation performance of photogenerated carriers. However, the wider forbidden band width (3.2eV) of the titanium dioxide nanoflower causes that the titanium dioxide nanoflower can only absorb ultraviolet light, and the photocatalytic performance of the titanium dioxide nanoflower is severely limited. At present, researchers propose different strategies to widen the light absorption range of the titanium dioxide nanoflower, and strategies such as noble metal modification, metal or nonmetal ion doping, narrow-bandgap semiconductor compounding and the like are successfully reported, so that the titanium dioxide nanoflower has good photocatalytic activity in a visible light region. At present, it is considered as an effective way to introduce defects into the titanium dioxide nanomaterial to broaden the light absorption range thereof. For example, the introduction of oxygen vacancies into the titanium dioxide crystal lattice can widen the light absorption range of the titanium dioxide crystal lattice, because the introduction of oxygen vacancies can form a shallow donor energy level near the valence band of the titanium dioxide, which means that photons in the visible light region can also excite the titanium dioxide with oxygen-rich vacancy defects, thereby effectively widening the absorption range of the titanium dioxide in the visible light region. Therefore, the introduction of oxygen vacancies in titanium dioxide nanoflower crystals is a very effective strategy to increase the photocatalytic activity of titanium dioxide.
At present, a plurality of methods for preparing titanium dioxide nanoflower materials are reported, and the methods mainly comprise a gas phase method, a hydrothermal method, a chemical precipitation method, a hydrolysis method, a sol-gel method, a microemulsion method and the like. However, a preparation method for introducing oxygen vacancies into titanium dioxide nanoflowers has not been reported, and therefore, it is necessary to develop a simple and convenient method for preparing oxygen-vacancy-rich titanium dioxide nanoflowers. Herein, a one-step simple solvothermal method is employed to introduce oxygen vacancies into the titanium dioxide nanoflowers. The method has the advantages of simple and convenient preparation, controllable oxygen vacancy concentration, high product purity, controllable size of the titanium dioxide nanoflower and the like.
Disclosure of Invention
The invention aims to solve the problems that the photocatalytic efficiency is low due to weak light absorption of titanium dioxide, the monodispersity of the prepared titanium dioxide nanoflower is poor, and the size distribution of a product is wide in the prior art.
The invention adopts the following technical scheme: a preparation method of oxygen-enriched vacancy titanium dioxide nanoflowers comprises the following steps: adding isopropanol into diethylenetriamine, uniformly stirring, adding diisopropyl di (acetylacetonate) titanate, uniformly stirring, pouring into a reaction kettle, carrying out heat treatment at the temperature of 150-220 ℃ for 12-36 hours, washing, and drying to obtain the oxygen-enriched vacancy titanium dioxide nanoflower material.
Furthermore, the volume ratio of the isopropanol, the diethylenetriamine and the diisopropyl bis (acetylacetonate) titanate is 1260-2520: 1-10: 45-360.
Further, the volume ratio of isopropanol, diethylenetriamine and diisopropyl bis (acetylacetonate) titanate is 1260:1:45, the reaction temperature is 200 ℃, and the reaction time is 24 hours.
The oxygen-enriched vacancy titanium dioxide nanoflower is composed of titanium dioxide nanosheets, wherein the titanium dioxide nanosheets are anatase phases and are 2-9 nm in thickness.
The invention has the beneficial effects that: the invention provides a simple preparation method for preparing an oxygen-rich vacancy titanium dioxide nanoflower material, which is characterized in that a large number of oxygen vacancies are simply and conveniently introduced into a titanium dioxide nanoflower, and the size and the shape of the titanium dioxide nanoflower material can be optimized by adjusting the addition of diethylenetriamine. The oxygen-enriched vacancy titanium dioxide nanoflower material is formed by self-assembling anatase titanium dioxide nanosheets and has a three-dimensional hierarchical structure, so that the absorption range of visible light of the titanium dioxide nanoflower can be expanded, the multiple scattering performance of light is improved, photoelectrons are transferred quickly, and more adsorption sites and reaction sites are increased. On the other hand, the oxygen-rich vacancy titanium dioxide nanoflower contains a large number of oxygen vacancies, and the oxygen vacancies can widen the absorption range of the oxygen vacancies in a visible light region, so that the photocatalytic performance of the oxygen-rich vacancy titanium dioxide nanoflower is improved. In addition, the material has simple preparation method, and the nano flower hierarchical structure and size are easy to control and are beneficial to industrial production. Therefore, the invention greatly reduces the production cost of the titanium dioxide nanoflower, obviously improves the photocatalytic performance of the titanium dioxide nanoflower and has great application prospect.
Drawings
Fig. 1 is a Scanning Electron Microscope (SEM) picture of the oxygen-rich vacancy titanium dioxide nanoflowers prepared in example 1.
FIG. 2 is a Transmission Electron Microscope (TEM) picture of the oxygen-rich vacancy titanium dioxide nanoflower prepared in example 1.
FIG. 3 is an X-ray diffraction pattern (XRD) of vacancy rich titanium dioxide produced in example 1.
FIG. 4 shows the Electron Paramagnetic Resonance (EPR) spectrum of the vacancy-rich titanium dioxide nanoflower prepared in example 1.
Fig. 5 is a Scanning Electron Microscope (SEM) picture of the oxygen-rich vacancy titanium dioxide nanoflowers prepared in example 2.
Fig. 6 is a Scanning Electron Microscope (SEM) picture of the oxygen-rich vacancy titanium dioxide nanoflowers prepared in example 3.
FIG. 7 is a graph showing hydrogen production by hydrolysis when the oxygen-rich vacancy titanium dioxide nanoflowers prepared in example 5 are used as a photocatalyst.
The specific implementation mode is as follows:
the present invention will be further described with reference to the following examples. The following examples are intended to illustrate the present invention, but not to limit the present invention, and any modifications and changes made within the spirit of the present invention and the scope of the claims fall within the scope of the present invention.
Example 1:
to 31.5mL of isopropyl alcohol was added 0.025mL of diethylenetriamine (EDTA), and the mixture was stirred for 10 min. To the solution was added 1.125mL of diisopropyl di (acetylacetonate) titanate. Stirring was continued for 10 min. The obtained mixed solution was poured into a reaction vessel and solvent-heat treated at 200 ℃ for 24 hours. And after the reaction is finished, washing the precipitate with deionized water and absolute ethyl alcohol for three times respectively, placing the washed precipitate in a 60 ℃ oven, and drying the washed precipitate for 24 hours to obtain the oxygen-enriched vacancy titanium dioxide nanoflower material.
Fig. 1 and 2 are a Scanning Electron Microscope (SEM) picture and a Transmission Electron Microscope (TEM) picture of the oxygen-rich vacancy titanium dioxide nanoflower prepared in example 1, respectively, from which it can be clearly seen that the size of the oxygen-rich vacancy titanium dioxide nanoflower is 500 to 1000nm, which is formed by self-assembly of ultrathin titanium dioxide nanosheets, and the thickness of the nanosheets is 2 to 9 nm.
FIG. 3 is an X-ray diffraction pattern (XRD) of vacancy rich titanium dioxide nanoflowers prepared in example 1, from which it can be seen that the material diffraction pattern coincides with the characteristic peaks of standard anatase phase titanium dioxide.
Fig. 4 is a paramagnetic resonance spectrum (EPR) diagram of the vacancy-rich titanium dioxide nanoflower prepared in example 1, and it can be seen that the vacancy-rich titanium dioxide nanoflower prepared is rich in a large number of oxygen vacancies.
Example 2:
to 31.5mL of the isopropyl alcohol solution, 0.05mL of diethylenetriamine (EDTA) was added and the mixture was stirred for 10 min. To the solution was added 1.125mL of diisopropyl di (acetylacetonate) titanate. Stirring was continued for 10 min. The resulting mixed solution was poured into a reaction vessel and subjected to solvothermal treatment at 150 ℃ for 36 hours. And after the reaction is finished, washing the precipitate with deionized water and absolute ethyl alcohol for three times respectively, placing the washed precipitate in a 60 ℃ oven, and drying the washed precipitate for 24 hours to obtain the oxygen-enriched vacancy titanium dioxide nanoflower material.
Fig. 5 is a Scanning Electron Microscope (SEM) picture of the oxygen-rich vacancy titanium dioxide nanoflower prepared in example 2, and it can be seen from the figure that the size of the titanium dioxide nanoflower is 100-300 nm, the titanium dioxide nanoflower is formed by self-assembling ultrathin titanium dioxide nanosheets, the thickness of the nanosheets is 2-9 nm, and the size is significantly reduced compared to the titanium dioxide nanoflower obtained in example 1. Further, XRD test and EPR test are carried out on the product, and the result shows that the material is anatase and is rich in a large number of oxygen vacancies.
Example 3:
to 31.5mL of the isopropanol solution was added 1.125mL of diisopropyl di (acetylacetonate) titanate. Stirring for 10 min. The obtained mixed solution was poured into a reaction vessel and solvent-heat treated at 200 ℃ for 24 hours. And after the reaction is finished, washing the precipitate with deionized water and absolute ethyl alcohol for three times respectively, placing the washed precipitate in a 60 ℃ oven, and drying the washed precipitate for 24 hours to obtain a sample.
Fig. 6 is a Scanning Electron Microscope (SEM) picture of the sample prepared in this example, from which it is apparent that, during the preparation process, no diethylenetriamine is added, and the prepared titanium dioxide does not form a hierarchical structure but exists in the form of particles, indicating that the morphology and size of the oxygen-rich vacancy titanium dioxide nanoflowers can be controlled by the amount of added diethylenetriamine.
Example 4:
to 31.5mL of isopropyl alcohol was added 0.025mL of diethylenetriamine (EDTA), and the mixture was stirred for 10 min. To the solution was added 1.125mL of diisopropyl di (acetylacetonate) titanate. Stirring was continued for 10 min. The resulting mixed solution was poured into a reaction vessel and subjected to solvothermal treatment at 220 ℃ for 12 hours. And after the reaction is finished, washing the precipitate with deionized water and absolute ethyl alcohol for three times respectively, placing the washed precipitate in a 60 ℃ oven, and drying the washed precipitate for 24 hours to obtain the oxygen-enriched vacancy titanium dioxide nanoflower material.
The obtained material is in a nanoflower structure, the size of the titanium dioxide nanoflower is 500-1000 nm, the titanium dioxide nanoflower is formed by self-assembly of ultrathin titanium dioxide nanosheets, the thickness of each nanosheet is 2-9 nm, XRD (X-ray diffraction) tests and EPR (ethylene propylene rubber) tests are carried out on the product, and the result shows that the material is anatase and is rich in a large number of oxygen vacancies.
Example 5:
the oxygen-enriched vacancy titanium dioxide nanoflower prepared by the invention can be used as a photocatalyst for efficiently decomposing water to produce hydrogen by photocatalysis, and the specific experimental process is as follows: under a full spectrum, 50mg of the oxygen-rich vacancy titanium dioxide nanoflower prepared in example 1 is ultrasonically dispersed in 100mL of 30% (v/v) methanol solution, vacuum pumping is performed, samples are taken every 1 hour of illumination time, and gas is detected by gas chromatography. Finally, a graph of hydrogen production by photocatalytic decomposition of the oxygen-rich vacancy titanium dioxide nanoflower photocatalyst under a simulated light source is drawn, as shown in fig. 7, it can be known that the oxygen-rich vacancy titanium dioxide nanoflower has an excellent effect on hydrogen production by water decomposition under the excitation of simulated light. The light was irradiated for 5 hours, and the hydrogen production was 120.5. mu. mol/g.
Claims (3)
1. A preparation method of oxygen-enriched vacancy titanium dioxide nanoflowers is characterized by comprising the following steps: adding isopropanol into diethylenetriamine, uniformly stirring, adding diisopropyl di (acetylacetonate) titanate, uniformly stirring, pouring into a reaction kettle, carrying out heat treatment at 150-220 ℃ for 12-36 hours, washing, and drying to obtain the oxygen-rich vacancy titanium dioxide nanoflower material, wherein the oxygen-rich vacancy titanium dioxide nanoflower material consists of titanium dioxide nanosheets, and the titanium dioxide nanosheets are anatase phases and have the thickness of 2-9 nm.
2. The method according to claim 1, wherein the volume ratio of isopropyl alcohol, diethylenetriamine and diisopropyl bis (acetylacetonate) titanate is 1260 to 2520:1 to 10:45 to 360.
3. The method according to claim 2, wherein the volume ratio of isopropyl alcohol, diethylenetriamine and diisopropyl di (acetylacetonate) titanate is 1260:1:45, the reaction temperature is 200 ℃, and the reaction time is 24 hours.
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| CN109663610B (en) * | 2018-11-20 | 2022-04-08 | 浙江理工大学上虞工业技术研究院有限公司 | Preparation method of two-dimensional carbon nitride/two-dimensional titanium dioxide composite material |
| CN109499597B (en) * | 2018-11-20 | 2022-04-01 | 浙江理工大学上虞工业技术研究院有限公司 | Preparation method of porous titanium dioxide/carbon nitride nanoparticle composite material |
| CN109574069B (en) * | 2018-11-21 | 2021-10-12 | 上海大学 | Carbon quantum dot induced titanium dioxide hierarchical nanostructure and preparation method thereof |
| CN109718752B (en) * | 2019-01-27 | 2021-11-12 | 安徽大学 | graphene/TiO2Nanocomposite and method for preparing same |
| CN110589883A (en) * | 2019-09-23 | 2019-12-20 | 安徽师范大学 | Two-dimensional layered titanium dioxide nano material rich in oxygen holes, preparation method and application thereof |
| CN110624527A (en) * | 2019-10-14 | 2019-12-31 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of three-dimensional colored titanium dioxide photocatalytic material, product and application thereof |
| CN111545184A (en) * | 2020-03-31 | 2020-08-18 | 上海电力大学 | Preparation method of oxygen-enriched vacancy titanium dioxide, product and application thereof |
| CN112892515A (en) * | 2021-01-29 | 2021-06-04 | 浙江大学 | All-optical-response titanium dioxide nanotube photocatalyst rich in surface oxygen vacancies and low-temperature preparation method and application thereof |
| CN112939053B (en) * | 2021-01-29 | 2022-11-11 | 浙江大学 | Method for preparing transition metal oxide material containing oxygen vacancy |
| CN115140765B (en) * | 2021-03-30 | 2023-08-01 | 中国科学院大连化学物理研究所 | Method for preparing oxygen vacancy pair defects on surface of rutile titanium oxide (110) |
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| "Hierarchical spheres assembled from large ultrathin anatase TiO2 nanosheets for photocatalytic hydrogen evolution from water splitting";Zixuan Ding et al.;《International Journal of Hydrogen Energy》;20180614;第43卷;第13190-13199页 * |
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