CN115974146A - Preparation method of (001) oriented rod-shaped anatase TiO2 mesocrystal - Google Patents
Preparation method of (001) oriented rod-shaped anatase TiO2 mesocrystal Download PDFInfo
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- CN115974146A CN115974146A CN202211551231.2A CN202211551231A CN115974146A CN 115974146 A CN115974146 A CN 115974146A CN 202211551231 A CN202211551231 A CN 202211551231A CN 115974146 A CN115974146 A CN 115974146A
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- oriented rod
- anatase tio2
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 91
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 27
- 238000003756 stirring Methods 0.000 claims abstract description 22
- 238000006243 chemical reaction Methods 0.000 claims abstract description 21
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims abstract description 10
- ITHZDDVSAWDQPZ-UHFFFAOYSA-L barium acetate Chemical compound [Ba+2].CC([O-])=O.CC([O-])=O ITHZDDVSAWDQPZ-UHFFFAOYSA-L 0.000 claims abstract description 10
- 239000008367 deionised water Substances 0.000 claims abstract description 8
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 239000002243 precursor Substances 0.000 claims abstract description 8
- 238000005406 washing Methods 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000002904 solvent Substances 0.000 claims abstract description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 7
- 238000004729 solvothermal method Methods 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 2
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 230000003115 biocidal effect Effects 0.000 abstract 1
- 230000001699 photocatalysis Effects 0.000 abstract 1
- 238000007146 photocatalysis Methods 0.000 abstract 1
- 230000003197 catalytic effect Effects 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 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 description 1
- 239000000969 carrier Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 238000000024 high-resolution transmission electron micrograph Methods 0.000 description 1
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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Abstract
The invention discloses a preparation method of (001) oriented rod-shaped anatase TiO2 mesocrystals, wherein a butyl titanate precursor and tetraethyl orthosilicate are mixed and stirred according to a certain proportion; stirring and dissolving barium acetate in an acetic acid solvent; then mixing the two solutions, and reacting for several hours under the condition of 180 ℃ solvent heat to obtain a white sample; and (001) removing and washing a sample by using deionized water to obtain the (001) oriented rod-shaped anatase TiO2 mesocrystal, wherein the length of the mesocrystal is 80-120nm, and the width of the mesocrystal is 18-25nm. The obtained anatase T iO2 mesocrystal has high crystallinity, large specific surface area and specific (001) oriented growth, is suitable for the fields of photocatalysis, antibiosis, environmental protection, photoelectric conversion and the like, and has very wide application prospect.
Description
Technical Field
The invention belongs to the technical field of functional materials, and relates to a preparation method of (001) oriented rod-shaped anatase TiO2 mesocrystals.
Background
Anatase TiO2 is a typical semiconductor material, has good stability, no toxicity, low price, strong light absorption capacity and excellent photoelectric specificity, can be widely applied to various fields such as environmental protection, cosmetics, coatings, energy conversion, catalysis, self-cleaning and the like, is always popular in the research of nano materials at home and abroad, and is often required to have larger specific surface area and good crystallinity when being used for sewage treatment, photoelectric conversion and catalytic materials so as to increase the contact area and the carrier transmission speed and improve the catalytic efficiency or the conversion efficiency.
Mesocrystals, which are an emerging class of materials, attract people's attention, have special structures, properties and atypical crystallization processes different from traditional single crystals and polycrystals, are generally formed by assembling, arranging and growing nano-crystalline particles along a certain direction, can have high crystallinity and large specific surface area at the same time, and have important application values in practical life use and industrial production.
Meanwhile, a great deal of recent documents report that the synergistic effect of the (001) orientation and the (101) direction of anatase TiO2 can greatly improve the spatial separation efficiency of carriers, electrons tend to move along the (101) direction, holes tend to move along the (001) direction, and the reduction of the recombination rate of electron-hole pairs is beneficial to the remarkable improvement of catalytic efficiency or photoelectric conversion efficiency.
Disclosure of Invention
The invention aims to provide a preparation method of (001) oriented rod-shaped anatase TiO2 mesocrystals, which is simple to operate, high in yield and easy to produce.
The technical scheme of the invention is as follows:
a preparation method of (001) oriented rod-shaped anatase TiO2 mesocrystals comprises the following specific steps:
step 1, uniformly mixing and stirring a tetrabutyl titanate precursor and tetraethyl orthosilicate;
step 2, stirring and dissolving barium acetate in an acetic acid solvent;
step 3, slowly adding the solution obtained in the step 2 into the system obtained in the step 1, and continuously stirring uniformly;
step 4, transferring the reaction system obtained in the step 3 to a reaction kettle for solvothermal reaction;
and 5, centrifugally washing the product obtained in the step 4 by deionized water and ethanol to obtain the (001) oriented rod-shaped anatase TiO2 mesocrystal.
Further, the mass ratio of tetraethyl orthosilicate to butyl titanate in the step 1 is 0.01-0.08;
further, the mass ratio of barium acetate to butyl titanate in the step 2 is 0.1-0.5, and the mass ratio of acetic acid to butyl titanate is 5;
further, the solvothermal reaction temperature in the step 4 is 180 ℃, and the reaction time is 10-16 hours.
Compared with the prior art, the invention has the beneficial effects that:
(1) The preparation method has low cost, easily obtained raw materials, simple and easily controlled process flow and large-scale synthesis production;
(2) The prepared anatase TiO2 rod-shaped mesocrystal is oriented along (001), uniform in size and monodispersity, has the characteristics of large specific surface area, high crystallinity and (001) orientation, and is greatly helpful for improving the catalytic efficiency, the energy conversion efficiency and the photoelectric conversion efficiency.
Drawings
FIG. 1 is an X-ray diffraction pattern of a rod-like anatase T iO2 mesocrystal synthesized in example 1;
FIG. 2 is a transmission electron microscope photograph of the rod-like anatase TiO2 mesocrystal synthesized in example 1;
FIG. 3 is a high resolution TEM image of anatase rod-like mesocrystals of TiO2 synthesized in example 1.
Detailed Description
The following detailed description of the preferred embodiments of the present invention, taken in conjunction with the accompanying drawings, will make the advantages and features of the invention easier to understand by those skilled in the art, and thus will clearly and clearly define the scope of the invention.
Referring to fig. 1-3, specific embodiments are provided:
example 1:
a preparation method of (001) oriented rod-shaped anatase TiO2 mesocrystals comprises the following steps:
step 1, mixing and stirring 2.0g of a butyl titanate precursor and 0.08g of tetraethyl orthosilicate for 1 hour;
step 2, stirring and dissolving 0.5g of barium acetate and 10g of acetic acid for 1 hour;
step 3, slowly adding the solution obtained in the step 2 into the system obtained in the step 1, and continuously stirring for 1 hour;
step 4, transferring the reaction system obtained in the step 3 into a reaction kettle, and reacting for 12 hours at 180 ℃;
and 5, centrifugally washing the product obtained in the step 4 by using deionized water and absolute ethyl alcohol to obtain the (001) oriented rod-shaped anatase TiO2 mesocrystal.
The X-ray diffraction pattern is shown in FIG. 1, the transmission electron micrograph is shown in FIG. 2, and the high-resolution transmission electron micrograph is shown in FIG. 3.
Example 2:
a preparation method of (001) oriented rod-shaped anatase TiO2 mesocrystals comprises the following steps:
step 1, mixing and stirring 2.0g of a butyl titanate precursor and 0.04g of tetraethyl orthosilicate for 1 hour;
step 2, stirring and dissolving 0.8g of barium acetate and 10g of acetic acid for 1 hour;
step 3, slowly adding the solution obtained in the step 2 into the system obtained in the step 1, and continuously stirring for 1 hour;
step 4, transferring the reaction system obtained in the step 3 into a reaction kettle, and reacting for 14 hours at 180 ℃;
and 5, centrifugally washing the product obtained in the step 4 by using deionized water and absolute ethyl alcohol to obtain the (001) oriented rod-shaped anatase TiO2 mesocrystal.
Example 3:
a preparation method of (001) oriented rod-shaped anatase TiO2 mesocrystals comprises the following steps:
step 1, mixing and stirring 4.0g of a butyl titanate precursor and 0.12g of tetraethyl orthosilicate for 1 hour;
step 2, stirring and dissolving 1.2g of barium acetate and 20g of acetic acid for 1 hour;
step 3, slowly adding the solution obtained in the step 2 into the system obtained in the step 1, and continuously stirring for 1 hour;
step 4, transferring the reaction system obtained in the step 3 into a reaction kettle, and reacting for 12 hours at 180 ℃;
and 5, centrifugally washing the product obtained in the step 4 by using deionized water and absolute ethyl alcohol to obtain the (001) oriented rod-shaped anatase TiO2 mesocrystal.
Example 4:
a preparation method of (001) oriented rod-shaped anatase TiO2 mesocrystals comprises the following steps:
step 1, mixing and stirring 2.0g of a butyl titanate precursor and 0.02g of tetraethyl orthosilicate for 1 hour;
step 2, stirring and dissolving 0.2g of barium acetate and 10g of acetic acid for 1 hour;
step 3, slowly adding the solution obtained in the step 2 into the system obtained in the step 1, and continuously stirring for 1 hour;
step 4, transferring the reaction system obtained in the step 3 into a reaction kettle, and reacting for 10 hours at 180 ℃;
and 5, centrifugally washing the product obtained in the step 4 by using deionized water and absolute ethyl alcohol to obtain the (001) oriented rod-shaped anatase TiO2 mesocrystal.
Example 5:
a preparation method of (001) oriented rod-shaped anatase TiO2 mesocrystals comprises the following steps:
step 1, mixing and stirring 2.0g of a butyl titanate precursor and 0.16g of tetraethyl orthosilicate for 1 hour;
step 2, stirring and dissolving 1.0g of barium acetate and 10g of acetic acid for 1 hour;
step 3, slowly adding the solution obtained in the step 2 into the system obtained in the step 1, and continuously stirring for 1 hour;
step 4, transferring the reaction system obtained in the step 3 into a reaction kettle, and reacting for 16 hours at 180 ℃;
and 5, centrifugally washing the product obtained in the step 4 by using deionized water and absolute ethyl alcohol to obtain the (001) oriented rod-shaped anatase TiO2 mesocrystal.
The above description is only a preferred embodiment of the present invention, and the scope of the present invention is not limited to the above embodiment, but equivalent modifications or changes made by those skilled in the art according to the present disclosure should be included in the scope of the present invention as set forth in the appended claims.
Claims (5)
1. A preparation method of (001) oriented rod-shaped anatase TiO2 mesocrystals is characterized by comprising the following steps: the method comprises the following specific steps:
step 1, mixing and stirring a butyl titanate precursor and tetraethyl orthosilicate uniformly;
step 2, stirring and dissolving barium acetate in an acetic acid solvent;
step 3, slowly adding the solution obtained in the step 2 into the system obtained in the step 1, and continuously stirring uniformly;
step 4, transferring the reaction system obtained in the step 3 to a reaction kettle for solvothermal reaction;
and 5, centrifugally washing the product obtained in the step 4 by deionized water and ethanol to obtain the (001) oriented rod-shaped anatase TiO2 mesocrystal.
2. The method for preparing (001) oriented rod-like anatase TiO2 mesocrystals according to claim 1, characterized in that: the mass ratio of tetraethyl orthosilicate to butyl titanate in the step 1 is 0.01-0.08.
3. The method for preparing (001) oriented rod-like anatase TiO2 mesocrystals according to claim 1, characterized in that: the mass ratio of barium acetate to butyl titanate in the step 2 is 0.1-0.5.
4. The method of preparing (001) oriented rod-like anatase TiO2 mesocrystals according to claim 1, characterized in that: the solvothermal reaction temperature in the step 4 is 180 ℃, and the reaction time is 10-16 hours.
5. The method of preparing (001) oriented rod-like anatase TiO2 mesocrystals according to claim 1, characterized in that: the length of the TiO2 mesocrystal is 80-120nm, and the width is 18-25nm.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202211551231.2A CN115974146A (en) | 2022-12-05 | 2022-12-05 | Preparation method of (001) oriented rod-shaped anatase TiO2 mesocrystal |
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| CN202211551231.2A CN115974146A (en) | 2022-12-05 | 2022-12-05 | Preparation method of (001) oriented rod-shaped anatase TiO2 mesocrystal |
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| CN202211551231.2A Pending CN115974146A (en) | 2022-12-05 | 2022-12-05 | Preparation method of (001) oriented rod-shaped anatase TiO2 mesocrystal |
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- 2022-12-05 CN CN202211551231.2A patent/CN115974146A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| XIAXIA YAO ET AL.: "Simultaneous photocatalytic degradation of ibuprofen and H2 evolution over Au/sheaf-like TiO2 mesocrystals", CHEMOSPHERE, vol. 261, 23 July 2020 (2020-07-23), pages 1 - 11, XP086307392, DOI: 10.1016/j.chemosphere.2020.127759 * |
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