CN111663183B - Quasi-single crystal titanium dioxide three-dimensional array containing micro-strain and preparation method thereof - Google Patents
Quasi-single crystal titanium dioxide three-dimensional array containing micro-strain and preparation method thereof Download PDFInfo
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- CN111663183B CN111663183B CN202010448726.7A CN202010448726A CN111663183B CN 111663183 B CN111663183 B CN 111663183B CN 202010448726 A CN202010448726 A CN 202010448726A CN 111663183 B CN111663183 B CN 111663183B
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 62
- 239000013078 crystal Substances 0.000 title claims abstract description 31
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title abstract description 6
- 239000002070 nanowire Substances 0.000 claims abstract description 21
- GROMGGTZECPEKN-UHFFFAOYSA-N sodium metatitanate Chemical compound [Na+].[Na+].[O-][Ti](=O)O[Ti](=O)O[Ti]([O-])=O GROMGGTZECPEKN-UHFFFAOYSA-N 0.000 claims abstract description 19
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims abstract description 5
- 238000010438 heat treatment Methods 0.000 claims abstract description 4
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 239000007864 aqueous solution Substances 0.000 claims description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- 241000282461 Canis lupus Species 0.000 claims description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 3
- 230000002378 acidificating effect Effects 0.000 claims description 3
- 238000002791 soaking Methods 0.000 claims description 3
- 229910052719 titanium Inorganic materials 0.000 claims description 3
- 239000010936 titanium Substances 0.000 claims description 3
- 239000002105 nanoparticle Substances 0.000 claims description 2
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 claims 1
- 239000011941 photocatalyst Substances 0.000 abstract description 6
- 239000003344 environmental pollutant Substances 0.000 abstract description 2
- 231100000719 pollutant Toxicity 0.000 abstract description 2
- 238000000151 deposition Methods 0.000 abstract 1
- 239000000463 material Substances 0.000 description 18
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 12
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 230000015556 catabolic process Effects 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- 230000001699 photocatalysis Effects 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 2
- 238000002524 electron diffraction data Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- DKAGJZJALZXOOV-UHFFFAOYSA-N hydrate;hydrochloride Chemical compound O.Cl DKAGJZJALZXOOV-UHFFFAOYSA-N 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000009281 ultraviolet germicidal irradiation Methods 0.000 description 1
- 239000012855 volatile organic compound Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/16—Oxides
- C30B29/22—Complex oxides
- C30B29/32—Titanates; Germanates; Molybdates; Tungstates
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/8678—Removing components of undefined structure
- B01D53/8687—Organic components
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- 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
- 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
-
- 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
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B19/00—Liquid-phase epitaxial-layer growth
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/16—Oxides
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
- C30B29/62—Whiskers or needles
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
- C30B7/10—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions by application of pressure, e.g. hydrothermal processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/70—Organic compounds not provided for in groups B01D2257/00 - B01D2257/602
- B01D2257/708—Volatile organic compounds V.O.C.'s
Abstract
The invention discloses a micro-strain containing quasi-single crystal titanium dioxide three-dimensional array and a preparation method thereof. Firstly, preparing a monocrystalline sodium titanate nanowire array by a hydrothermal method; then, depositing mesomorphic TiO on the surface of the monocrystal sodium titanate nanowire array2(ii) a Finally, proton exchange and heat treatment are carried out to convert the single crystal sodium titanate into single crystal TiO2And obtaining the final quasi-single crystal titanium dioxide three-dimensional array containing micro strain. The method utilizes mesogenic TiO2Epitaxial growth on the surface of single crystal sodium titanate nanowire, combined with lattice constant difference, on TiO2Introducing tensile strain; then converting the single crystal sodium titanate nanowire into single crystal TiO2Nanowire to obtain single-phase anatase TiO2And has a quasi-single crystal structure as a whole. Compared with the existing method for preparing TiO2Compared with the array technology, the TiO prepared by the method disclosed by the invention2Has the unique characteristics of three-dimensional hierarchical structure, quasi-single crystal structure and uniaxial tensile strain, can be used as a high-performance photocatalyst and is used in the fields of gas-phase pollutant treatment and the like.
Description
Technical Field
The invention relates to a micro-strain-containing quasi-single crystal titanium dioxide three-dimensional array and a preparation method thereof, which are expected to be applied to the fields of photocatalytic environment purification and the like.
Background
TiO2The nano material has potential application prospect in the fields of photocatalysis, solar batteries, lithium ion batteries, sodium ion batteries, gas sensors and the like. TiO 22Depending on its composition, phase structure, microstructure and strain state. The quasi-single crystal structure has excellent charge transmission performance; the three-dimensional array has higher specific surface area and abundant mass transfer channels; the electronic structure of the material can be changed by introducing proper strain into the material, so that the performance of the material can be regulated and controlled. Thus, TiO having the above three important characteristics are produced2The material has important significance and can be widely applied as a high-performance functional material.
Disclosure of Invention
The invention aims to provide a quasi-single crystal titanium dioxide three-dimensional array containing micro strain and a preparation method thereof.
The technical scheme of the invention is as follows:
a preparation method of a quasi-single crystal titanium dioxide three-dimensional array containing micro strain comprises the following steps:
1) carrying out hydrothermal reaction on a titanium sheet in a NaOH aqueous solution with the concentration of 1.25mol/L at 220 ℃ for 20h to obtain the single crystal sodium titanate nanowire array.
2) Putting the sodium titanate nanowire array into TiF with the concentration of 0.04mol/L, pH value of 24Reacting in an acidic aqueous solution at 60 ℃ for 3h to obtain the sodium titanate nanowire array/TiO2An array of mesogenic branches.
3) Sodium titanate nanowire array/TiO2Soaking the mesomorphic branch array in 0.1mol/L hydrochloric acid water solution for 2h for proton exchange, and then performing heat treatment at 450 ℃ for 1h to obtain the strain-containing quasi-single crystal TiO2A three-dimensional array.
The invention utilizes mesogenic TiO2Epitaxial growth on surface of single crystal sodium titanate nanowire, bondingDifference in lattice constant in TiO2Introducing tensile strain; then converting the single crystal sodium titanate nanowire into single crystal TiO2Nanowire to obtain single-phase anatase TiO2And has a quasi-single crystal structure as a whole. TiO prepared by the method disclosed by the invention2Meanwhile, the photocatalyst has a three-dimensional hierarchical structure, a quasi-single crystal structure and uniaxial tensile strain, and can be used as a high-performance photocatalyst for gas-phase pollutant degradation.
Drawings
FIG. 1 is a scanning electron micrograph of a three-dimensional array of titanium dioxide prepared in example 1;
FIG. 2 is an X-ray diffraction pattern of the three-dimensional array of titanium dioxide prepared in example 1;
FIG. 3 is a partial peak position of X-ray diffraction pattern of three-dimensional array of titanium dioxide prepared in example 1 and unstrained TiO2Comparing materials;
FIG. 4 is a TEM photograph of a three-dimensional array of titania prepared in example 1;
FIG. 5 is an electron diffraction pattern of a three-dimensional array of titanium dioxide prepared in example 1;
FIG. 6 shows the degradation of toluene by UV irradiation of the three-dimensional array of titanium dioxide prepared in example 1.
Detailed Description
The present invention will be further illustrated with reference to the following examples, but the present invention is not limited to the following examples.
Example 1
Carrying out hydrothermal reaction on a titanium sheet in a NaOH aqueous solution with the concentration of 1.25mol/L for 20h at 220 ℃ to obtain a sodium titanate nanowire array; putting the sodium titanate nanowire array into TiF with the concentration of 0.04mol/L, pH value of 24Reacting in an acidic aqueous solution at 60 ℃ for 3h to obtain the sodium titanate nanowire array/TiO2An array of particle branches; sodium titanate nanowire array/TiO2Soaking the particle branch array in 0.1mol/L hydrochloric acid aqueous solution for 2h, and then performing heat treatment at 450 ℃ for 1h to obtain the strain-containing quasi-single crystal TiO2A three-dimensional array.
Figure 1 is a scanning electron micrograph of the material obtained,the material can be seen to have a three-dimensional array structure, overall resembling the structure of a "wolf tooth stick", consisting of nanowires of the "trunk" and nanoparticles of the "branches". FIG. 2 is an X-ray diffraction pattern of the material obtained, which was retrieved and compared with a standard card, and which was a single phase anatase TiO2. FIG. 3 shows partial peak positions of X-ray diffraction pattern and unstrained TiO2Comparison of materials, it can be seen that the (200) peak position of the material is shifted to a small angular direction, indicating the presence of [100] within the material]Micro strain in the direction. Fig. 4 is a transmission electron microscope photograph of the material, which can further see the three-dimensional branch structure, and the overall appearance is similar to a wolf tooth stick. FIG. 5 is a selected electron diffraction pattern of the material as discrete diffraction points, but with "broadening" of the diffraction points, illustrating the material having a quasi-single crystal structure.
The effect experimental example of the quasi-single crystal titanium dioxide three-dimensional array containing micro strain as the photocatalyst comprises the following steps:
to further illustrate the application advantages of the microstrain-containing quasi-single crystal titanium dioxide three-dimensional array, the material prepared in example 1 is used as a photocatalyst, and the catalytic performance of the photocatalyst for degrading gas-phase toluene is tested. FIG. 6 shows the material (film area 4.5 cm)2) Under uv light irradiation (light source: PL-L18W/10/4P ultraviolet lamp) to degrade the toluene with the initial concentration of 730ppm, and the material can completely degrade the toluene with the initial concentration of 730ppm within 1 hour, has excellent photocatalytic performance, and is expected to be applied to the fields of degradation of volatile organic compounds and the like.
Claims (2)
1. A quasi-single crystal titanium dioxide three-dimensional array containing micro strain is characterized by comprising the following characteristics: the three-dimensional structure is a pseudo-single crystal structure which is a wolf tooth rod-shaped pseudo-single crystal structure formed by a titanium dioxide nanowire trunk and titanium dioxide nanoparticle branches, and the tensile strain in the direction of [100] exists.
2. A method for preparing a three-dimensional array of microstrain-containing quasi-monocrystalline titanium dioxide according to claim 1, comprising the steps of:
1) carrying out hydrothermal reaction on a titanium sheet in a NaOH aqueous solution with the concentration of 1.25mol/L at 220 ℃ for 20h to obtain a single crystal sodium titanate nanowire array;
2) putting the sodium titanate nanowire array into TiF with the concentration of 0.04mol/L, pH value of 24Reacting in an acidic aqueous solution at 60 ℃ for 3h to obtain the sodium titanate nanowire array/TiO2An array of mesogenic branches;
3) sodium titanate nanowire array/TiO2Soaking the mesomorphic branch array in 0.1mol/L hydrochloric acid aqueous solution for 2h for proton exchange, and then carrying out heat treatment at 450 ℃ for 1h to obtain the quasi-single crystal TiO containing microstrain2A three-dimensional array.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101704511A (en) * | 2009-11-20 | 2010-05-12 | 哈尔滨工业大学 | Preparation method of titanium dioxide nanotube (titanium dioxide nanowire) array heterojunction with visible-light catalytic activity |
| CN105355883A (en) * | 2015-11-18 | 2016-02-24 | 海南大学 | TiN / TiO2 core-shell nanowire array and preparation method |
| CN109967061A (en) * | 2019-02-20 | 2019-07-05 | 浙江大学 | In the method that titanium dioxide microporous surface selective deposition Homogenotic nanometer particle promotes photocatalytic activity |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101704511A (en) * | 2009-11-20 | 2010-05-12 | 哈尔滨工业大学 | Preparation method of titanium dioxide nanotube (titanium dioxide nanowire) array heterojunction with visible-light catalytic activity |
| CN105355883A (en) * | 2015-11-18 | 2016-02-24 | 海南大学 | TiN / TiO2 core-shell nanowire array and preparation method |
| CN109967061A (en) * | 2019-02-20 | 2019-07-05 | 浙江大学 | In the method that titanium dioxide microporous surface selective deposition Homogenotic nanometer particle promotes photocatalytic activity |
Non-Patent Citations (2)
| Title |
|---|
| Pseudocapacitance-Enhanced Li-Ion Microbatteries Derived by a TiN@TiO2 Nanowire Anode;Wei Wen et al.;《Chem》;20170309;第2卷;参见正文第4页第1段，第11页第4段-第12页第3段和图1 * |
| Titanium dioxide nanotrees for high-capacity lithium-ion microbatteries;Wei Wen et al.;《J. Mater. Chem. A》;20160731;第4卷;参见正文第3页图1 * |
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