CN113998733A - TiO with continuous two-dimensional nanosheet structure2Method for producing a material - Google Patents
TiO with continuous two-dimensional nanosheet structure2Method for producing a material Download PDFInfo
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- CN113998733A CN113998733A CN202111263396.5A CN202111263396A CN113998733A CN 113998733 A CN113998733 A CN 113998733A CN 202111263396 A CN202111263396 A CN 202111263396A CN 113998733 A CN113998733 A CN 113998733A
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- dimensional nanosheet
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- 239000000463 material Substances 0.000 title claims abstract description 37
- 239000002135 nanosheet Substances 0.000 title claims abstract description 26
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 27
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims abstract description 27
- 238000004729 solvothermal method Methods 0.000 claims abstract description 10
- 239000003960 organic solvent Substances 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 7
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 6
- 239000010936 titanium Substances 0.000 claims abstract description 6
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 23
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 10
- 238000002360 preparation method Methods 0.000 claims description 6
- 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 4
- 239000002064 nanoplatelet Substances 0.000 claims 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 abstract description 13
- 238000007146 photocatalysis Methods 0.000 abstract description 3
- 230000001699 photocatalysis Effects 0.000 abstract description 3
- 239000011806 microball Substances 0.000 abstract description 2
- 238000001816 cooling Methods 0.000 description 5
- 238000001035 drying Methods 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
- 238000005406 washing Methods 0.000 description 5
- 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 4
- 239000002086 nanomaterial Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 2
- 239000004005 microsphere Substances 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000013590 bulk material Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000007810 chemical reaction solvent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
Images
Classifications
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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
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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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
-
- 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
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
-
- 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 TiO with a continuous two-dimensional nanosheet structure2A method of preparing a material comprising: uniformly mixing a titanium source and an organic solvent, and carrying out solvothermal reaction for 12-24h at the temperature of 180-220 ℃ to obtain TiO with a special hollow structure2Micro-balls; the organic solvent is prepared from acetic acid and acetonitrile in a volume ratio of 1: (1-4). The invention also discloses TiO with a continuous two-dimensional nanosheet structure2A material. The invention prepares TiO with continuous two-dimensional nanosheet structure by a simple solvothermal method2The material has the advantages of mild reaction conditions, simple process, strong controllability and good reproducibility, and the prepared TiO has the advantages of2The material has wide application in the fields of solar cells, ion batteries, photocatalysis and the like.
Description
Technical Field
The invention relates to the technical field of inorganic nano material preparation, in particular to a preparation method of a TiO2 material with a continuous two-dimensional nanosheet structure.
Background
In recent years, with the rise of graphene materials, two-dimensional nanomaterials have attracted great research interests of broad researchers. The two-dimensional material has larger transverse dimension and thickness of atomic level, and can show the characteristics of high surface atomic ratio, anisotropic electrical property, adjustable band gap, high surface reactivity and the like. Compared with a bulk material, the coordination number, bond angle and bond length of atoms on the surface of the two-dimensional material are different, and abundant surface active sites can be provided for chemical reaction. Secondly, the specific surface area of the two-dimensional material is huge, and in the reaction process, the two-dimensional material has a larger contact area with a reaction solution, so that more reactants can be adsorbed, and the reaction can be promoted to be carried out more quickly. Again, the reduced thickness significantly reduces the distance that photogenerated charges migrate from the interior of the material to the surface of the material, thereby enabling faster reaction kinetics. And finally, the abundant defects on the surface of the two-dimensional material are utilized to carry out functional modification, so that the light absorption capacity of the material is improved, the charge separation and transfer efficiency is improved, and the surface oxidation-reduction reaction rate is accelerated. Due to unique electrical, optical and chemical properties, two-dimensional materials are widely applied to the fields of optoelectronic devices, catalysis, energy storage and conversion and the like.
TiO2Has the advantages of wide forbidden band width, no toxicity, good chemical stability and the like, and is widely applied to the fields of solar cells, ion batteries, photocatalysis, antibacterial materials and the like in recent years. Therefore, to further enhance TiO2The performance of the material is reasonably designed into TiO2Micro-nano structure, preparing TiO with two-dimensional nano structure2The material and the preparation method thereof are simplified, and the method has important significance.
Disclosure of Invention
Based on the technical problems in the prior art, the invention provides TiO with a continuous two-dimensional nanosheet structure2A method for preparing the material.
The invention provides TiO with a continuous two-dimensional nanosheet structure2A method of preparing a material comprising: uniformly mixing a titanium source and an organic solvent, and carrying out solvothermal reaction for 12-24h at the temperature of 180-220 ℃ to obtain TiO with a special hollow structure2Micro-balls; the organic solvent is prepared from acetic acid and acetonitrile in a volume ratio of 1: (1-4).
Preferably, the titanium source is tetra-n-butyl titanate, tetra-isopropyl titanate, or a combination thereof.
Preferably, the volume ratio of the titanium source to the organic solvent is 1: (20-30).
TiO with continuous two-dimensional nanosheet structure2The material is prepared by the preparation method.
Preferably, the TiO is2The material being formed of continuous two-dimensional TiO2Nanosheet, said two-dimensional TiO2The thickness of the nano-sheet is 10-15 nm.
The invention has the following beneficial effects:
the invention adopts the mixture of two conventional solvents of acetic acid and acetonitrile as a reaction solvent for the first time, and prepares TiO with a continuous two-dimensional nanosheet structure by a simple solvothermal method2The material has no template and post-treatment steps in the preparation process, has the advantages of mild reaction conditions, simple process, strong controllability and good reproducibility, and the prepared TiO has the advantages of2The material has wide application in the fields of solar cells, ion batteries, photocatalysis and the like.
Drawings
FIG. 1 shows TiO prepared in example 12SEM image of the material.
FIG. 2 shows TiO prepared in comparative example 12SEM image of the material.
Detailed Description
The technical solution of the present invention will be described in detail below with reference to specific examples.
Example 1
Uniformly mixing 10mL of acetic acid and 40mL of acetonitrile, adding 2mL of tetrabutyl titanate, uniformly stirring, adding into a reaction kettle, carrying out solvothermal reaction for 16h at 200 ℃, naturally cooling, centrifuging, washing and drying to obtain the TiO with the continuous two-dimensional nanosheet structure2The thickness of the nano-sheet is 10-15 nm.
Example 2
Uniformly mixing 20mL of acetic acid and 30mL of acetonitrile, adding 2mL of tetrabutyl titanate, uniformly stirring, adding into a reaction kettle, carrying out solvothermal reaction for 16h at 200 ℃, naturally cooling, centrifuging, washing and drying to obtain the TiO with the continuous two-dimensional nanosheet structure2The thickness of the nano-sheet is 10-15 nm.
Example 3
Adding 2mL of tetrabutyl titanate into 50mL of organic solvent (wherein the organic solvent is formed by mixing acetic acid and acetonitrile according to a volume ratio of 1: 1), uniformly stirring, adding into a reaction kettle, carrying out solvothermal reaction at 180 ℃ for 24h, naturally cooling, centrifuging, washing and drying to obtain the TiO with the continuous two-dimensional nanosheet structure2The thickness of the nano-sheet is 10-15 nm.
Example 4
Uniformly mixing 25mL of acetic acid and 25mL of acetonitrile, adding 2mL of tetra-n-butyl titanate, uniformly stirring, adding into a reaction kettle, carrying out solvothermal reaction for 12h at 220 ℃, naturally cooling, centrifuging, washing and drying to obtain TiO with a continuous two-dimensional nanosheet structure2The thickness of the nano-sheet is 10-15 nm.
Comparative example 1
Uniformly mixing 5mL of acetic acid and 45mL of acetonitrile, adding 2mL of tetrabutyl titanate, uniformly stirring, adding into a reaction kettle, carrying out solvothermal reaction for 16h at 200 ℃, naturally cooling, centrifuging, washing and drying to obtain TiO2A material.
FIG. 1 is the TiO prepared in example 12The material has a continuous two-dimensional nanosheet structure, and the thickness of the nanosheets is 10-15 nm. FIG. 2 is TiO prepared in comparative example 12Material, it can be seen that the material consists of nanoparticles and irregular microspheres, the size of the nanoparticles being<100nm, and the diameter of the microsphere is 1-2 μm.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (4)
1. TiO with continuous two-dimensional nanosheet structure2The preparation method of the material is characterized by comprising the following steps: uniformly mixing a titanium source and an organic solvent, and carrying out solvothermal reaction for 12-24h at the temperature of 180-220 ℃ to obtain TiO with a special hollow structure2Micron meterA ball; the organic solvent is prepared from acetic acid and acetonitrile in a volume ratio of 1: (1-4).
2. TiO with continuous two-dimensional nanoplatelet structure according to claim 12A method of preparing a material, characterized in that the titanium source is tetra-n-butyl titanate, tetra-isopropyl titanate, or a combination thereof.
3. TiO with continuous two-dimensional nanosheet structure2A material produced by the production method according to claim 1 or 2.
4. TiO with continuous two-dimensional nanoplatelet structures according to claim 32Material, characterized in that the TiO is2The material being formed of continuous two-dimensional TiO2Nanosheet, said two-dimensional TiO2The thickness of the nano-sheet is 10-15 nm.
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Citations (9)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1749172A (en) * | 2004-09-15 | 2006-03-22 | 中国科学院合肥物质科学研究院 | The preparation method of titanium dioxide nano mesoporous balls |
JP2006290680A (en) * | 2005-04-11 | 2006-10-26 | National Institute Of Advanced Industrial & Technology | Spherical nanoparticle porous body and method for synthesizing the same |
CN103896330A (en) * | 2012-12-28 | 2014-07-02 | 中国科学院上海硅酸盐研究所 | Modified titanium dioxide, preparation method thereof and solar cell prepared thereby |
CN104787800A (en) * | 2015-04-14 | 2015-07-22 | 济南大学 | Flower-ball-shaped titanium dioxide and preparation method thereof |
CN105399140A (en) * | 2015-11-26 | 2016-03-16 | 遵义医学院 | Preparation method for anatase nano TiO2 by using titanium tetrachloride-acetonitrile as intermediate |
US20170267542A1 (en) * | 2014-08-20 | 2017-09-21 | Beijing Normal University | Synthesis method for tio2 nanocrystal |
CN107278198A (en) * | 2014-12-23 | 2017-10-20 | 埃西勒国际通用光学公司 | A kind of continuous current method for being used to manufacture the metal oxide nanoparticles that surface is modified by supercritical solvent thermal synthesis |
CN110124701A (en) * | 2019-06-25 | 2019-08-16 | 泉州师范学院 | A kind of preparation method and applications of molybdenum disulfide quantum dot/titanium dioxide nanoplate composite photo-catalyst |
WO2019195916A1 (en) * | 2018-04-13 | 2019-10-17 | Nanophyll Inc. | Self-cleaning and anti-fouling graphene oxide/tio2 photoactive coating and large scale bonding-to- surface process thereof |
-
2021
- 2021-10-28 CN CN202111263396.5A patent/CN113998733B/en active Active
Patent Citations (9)
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CN1749172A (en) * | 2004-09-15 | 2006-03-22 | 中国科学院合肥物质科学研究院 | The preparation method of titanium dioxide nano mesoporous balls |
JP2006290680A (en) * | 2005-04-11 | 2006-10-26 | National Institute Of Advanced Industrial & Technology | Spherical nanoparticle porous body and method for synthesizing the same |
CN103896330A (en) * | 2012-12-28 | 2014-07-02 | 中国科学院上海硅酸盐研究所 | Modified titanium dioxide, preparation method thereof and solar cell prepared thereby |
US20170267542A1 (en) * | 2014-08-20 | 2017-09-21 | Beijing Normal University | Synthesis method for tio2 nanocrystal |
CN107278198A (en) * | 2014-12-23 | 2017-10-20 | 埃西勒国际通用光学公司 | A kind of continuous current method for being used to manufacture the metal oxide nanoparticles that surface is modified by supercritical solvent thermal synthesis |
CN104787800A (en) * | 2015-04-14 | 2015-07-22 | 济南大学 | Flower-ball-shaped titanium dioxide and preparation method thereof |
CN105399140A (en) * | 2015-11-26 | 2016-03-16 | 遵义医学院 | Preparation method for anatase nano TiO2 by using titanium tetrachloride-acetonitrile as intermediate |
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