CN109052464B - High-temperature phase TiO2(B) Method for producing a material - Google Patents
High-temperature phase TiO2(B) Method for producing a material Download PDFInfo
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- 229910010251 TiO2(B) Inorganic materials 0.000 title claims abstract description 35
- 239000000463 material Substances 0.000 title claims abstract description 22
- 238000004519 manufacturing process Methods 0.000 title description 3
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000002360 preparation method Methods 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000002243 precursor Substances 0.000 claims abstract description 11
- 238000003756 stirring Methods 0.000 claims abstract description 10
- 230000003647 oxidation Effects 0.000 claims abstract description 8
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 8
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 claims abstract description 6
- 239000012153 distilled water Substances 0.000 claims abstract description 4
- 238000001704 evaporation Methods 0.000 claims abstract description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical group F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 30
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 claims description 11
- 239000010936 titanium Substances 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 9
- 229910000040 hydrogen fluoride Inorganic materials 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 6
- 239000011775 sodium fluoride Substances 0.000 claims description 6
- 239000000725 suspension Substances 0.000 claims description 6
- 235000013024 sodium fluoride Nutrition 0.000 claims 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 claims description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 229910052719 titanium Inorganic materials 0.000 claims description 2
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 claims description 2
- 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 2
- YONPGGFAJWQGJC-UHFFFAOYSA-K titanium(iii) chloride Chemical compound Cl[Ti](Cl)Cl YONPGGFAJWQGJC-UHFFFAOYSA-K 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 10
- 230000008859 change Effects 0.000 abstract description 5
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 abstract description 4
- 229910001416 lithium ion Inorganic materials 0.000 abstract description 4
- 230000001699 photocatalysis Effects 0.000 abstract description 3
- 238000007146 photocatalysis Methods 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 21
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 9
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 8
- 239000008367 deionised water Substances 0.000 description 8
- 229910021641 deionized water Inorganic materials 0.000 description 8
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 238000000349 field-emission scanning electron micrograph Methods 0.000 description 6
- 239000000706 filtrate Substances 0.000 description 6
- 238000001027 hydrothermal synthesis Methods 0.000 description 6
- 239000007787 solid Substances 0.000 description 5
- 230000007704 transition Effects 0.000 description 5
- 230000007935 neutral effect Effects 0.000 description 4
- 238000000967 suction filtration Methods 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- 239000002074 nanoribbon Substances 0.000 description 3
- 230000009466 transformation Effects 0.000 description 3
- 230000009471 action Effects 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000005530 etching Methods 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 239000003112 inhibitor Substances 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000004729 solvothermal method Methods 0.000 description 2
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000008034 disappearance Effects 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 229920003048 styrene butadiene rubber Polymers 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 230000001131 transforming effect Effects 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
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
-
- 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
-
- B01J35/33—
-
- B01J35/39—
-
- 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
- C01G23/07—Producing by vapour phase processes, e.g. halide oxidation
Abstract
The invention discloses high-temperature phase TiO2(B) The preparation method of the material comprises the steps of preparing TiO by a traditional method2(B) Precursor or pure phase TiO2(B) Then fluoride, distilled water and TiO2(B) Precursor or pure phase TiO2(B) Uniformly mixing and stirring, slowly evaporating to dryness, and then performing high-temperature thermal oxidation treatment in the atmosphere to obtain high-temperature phase TiO with excellent stability2(B) In that respect The preparation method is simple, the raw materials are low in price, the materials do not have complete phase change at a higher temperature, the thermal stability is good, the green and environment-friendly effects are achieved, and the preparation method can be effectively applied to the fields of photocatalysis, electrocatalysis, photoelectrocatalysis, lithium ion batteries and the like.
Description
Technical Field
The invention belongs to the technical field of photocatalytic degradation of pollutants, and particularly relates to high-temperature phase TiO2(B) A method for preparing the material.
Background
TiO2(B) The titanium dioxide is a metastable titanium oxide homogeneous variant with smaller density and loose structure than anatase and rutile, and has attracted attention in the fields of lithium ion batteries, capacitors, sensors, photocatalysis, photoelectrocatalysis and the like. At present, one can prepare TiO by various methods2(B) The conventional preparation method is acetic acid solvothermal method (Changhua Wang, XitongZhang and Yichun Liu. Cooexistance of an anatase/TiO)2(B) heterojunction and anexposed (001) facet in TiO2nanoribbon photocatalysts synthesized via afluorine-free route and topotactic transformation[J]Nanoscale, 2014, 6: 5329-one 5337.), strong alkali hydrothermal method (Yan X, Zhang Y, Zhu K, et al2(B)nanoribbons using the styrene butadiene rubber andsodium carboxyl methyl cellulose water binder [J]Journal of Power Sources,2014, 246: 95-102.), ethylene glycol Solvothermal method (Cellpover, Linghui)Hydro-thermal synthesis of high purity TiO from Qin Wei Wen Xiao2(B) Study of nanowires and lithium cell Properties thereof [ J]Functional materials, 2015,9(46): 09148-2-B as anode material[J]J, Cent, South Univ. technol.2011, 18: 406-2(B): An Anode for Lithium-Ion Batteries[J]2012, 124: 2206-2-B nanoribbon thin films for dye-sensitized solar cells[J]Thinsloid Films, 2010, 519 (2): 662-665), and the like. Among these methods, hydrothermal methods are attracting much attention because of their simple preparation method and low cost. However, these methods produce TiO2(B) After the temperature is over 500 ℃, the crystal phase can be gradually transformed into an anatase phase, thereby limiting the application of the anatase phase in some fields. At present, TiO inhibition at high temperature is not available2(B) And (5) reporting phase transition.
Disclosure of Invention
The invention aims to provide high-temperature phase TiO2(B) A method for preparing the material.
Aiming at the purposes, the technical scheme adopted by the invention is as follows: fluoride and TiO2(B) Precursor or pure phase TiO2(B) Adding distilled water, stirring for 1-10 h, drying the obtained turbid liquid in a drying oven by distillation, and performing thermal oxidation treatment at 600-950 ℃ in a muffle furnace in an atmospheric atmosphere to obtain high-temperature phase TiO2(B) A material.
The fluoride is hydrofluoric acid or sodium fluoride, and the mass concentration of hydrogen fluoride or sodium fluoride in the obtained suspension is preferably 0.1 to 0.5%.
In the above production method, fluoride and TiO are preferably used2(B) Precursor or pure phase TiO2(B) Adding distilled water and stirring for 4-6 h.
In the preparation method, the evaporation temperature is 60-90 ℃.
In the preparation method, the thermal oxidation treatment temperature is preferably 700-800 ℃, the time is 1-3 h, and the heating rate is 3-10 ℃/min.
The above pure phase of TiO2(B) The titanium source is any one or a mixture of more than two of isopropyl titanate, titanium tetra-n-butoxide, titanium trichloride and titanium tetrachloride.
The above TiO2(B) The precursor is H2Ti4O9、H2Ti2O5、H2Ti5O11And the like.
The invention has the following beneficial effects:
the invention can greatly slow down TiO by the participation of phase transition inhibitor HF or sodium fluoride2(B) Phase transformation process, relatively more TiO is still remained under high temperature condition2(B) And, the presence of this structure promotes the formation of TiO at high temperatures2(B) A/anatase heterogeneous junction structure.
The preparation method is simple, the raw materials are low in price, and the obtained TiO2(B) The material has good thermal stability, does not generate phase change at higher temperature, and can be effectively applied to the fields of photocatalysis, electrocatalysis, lithium ion batteries and the like.
Drawings
FIG. 1 is an XRD diffraction pattern of samples obtained in examples 1 to 3 and comparative examples 1 to 3.
FIG. 2 is a field emission scanning electron micrograph of the sample obtained in example 1.
FIG. 3 is a field emission scanning electron micrograph of the sample obtained in example 2.
FIG. 4 is a field emission scanning electron micrograph of the sample obtained in example 3.
FIG. 5 is a field emission scanning electron micrograph of the sample obtained in comparative example 1.
FIG. 6 is a field emission scanning electron micrograph of the sample obtained in comparative example 2.
FIG. 7 is a field emission scanning electron micrograph of the sample obtained in comparative example 3.
Detailed Description
The invention will be further described in detail with reference to the following figures and examples, but the scope of the invention is not limited to these examples.
Example 1
6 mL of titanium tetra-n-butoxide and 3mL of acetic acid were added to 20 mL of ethylene glycol, and the mixture was stirred uniformly for 15 min, then 30mL of a 15 mol/L aqueous NaOH solution was added, and stirring was continued for 10 min. Transferring the obtained mixed solution to a 100 mL hydrothermal reaction kettle, placing the kettle in an oven, keeping the temperature of the kettle at 180 ℃ for 12 h, naturally cooling the kettle to room temperature, taking out the kettle, performing suction filtration, washing the obtained product to be neutral by using deionized water and ethanol, stirring the obtained filtrate in 300 mL 0.1 mol/L HCl aqueous solution for 12 h, performing suction filtration, washing the filtrate to be neutral by using the deionized water and ethanol, and drying the filtrate at 80 ℃ for 12 h to obtain TiO2(B) Precursor H2Ti4O9. 0.3 g of TiO2(B) Precursor H2Ti4O9Dispersing the hydrogen fluoride and 0.01 mL of hydrofluoric acid (the mass fraction of the hydrogen fluoride is 49%) in 10mL of deionized water, placing the deionized water in a 20 mL small crucible, and uniformly stirring for 4 h to form uniformly dispersed suspension, wherein the mass fraction of the hydrogen fluoride in the obtained suspension is 0.1%; then putting the mixture into a drying oven for drying for 8 h at the temperature of 80 ℃, grinding the obtained white solid, and then putting the ground white solid into a muffle furnace for thermal oxidation treatment for 2 h at the temperature of 750 ℃ in the atmosphere to obtain high-temperature phase TiO2(B) Materials, noted 0.1% F-HT.
Example 2
In this example, the amount of hydrofluoric acid used was 0.03 mL, and the other steps were the same as in example 1 to obtain high-temperature phase TiO2(B) Material, 0.3% F-HT.
Example 3
In this example, the amount of hydrofluoric acid used was 0.05 mL, and the other steps were the same as in example 1 to obtain high-temperature phase TiO2(B) Material, 0.5% F-HT.
Comparative example 1
The procedure was the same as in example 1 except that hydrofluoric acid was not added, and the obtained sample was marked as 0.0% F-HT.
Comparative example 2
The amount of hydrofluoric acid used was 0.1mL, the procedure was otherwise the same as in example 1, and the resulting sample was reported as 1.0% F-HT.
Comparative example 3
The amount of hydrofluoric acid used was 0.3mL, the procedure was otherwise the same as in example 1, and the resulting sample was reported as 3.0% F-HT.
Example 4
In this example, the hydrofluoric acid in example 2 was replaced with 0.03 g of sodium fluoride, and the other steps were the same as in example 2 to obtain high-temperature phase TiO2(B) A material.
Example 5
6 mL of titanium tetra-n-butoxide and 3mL of acetic acid were added to 20 mL of ethylene glycol, and the mixture was stirred uniformly for 15 min, then 30mL of a 15 mol/L aqueous NaOH solution was added, and stirring was continued for 10 min. Transferring the obtained mixed solution to a 100 mL hydrothermal reaction kettle, placing the hydrothermal reaction kettle in an oven, keeping the temperature of 180 ℃ for 12 h, naturally cooling to room temperature, taking out, carrying out suction filtration, washing the obtained product to be neutral by using deionized water and ethanol, stirring the obtained filtrate in 300 mL 0.1 mol/L HCl aqueous solution for 12 h, carrying out suction filtration, washing the filtrate to be neutral by using the deionized water and the ethanol, drying the filtrate at 80 ℃ for 12 h, placing the solid in a muffle furnace, carrying out thermal oxidation treatment at 400 ℃ in the atmosphere, and obtaining pure-phase TiO2(B) In that respect 0.3 g of pure phase TiO2(B) Dispersing the hydrogen fluoride and 0.03 mL of hydrofluoric acid (the mass fraction of the hydrogen fluoride is 49%) in 10mL of deionized water, placing the deionized water in a 20 mL small crucible, and uniformly stirring for 4 h to form uniformly dispersed suspension, wherein the mass fraction of the hydrogen fluoride in the obtained suspension is 0.3%; then putting the mixture into a drying oven for drying for 8 h at the temperature of 80 ℃, grinding the obtained white solid, and then putting the ground white solid into a muffle furnace for thermal oxidation treatment for 2 h at the temperature of 750 ℃ in the atmosphere to obtain high-temperature phase TiO2(B) A material.
The inventors carried out XRD diffraction pattern and field emission scanning electron microscope tests on the samples obtained in examples 1-3 and comparative examples 1-3, and the results are shown in FIGS. 1-7.
As can be seen from FIG. 1, TiO sample of comparative example 12(B) Complete phase transition to anatase at 750 ℃. According to the TiO in the figure2(B) (JCPDS 46-1238) and anatase (JCPDS 21-1272) Standard cards it can be seen that TiO in the sample is gradually increased (0.1% -0.3 wt%) with hydrofluoric acid addition2(B) The phase gradually appears, which shows that the phase change degree of the structure is weakened under the action of HF, and partial phase structure is maintained. This is because of the addition of F-So that the surface energy of the material is reduced and the phase transition requires higher temperature and energy. While TiO when the amount of HF continued to increase (0.5 wt% to 3.0 wt%), the amount of HF continued to increase2(B) The content starts to decrease until it becomes anatase completely. According to the standard curve of XRD, TiO in the sample containing 0.3 percent of HF at 750 ℃ can be calculated2(B) Has an anatase content of 50.5% and 49.5%. The figure shows that the presence of a small amount of HF does act as a phase transition inhibitor, which can retain part of the TiO at high temperatures of 750 deg.C2(B) Phase, however, with increasing HF concentration, due to HF vs. TiO2The etching effect of the structure is accelerated to TiO2(B) The phase transformation progresses, thereby completely transforming into an anatase phase.
As can be seen from FIGS. 2 to 7, the 0.0% F-HT samples showed a rod-like appearance with more particles stacked, with fibrous TiO with increasing HF content2(B) The structure is gradually obvious, and the content of HF is continuously increased, so that the structure can be obviously seen to TiO2And (3) the fibrous structure of the sample gradually disappears under the etching action of the sample, and finally the sample becomes an agglomerated granular sample. In combination with XRD data we can see that the anatase sample is mainly in granular morphology, while TiO2(B) The sample was a fibrous structure. In the sample without HF (0.0% F-HT), although TiO2(B) The whole phase changed to anatase phase, and TiO was still observed2(B) Fibrous structure of precursor, and when HF sample (3.0% F-HT), TiO2(B) Complete phase change to anatase is accompanied by the disappearance of the fibrous structure of the precursor. In sample 0.3% F-HT, both TiO and2(B) the fibrous structure of (a) further comprises partially phase-changed anatase particles to form a plurality of heterogeneous structures. Therefore, a large number of distinct hetero-junction structures are formed in the material during the phase change.
Claims (6)
1. High-temperature phase TiO2(B) The preparation method of the material is characterized by comprising the following steps: fluoride and TiO2(B) Precursor or pure phase TiO2(B) Adding distilled water and stirringStirring for 1-10 h, evaporating the obtained turbid liquid in an oven to dryness, and performing thermal oxidation treatment in a muffle furnace at 600-950 ℃ in an atmosphere to obtain high-temperature phase TiO2(B) A material;
the fluoride is hydrofluoric acid or sodium fluoride, and the mass concentration of the hydrogen fluoride or the sodium fluoride in the obtained suspension is 0.1-0.5%.
2. High temperature phase TiO according to claim 12(B) The preparation method of the material is characterized by comprising the following steps: the stirring time is 4-6 h.
3. High temperature phase TiO according to claim 12(B) The preparation method of the material is characterized by comprising the following steps: the drying temperature is 60-90 ℃.
4. High temperature phase TiO according to claim 12(B) The preparation method of the material is characterized by comprising the following steps: the thermal oxidation treatment temperature is 700-800 ℃, the time is 1-3 h, and the heating rate is 3-10 ℃/min.
5. The high temperature phase TiO according to any one of claims 1 to 42(B) The preparation method of the material is characterized by comprising the following steps: the pure phase of TiO2(B) The titanium source is any one or a mixture of more than two of isopropyl titanate, titanium tetra-n-butoxide, titanium trichloride and titanium tetrachloride.
6. The high temperature phase TiO according to any one of claims 1 to 42(B) The preparation method of the material is characterized by comprising the following steps: the TiO is2(B) The precursor is H2Ti4O9、H2Ti2O5Or H2Ti5O11。
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102040190A (en) * | 2009-10-14 | 2011-05-04 | 嵇天浩 | Simple preparation for massive nitrogen (N)-doped TiO2 (B) nanowires/belts |
| CN102531050A (en) * | 2010-12-30 | 2012-07-04 | 北京大学 | Method for preparing TiO2 (B) nano wires and application of prepared TiO2 (B) nano wires |
| CN104649319A (en) * | 2015-03-02 | 2015-05-27 | 北华大学 | Method for preparing TiO2(B) nano-sponge |
| CN106938856A (en) * | 2016-01-05 | 2017-07-11 | 首都师范大学 | A kind of ring-type TiO2(B) and preparation method thereof |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102040190A (en) * | 2009-10-14 | 2011-05-04 | 嵇天浩 | Simple preparation for massive nitrogen (N)-doped TiO2 (B) nanowires/belts |
| CN102531050A (en) * | 2010-12-30 | 2012-07-04 | 北京大学 | Method for preparing TiO2 (B) nano wires and application of prepared TiO2 (B) nano wires |
| CN104649319A (en) * | 2015-03-02 | 2015-05-27 | 北华大学 | Method for preparing TiO2(B) nano-sponge |
| CN106938856A (en) * | 2016-01-05 | 2017-07-11 | 首都师范大学 | A kind of ring-type TiO2(B) and preparation method thereof |
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