CN109052464A - A kind of high-temperature-phase TiO2(B) preparation method of material - Google Patents
A kind of high-temperature-phase TiO2(B) preparation method of material Download PDFInfo
- Publication number
- CN109052464A CN109052464A CN201810904360.2A CN201810904360A CN109052464A CN 109052464 A CN109052464 A CN 109052464A CN 201810904360 A CN201810904360 A CN 201810904360A CN 109052464 A CN109052464 A CN 109052464A
- Authority
- CN
- China
- Prior art keywords
- temperature
- tio
- preparation
- phase
- phase tio
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 229910010251 TiO2(B) Inorganic materials 0.000 title claims abstract description 33
- 239000000463 material Substances 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 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
- 238000007796 conventional method Methods 0.000 claims abstract description 5
- 239000012153 distilled water Substances 0.000 claims abstract description 4
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 25
- 238000000034 method Methods 0.000 claims description 17
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 12
- 229960002050 hydrofluoric acid Drugs 0.000 claims description 11
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 claims description 11
- 239000010936 titanium Substances 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- 239000000725 suspension Substances 0.000 claims description 8
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 7
- 229910000040 hydrogen fluoride Inorganic materials 0.000 claims description 6
- 230000008569 process Effects 0.000 claims description 6
- 239000011775 sodium fluoride Substances 0.000 claims description 6
- 235000013024 sodium fluoride Nutrition 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 5
- 238000001652 electrophoretic deposition Methods 0.000 claims description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 3
- 239000001257 hydrogen Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 238000003836 solid-state method Methods 0.000 claims description 3
- 229910052719 titanium Inorganic materials 0.000 claims description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 229910052739 hydrogen 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
- YONPGGFAJWQGJC-UHFFFAOYSA-K titanium(iii) chloride Chemical compound Cl[Ti](Cl)Cl YONPGGFAJWQGJC-UHFFFAOYSA-K 0.000 claims description 2
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 claims 1
- 150000002009 diols Chemical class 0.000 claims 1
- 229910052731 fluorine Inorganic materials 0.000 claims 1
- 239000011737 fluorine Substances 0.000 claims 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims 1
- 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 1
- 230000009466 transformation Effects 0.000 abstract description 7
- 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 4
- 238000007146 photocatalysis Methods 0.000 abstract description 3
- 238000006555 catalytic reaction Methods 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 230000001681 protective effect Effects 0.000 abstract 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 20
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 239000008367 deionised water Substances 0.000 description 5
- 229910021641 deionized water Inorganic materials 0.000 description 5
- 229910010455 TiO2 (B) Inorganic materials 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 4
- 235000019441 ethanol Nutrition 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 230000007704 transition Effects 0.000 description 4
- 239000002074 nanoribbon Substances 0.000 description 3
- 229910003075 TiO2-B Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 239000000706 filtrate Substances 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 239000003112 inhibitor Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 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
- 239000002253 acid Substances 0.000 description 1
- 230000009471 action Effects 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
- 230000015556 catabolic process Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- -1 isopropyl Ester Chemical class 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 125000004108 n-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- 238000000643 oven drying Methods 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 229920003048 styrene butadiene rubber Polymers 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
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
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/33—Electric or magnetic properties
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Geology (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Inorganic Chemistry (AREA)
- Environmental & Geological Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Catalysts (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention discloses a kind of high-temperature-phase TiO2(B) preparation method of material first passes through conventional method preparation TiO2(B) presoma or pure phase TiO2(B), then by fluoride, distilled water and TiO2(B) presoma or pure phase TiO2(B) it is mixed evenly, is slowly evaporated, then high-temperature thermal oxidation is handled under atmospheric atmosphere, and the high-temperature-phase TiO of excellent in stability can be obtained2(B).Preparation method of the present invention is simple, and the prices of raw materials are cheap, and complete phase transformation does not occur at relatively high temperatures for material, and thermal stability is good, environmentally protective, can be efficiently applied to the fields such as photocatalysis, electro-catalysis, photoelectrocatalysis, lithium ion battery.
Description
Technical field
The invention belongs to photocatalytic pollutant degradation technical fields, and in particular to a kind of high-temperature-phase TiO2(B) system of material
Preparation Method.
Background technique
TiO2It (B) is a kind of metasable state titanium oxide homogeneity variant smaller than anatase and rutile density, loosely organized,
The fields such as lithium ion battery, capacitor, sensor and photocatalysis, photoelectrocatalysis are concerned.People can be by each at present
Kind of method prepares TiO2(B), traditional preparation method has acetic acid solvent thermal method (Changhua Wang, Xintong Zhang
and Yichun Liu.Coexistence of an anatase/TiO2(B)heterojunction and an exposed
(001)facet in TiO2nanoribbon photocatalysts synthesized via a fluorine-free
Route and topotactic transformation [J] .Nanoscale, 2014,6:5329-5337.), highly basic hydro-thermal
Method (Yan X, Zhang Y, Zhu K, et al.Enhanced electrochemical properties of TiO2(B)
nanoribbons using the styrene butadiene rubber and sodium carboxyl methyl
Cellulose water binder [J] .Journal of Power Sources, 2014,246:95-102.), ethylene glycol it is molten
(Luo Xiaoxiao, woods rises dazzles agent thermal method, and Qin Wei, Wen Xiaogang hydro-thermal method synthesizes high-purity Ti O2(B) nano wire and its lithium electrical property are ground
Study carefully [J] functional material, 2015,9 (46): 09148-09152.), high temperature solid-state method (WANG Xin-yu (Wang Xinyu), XIE
Ke-yu (Xie Keyu), LI Jie (Lee's Jie), LAI Yan-qing (Lai Yanqing), ZHANG Zhi-an (Zhang Zhian), LIU Ye-
Xiang (Liu Yexiang) .Synthesis and electrochemical performance of TiO2-B as anode
Material [J] .J.Cent.South Univ.Technol.2011,18:406-410.), sol-gal process (Yu Ren,
Zheng Liu,Frédérique Pourpoint,A.Robert Armstrong,Clare P.Grey,and Peter G.
Bruce*.Nanoparticulate TiO2(B):An Anode for Lithium-Ion Batteries[J].2012,
124:2206-2209.), electrophoretic deposition (CC Tsai, YY Chu, H Teng.A simple electrophoretic
deposition method to prepare TiO2-B nanoribbon thin films for dye-sensitized
Solar cells [J] .Thin Solid Films, 2010,519 (2): 662-665.) etc..In these methods hydro-thermal method because
Preparation method is simple, at low cost and be concerned.But the TiO that these methods are prepared2(B) brilliant after temperature is 500 DEG C or more
It meets and is gradually converted into Anatase, limit it in the application in some fields.There has been no inhibit TiO at high temperature at present2(B)
The report of phase transformation.
Summary of the invention
The object of the present invention is to provide a kind of high-temperature-phase TiO2(B) preparation method of material.
For above-mentioned purpose, the technical scheme adopted by the invention is that: by fluoride and TiO2(B) presoma or pure phase
TiO2(B) be added in distilled water and stir 1~10h, gained suspension is put into be evaporated in baking oven after, be placed in Muffle furnace in atmosphere
Lower 600~950 DEG C of thermal oxidations are enclosed, high-temperature-phase TiO is obtained2(B) material.
Above-mentioned fluoride is hydrofluoric acid or sodium fluoride, the preferably mass concentration of hydrogen fluoride or sodium fluoride in gained suspension
It is 0.1%~0.5%.
In above-mentioned preparation method, preferably by fluoride and TiO2(B) presoma or pure phase TiO2(B) it is added in distilled water and stirs
Mix 4~6h.
In above-mentioned preparation method, the evaporated temperature is 60~90 DEG C.
In above-mentioned preparation method, preferably thermal oxidation temperature is 700~800 DEG C, and the time is 1~3h, heating rate 3
~10 DEG C/min.
The TiO of above-mentioned pure phase2(B) it is prepared using conventional method, wherein conventional method is acetic acid solvent thermal method, highly basic
Hydro-thermal method, ethylene glycol solvent thermal method, high temperature solid-state method, sol-gal process or electrophoretic deposition, titanium source used are metatitanic acid isopropyl
Ester, four n-butyl titaniums, titanium trichloride, any one in titanium tetrachloride or two or more mixtures.
Above-mentioned TiO2(B) presoma is H2Ti4O9、H2Ti2O5、H2Ti5O11Deng.
Beneficial effects of the present invention are as follows:
The present invention can largely slow down TiO by the participation of phase transformation inhibitor HF or sodium fluoride2(B) phase transition process,
Still retain relatively large number of TiO under the high temperature conditions2(B), also, the presence of the structure promotes and forms TiO under high temperature2(B)/
Anatase out-phase junction structure.
Preparation method of the present invention is simple, and the prices of raw materials are cheap, gained TiO2(B) material thermal stability is good, in higher temperatures
It is not undergone phase transition under degree, the fields such as photocatalysis, electro-catalysis, lithium ion battery can be efficiently applied to.
Detailed description of the invention
Fig. 1 is the XRD diffraction pattern of 1~3 gained sample of Examples 1 to 3 and comparative example.
Fig. 2 is the field emission scanning electron microscope figure of 1 gained sample of embodiment.
Fig. 3 is the field emission scanning electron microscope figure of 2 gained sample of embodiment.
Fig. 4 is the field emission scanning electron microscope figure of 3 gained sample of embodiment.
Fig. 5 is the field emission scanning electron microscope figure of 1 gained sample of comparative example.
Fig. 6 is the field emission scanning electron microscope figure of 2 gained sample of comparative example.
Fig. 7 is the field emission scanning electron microscope figure of 3 gained sample of comparative example.
Specific embodiment
The present invention is described in more detail with reference to the accompanying drawings and examples, but protection scope of the present invention is not limited only to
These embodiments.
Embodiment 1
Tetra- n-butyl titanium of 6mL and 3mL acetic acid are added in 20mL ethylene glycol, then 30mL is added in uniform stirring 15min
15mol/L NaOH aqueous solution continues to stir 10min.Gained mixed liquor is transferred to 100mL hydrothermal reaction kettle, is placed in baking oven
In after 180 DEG C of heat preservation 12h, cooled to room temperature is taken out, and filters and is washed till products therefrom with deionized water and ethyl alcohol
Property, obtained filtrate stirs 12h in 300mL 0.1mol/L HCL aqueous solution, filter, and is washed till with deionized water and ethyl alcohol
After property, 80 DEG C of dry 12h obtain TiO2(B) presoma H2Ti4O9.By 0.3g TiO2(B) presoma H2Ti4O9With 0.01mL hydrogen
Fluoric acid (mass fraction of hydrogen fluoride is 49%) is scattered in 10mL deionized water, is placed in 20mL small crucible uniform stirring 4h, shape
At finely dispersed suspension, the mass fraction of hydrogen fluoride is 0.1% in gained suspension；It is then placed in 80 DEG C of baking oven drying
8h, obtained white solid grinding are placed on the lower 750 DEG C of thermal oxidation 2h of Muffle furnace atmospheric atmosphere, obtain high-temperature-phase TiO2
(B) material is denoted as 0.1%F-HT.
Embodiment 2
In the present embodiment, the dosage of hydrofluoric acid is 0.03mL, other steps are same as Example 1, obtain high-temperature-phase TiO2
(B) material is denoted as 0.3%F-HT.
Embodiment 3
In the present embodiment, the dosage of hydrofluoric acid is 0.05mL, other steps are same as Example 1, obtain high-temperature-phase TiO2
(B) material is denoted as 0.5%F-HT.
Comparative example 1
Do not add hydrofluoric acid, other steps are same as Example 1, and gained sample is labeled as 0.0%F-HT.
Comparative example 2
The dosage of hydrofluoric acid is 0.1mL, other steps are same as Example 1, and gained sample is denoted as 1.0%F-HT.
Comparative example 3
The dosage of hydrofluoric acid is 0.3mL, other steps are same as Example 1, and gained sample is denoted as 3.0%F-HT.
Embodiment 4
In the present embodiment, with the hydrofluoric acid in 0.03g sodium fluoride alternative embodiment 2, other steps are identical as embodiment 2,
Obtain high-temperature-phase TiO2(B) material.
Embodiment 5
Tetra- n-butyl titanium of 6mL and 3mL acetic acid are added in 20mL ethylene glycol, then 30mL is added in uniform stirring 15min
15mol/L NaOH aqueous solution continues to stir 10min.Gained mixed liquor is transferred to 100mL hydrothermal reaction kettle, is placed in baking oven
In after 180 DEG C of heat preservation 12h, cooled to room temperature is taken out, and filters and is washed till products therefrom with deionized water and ethyl alcohol
Property, obtained filtrate stirs 12h in 300mL 0.1mol/L HCL aqueous solution, filter, and is washed till with deionized water and ethyl alcohol
After property, solid is placed in Muffle furnace 400 DEG C of thermal oxidations under atmospheric atmosphere by 80 DEG C of dry 12h, obtains pure phase TiO2
(B).By 0.3g pure phase TiO2(B) 10mL deionization is scattered in 0.03mL hydrofluoric acid (mass fraction of hydrogen fluoride is 49%)
In water, it is placed in 20mL small crucible uniform stirring 4h, forms finely dispersed suspension, the quality of hydrogen fluoride in gained suspension
Score is 0.3%；80 DEG C of drying 8h of baking oven are then placed in, obtained white solid grinding is placed under Muffle furnace atmospheric atmosphere
750 DEG C of thermal oxidation 2h, obtain high-temperature-phase TiO2(B) material.
Inventor has carried out XRD diffraction pattern and field emission scanning electron microscope to Examples 1 to 3 and 1~3 gained sample of comparative example
Test, the result is shown in Figure 1~7.
As seen from Figure 1, the sample TiO of comparative example 12(B) mutually become anatase completely at 750 DEG C.According to the TiO in figure2
(B) (JCPDS 46-1238) and anatase (JCPDS 21-1272) standard card can be seen that the amount being added with hydrofluoric acid
Gradually increase TiO in (0.1%-0.3wt%) sample2(B) it mutually gradually appears, illustrates structure phase transformation journey under the action of HF
Degree weakens, and part phase structure is maintained.This is because the F being added-The surface of material enable to reduce, phase transition then needs more
High temperature and energy.And when the amount of HF continues growing (0.5wt%- 3.0wt%), TiO2(B) content start reduce until
Become anatase completely.It can be calculated in 750 DEG C of samples containing 0.3%HF according to the standard curve of XRD, TiO2(B) content
It is 50.5%, anatase content 49.5%.The chart is bright, and phase transformation inhibitor is played the role of in the presence of a small amount of HF really, can
Still to retain part TiO under 750 DEG C of high temperature2(B) phase, however as the increase of HF concentration, since HF is to TiO2The quarter of structure
Erosion effect, accelerates TiO instead2(B) process of phase transformation, so that it be made to be completely transformed into Anatase.
By Fig. 2~7 as it can be seen that 0.0%F-HT sample shows the rodlike appearance of more particle packing, with the increasing of HF amount
Add, fibrous TiO2(B) structure is gradually obvious, continues growing the amount of HF, it can clearly be seen that it is to TiO2The etching of sample
Effect, sample fiber shape structure fade away, and finally become the graininess sample reunited.In conjunction with XRD data it will be seen that
Anatase sample is mainly graininess pattern, and TiO2(B) sample is fibrous structure.(the 0.0%F- in the sample without HF
HT), although TiO2(B) all mutually become Anatase, still it can be observed that TiO2(B) fibrous structure of presoma, and when height
Concentration HF sample (3.0%F-HT), TiO2(B) mutually become disappearing for anatase simultaneous precursor fibre shape structure completely
It loses.In sample 0.3%F-HT, TiO is both contained2(B) fibrous structure contains the anatase particles of partial phase change again,
Form a large amount of out-phase junction structure.Therefore, a large amount of apparent out-phase junction structures are formd in the material in phase transition process.
Claims (8)
1. a kind of high-temperature-phase TiO2(B) preparation method of material, it is characterised in that: by fluoride and TiO2(B) presoma or pure phase
TiO2(B) be added in distilled water and stir 1~10h, gained suspension is put into be evaporated in baking oven after, be placed in Muffle furnace in atmosphere
Lower 600~950 DEG C of thermal oxidations are enclosed, high-temperature-phase TiO is obtained2(B) material.
2. high-temperature-phase TiO according to claim 12(B) preparation method of material, it is characterised in that: the fluoride is hydrogen
Fluoric acid or sodium fluoride.
3. high-temperature-phase TiO according to claim 22(B) preparation method of material, it is characterised in that: fluorine in gained suspension
The mass concentration for changing hydrogen or sodium fluoride is 0.1%~0.5%.
4. high-temperature-phase TiO according to claim 12(B) preparation method of material, it is characterised in that: the time of the stirring
For 4~6h.
5. high-temperature-phase TiO according to claim 12(B) preparation method of material, it is characterised in that: the evaporated temperature
It is 60~90 DEG C.
6. high-temperature-phase TiO according to claim 12(B) preparation method of material, it is characterised in that: the thermal oxidation
Temperature is 700~800 DEG C, and the time is 1~3h, and heating rate is 3~10 DEG C/min.
7. high-temperature-phase TiO described in any one according to claim 1~62(B) preparation method of material, it is characterised in that: institute
State the TiO of pure phase2(B) it is prepared using conventional method, wherein conventional method is acetic acid solvent thermal method, highly basic hydro-thermal method, second
Diol solvent thermal method, high temperature solid-state method, sol-gal process or electrophoretic deposition, titanium source used are isopropyl titanate, four positive fourths
Alcohol titanium, titanium trichloride, any one in titanium tetrachloride or two or more mixtures.
8. high-temperature-phase TiO described in any one according to claim 1~62(B) preparation method of material, it is characterised in that: institute
The TiO stated2(B) presoma is H2Ti4O9、H2Ti2O5Or H2Ti5O11。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810904360.2A CN109052464B (en) | 2018-08-09 | 2018-08-09 | High-temperature phase TiO2(B) Method for producing a material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810904360.2A CN109052464B (en) | 2018-08-09 | 2018-08-09 | High-temperature phase TiO2(B) Method for producing a material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN109052464A true CN109052464A (en) | 2018-12-21 |
| CN109052464B CN109052464B (en) | 2020-10-16 |
Family
ID=64683152
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810904360.2A Active CN109052464B (en) | 2018-08-09 | 2018-08-09 | High-temperature phase TiO2(B) Method for producing a material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109052464B (en) |
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 |
-
2018
- 2018-08-09 CN CN201810904360.2A patent/CN109052464B/en active Active
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 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN109052464B (en) | 2020-10-16 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Gao et al. | Preparation and electrochemical characterization of anatase nanorods for lithium-inserting electrode material | |
| Zhang et al. | Increasing the oxygen vacancy density on the TiO2 surface by La-doping for dye-sensitized solar cells | |
| CN102208658B (en) | Method for preparing nanometer Ti4O7 particles | |
| Wang et al. | Improving photocatalytic H2 evolution of TiO2 via formation of {001}–{010} quasi-heterojunctions | |
| CN111646500B (en) | 2D porous TiO rich in surface defects 2 Nanosheets and preparation method thereof | |
| Sugimoto et al. | Formation mechanism of amorphous TiO2 spheres in organic solvents. 1. Roles of ammonia | |
| Yang et al. | Control of nucleation in solution growth of anatase TiO2 on glass substrate | |
| CN103626179A (en) | Method for preparing nanometer zirconium carbide powder | |
| WO2016026339A1 (en) | Synthesis method for tio2 nanocrystal | |
| CN104923230A (en) | Titanium dioxide/ferroferric oxide nanocomposite and preparation method therefor | |
| CN104402047B (en) | Expose the rutile TiO that crystal face is controlled 2nanometer rod is self-assembled into the method for microballoon | |
| Zhang et al. | Template-free scalable synthesis of TiO 2 hollow nanoparticles for excellent photoelectrochemical applications | |
| Gao et al. | Enhanced visible-light-driven photocatalytic H2-production activity of CdS-loaded TiO2 microspheres with exposed (001) facets | |
| CN105070522B (en) | Graphene/titania nanotube prepares flexible bending folding thin-film electrode | |
| Deng et al. | TiO2/reduced hydroxylated graphene nanocomposite photocatalysts: Improved electron–hole separation and migration | |
| CN109019693B (en) | Monoclinic phase WO3Preparation method of nano cuboid and photocatalytic application thereof | |
| CN109052464A (en) | A kind of high-temperature-phase TiO2(B) preparation method of material | |
| Wang et al. | Hydrothermal synthesis of SnO2 nanoflower arrays and their optical properties | |
| Feng et al. | Electrospinning of TiO2 nanofibers: the influence of Li and Ca doping and vacuum calcination | |
| Silva et al. | Electronic structure, morphological aspects, optical and electrochemical properties of RuO 2 nanocrystals | |
| KR100836710B1 (en) | Method for preparing nano particle powder of titanium dioxide for dye-sensitized solar cell by sol-gel combustion hybrid method | |
| CN109110806A (en) | A kind of method of controlledly synthesis different crystal forms strawberry-like titanium dioxide nano material | |
| CN106914235A (en) | A kind of Graphene Re TiO2The preparation method of multiple elements design nano-tube material | |
| Kim et al. | Dehydration of Alginic Acid Cryogel by TiCl4 vapor: Direct Access to Mesoporous TiO2@ C Nanocomposites and Their Performance in Lithium‐Ion Batteries | |
| CN106345443A (en) | Photocatalysis material with nano TiO2 loaded on kieselguhr white carbon black used as carrier and preparation method of photocatalysis material |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |