CN1118587C - Process for preparing hydrophobic rutile film by reinforced and magnetically controlled DC sputtering - Google Patents
Process for preparing hydrophobic rutile film by reinforced and magnetically controlled DC sputtering Download PDFInfo
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- CN1118587C CN1118587C CN 00127814 CN00127814A CN1118587C CN 1118587 C CN1118587 C CN 1118587C CN 00127814 CN00127814 CN 00127814 CN 00127814 A CN00127814 A CN 00127814A CN 1118587 C CN1118587 C CN 1118587C
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Abstract
The present invention relates to a method for preparing hydrophobic rutile film by reinforced and magnetically controlled DC sputtering, which is characterized in that reinforced DC sputtering conditions adopt highly magnetically-controlled Ti target sputtering, and are combined with the conditions of highly sputtering current density, high temperature of basal plates, low working air pressure and high oxygen partial pressure to ensure the sufficient ionization and the oxidation of a thin film of deposition, make the sputtering stable and improve the deposition rate. A TiO2 thin film prepared by the present invention has a rutile polycrystalline structure containing a little of anatase, has the advantages of favorable friction resistance and hydrophobic characteristic, and very good surface adhesion, can be used for surface coating of the materials of lenses made of glass, ceramic, cladding glass, automobile rear view mirrors, etc., and can also be used for preparing some biologic medicine materials.
Description
Technical field
The present invention relates to a kind of preparation method of nano titanium dioxide thin film materials; relate in particular to a kind of titanium deoxid film reinforced and magnetically controlled DC sputtering preparation method with rutile structure; the film of the present invention's preparation can be used for environment protection, engineering and biological medicine material, belongs to field of material engineering technology.
Background technology
Titanium dioxide (TiO
2) the surface under UV-irradiation, can have good hydrophilicity can and the ability of decomposing organic matter matter, this class material can produce free electron and hole under ultraviolet irradiation, thereby has a very strong photoxidation restoring function, various organic compound of oxidable decomposition and part inorganics, can destroy the cytolemma of bacterium and solidify the protein of virus, have extremely strong antifouling, sterilization and deodorization functions.Because the ability of the hydrophilic and decomposing organic matter matter of titanium dioxide makes that the Application Areas of photocatalysis material of titanium dioxide is very extensive: the processing of automatically cleaning, antifog, sterilization, antifouling, deodorizing, purifying air, water etc.
Photocatalysis material of titanium dioxide has three kinds of forms, liquid state, powder particle attitude and film attitude.Two kinds of method preparations of available chemistry and physics.In the prior art, chemical process is to prepare the most general method of titanium dioxide at present, R.Wang in 1997, Deng at Nature Vol.388,431 (1997) go up report successfully prepares the titanium deoxid film with strong katalysis with the method for chemistry, have received increasing attention, but the life-span with the film of chemical process preparation is very limited, the performance and the use range of the product of chemical process preparation also have significant limitation in addition, some product must be with the preparation method of physics as a supplement, with performance and the use range of enriching titanium dioxide product.Discover titanium dioxide (TiO
2) film except having good photocatalysis characteristic, the titanium dioxide (TiO that utilizes physical method (magnetron sputtering) under certain processing condition, to prepare
2) film, also have extraordinary hydrophobic property, and this specific character can't be because of the irradiation of UV-light changing to some extent, this has just greatly expanded titanium dioxide (TiO
2) practical application area of film.It is not very general preparing optically catalytic TiO 2 film with physical method at present, and physical method is varied, wherein is the method that adopts usually at present with the magnetron sputtering.But, because this method adopts general reactive sputtering, very strict to processing requirement, if it is improper that technology and technical finesse have slightly, prepared material just has obvious defects, composition is uncontrollable, sticking power and compactness is poor, rub resistance not, and particularly prepared titanium deoxid film is after friction, and its some physicals obviously reduces even completely dissolve.In addition, prepare the general technology of titanium deoxid film at present, also exist oxidation incomplete, sedimentation rate is low, problems such as sputter instability.Therefore, must improve its preparation technology and technology,, improve its practical application to improve the quality of film.
Summary of the invention
The objective of the invention is to above-mentioned deficiency, a kind of processing method of new preparation titanium dioxide hydrophobic rutile film is provided,, improve the performance of film, be more suitable for actual needs, expand its range of application to improve the quality of film at prior art.
For realizing such purpose, must improve the magnetic control degree of the plasma body on target surface, make that the energy of sputtered atom is more concentrated, adopt high current density, low operating air pressure and high keto sectional pressure simultaneously, to guarantee the abundant oxidation of sufficient ionization and deposit film, overcome oxygen partial pressure simultaneously when higher, the sputter instability that oxidation brought on target surface improves deposition.In addition, big deposition helps to reduce the content of gas molecule in the film, if oxygen molecule is activated or ionization preferably, and the lower words of operating air pressure, oxonium ion can further act on (with the suitable height of time substrate temperature) on the deposit film, forms high-quality thin film of titanium oxide.
The present invention has strengthened the direct magnetic control condition, adopt the sputter of high magnetic control titanium target, and prepare titanium deoxid film in conjunction with high sputtering current density, high substrate temperature, low operating air pressure and high keto sectional pressure condition, concrete technical scheme is as follows: adopt the sputter of titanium target, target Surface field intensity is 1000 Gausses, target surface is 7cm to the distance of substrate, and underlay substrate can adopt silicon chip, glass, pottery and tinsel etc.Toast vacuum chamber during preparation earlier, treat that base vacuum is evacuated to 1 * 10
-3Behind the Pa, near sputtering target, feed argon gas, keep Ar Pressure to be about 1Pa, increase the electric voltage ionization argon gas and produce glow discharge, regulate Ar Pressure to 0.4Pa, after sputter is stable, near aerating oxygen substrate, so that form pressure gradient at vacuum chamber, oxygen molecule is easy to be activated or ionization under this condition, operating air pressure still maintains 0.4Pa, intrinsic standoff ratio O
2: Ar=1: 1.Regulating voltage makes the sputtering current density of this moment be about 50mA/cm
2, deposition is about 0.7nm/s at this moment, if substrate temperature is controlled near 360 degree, the titanium deoxid film for preparing under this condition has the rutile polycrystalline structure that contains small amount of anatase.Experiment finds that the best effort air pressure during sputter is 0.4Pa (O
2: Ar=1: 1), its surface condition of titanium deoxid film best (hardness, density, homogeneity, sticking power the best) that scanning electron microscope and relevant contrast experiment's discovery prepare under this condition.Film thickness can determine that with depositing time film is thick more as required, and characteristic is outstanding more, and thickness is 100nm at least.
Obtain by X light diffracting analysis, prepared titanium deoxid film is 360 when spending at substrate temperature, forms the rutile polycrystalline structure that contains small amount of anatase easily, the hydrophobic property that the film of this structure has good rub resistance and gives prominence to very much.
Adopt the titanium deoxid film (the film thickness scope is 100-2000nm) of the inventive method preparation, following effect is arranged: when substrate was tilting, water did not have on substrate and stops, and hydrophobic effect is very obvious.In addition aspect rub resistance, after the titanium deoxid film friction of usual way preparation, its hydrophobic property obviously reduces even completely dissolve, and be greatly improved in this respect with the titanium deoxid film of the inventive method preparation, friction, its hydrophobic property of washing back are not seen reduction, and the raising of this and film quality has very big relation.In addition, the hydrophobic property of the titanium deoxid film of the present invention's preparation can not change to some extent because of the irradiation of UV-light, and can not mildew, and this has just greatly expanded the practical application area of titanium deoxid film.
The present invention has strengthened the magnetic control degree of sputtering target surface plasma, has improved the energy and the free path of deposition and atomic, and oxidation is more abundant, sputter is also highly stable, depositing of thin film speed and quality improve a lot, and the physicals of film also has big improvement, is more suitable for actual needs.
The film of the present invention's preparation can be used for glass mirror, pottery, and the surface coating of materials such as cladding glass and automobile rearview mirror also can be used for preparing some biological medicine material.
Below in conjunction with embodiment technical scheme of the present invention is further described.
Embodiment
Preparation titanium dioxide hydrophobic film adopts the sputter of titanium target under high current density, low operating air pressure condition, and target Surface field intensity is 1000 Gausses, and target surface is 7cm to the distance of substrate, and substrate adopts silicon chip.Toast vacuum chamber during preparation earlier, treat that base vacuum is evacuated to 1 * 10
-3Behind the Pa, feed the 1Pa argon gas near sputtering target, voltage adds to 500 volts of ionization argon gas and produces glow discharge, regulates Ar Pressure to 0.4Pa, and after sputter was stable, near aerating oxygen substrate, operating air pressure maintained 0.4Pa (O
2: Ar=1: 1), regulating voltage, making sputtering current density is 50mA/cm
2, substrate temperature is controlled at 360 degree, and this moment, deposition was 0.7nm/s.
The titanium deoxid film for preparing under this processing condition has the rutile polycrystalline structure that contains small amount of anatase, has good rub resistance and hydrophobic property, and surface adhesion force is very good.
Claims (1)
1, a kind of reinforced and magnetically controlled DC sputtering preparation method of hydrophobic rutile film, it is characterized in that strengthening the d.c. sputtering condition, adopt the sputter of high magnetic control titanium target, and in conjunction with high sputtering current density, high substrate temperature, low operating air pressure and high keto sectional pressure condition, titanium target Surface field intensity is 1000 Gausses, target surface to the distance of substrate is 7cm, toasts vacuum chamber, base vacuum to 1 * 10 during preparation earlier
-3Behind the Pa, feed argon gas near sputtering target, the maintenance Ar Pressure is 1Pa, increases the electric voltage ionization argon gas and produces glow discharge, regulates Ar Pressure to 0.4Pa, after sputter is stable, and near aerating oxygen substrate, operating air pressure maintains 0.4Pa, intrinsic standoff ratio O
2: Ar=1: 1, regulating voltage, making sputtering current density is 50mA/cm
2, substrate temperature is controlled at 360 degree, and deposition is 0.7nm/s.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 00127814 CN1118587C (en) | 2000-12-07 | 2000-12-07 | Process for preparing hydrophobic rutile film by reinforced and magnetically controlled DC sputtering |
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| Application Number | Priority Date | Filing Date | Title |
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| CN 00127814 CN1118587C (en) | 2000-12-07 | 2000-12-07 | Process for preparing hydrophobic rutile film by reinforced and magnetically controlled DC sputtering |
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| CN1309190A CN1309190A (en) | 2001-08-22 |
| CN1118587C true CN1118587C (en) | 2003-08-20 |
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| CN 00127814 Expired - Fee Related CN1118587C (en) | 2000-12-07 | 2000-12-07 | Process for preparing hydrophobic rutile film by reinforced and magnetically controlled DC sputtering |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWI372140B (en) * | 2003-01-28 | 2012-09-11 | Koninkl Philips Electronics Nv | Method of producing transparent titanium oxide coatings having a rutile structure |
| CN1302148C (en) * | 2004-07-12 | 2007-02-28 | 广州粤海真空技术有限公司 | Preparation method for TiOxNy highly effective solar photo-thermal conversion film |
| CN100413545C (en) * | 2005-08-11 | 2008-08-27 | 上海交通大学 | Method for preparing TiO2-HA biological medical nanometer structured film |
| CN100406611C (en) * | 2005-08-11 | 2008-07-30 | 上海交通大学 | Method of preparing nano-structure bioactive titanium metal film |
| CN100345599C (en) * | 2005-08-11 | 2007-10-31 | 上海交通大学 | Prepn process of biomedical active TiO2 film |
| CN111945120A (en) * | 2020-07-23 | 2020-11-17 | 江苏理工学院 | In-situ preparation method and application of super-hydrophobic titanium film |
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