CN110295354A - A kind of direct current reaction magnetron sputtering deposition method of transition metal oxide film - Google Patents
A kind of direct current reaction magnetron sputtering deposition method of transition metal oxide film Download PDFInfo
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- CN110295354A CN110295354A CN201910716179.3A CN201910716179A CN110295354A CN 110295354 A CN110295354 A CN 110295354A CN 201910716179 A CN201910716179 A CN 201910716179A CN 110295354 A CN110295354 A CN 110295354A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/0021—Reactive sputtering or evaporation
- C23C14/0036—Reactive sputtering
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/08—Oxides
- C23C14/083—Oxides of refractory metals or yttrium
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/54—Controlling or regulating the coating process
- C23C14/548—Controlling the composition
Abstract
The invention discloses a kind of direct current reaction magnetron sputtering deposition methods of transition metal oxide film, include the following steps: the cathode for being equipped with transition metal target being connected to external dc power, suitable sedimentary condition is set, DC power supply is opened and generates plasma；It is stepped up or reduces and enter the indoor reaction gas flow of vacuum sputtering chamber, obtain a particular kind of relationship curve about target voltage and reaction gas flow；According to the relation curve by the reactive sputtering region division of reaction gas zero point to target voltage highest point be metal area, it is metal oxide area by the reactive sputtering region division after target voltage highest point, the corresponding reaction gas flow in target voltage highest point is inflection point reaction gas flow, and the operating point codetermined by multiple technological parameters is obtained near inflection point reaction gas flow；Reactive magnetron sputtering is carried out under the operating point to prepare the transition metal oxide material haveing excellent performance.The present invention relates to technical field of film preparation.
Description
Technical field
The present invention relates to technical field of film preparation, in particular to the direct current reaction magnetic of a kind of transition metal oxide film
Control sputter deposition.
Background technique
Transition metal oxide such as tungsten oxide (WOx), molybdenum oxide (MoOx), tantalum oxide (TaOx), niobium oxide (NbOx) and
Aoxidize tungsten (Mo1-yWyOx) etc. since it is special with different material properties such as carrier transport selectivity, high work content, high dielectric
Property, high light transmission rate and ion it is embeddable or abjection etc. characteristics thus be widely used in electrochromic device, solar cell,
In full thin film solid state capacitor, photoelectric sensor and transistor etc., play an important role.For example, in electrochromic device
In, metal oxide such as tungsten oxide (WOx) it is used as the photochromic layer of full thin film solid state electrochromic device, and tantalum oxide (TaOx)
Then using the ion transport layers of hydrogen ion transmission.In addition, the transition metal oxide such as MoO of high work content can be usedxAnd WOxEqual materials
Material is applied in thin-film solar cells as used in cadmium telluride (CdTe) solar battery, copper indium gallium selenide (CIGS) solar battery
In the contact performance and carrier transmission performance that adjust material.Currently, usually preparing one layer or multilayer transition metal oxide
Applied in crystal-silicon solar cell, effect, anti-reflection effect, front-surface field and back surface field are passivated to electrode surface and made
With, and with crystalline silicon material form the various effects such as p-n heterojunction.Metal oxide such as TaOxFilm is in thin film transistor (TFT)
Excellent switch performance etc. is realized as dielectric material.
Magnetically controlled sputter method is widely used in the preparation of transition metal oxide material, and wherein using the anti-of metal targets
Answer magnetically controlled sputter method that fast deposition may be implemented, the features such as material composition is easily adjusted.Nevertheless, using reaction magnetocontrol sputtering side
Technique is relative complex when method prepares transition metal oxide, and the sedimentary condition of one side reaction magnetocontrol sputtering process such as sputters function
Rate, operating air pressure, reaction gas flow, underlayer temperature etc. interdepend；On the other hand, reactive sputtering process may have multiple
The material of reaction interval such as metal area, transition region, oxide region etc., the preparation of differential responses section has different material properties.
Different transition metal oxide materials have the characteristics that different reactive sputtering areas, and the material of optimization characteristics is in specifically reaction magnetic
Prepared by the operating point for controlling the reactive sputtering section of sputtering process completes, and how to determine the reactive sputtering in specific reactive sputtering section
Operating point is particularly significant.
Summary of the invention
It is an object of the invention to overcome the deficiencies of existing technologies and insufficient, provides and a kind of utilize target voltage monitor mode
It monitors target material surface state, and then obtains the work codetermined by multiple technological parameters near inflection point reaction gas flow
Point carries out reactive magnetron sputtering under the operating point to prepare the transition metal oxide material haveing excellent performance.
The purpose of the present invention can be achieved through the following technical solutions: a kind of direct current reaction of transition metal oxide film
Magnetron sputtering deposition method includes the following steps: the cathode for being equipped with transition metal target being connected to external dc power, set
Suitable sedimentary condition opens DC power supply and generates plasma；It is stepped up or reduces and is indoor into vacuum sputtering chamber
Reaction gas flow obtains a particular kind of relationship curve about target voltage and reaction gas flow；According to the relation curve
It is metal area by the reactive sputtering region division of reaction gas flow zero point to target voltage highest point, after target voltage highest point
Reactive sputtering region division be metal oxide area, the corresponding reaction gas flow in target voltage highest point be inflection point reaction gas
Flow obtains the operating point codetermined by multiple technological parameters near inflection point reaction gas flow；Under the operating point into
Row reactive magnetron sputtering is to prepare the transition metal oxide material haveing excellent performance.
As a preferred technical solution, in the metal area, target voltage increases with the increase of reaction gas flow,
In the metal oxide area, target voltage keeps relative stability with the increase of reaction gas flow.
Dynamic deposition rate and dynamic deposition rate highest point in reaction gas flow curve as a preferred technical solution,
Corresponding inflection point reaction gas flow position, with the inflection point reaction gas flow position in the curve of target voltage and reaction gas flow
It is equipped with deviation.
The metal area has low light transmission rate as a preferred technical solution, and the metal oxide area has height
Light transmission rate.
As a preferred technical solution, under inflection point reaction gas flow, the surface topography of metal-oxide film with
The raising of air pressure becomes loose from compact, or even slight crack occurs under highest operating air pressure.
As a preferred technical solution, the particular kind of relationship curve can also be target voltage and reaction gas partial pressure curves or
Target voltage and reaction gas content curve.
The metallic target is for single tungsten target, included a tantalum target, molybdenum target or niobium target and by these gold as a preferred technical solution,
Belong to the binary or multicomponent alloy target of composition.The transition metal oxide be metallic tungsten oxide, molybdenum oxide, tantalum oxide or
Niobium oxide and the binary being made of tungsten, tantalum, molybdenum and niobium or multi-element alloy oxide film.
The sedimentary condition includes power, operating air pressure, underlayer temperature and working distance as a preferred technical solution,
From.
Reaction gas is oxygen as a preferred technical solution,.
Compared with the prior art, the invention has the following advantages and beneficial effects:
1. the present invention is divided into metal area and gold using the state of target voltage monitor mode monitoring target, by sputtering conversion zone
Belong to oxide region, preferably operating point is obtained near inflection point reaction gas flow, oxo transition metal is realized at the operating point
Compound is closed stablizing for object material and is prepared, and the material property of optimization is obtained.
2. using the transition metal oxide film preparation process characteristic (oxygen flow-target voltage) and phase of this method preparation
The material property answered includes that deposition rate, optical characteristics, surface topography and crystal structure etc. are not only adapted to the oxygen enumerated
Change W film, tantalum oxide films, while being also suitable for Electrochromic Molybdenum Oxide Coatings, columbium oxide film and being made of tungsten, tantalum, molybdenum and niobium
Binary or multi-element alloy oxide film, the scope of application are wider.
3. single metal oxide and multi-element metal oxide thin-film material may be implemented in the present invention preparation and performance
Optimization, can be widely applied to include the devices such as solar cell, electrochromic device, supercapacitor, photoelectric sensor, transistor
In.
Detailed description of the invention
Fig. 1 is to prepare tungsten oxide (WO using reaction magnetocontrol sputtering in the embodiment of the present invention onex) film when in different works
Make the relation curve of the target voltage and oxygen flow under air pressure, and prepared under different operating air pressure and different oxygen flows
The dynamic deposition rate curve of tungsten oxide film.
Fig. 2 is the oxidation prepared in the case where operating air pressure is 0.5Pa and under different oxygen flows in the embodiment of the present invention one
The light transmission rate curve of W film.
Fig. 3 is in the embodiment of the present invention one in different operating air pressure (0.5Pa, 2.0Pa, 4.0Pa, 6.0Pa) and different
Light transmission rate of the tungsten oxide film prepared under oxygen flow in 400-800nm wave-length coverage.
Fig. 4 is in the embodiment of the present invention one in different operating air pressure (0.5Pa, 2.0Pa, 4.0Pa, 6.0Pa) and selection target
The x-ray diffraction spectrogram of the tungsten oxide film prepared under the oxygen flow at corner position in voltage-oxygen flow curve and
Corresponding surface topography map.
Fig. 5 is in the embodiment of the present invention one in different operating air pressure (0.5Pa, 2.0Pa, 4.0Pa, 6.0Pa) and selection target
The tungsten oxide film prepared under the oxygen flow at corner position in voltage-oxygen flow curve is applied to full thin film solid state electricity
The electrochromic property of mutagens color device.
Fig. 6 is when preparing tantalum oxide films using reaction magnetocontrol sputtering in the embodiment of the present invention two in different operating air pressures
Under target voltage and oxygen flow relation curve.
Fig. 7 is to use reaction magnetocontrol sputtering when preparing tantalum oxide films at 0.5Pa and 2.0Pa in the embodiment of the present invention two
With target voltage, oxygen partial pressure and the corresponding dynamic deposition rate under different oxygen flows.
Fig. 8 is in the embodiment of the present invention two in different operating air pressure (0.5Pa, 1.0Pa, 2.0Pa, 4.0Pa) and selection target
The x-ray diffraction spectrogram of the tantalum oxide films prepared under the oxygen flow at corner position in voltage-oxygen flow curve and
Corresponding surface topography map.
Specific embodiment
Present invention will now be described in further detail with reference to the embodiments and the accompanying drawings, but embodiments of the present invention are unlimited
In this.
Embodiment one
Tungsten oxide film is prepared using the target voltage monitor mode in the present invention, and as electrochromic layer applied to complete thin
In film solid electrochromic device, device architecture is glass substrate/ITO (transparent electrode layer)/NiOx(ion storage)/TaOx
(solid electrolyte layer)/WOx(electrochromic layer)/ITO (transparent electrode layer).Firstly, passing through tune under different operating air pressures
Oxygen flow (changing from 0sccm to 20sccm) is saved, the variation of corresponding target voltage is measured, wherein sputtering power is 200W holding
Constant, substrate does not heat.Fig. 1 is to prepare tungsten oxide (WO using reaction magnetocontrol sputteringx) film when under different operating air pressures
Target voltage and oxygen flow relation curve.With the increase of oxygen flow, target voltage increases.Then, with oxygen flow
The target voltage that continues growing reach a high point, then keep relative stability.By oxygen zero point to the reaction of target voltage highest point
Sputter area is divided into metal area, is metal oxide area, target electricity by the reactive sputtering region division after target voltage highest point
Pressing the corresponding oxygen flow in highest point is inflection point oxygen flow.
Target voltage in metal area increases as oxygen flow increases, and this is mainly due to the increasings with oxygen flow
The content (occupied area ratio) of the metal oxide on target surface is added to increase, and the secondary rate of tungsten oxide is than metal
Secondary rate is low, and so as to cause the electric current under firm power as oxygen flow is reduced, target voltage is increased.In gold
The target surface for belonging to oxide region is almost covered by tungsten oxide constituent.With the raising of operating air pressure, peak target electricity
Oxygen flow (inflection point oxygen flow) needed for pressure reduces (being moved to the left), this has with the partial pressure of oxygen increase under high operating air pressure
It closes.It is easier to cause the oxidation on metallic target surface under the conditions of high oxygen partial pressures, to reach high target under small oxygen flow
Voltage.
As shown in Figure 1, the Dynamic deposition speed of the tungsten oxide film prepared under different operating air pressure and different oxygen flows
Rate reduces afterwards as the increase of oxygen flow first increases.Inflection point oxygen flow position is deviateed in dynamic deposition rate highest point, low
Under oxygen flow raised dynamic deposition rate mainly due to the raising of voltage cause sputtering particle energy increase so as to cause
Sputtering yield increases.In addition, the sputtering yield due to oxide itself is lower than the sputtering yield of metal, with oxygen flow
Increase target material surface oxide content to increase, so as to cause deposition rate reduction.To obtain larger dynamic deposition rate, can turn
Point oxygen flow is biased to obtain at the position of metal area by oxygen flow, sputtering power, operating air pressure, underlayer temperature, working distance
From etc. the operating point that codetermines of multiple technological parameters, the operating point by the tungsten oxide film dynamic deposition rate of acquisition compared with
Greatly.
As shown in Fig. 2, the tungsten oxide film prepared in the case where operating air pressure is 0.5Pa as its is whole for the increase of oxygen flow
Light transmission rate in a wave-length coverage increases, and reaches high value in inflection point oxygen stream magnitude.This rule is suitable for other work
The tungsten oxide film prepared under air pressure series.As shown in figure 3, operating air pressure be 0.5Pa, 2.0Pa, 4.0Pa and 6.0Pa and
Light transmission rate of the tungsten oxide film prepared under different oxygen flows in 400-800nm wave-length coverage is with oxygen flow
Increase and quickly increase, then keeps a metastable value.It follows that can be with by target voltage-oxygen flow curve
Fast and effeciently setting obtains the reaction magnetic control with the metal oxide materials of high light transmission rate and opposite high deposition rate
Sputter area and correspondingly deposited condition (including most important inflection point oxygen stream magnitude).
By choosing the relatively high tungsten oxide of transmitance prepared under the conditions of oxygen flow at inflection point under different operating air pressure
Film compares its crystal structure and surface topography.As shown in figure 4, non crystalline structure is presented in all oxides film.Nevertheless,
With the raising of air pressure, the surface topography of film becomes loose from compact, or even slight crack occurs in high operating air pressure.
And of a relatively loose tungsten oxide film is excellent electroluminescent applied to may be implemented in full thin film solid state electrochromic device
Discoloration.Because of a relatively loose tungsten oxide film has more crystal boundaries, crystal boundary provides the channel of ion transport.More
Ion can be embedded in the area of space of tungsten oxide crystals, in conjunction with the external electrical (electroneutral for keeping material internal) of injection
To change the relationship between energy levels of material, the color shifting properties of material are realized.Under selection different operating air pressure at inflection point under oxygen flow
The tungsten oxide film of preparation is applied in full thin film solid state electrochromic device as electrochromic layer.Device architecture is glass lined
Bottom/ITO (transparent electrode layer)/NiOx(ion storage)/TaOx(solid electrolyte layer)/WOx(electrochromic layer)/ITO is (thoroughly
Prescribed electrode layer)) electrochromic property.As shown in figure 5, joint electrochemical workstation and spectrophotometer (are surveyed using dynamics
Amount mode) measure the variation that electrochromic device (changes voltage) at any time for the light transmission rate at 600nm in wavelength.It can see
Out, the tungsten oxide film prepared in the case where operating air pressure is 4.0Pa is applied in full thin film solid state electrochromic device with highest
Light modulation range (performance).
The target voltage during reaction magnetocontrol sputtering-oxygen flow curve under different materials and different sedimentary conditions is not
Together, the reactive sputtering region of division also will be different.By means of the present invention, target is fast and effeciently monitored in not synsedimentary item
Surface state under part, the metal oxide prepared by reaction magnetocontrol sputtering method in the operating point in different reactive sputtering areas
Film will obtain different material properties.The work codetermined by multiple technological parameters is obtained near inflection point reaction gas flow
Make a little, can fast and effeciently optimize material properties and promotes corresponding device performance.
Embodiment two
It is used in embodiment one and prepares the same method of tungsten oxide film and prepare tantalum oxide films, sputtering power is
200W is kept constant, and substrate is heating.Fig. 6 is to pass through under different operating air pressures (0.5Pa, 1.0Pa, 2.0Pa, 4.0Pa)
It adjusts oxygen flow to change from 0sccm to 16sccm, measures the change curve of corresponding target voltage.Using reaction magnetocontrol sputtering side
Method prepares tantalum oxide films and acquisition target voltage and oxygen flow relation curve when preparing tungsten oxide film are very alike.Equally,
With the increase of oxygen flow, target voltage increases.Then, as the target voltage that continues growing of oxygen flow reaches a high point,
It then keeps relative stability, at this moment target surface is almost covered by tantalum oxide ingredient.Equally, for the preparation of tantalum oxide films
For, reactive sputtering zoning can be divided into metal area and metal oxide area by dividing by target voltage-oxygen flow.By such
Method fast and effeciently monitors surface state of the target under different sedimentary conditions, by reaction magnetocontrol sputtering method in difference
Reactive sputtering area operating point preparation metal-oxide film will obtain different material properties.
Fig. 7 is to prepare tantalum oxide (TaO using reaction magnetocontrol sputteringx) film when at 0.5Pa and 2.0Pa and different oxygen
Target voltage, oxygen partial pressure and corresponding dynamic deposition rate under flow.Equally, in different operating air pressure and different oxygen streams
The dynamic deposition rate of the lower tantalum oxide films prepared of amount reduces afterwards as the increase of oxygen flow first increases.Dynamic deposition rate
Inflection point oxygen flow position is deviateed in highest point, and the tungsten oxide prepared in changing rule and embodiment one is consistent.Partial pressure of oxygen with
The increase of oxygen flow and increase.
Fig. 8 is under the operating air pressure of 0.5Pa, 1.0Pa, 2.0Pa and 4.0Pa and in corresponding target voltage-oxygen flow
X-ray diffraction spectrum (XRD) figure of the tantalum oxide films prepared under the oxygen flow at corner position in curve and corresponding table
Face shape appearance figure (scanning electron microscope, that is, SEM figure).All tantalum oxide films are non crystalline structure.Meanwhile with the increase of air pressure,
Tantalum oxide films surface topography changes from fine and close appearance to the thin cellular of pine.The tantalum oxide films prepared under hyperbar are conducive to water
Absorption, dissolution and the transmission of internal proton of molecule are applied to all solid state electricity to realize high ion (proton) electric conductivity
High electro-optic response rate may be implemented in mutagens color device.The tantalum oxide films prepared at 2Pa are applied to all solid state electroluminescent
Electroluminescent device can obtain highest smooth adjustable range.
In addition, using the transition metal oxide film preparation process characteristic (oxygen flow-target electricity of the method for the present invention preparation
Pressure) and corresponding material property include that deposition rate, optical characteristics, surface topography and crystal structure etc. are not only adapted to arrange
Tungsten oxide film, the tantalum oxide films of act, while being also suitable for Electrochromic Molybdenum Oxide Coatings, columbium oxide film and by tungsten, tantalum, molybdenum and niobium
The binary or multi-element alloy oxide film of composition.
The embodiments described above only express several embodiments of the present invention, and the description thereof is more specific and detailed, but simultaneously
Limitations on the scope of the patent of the present invention therefore cannot be interpreted as.It should be pointed out that for those of ordinary skill in the art
For, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to guarantor of the invention
Protect range.Therefore, the scope of protection of the patent of the invention shall be subject to the appended claims.
Claims (10)
1. a kind of direct current reaction magnetron sputtering deposition method of transition metal oxide film, which is characterized in that including walking as follows
It is rapid:
The cathode for being equipped with transition metal target is connected to external dc power, sets suitable sedimentary condition, opens direct current
Source generates plasma；
It is stepped up or reduces and enter the indoor reaction gas flow of vacuum sputtering chamber, obtain one about target voltage and reaction
The particular kind of relationship curve of gas flow；
According to the relation curve by the reactive sputtering region division of reaction gas flow zero point to target voltage highest point be metal
Reactive sputtering region division after target voltage highest point is metal oxide area, the corresponding reaction in target voltage highest point by area
Gas flow is inflection point reaction gas flow, and acquisition is codetermined by multiple technological parameters near inflection point reaction gas flow
Operating point；
Reactive magnetron sputtering is carried out under the operating point to prepare the transition metal oxide material haveing excellent performance.
2. deposition method according to claim 1, which is characterized in that in the metal area, target voltage is with reaction gas
The increase of body flow and increase, in the metal oxide area, target voltage keeps opposite with the increase of reaction gas flow
Stablize.
3. deposition method according to claim 1, which is characterized in that in dynamic deposition rate and reaction gas flow curve
Dynamic deposition rate highest point corresponding inflection point reaction gas flow position, and in the curve of target voltage and reaction gas flow
There is deviation in inflection point reaction gas flow position.
4. deposition method according to claim 1, which is characterized in that the metal area has low light transmission rate, described
Metal oxide area has high light transmission rate.
5. deposition method according to claim 1, which is characterized in that under inflection point reaction gas flow, metal oxide
The surface topography of film becomes loose from compact, or even slight crack occur under highest operating air pressure with the raising of air pressure.
6. deposition method according to claim 1, which is characterized in that the particular kind of relationship curve can also be target voltage and
Reaction gas partial pressure curves or target voltage and reaction gas content curve.
7. deposition method according to claim 1, which is characterized in that the metallic target be single tungsten target, included a tantalum target, molybdenum target or
Person's niobium target and the binary being made of these metals or multicomponent alloy target.
8. deposition method according to claim 1, which is characterized in that the transition metal oxide be metallic tungsten oxide,
Molybdenum oxide, tantalum oxide or niobium oxide and the binary being made of tungsten, tantalum, molybdenum and niobium or multi-element alloy oxide film.
9. deposition method according to claim 1, which is characterized in that the sedimentary condition includes power, work gas
Pressure, underlayer temperature and operating distance.
10. -9 described in any item deposition methods according to claim 1, which is characterized in that reaction gas is oxygen.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109449247A (en) * | 2018-09-11 | 2019-03-08 | 暨南大学 | Tin dope Electrochromic Molybdenum Oxide Coatings, wide spectrum photodetector array based on tin dope Electrochromic Molybdenum Oxide Coatings and preparation method thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS59208815A (en) * | 1983-05-13 | 1984-11-27 | Kyocera Corp | Buried composite target in magnetron sputtering apparatus |
| CN101333643A (en) * | 2007-06-26 | 2008-12-31 | 衡阳市真空机电设备有限公司 | Reactive sputtering knee voltage control process for energy-conserving high-efficiency solar thermal-collecting tube coating machine |
| CN101694328A (en) * | 2009-10-28 | 2010-04-14 | 董晏伯 | Multitarget and high temperature and oxidation resisting solar energy absorbing membranous layer and production method thereof |
| US20100276282A1 (en) * | 2002-09-30 | 2010-11-04 | Miasole | Manufacturing Apparatus and Method for Large-Scale Production of Thin-Film Solar Cells |
| CN104278246A (en) * | 2014-10-28 | 2015-01-14 | 佳木斯大学 | Method of preparing DLC film on substrate surface |
| CN109402565A (en) * | 2018-10-11 | 2019-03-01 | 暨南大学 | A kind of growing method of nickel oxide film, nickel oxide film and its photoelectric device |
-
2019
- 2019-08-05 CN CN201910716179.3A patent/CN110295354A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS59208815A (en) * | 1983-05-13 | 1984-11-27 | Kyocera Corp | Buried composite target in magnetron sputtering apparatus |
| US20100276282A1 (en) * | 2002-09-30 | 2010-11-04 | Miasole | Manufacturing Apparatus and Method for Large-Scale Production of Thin-Film Solar Cells |
| CN101333643A (en) * | 2007-06-26 | 2008-12-31 | 衡阳市真空机电设备有限公司 | Reactive sputtering knee voltage control process for energy-conserving high-efficiency solar thermal-collecting tube coating machine |
| CN101694328A (en) * | 2009-10-28 | 2010-04-14 | 董晏伯 | Multitarget and high temperature and oxidation resisting solar energy absorbing membranous layer and production method thereof |
| CN104278246A (en) * | 2014-10-28 | 2015-01-14 | 佳木斯大学 | Method of preparing DLC film on substrate surface |
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| CN109449247A (en) * | 2018-09-11 | 2019-03-08 | 暨南大学 | Tin dope Electrochromic Molybdenum Oxide Coatings, wide spectrum photodetector array based on tin dope Electrochromic Molybdenum Oxide Coatings and preparation method thereof |
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