CN100522820C - Process for preparing TiO2 nano cluster - Google Patents
Process for preparing TiO2 nano cluster Download PDFInfo
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- CN100522820C CN100522820C CNB2006101236873A CN200610123687A CN100522820C CN 100522820 C CN100522820 C CN 100522820C CN B2006101236873 A CNB2006101236873 A CN B2006101236873A CN 200610123687 A CN200610123687 A CN 200610123687A CN 100522820 C CN100522820 C CN 100522820C
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- titanium
- nano cluster
- tio
- film
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Abstract
The invention discloses a making method of titanium oxide nanometer cluster, which is characterized by the following: utilizing molecular beam equipment to grow titanium oxide on the substrate and metal film simultaneously; reacting titanium atom and oxygen completely; forming nanometer cluster evenly in the passivating film randomly; controlling the size of nanometer cluster through controlling the flow of MBE beam source.
Description
Technical field
The present invention relates to the TiO 2 nano cluster material, particularly relate to a kind of preparation method of TiO 2 nano cluster.
Background technology
The preparation of nano material is an important field of research, has preparation method's ubiquity complex steps of TiO 2 nano cluster now, is difficult to control the problems such as size of TiO 2 nano cluster size.
Summary of the invention
The objective of the invention is to overcome the deficiency that existing TiO 2 nano cluster preparation method exists, provide a kind of step simple, can control the size of TiO 2 nano cluster size, realize the preparation method of varied nano-meter characteristic.
To achieve these goals, the present invention utilizes radio-frequency plasma molecular beam epitaxial device (RF-MBE) preparation TiO 2 nano cluster.Molecular beam epitaxial device (MBE) is that (vacuum tightness is the highest can to reach 10 to high-vacuum apparatus
-12Mbar).The inert metal film of growth of passivation on substrate, and grow simultaneously titanium and oxygen, titanium and oxygen reaction generate titanium dioxide.Substrate is SrTiO
3, MgO or LaAlO
3
Because the characteristics of molecular beam epitaxial device are accurately to control the growth or the preparation of epitaxial film in the precision of atomic level, so can accurately control the thickness (from nanometer to the micron number magnitude) of inert metal film and TiO 2 nano cluster how much.Can be on high electron energy diffractometer (RHEED) supervising in growth and the preparation process on the throne real-time monitoring.
The preferred gold thin film of inert metal film.The golden film of growth on the inherent substrate of MBE growth chamber, gold atom does not react with oxygen (being produced by radio-frequency (RF) plasma generator) when 450 ℃ of temperature, oxygen is only selected the titanium atom of easy oxidation, enough relaxation times are being arranged, under the situation of the abundant reaction of space and sufficient oxygen, titanium atom and oxygen reaction form TiO 2 nano cluster.
When TiO 2 nano cluster prepares, the atomic molar ratio that comes out in the electron gun stove of gold metal and titanium metal is about 10:1, titanium and oxygen fully react the formation TiO 2 nano cluster under 450 ℃ of utmost points prepare at a slow speed, and are randomly dispersed in equably in the golden film (golden here film can be done and support and passive film).Control electron gun furnace temperature can control atomic quantity on the substrate than so that the size and the concentration in film of control TiO 2 nano cluster size.
Compared with prior art, the present invention has following beneficial effect: utilize method of the present invention to prepare TiO 2 nano cluster, can control the thickness (being the control growing time) of film, and then the size of control TiO 2 nano cluster amount; Thereby can control the size of the flow control nanocluster of MBE electron gun stove titanium.The preparation method is simple, can realize the preparation of varied nano-meter characteristic, supports that at gold nano particle is evenly distributed in the film in the passive film.Utilize this TiO 2 nano cluster to realize nano effect such as catalysis etc.
Description of drawings
Fig. 1 is the TiO 2 nano cluster structural representation;
The golden titanium on the x-ray photoelectron spectroscopy that Fig. 2 measures for epitaxial structure (XPS) and the valence state of oxygen.
Embodiment
In molecular beam epitaxial device (MBE) growth, the growth temperature of the electron gun stove of gold and titanium is respectively 1300 and 1100 ℃.At SrTiO
3The metallic film of growth of passivation on the substrate, in the time of 450 ℃, gold atom does not react with oxygen but forms the passive metal film of supporting cluster, and titanium atom and oxygen fully react,, under nonreactive gold atom situation, form nanocluster and evenly be randomly dispersed in the golden passive film in titanium atom quantity.The control growing time is the thickness of may command film, i.e. the size of may command TiO 2 nano cluster amount; Thereby can control the size of the flow control nanocluster of MBE electron gun stove titanium.
The cross section of gained TiO 2 nano cluster such as Fig. 1, SrTiO
3Golden film is arranged on the substrate, and TiO 2 nano cluster is evenly distributed in the golden film of extension.
Gold does not react with oxygen, titanium and oxygen reaction form titanium dioxide nano material, valence state on the x-ray photoelectron spectroscopy shown in Figure 2 (XPS) can reflect, the gold film does not have oxidized valence state, and titanium and oxygen have ionic valence condition to form titanic oxide material, and oxygen and titanium can form the TiO 2 nano cluster structure.
Claims (2)
1, a kind of preparation method of TiO 2 nano cluster, it is characterized in that in MBE equipment, in the time of 450 ℃ on substrate the gold thin film of growth of passivation, the atomic molar ratio that comes out in and the titanium dioxide of titanium and the oxidation reaction of growing simultaneously, gold and the electron gun stove of titanium is 10:1.
2, preparation method according to claim 1 is characterized in that described substrate is SrTiO
3, MgO or LaAlO
3
Priority Applications (1)
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CNB2006101236873A CN100522820C (en) | 2006-11-22 | 2006-11-22 | Process for preparing TiO2 nano cluster |
Applications Claiming Priority (1)
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---|---|---|---|
CNB2006101236873A CN100522820C (en) | 2006-11-22 | 2006-11-22 | Process for preparing TiO2 nano cluster |
Publications (2)
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CN101007652A CN101007652A (en) | 2007-08-01 |
CN100522820C true CN100522820C (en) | 2009-08-05 |
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CNB2006101236873A Expired - Fee Related CN100522820C (en) | 2006-11-22 | 2006-11-22 | Process for preparing TiO2 nano cluster |
Country Status (1)
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CN (1) | CN100522820C (en) |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1670919A (en) * | 2005-05-16 | 2005-09-21 | 中国科学院物理研究所 | Method for preparing high-quality zinc polarity ZnO single crystal film on magnesium aluminate substrate |
JP2006218411A (en) * | 2005-02-10 | 2006-08-24 | Sumitomo Seika Chem Co Ltd | Nitrogen-doped titanium oxide having photocatalyst action and its production method |
-
2006
- 2006-11-22 CN CNB2006101236873A patent/CN100522820C/en not_active Expired - Fee Related
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2006218411A (en) * | 2005-02-10 | 2006-08-24 | Sumitomo Seika Chem Co Ltd | Nitrogen-doped titanium oxide having photocatalyst action and its production method |
CN1670919A (en) * | 2005-05-16 | 2005-09-21 | 中国科学院物理研究所 | Method for preparing high-quality zinc polarity ZnO single crystal film on magnesium aluminate substrate |
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CN101007652A (en) | 2007-08-01 |
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Granted publication date: 20090805 Termination date: 20101122 |