CN1904137A - Quasi-mono-dimension nano-structure of low sublimation temperature high deposition temperature metallic oxide and its thin film preparation method - Google Patents
Quasi-mono-dimension nano-structure of low sublimation temperature high deposition temperature metallic oxide and its thin film preparation method Download PDFInfo
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- CN1904137A CN1904137A CN 200610036916 CN200610036916A CN1904137A CN 1904137 A CN1904137 A CN 1904137A CN 200610036916 CN200610036916 CN 200610036916 CN 200610036916 A CN200610036916 A CN 200610036916A CN 1904137 A CN1904137 A CN 1904137A
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Abstract
This invention relates to a process for preparing metal oxide quasi-one-dim nanometer structure which has low sublimation temperature and high depositing temperature. The feature is that evaporative source evaporating and depositing on the substrate sole to form the output when in the vacuum and depositing temperature higher then evaporative source temperature. Depositing sole located in high temperature region, metal evaporating source located in low temperature. Input small amounts of oxygen, through reaction to form oxide and deposit on the sole to form the output
Description
Technical field
The present invention relates to the preparation method of a kind of low sublimation temperature temperature high deposition metal oxide quasi-one dimensional nanostructure and film thereof.This method is applicable to the quasi-one-dimensional nanometer material for preparing certain quasi-metal oxides such as magnesium oxide, zinc oxide, chromic oxide under vacuum condition, and the feature of this metalloid is: the sublimation temperature of metal is less than the formation temperature of its oxide compound quasi-one dimensional nanostructure under the certain vacuum degree.
Technical background
Metal oxide materials has important application in electron device, for example magnesium oxide has superior secondary electron emission characteristic, especially has a wide range of applications in the plasma panel display spare in electron device.Nano material is because scale effect can make material have unique performance on Electronic Performance, mechanical property and chemical property, for example quasi-one-dimensional nanometer material may make bill of material reveal good electronic emission performance because its big length-to-diameter ratio is brought strong electric field reinforcing effect.Be object with magnesium oxide below, the technology of preparing background of quasi-one-dimensional nanometer material is described.
The preparation method of magnesium oxide quasi-one-dimensional nanometer material has chemical vapor deposition (CVD) method, molecular beam epitaxy (MBE) method, solution method etc.In CVD method and MBE method; usually need to feed a large amount of argon gas as shielding gas; and form certain air pressure, then 800～950 ℃ of heating evaporation source MAGNESIUM METAL, oxidation afterwards also is being positioned at formation of deposits magnesium oxide quasi-one-dimensional nanometer material on the substrate of cold zone.But the someone reports that adopting underlayer temperature to be higher than the evaporation source method of temperature in a vacuum prepares magnesium oxide quasi-one dimensional nanostructure and film thereof as yet at present.
Technological invention
The preparation method of low sublimation temperature temperature high deposition metal oxide quasi-one dimensional nanostructure of the present invention and film thereof may further comprise the steps:
(1) cleaning base plate is removed the impurity on the substrate;
(2) substrate is placed the high-temperature zone, and the metal evaporation sources that will hang down sublimation temperature is positioned over cold zone, then substrate and evaporation source is placed in the vacuum unit together, vacuum unit is evacuated to the certain vacuum degree;
(3) substrate is warming up to certain temperature T
1, the evaporation source metal is warming up to certain temperature T
2, insulation for some time t
1T wherein
1And T
2Need satisfy following condition: T
2Sublimation temperature T more than or equal to evaporation source
0, T
1Greater than T
2, i.e. T
0≤ T
2＜T
1
(4) feed a certain amount of oxygen then, and insulation for some time t
2Stop logical oxygen at last, lower the temperature and be cooled to room temperature.
The present invention has important meaning to method and the technology that the development vacuum condition prepares quasi-one-dimensional nanometer material down, and it is simple that the present invention simultaneously prepares the required equipment of nanostructure, and cost is low, and is easy to realize the controlled preparation of nanostructure.
Description of drawings
Fig. 1 is the SEM photo that utilizes the bitter earth nano rod film of method for preparing.
Fig. 2 is the XRD analysis result who utilizes the bitter earth nano rod film of method for preparing.
Fig. 3 is TEM photo and the electron diffraction photo that utilizes the magnesium oxide nanometer rod of method for preparing.
Fig. 4 is the field emission characteristic curve (I-V curve and FN curve) that utilizes the bitter earth nano rod film of method for preparing.
Fig. 5 is the SEM photo that utilizes the bitter earth nano awl film of method for preparing.
Fig. 6 is the SEM photo that utilizes the junction type bitter earth nano rod film of method for preparing.
Embodiment for example
The preparation of embodiment 1 bitter earth nano rod film
With (100) silicon chip as substrate, ultrasonic cleaning 5 minutes in acetone earlier, ultrasonic cleaning 5 minutes in dehydrated alcohol then.
Silicon chip is put into tungsten boat (120 * 20 * 0.3mm
3) in; Twine the metal magnesium ribbon with tungsten bar or ceramic plate, be placed on silicon chip directly over, the distance of the two is 1mm～5mm.Above-mentioned mounted tungsten boat is put into vacuum unit, vacuum unit is evacuated to the vacuum tightness of 4-5Pa, keep this vacuum tightness then.
The tungsten boat is heated to certain temperature T
1(T
1=700-900 ℃), the temperature T of while evaporation source MAGNESIUM METAL
2Reach 430 ℃ of its sublimation temperatures, be incubated 5 minutes then.
Follow aerating oxygen, flow velocity is about 5-10sccm, and is incubated 20 minutes.
Stop logical oxygen at last, lower the temperature and be cooled to room temperature.
To by prepared magnesium oxide quasi-one dimensional nanostructure and the film thereof that goes out of above-mentioned steps, characterize and analyze with scanning electron microscope (SEM), X-ray diffraction (XRD) and transmission electron microscope (TEM), tested its field emission performance simultaneously.Be described further below in conjunction with accompanying drawing.
Fig. 1 is the SEM photo that utilizes the bitter earth nano rod film of method for preparing.See from figure: prepared nano-rod film length is 1～3 μ m, and diameter is between 100～300nm, and it is more even to distribute.
Fig. 2 is the XRD analysis result who utilizes the bitter earth nano rod film of method for preparing.XRD shows that prepared nanometer rod is a magnesium oxide single crystal.
Fig. 3 is TEM photo and the electron diffraction photo that utilizes the magnesium oxide nanometer rod of method for preparing.See from electron-diffraction diagram: the prepared magnesium oxide nanometer rod crystalline direction of growth is [100] direction.
Fig. 4 is the field emission characteristic curve (I-V curve and FN curve) that utilizes the bitter earth nano rod film of method for preparing.The unlatching electric field of this sample is that (emission is 10 μ A/cm to 7.3MV/m
2), maximum current density is 7.537mA/cm
2
The preparation of embodiment 2 bitter earth nanos awl film
The preparation method is similar to the method for embodiment 1, and difference is in the evaporation source temperature T
2Different with the flux values of aerating oxygen.That is: use (100) silicon chip as substrate, and carry out clean; Cleaned silicon chip is put into the tungsten boat, evaporation source metal magnesium ribbon be placed on silicon chip directly over; Above-mentioned mounted tungsten boat is put into vacuum unit, and be evacuated to 4-5Pa; The tungsten boat is heated to temperature T
1(T
1=700-900 ℃), evaporation source MAGNESIUM METAL temperature T
2Reach 600 ℃, be incubated 5 minutes then; Follow aerating oxygen, flow velocity is about 20sccm, and is incubated 20 minutes; Stop logical oxygen at last, lower the temperature and be cooled to room temperature.
Fig. 5 is the bitter earth nano awl film SEM photo that utilizes method for preparing.
The preparation of embodiment 3 junction type bitter earth nano rod films
The preparation method is similar to the method for embodiment 1, and difference is the flux values difference of aerating oxygen.That is: use (100) silicon chip as substrate, and carry out clean; Cleaned silicon chip is put into the tungsten boat, evaporation source metal magnesium ribbon be placed on silicon chip directly over; Above-mentioned mounted tungsten boat is put into vacuum unit, and be evacuated to 4-5Pa; The tungsten boat is heated to temperature T
1(T
1=700-900 ℃), the temperature T of heating evaporation source MAGNESIUM METAL
2Reach 430 ℃ of its sublimation temperatures, be incubated 5 minutes then; Follow aerating oxygen, flow velocity is about 20sccm, and is incubated 20 minutes; Stop logical oxygen at last, lower the temperature and be cooled to room temperature.
Fig. 6 is the SEM photo that utilizes the junction type bitter earth nano rod film of method for preparing.
Preparation method's analysis of quasi-one-dimensional nanometer materials such as embodiment 4 zinc oxide, chromic oxide
Similar to MAGNESIUM METAL, the low-temperature distillation phenomenon can take place in metals such as zinc, chromium in vacuum environment, and vacuum tightness is high more, and sublimation temperature is low more.In addition, according to document
1,2Report, adopt the preparation temperature of the prepared zinc oxide quasi-one-dimensional nanometer material of CVD or PVD (physical vapor deposition) method all to be higher than the sublimation temperature of zinc in vacuum condition, and this phenomenon is identical with the phenomenon that magnesium oxide quasi-one-dimensional nanometer material preparation process in embodiments of the invention 1 and 2 is taken place, therefore, adopt the method for foregoing invention, can prepare the quasi-one-dimensional nanometer material of certain quasi-metal oxides such as zinc oxide, chromic oxide equally.
Reference:
1.P.X.Gao，Z.L.Wang，J.Phys.Chem.B?2004，108，7534-7537
2.X.Wang，et?al，Appl.Phys.Lett.，2004，84，4941
Claims (4)
1, a kind of method for preparing low sublimation temperature temperature high deposition metal oxide quasi-one dimensional nanostructure and film thereof is characterized in that: in a vacuum, substrate temperature is higher than under the evaporation source temperature condition, makes its evaporation by the heating of metal source; Aerating oxygen makes the metal and the oxygen reaction that are evaporated form the respective metal oxide compound, and is deposited on formation metal oxide quasi-one dimensional nanostructure and film thereof on the substrate then.
2, the method for preparing metal oxide quasi-one dimensional nanostructure and film thereof that claim 1 is narrated, its processing step is:
(1) cleaning base plate is removed the impurity on the substrate;
(2) substrate is placed the high-temperature zone, and the metal evaporation sources that will hang down sublimation temperature is positioned over cold zone, then substrate and evaporation source is placed in the vacuum unit together, vacuum unit is evacuated to below the 10Pa;
(3) substrate is warming up to certain temperature T
1, the evaporation source metal is warming up to the temperature T of its distillation
2, and insulation, wherein T
1And T
2Need satisfy following condition: T
2Sublimation temperature T more than or equal to evaporation source
0, T
1Greater than T
2, i.e. T
0≤ T
2＜T
1
(4) feed the oxygen of flow less than 20sccm, and insulation; Reaction finishes, and stops logical oxygen, lowers the temperature and is cooled to room temperature.
3, the preparation method of described metal oxide quasi-one dimensional nanostructure of claim 2 and film thereof, it is characterized in that: the underlay substrate temperature is higher than the evaporation source temperature.
4, prepared metal oxide quasi-one dimensional nanostructure and the film thereof of claim 1 or 2 described methods has application in electron device.
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|---|---|---|---|
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101805883B (en) * | 2009-02-13 | 2012-06-06 | 比亚迪股份有限公司 | Film plating plate and preparation method thereof |
| CN108565132A (en) * | 2018-05-15 | 2018-09-21 | 中国科学院深圳先进技术研究院 | A kind of fibrous material and preparation method thereof with metal oxide nanostructure |
-
2006
- 2006-08-03 CN CN 200610036916 patent/CN1904137A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101805883B (en) * | 2009-02-13 | 2012-06-06 | 比亚迪股份有限公司 | Film plating plate and preparation method thereof |
| CN108565132A (en) * | 2018-05-15 | 2018-09-21 | 中国科学院深圳先进技术研究院 | A kind of fibrous material and preparation method thereof with metal oxide nanostructure |
| CN108565132B (en) * | 2018-05-15 | 2019-09-27 | 中国科学院深圳先进技术研究院 | A kind of fibrous material and preparation method thereof with metal oxide nanostructure |
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Open date: 20070131 |