CN1974014A - Process of preparing nitrogen doped nanometer titania - Google Patents
Process of preparing nitrogen doped nanometer titania Download PDFInfo
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- CN1974014A CN1974014A CN 200610147257 CN200610147257A CN1974014A CN 1974014 A CN1974014 A CN 1974014A CN 200610147257 CN200610147257 CN 200610147257 CN 200610147257 A CN200610147257 A CN 200610147257A CN 1974014 A CN1974014 A CN 1974014A
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- titania
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- tin
- doped nanometer
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Abstract
The present invention belongs to the field of titania photocatalysis technology, and is especially preparation process of nitrogen doped nanometer titania. By using titanium nitride powder as material and through heat oxidation treatment at the temperature of 450-600 deg.c for 1-21 hr, nanometer rutile type titania is produced. The preparation process is simple uses no toxic NH3, and the prepared titania material may be used in photocatalysis, solar cell, phtotocatalytically decomposing water to prepare hydrogen and other fields.
Description
Technical field
The invention belongs to the optically catalytic TiO 2 technical field, be specifically related to a kind of new method for preparing nitrogen doped nanometer titania by the compound titanium nitride.
Background technology
Found semiconductor titanium dioxide since splitting water into hydrogen and oxygen under the UV-irradiation from 1972, titanium dioxide has been subjected in the material field paying attention to very widely.TiO
2Can be used for many aspects such as photocatalysis to degrade organic matter, sterilizing, sewage disposal, air cleaning, at present, nano-TiO
2Preparation method's research become a very active problem of photocatalysis new material exploitation.Because TiO
2Big (the 3.2eV anatase type of energy gap, 3.0eV rutile-type), absorption difference to visible light, limited its range of application greatly, adopted doping metals or nonmetallic mode to increase its visible light activity usually, having of reporting at present is nonmetal as C, N, the doping of elements such as S and Fe, Cr, the doping of Sb and the multiple metallic element of rare earth element etc.The nitrogen-doped nanometer TiO that has reported
2The preparation method of film has multiple, and for example ion injection method is introduced NH in presoma
3, or at NH
3Heat treatment TiO in the atmosphere
2Film can obtain nitrogen-doped nanometer TiO
2Film.But there are some shortcomings in these methods, as NH
3Toxicity problem.The present invention proposes a kind of new method, prepares the nanostructured TiO that nitrogen mixes by compound TiN
2, method is simple, has avoided using poisonous NH
3
Summary of the invention
The objective of the invention is to propose a kind of technology simple, without NH
3The method for preparing nitrogen doped nanometer titania.
The method for preparing nitrogen doped nanometer titania that the present invention proposes, be to be raw material with the titanium nitride powder, carry out thermal oxidation, the control temperature is 450 ℃～600 ℃, oxidization time is 1-21 hour, the color of titanium nitride changes, and forms the titanium dioxide (TiO with rutile type nano structure
2).
Among the present invention, thermal oxide can be adopted muffle furnace, perhaps thermogravimetric analyzer etc.
Among the present invention, the raw material titanium nitride powder can micron or nanometer grade powder.
Experiment shows that the nitrogen-doped titanium dioxide that is prepared by the inventive method has rutile crystal type and the typical semi-conductive feature of n type.
1. under white light, with the doped Ti O of this method preparation
2Show tangible photovoltage, as shown in Figure 1, Fig. 1 obtains TiO after the titanium nitride heat treatment
2The photovoltage curve of electrode.The result shows, the nitrogen doped Ti O of preparation
2Have the semi-conductive feature of typical n type, can be applied at aspects such as photocatalysis, solar cell, light hydrogen production by water decomposition.
2. in air atmosphere the TiN material is carried out thermogravimetric analysis with 10 ℃/min of heating rate, the thermogravimetric curve that obtains as shown in Figure 2.As can be seen from the figure, along with the rising of temperature, TiN is oxidized, shows a process that continues weightening finish, and this is to generate the TiN that nitrogen mixes gradually
XO
YProcess.After 600 ℃, weight increases sharply, and shows that the oxidized speed of TiN increases rapidly.
3. prepare nitrogen doped Ti O by this method
2The XRD test shows of material, 600 ℃ of heat treatment oxidations promptly have the TiO of rutile crystal type structure after 1 hour
2Generate.Fig. 3 is 600 ℃ of thermal oxide titanium nitride different times (a) 0 hour; (b) 3 hours; (c) the nanostructured TiO of preparation in 9 hours
2XRD spectrum.As can be seen from the figure, with the increase of oxidization time, the TiO of rutile crystal type structure
2Diffraction maximum increase gradually, show TiO
2Crystallization be tending towards complete.
4. to prepared nitrogen doped Ti O
2The SEM test shows, possess loose nanostructured (Fig. 4), its big surface area is laid a good foundation for improving photoelectric activity and photocatalytic activity.
Description of drawings
Fig. 1 is with the nanostructured TiO of the present invention's preparation
2The photovoltage curve of electrode.
The TG curve of Fig. 2 heated oxide TiN process under air atmosphere has shown that weight increases situation under the different temperatures.
The following 600 ℃ of thermal oxide titanium nitride different times of Fig. 3 air atmosphere ((a) 0 hour; (b) 3 hours; (c) 9 hours) preparation nano-TiO
2XRD spectrum.O represents TiN, and R represents the TiO of rutile structure
2
Before the thermal oxide of Fig. 4 titanium nitride (A), and 600 ℃ of thermal oxides 3 hours (B), the nanostructured TiO of 9 hours (C) preparation
2SEM figure.
The nitrogen-doped nanometer TiO of the following 450 ℃ of thermal oxide titanium nitrides of Fig. 5 air atmosphere preparation in 21 hours
2XRD spectrum.O represents TiN, and R represents the TiO of rutile structure
2, A represents anatase structured TiO
2
The specific embodiment
Embodiment 1: titanium nitride (TiN) powder is placed muffle furnace, heat treated is 3 hours under the atmosphere of 600 ℃ air, and the color of TiN changes, and becomes Dark grey by the dark yellow of nitride powder, the XRD test shows, part TiN changes the TiO of rutile-type into
2Powder.Through the XRD spectrum of 600 ℃ of heat treatments after 3 hours is shown in Fig. 3 (b).
Embodiment 2: titanium nitride (TiN) powder is placed muffle furnace, heat treated is 9 hours under the atmosphere of 500 ℃ air, the color of TiN changes, dark yellow by nitride powder becomes light grey SEM test shows, through after the thermal oxide, change the nanostructured TiO of loose porous shape into by ganoid TiN powder structure
2, Fig. 4 (C), with the increase of oxidization time, loose porous shape is more obvious.
Embodiment 3: nitride powder is placed crucible, carry out thermogravimetric analysis under the atmosphere of air, obtain nitrogen-doped nanometer TiO
2Weight-the temperature curve of thermal oxidation process as shown in Figure 2.
Embodiment 4: titanium nitride (TiN) powder is placed muffle furnace, and heat treated is 21 hours under the atmosphere of 450 ℃ air, and the color of TiN changes, and becomes dark brown red by the dark yellow of nitride powder, and the XRD test shows has the TiO of rutile-type
2TiO with the anatase type
2Characteristic peak occur, show that TiN partly changes TiO into
2, see shown in Figure 5.
Claims (1)
1, a kind of preparation method of nitrogen doped nanometer titania, it is characterized in that with the nitrogenous fertilizer titanium powder be raw material, carry out thermal oxidation, the control temperature is 450 ℃～600 ℃, oxidization time is 1-21 hour, the color of titanium nitride changes, and forms the titanium dioxide with rutile type nano structure.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200610147257 CN1974014A (en) | 2006-12-14 | 2006-12-14 | Process of preparing nitrogen doped nanometer titania |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200610147257 CN1974014A (en) | 2006-12-14 | 2006-12-14 | Process of preparing nitrogen doped nanometer titania |
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|---|---|
| CN1974014A true CN1974014A (en) | 2007-06-06 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101513610B (en) * | 2009-02-20 | 2010-12-29 | 复旦大学 | Method for preparing C-N codope nano TiO2 photocatalyst |
| CN102039131A (en) * | 2011-01-07 | 2011-05-04 | 华东理工大学 | Catalyst for generating hydrogen by visible light photocatalytic reduction of water, and preparation method thereof |
| CN102553626A (en) * | 2011-12-29 | 2012-07-11 | 复旦大学 | Preparation method of carbon-nitrogen-codoped TiO2 nano catalysis material |
| CN105498822A (en) * | 2015-12-21 | 2016-04-20 | 中国工程物理研究院核物理与化学研究所 | Preparation method for nitrogen-doped anatase titanium dioxide |
-
2006
- 2006-12-14 CN CN 200610147257 patent/CN1974014A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101513610B (en) * | 2009-02-20 | 2010-12-29 | 复旦大学 | Method for preparing C-N codope nano TiO2 photocatalyst |
| CN102039131A (en) * | 2011-01-07 | 2011-05-04 | 华东理工大学 | Catalyst for generating hydrogen by visible light photocatalytic reduction of water, and preparation method thereof |
| CN102039131B (en) * | 2011-01-07 | 2013-01-09 | 华东理工大学 | Catalyst for generating hydrogen by visible light photocatalytic reduction of water, and preparation method thereof |
| CN102553626A (en) * | 2011-12-29 | 2012-07-11 | 复旦大学 | Preparation method of carbon-nitrogen-codoped TiO2 nano catalysis material |
| CN105498822A (en) * | 2015-12-21 | 2016-04-20 | 中国工程物理研究院核物理与化学研究所 | Preparation method for nitrogen-doped anatase titanium dioxide |
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