CN102140687A - Preparation method of single-crystal titanium dioxide - Google Patents
Preparation method of single-crystal titanium dioxide Download PDFInfo
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- CN102140687A CN102140687A CN 201110054178 CN201110054178A CN102140687A CN 102140687 A CN102140687 A CN 102140687A CN 201110054178 CN201110054178 CN 201110054178 CN 201110054178 A CN201110054178 A CN 201110054178A CN 102140687 A CN102140687 A CN 102140687A
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- titanium dioxide
- single crystal
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- crystal titanium
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Abstract
The invention relates to a preparation method of single-crystal titanium dioxide with a high-index crystal face, which utilizes a TiCl4 gaseous oxidation method for preparing the single-crystal titanium dioxide granules, wherein the synthesized titanium dioxide is in an anatase structure and mainly contains octahedron formed from double pyramids, the granule size is 1-10 micrometers, the crystal face exposed outside is mainly (105) crystal face. The titanium dioxide single-crystal granule with high-index crystal face structure has important application in the fields of environmental science and new energy sources.
Description
Technical field
The present invention relates to a kind of single crystal titanium dioxide material, it is the octahedral structure of being made up of high index (105) crystal face, and this product has very important purposes in environment protection and clean energy field.
Background technology
Energy shortage and environmental pollution are the human at present two large problems of being badly in need of solution.We need be energy-conservation on the one hand, reduces the consumption of the energy, and use reproducible clean energy as much as possible; We must reduce the discharging of pollutent on the other hand, eliminate environmental pollution.Sunlight is a clean energy, how sunlight is changed into the energy of our convenient use and utilizes sunlight to eliminate the focus that environmental pollution becomes research.Semiconductor functional material has special advantages aspect the sunlight absorbing and utilize.For example utilize anatase type titanium oxide can make dye-sensitized cell, sunlight is converted to our the convenient electric energy that uses.Anatase titanium dioxide TiO
2In photocatalytic degradation pollutent field very important purposes is arranged also.Rayed TiO when certain wavelength
2During crystal, if the energy of photon is greater than TiO
2Energy gap, TiO
2After absorbing photon, the electronics on its valence band is subjected to optical excitation will transit to conduction band, thereby forms light induced electron at conduction band, forms photohole on valence band.Photohole has very high reactive behavior, can be CO with the organic pollutant mineralising
2And H
2O, thus reach the purpose of removal of pollutants.
Anatase titanium dioxide TiO
2No matter be to be used for the fuel sensitization solar battery, still be applied to photocatalyst, all have the problem of inefficiency at present, this one side and anatase titanium dioxide TiO
2Crystalline structure relevant, the crystal face that also exposes with crystal is relevant on the other hand.Yet from the angle of crystal chemistry, crystal growth need be satisfied minimum surface energy principle, and the high reactivity face often disappears in process of growth fast.Usually the crystal face of prepared anatase-type titanium oxide monocrystalline mainly is made of thermodynamically stable (101) face.So, TiO
2The crystalline reactive behavior is all lower.Control anatase titanium dioxide TiO
2Crystal face growth, we have done number of research projects, utilize that the method for wet-chemical is synthetic to have an anatase type titanium oxide (Anatase TiO that a large amount of (001) faces expose
2Single crystals with a large percentage of reactive facets. Nature. 2008. 453,638-641; Solvothermal Synthesis and Photoreactivity of Anatase TiO
2Nanosheets with Dominant 001} Facets. J. Am. Chem. Soc. 2009.131:4078-4083).The high index crystal face has unique atomic structure, has more step and more unsaturated link(age), and these structures can be as the reactive activity point.
The present invention utilizes TiCl
4The titanium oxide with high index crystal face is prepared in gaseous oxidation, and synthetic method is simple, and starting material are selected extensively, and preparation cost is cheap, is fit to very much amplify carry out suitability for industrialized production.
Summary of the invention
It is cheap to the objective of the invention is to develop a kind of preparation cost, has the preparation method of the monocrystalline titan oxide particles of high index crystal face.
A kind of synthetic method of single crystal titanium dioxide comprises following steps:
The carrier gas of 0.1～0.6 L/min is fed in the titanium source presoma of 70～140 ° of C, and the steam of well-mixed carrier gas and described titanium source presoma enters into the tube furnace of 800～1500 ° of C by reactor; Reacted 10～60 minutes, and obtained the single crystal titanium dioxide particle;
Described carrier gas is one or more in nitrogen, argon gas and the oxygen.
Described titanium source presoma is a titanium tetrachloride.
Described reactor has spirane structure, and its screw diameter is slightly less than the diameter of described tube furnace heating tube.
Described single crystal titanium dioxide is an anatase structures, based on the octahedron of two pyramids formation; Described octahedral eight crystal faces are high index (105) crystal face; Described single crystal titanium dioxide granular size is 1～10 micron.
With existing monocrystalline TiO
2Product is compared, and the present invention has the following advantages: building-up process is simple, and starting material are selected extensively, and are with low cost.
Description of drawings
Fig. 1 is a preparation method's of the present invention schematic flow sheet;
Fig. 2 is the XRD figure spectrum of embodiment 1 synthetic titanium dioxide granule;
Fig. 3 is the stereoscan photograph of embodiment 1 synthetic titanium dioxide granule;
Fig. 4 is the stereoscan photograph of embodiment 2 synthetic titanium dioxide granules;
Fig. 5 is the stereoscan photograph of embodiment 3 synthetic titanium dioxide granules;
Fig. 6 is the stereoscan photograph of embodiment 4 synthetic titanium dioxide granules;
Fig. 7 is the stereoscan photograph of embodiment 5 synthetic titanium dioxide granules.
Embodiment
Below by embodiment the present invention is specifically described.Be necessary to be pointed out that at this; following examples only are used for that the invention will be further described; can not be interpreted as limiting the scope of the invention, some nonessential improvement and adjustment that the professional and technical personnel in this field content according to the present invention is made still belong to protection scope of the present invention.
Embodiment 1
Preparation method's schema of single crystal titanium dioxide of the present invention as shown in Figure 1.With oxygen dewater, purifying, through spinner-type flowmeter metering back (flow is 0.2 L/min), 98 ° of C(70～140 ° C that are passed into the oil bath heating all can) TiCl
4In, bubbling carries a certain amount of TiCl
4Steam enters into the tube furnace of certain temperature (1000 ° of C) by reactor, reacts collecting granules in bag filter 30 minutes.Fig. 2 is the XRD diffracting spectrum of this sample.As can be seen, the synthetic titanium oxide is an anatase structures under this condition, and very a spot of rutile particles is arranged.Fig. 3 is the stereoscan photograph of this sample, and as can be seen, the monocrystalline titanium oxide is an octahedral structure, and the surface is cleaned very much, does not have other impurity to exist basically, and the particulate size is about 1～2 μ m.
With oxygen dewater, purifying, through spinner-type flowmeter metering back (flow is 0.2 L/min), be passed into the TiCl of oil bath heating (98 ° of C)
4In, bubbling carries a certain amount of TiCl
4Steam enters into the tube furnace of certain temperature (800 ° of C) by reactor, reacts collecting granules in bag filter 10 minutes.Fig. 4 is the stereoscan photograph of this sample, and as can be seen, titan oxide particles is an octahedral structure, and size is about 1～2 μ m, has a small amount of irregular small-particle to be adsorbed on octahedral surface.
Embodiment 3
With oxygen (flow is 0.3 L/min) and nitrogen (flow is 0.2 L/min) dewater, purifying, behind the thorough mixing, be passed into the TiCl of oil bath heating (80 ° of C)
4In, bubbling carries a certain amount of TiCl
4Steam enters into the tube furnace of certain temperature (1000 ° of C) by reactor, reacts collecting granules in bag filter 30 minutes.Fig. 5 is the stereoscan photograph of this sample, and as can be seen, titan oxide particles is an octahedral structure, and size is 1～2 μ m, has a small amount of irregular small-particle to be adsorbed on octahedral surface.
Embodiment 4
With oxygen (flow is 0.2 L/min) and argon gas gas (flow is 0.2 L/min) dewater, purifying, behind the thorough mixing, be passed into the TiCl of oil bath heating (130 ° of C)
4In, bubbling carries a certain amount of TiCl
4Steam enters into the tube furnace of certain temperature (1000 ° of C) by reactor, reacts collecting granules in bag filter 50 minutes.Fig. 6 is the stereoscan photograph of this sample, and as can be seen, titan oxide particles is an octahedral structure, and size is 1～2 μ m, has more irregular small-particle to be adsorbed on octahedral surface.
Embodiment 5
With oxygen dewater, purifying, through spinner-type flowmeter metering back (flow is 0.2 L/min), be passed into the TiCl of oil bath heating (98 ° of C)
4In, bubbling carries a certain amount of TiCl
4Steam, enter into the tube furnace of certain temperature (1300 ° of C) by reactor, reacted 30 minutes, collecting granules Fig. 7 is the stereoscan photograph of this sample in bag filter, as can be seen, the monocrystalline titanium oxide is an octahedral structure, has more irregular small-particle to be adsorbed on octahedral surface, and the particulate size is about 1～5 μ m.
The temperature of above-mentioned oil bath heating all can between 70～140 ° of C; The combination that the above-mentioned oxygen of using can use nitrogen, argon gas or their three kinds of gases to form substitutes.
Claims (4)
1. the synthetic method of a single crystal titanium dioxide is characterized in that, comprises following steps:
The carrier gas of 0.1～0.6 L/min is fed in the titanium source precursor solution of 70～140 ° of C, and the steam of well-mixed carrier gas and described presoma enters into the tube furnace of 800～1500 ° of C by reactor; Reacted 10～60 minutes, and obtained the single crystal titanium dioxide particle;
Described carrier gas is one or more in nitrogen, argon gas and the oxygen.
2. the preparation method of single crystal titanium dioxide according to claim 1 is characterized in that, described titanium source presoma is a titanium tetrachloride.
3. the preparation method of single crystal titanium dioxide according to claim 1 is characterized in that, described reactor has spirane structure, and its screw diameter is slightly less than the diameter of described tube furnace heating tube.
4. the preparation method of the described single crystal titanium dioxide of root root claim 1 is characterized in that, described single crystal titanium dioxide is an anatase structures, based on the octahedron of two pyramids formation; Described octahedral eight crystal faces are high index (105) crystal face; Described single crystal titanium dioxide granular size is 1～10 micron.
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| CN201110054178.0A CN102140687B (en) | 2011-03-08 | 2011-03-08 | Preparation method of single-crystal titanium dioxide |
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| CN201110054178.0A CN102140687B (en) | 2011-03-08 | 2011-03-08 | Preparation method of single-crystal titanium dioxide |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102995120A (en) * | 2012-12-12 | 2013-03-27 | 国家纳米科学中心 | Nanometer TiO2 monocrystalline material, preparation method and application thereof |
| CN104341002A (en) * | 2013-07-30 | 2015-02-11 | 昭和电工株式会社 | Titanium oxide particle and preparation method thereof |
| CN106698503A (en) * | 2015-11-13 | 2017-05-24 | 中国石油化工股份有限公司 | Synthetic method of titanium dioxide nano-powder |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1245144A (en) * | 1999-08-27 | 2000-02-23 | 华东理工大学 | Process for preparing nm-class TiO2 |
-
2011
- 2011-03-08 CN CN201110054178.0A patent/CN102140687B/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1245144A (en) * | 1999-08-27 | 2000-02-23 | 华东理工大学 | Process for preparing nm-class TiO2 |
Non-Patent Citations (4)
| Title |
|---|
| 《功能材料》 20001231 施利毅等 TiCl_4高温气相氧化合成纳米二氧化钛颗粒的研究I.颗粒晶型结构控制 622-624 第31卷, 第6期 * |
| 《功能材料》 20001231 施利毅等 TiCl_4高温气相氧化合成纳米二氧化钛颗粒的研究II.颗粒粒度控制 625-627 第31卷, 第6期 * |
| 《现代涂料与涂装》 20060630 魏绍东等 以TiCl4为原料制备纳米TiO2的研究进展--气相法 43-46 , * |
| 《金属学报》 20000331 施利毅等 高温气相反应合成金红石型纳米TiO_2颗粒的研究 295-299 第36卷, 第3期 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102995120A (en) * | 2012-12-12 | 2013-03-27 | 国家纳米科学中心 | Nanometer TiO2 monocrystalline material, preparation method and application thereof |
| CN102995120B (en) * | 2012-12-12 | 2015-05-20 | 国家纳米科学中心 | Nanometer TiO2 monocrystalline material, preparation method and application thereof |
| CN104341002A (en) * | 2013-07-30 | 2015-02-11 | 昭和电工株式会社 | Titanium oxide particle and preparation method thereof |
| CN106698503A (en) * | 2015-11-13 | 2017-05-24 | 中国石油化工股份有限公司 | Synthetic method of titanium dioxide nano-powder |
| CN106698503B (en) * | 2015-11-13 | 2018-03-16 | 中国石油化工股份有限公司 | A kind of synthetic method of titanic oxide nano |
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| CN102140687B (en) | 2014-04-09 |
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