CN103789738B - WO3cluster-beam deposition system and utilize it to prepare WO3the method of thin film - Google Patents
WO3cluster-beam deposition system and utilize it to prepare WO3the method of thin film Download PDFInfo
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- CN103789738B CN103789738B CN201410017311.9A CN201410017311A CN103789738B CN 103789738 B CN103789738 B CN 103789738B CN 201410017311 A CN201410017311 A CN 201410017311A CN 103789738 B CN103789738 B CN 103789738B
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Abstract
The invention discloses a kind of WO3Cluster-beam deposition system and utilize it to prepare WO3The method of thin film, comprises the steps: 1), select WO3Ceramic target is as sputtering target material；2) it is fixed on the substrate pedestal of fine vacuum settling chamber after, substrate being cleaned；3), utilize mechanical pump and molecular pump forvacuum, make the vacuum pressure of settling chamber less than or equal to 1 × 10‑5Pa；4), in cluster source chamber sidewall pipeline, it is passed through liquid nitrogen, it is passed through noble gas Ar gas and He gas respectively by sputter gas entrance and buffer gas entrance, the pressure making cluster source chamber reaches 100～500Pa, using shielding power supply, the W ion sputtered and O ion are continually colliding with He atom in cluster source chamber by air accumulation method and gradually grow into WO3Cluster；5) WO formed3Orientation Cluster Beam aligning substrate starts deposition, and sedimentation rate is 0.1～0.5/s, and sedimentation time is 10～30 minutes, forms the WO that thickness is 100～200 nanometers on substrate3Clusters Films；6) WO obtained3Clusters Films is annealed 5～10 minutes at 400～600 DEG C through rapid thermal processing system.
Description
Technical field
The present invention relates to a kind of WO3Cluster-beam deposition system and utilize it to prepare WO3The method of thin film.
Background technology
WO3Be a kind of n-type metal oxide semiconductor, be also a kind of important functional material simultaneously, have photochromic,
The characteristics such as electrochromism, air-sensitive, photocatalysis.Particularly in photocatalysis research field, with traditional TiO2, the broad stopband such as ZnO half
Conductor catalysis material is compared, WO3Band gap is 2.4～2.8 eV, can absorb visible ray and realize visible light catalytic；And its chemistry
Stable performance, under room temperature not with acid and alkali reaction, photoetch will not occur.These advantages make WO3Catalysis material shows huge
Big application potential.It addition, China is the country that tungsten ore resource is the abundantest in the world, its tungsten resource gross reserves is 1,150,000 tons, for
WO3Provide abundant source.WO3Thin film is widely used, such as display device, energy-conservation color-changing window, information storage
Device, gas sensor, pH meter, as visible light catalytic material degradation of contaminant and photodissociation Aquatic product hydrogen etc..
At present, common preparation WO3The method of thin film has: sol-gel process (J. Amer. Chem. Soc., 2001,
123,10639), magnetron sputtering method (J. Appl. Phys. 2000,87,177；Chinese patent 200610014902.6),
Vacuum vapor deposition method (Chinese patent 01107472.8), atomic layer deposition method (J. Amer. Chem. Soc., 2006,128,
9638), chemical vapour deposition technique (Chem. Mater., 2003,15,2786), electrodeposition process (Adv. Mater.,
2003, 15, 1269；Chinese patent 201310033459.7), direct growth method (Nanotechnology. 2008,19,
065704；Chinese patent 200910157787.1) etc..Wherein, most study is sol-gel process, conventional sol-gel
Method technique includes the alkoxide hydrolysis of tungsten, the ion exchange of tungstates, tungsten powder peroxidating poly-wolframic acid method etc., and such as, China is specially
Profit 200910311691.6 reports soluble in water for many for water solublity Polytungstates, adds dispersant and modifying agent prepares forerunner
Liquid, uses dip-coating method or spin-coating method to carry out plated film at substrate surface, and nanometer WO is prepared in high-temperature calcination subsequently3The side of thin film
Method；The Chinese patent of Application No. 00131023.2 reports a kind of employing ion exchange and prepares WO3Colloidal sol, carries on substrate
Coating is drawn to prepare gas-discoloration WO3The method of thin film；Chinese patent 200810197305.0 discloses and utilizes ion to hand over one
Change method synthesis wolframic acid, then prepare photochromic WO under derivant malic acid effect3The method of thin film；Application No.
200810197795.4 Chinese patent disclose and a kind of utilize nucleator to prepare photochromic for tiny balloon of microscopic appearance
WO3The method of thin film；Chinese patent 201110185188.8 provides a kind of being dissolved in hydrogen peroxide by tungsten powder and peroxidating water occurs
Bath reaction, then substrate is immersed in pulling film forming in colloidal sol, annealing obtains WO subsequently3The method of thin film.Generally speaking, molten
Glue-gel method film-forming apparatus is relatively easy, low cost, but the problem of the method maximum is that film is poor with substrate adhesion, makes
During with, film is easy to fall off, in annealing process, and the organic volatilization of gel and the destruction of polymer backbone, more it is easily caused thin film
There is crack in be full of cracks, and additionally the method repeatability is not the best enough, limits WO3The actual application of thin film.
Summary of the invention
The technical problem to be solved is: provide a kind of WO3Cluster-beam deposition system and utilize it to prepare WO3
The method of thin film.
In order to solve above-mentioned technical problem, the technical solution used in the present invention is: WO3Cluster-beam deposition system, including:
Housing, is disposed with cluster source chamber, first order difference vacuum chamber, second level difference vacuum chamber in described housing from front to back
And settling chamber, substrate pedestal and crystal oscillator it is respectively arranged with in the inside of described settling chamber, described crystal oscillator is arranged
In the front end of substrate pedestal, substrate is arranged on described substrate pedestal, true in described first order difference vacuum chamber, second level difference
It is connected to molecular pump, in described first order difference vacuum chamber, second level difference vacuum chamber and deposition on empty room and settling chamber
Being respectively arranged with aerodynamics nozzle inside the front end of room, connecting in described cluster source chamber has mechanical pump, in described cluster
The front end of source chamber is provided with atomizer, WO3Ceramic target is arranged on the rear end of described atomizer, after described atomizer
End WO3The outside of ceramic target is provided with the target head screening cover cooperated with it, and connecting in described cluster source chamber has cushion gas
Body entrance, sputter gas entrance and liquid nitrogen entrance.
In order to preferably solve above-mentioned technical problem, the further technical scheme that the present invention uses is: utilize WO3Cluster beam
Stream depositing system prepares WO3Thin film method, comprise the steps:
1), WO is selected3Ceramic target is as sputtering target material；
2) it is fixed on the substrate pedestal of fine vacuum settling chamber after, substrate being cleaned；
3), utilize mechanical pump and molecular pump forvacuum, make the vacuum pressure of settling chamber less than or equal to 1 ×
10-5Pa；4), in cluster source chamber sidewall pipeline, it is passed through liquid nitrogen, after the cooling fully of cluster source chamber lateral compartments, point
It is not passed through noble gas Ar gas and He gas by sputter gas entrance and buffer gas entrance, respectively as sputter gas and buffering
Gas, makes the pressure of cluster source chamber reach 100～500Pa, under this air pressure, uses shielding power supply so that it is sputter, spatter
W ion and the O ion of injection are continually colliding with He atom in cluster source chamber by air accumulation method and gradually grow into WO3
Cluster, the WO of formation3Cluster buffered gas He gas is carried through first order difference vacuum chamber, second level difference vacuum chamber and sinks
The aerodynamics nozzle of long-pending room sprays and forms the WO of collimation3Orientation Cluster Beam；
5) WO formed3Orientation Cluster Beam aligning substrate starts deposition, and sedimentation rate is 0.1～0.5/s, during deposition
Between be 10～30 minutes, forming thickness on substrate is the WO of 100～200 nanometers3Clusters Films；
6) WO obtained3Clusters Films is annealed 5～10 minutes at 400～600 DEG C through rapid thermal processing system.
In order to preferably solve above-mentioned technical problem, the further technical scheme that the present invention uses is: described WO3Pottery
A diameter of 50mm of target, thickness is 3mm.
In order to preferably solve above-mentioned technical problem, the further technical scheme that the present invention uses is: described substrate can
Select quartz glass plate, (100) oriented single crystal Si, lucite or PET film.
In order to preferably solve above-mentioned technical problem, the further technical scheme that the present invention uses is: described sputtering electricity
Source is unipolar pulse DC source.
In order to preferably solve above-mentioned technical problem, the further technical scheme that the present invention uses is: described one pole arteries and veins
Rush the adjustable parameter scope of DC source be respectively as follows: sputtering voltage 350～400V, sputtering current 0.2～0.5A, frequency 30～
50kHz, dutycycle 60～80%, buffer gas He throughput is 30～60sccm, sputter gas Ar throughput be 60～
100sccm。
In order to preferably solve above-mentioned technical problem, the further technical scheme that the present invention uses is: described cluster source
The cooling length set point of outside chamber is 60～90mm.
In order to preferably solve above-mentioned technical problem, the further technical scheme that the present invention uses is: described is annealed
Journey is at N2Atmosphere completes.
The invention have the advantage that above-mentioned WO3Cluster-beam deposition system and utilize it to prepare WO3The method of thin film, technique letter
Single, low cost of manufacture, it is achieved that to WO3Film dimensions and the control of uniformity, and the WO formed3Thin film and substrate adhesion
Good.
Accompanying drawing explanation
Fig. 1 is WO of the present invention3Cluster-beam deposition system and utilize it to prepare WO3WO in the method for thin film3Cluster Beam sinks
The structural representation of long-pending system.
In figure: 1, housing, 2, cluster source chamber, 3, first order difference vacuum chamber, 31, second level difference vacuum chamber, 4, deposition
Room, 5, substrate pedestal, 6, crystal oscillator, 7, substrate, 8, molecular pump, 9, aerodynamics nozzle, 10, mechanical pump, 11, atom
Change device, 12, WO3Ceramic target, 13, target head screening cover, 14, buffer gas entrance, 15, sputter gas entrance, 16, liquid nitrogen entrance.
Fig. 2 is the WO of embodiment 1 preparation3Thin film X-ray diffraction spectrogram.
Fig. 3 is the WO of embodiment 1 preparation3Film scanning electron micrograph.
Fig. 4 is the WO of embodiment 1 preparation3Thin film atomic force microscopy.
Detailed description of the invention
The particular content of the present invention is described in detail below by the drawings and specific embodiments.
As it is shown in figure 1, WO3Cluster-beam deposition system, including: housing 1, set the most successively in described housing 1
It is equipped with cluster source chamber 2, first order difference vacuum chamber 3, second level difference vacuum chamber 31 and settling chamber 4, in described settling chamber 4
Portion is respectively arranged with substrate pedestal 5 and crystal oscillator 6, and described crystal oscillator 6 is arranged on the front end of substrate pedestal 5, substrate 7
It is arranged on described substrate pedestal 5, described first order difference vacuum chamber 3, second level difference vacuum chamber 3 and settling chamber 4 divide
Lian Jie there is not molecular pump 8, inside the front end of described first order difference vacuum chamber 3, second level difference vacuum chamber 31 and settling chamber 4
Being respectively arranged with aerodynamics nozzle 9, connecting in described cluster source chamber 2 has mechanical pump 10, before described cluster source chamber 2
End is provided with atomizer 11, WO3Ceramic target 12 is arranged on the rear end of described atomizer 11, after described atomizer 11
End WO3The outside of ceramic target 12 is provided with the target head screening cover 13 cooperated with it, and in described cluster source chamber 2, connection has slow
Rush gas access 14, sputter gas entrance 15 and liquid nitrogen entrance 16.
Utilize WO3Cluster-beam deposition system prepares WO3Thin film method, comprise the steps:
1), WO is selected3Ceramic target 12 is as sputtering target material；
2) it is fixed on after, substrate 7 being cleaned on the substrate pedestal 5 of fine vacuum settling chamber 4；
3), utilize mechanical pump 10 and molecular pump 8 forvacuum, make the vacuum pressure of settling chamber 4 be less than or equal to
1×10-5Pa；
4), in cluster source chamber 2 sidewall pipeline, it is passed through liquid nitrogen, after the cooling fully of cluster source chamber 2 lateral compartments, leads to respectively
Cross sputter gas entrance 15 and buffer gas entrance 14 is passed through noble gas Ar gas and He gas, respectively as sputter gas and buffering
Gas, makes the pressure of cluster source chamber 2 reach 100～500Pa, under this air pressure, uses shielding power supply so that it is sputter,
The W ion and the O ion that sputter are continually colliding with He atom in cluster source chamber 2 by air accumulation method and gradually grow into
WO3Cluster, the WO of formation3Cluster buffered gas He gas is carried through first order difference vacuum chamber 3, second level difference vacuum chamber
31 and the aerodynamics nozzle 9 of settling chamber 4 spray and form the WO of collimation3Orientation Cluster Beam；
5) WO formed3Orientation Cluster Beam aligning substrate 7 starts deposition, and sedimentation rate is 0.1～0.5/s, during deposition
Between be 10～30 minutes, forming thickness on substrate 7 is the WO of 100～200 nanometers3Clusters Films；
6) WO obtained3Clusters Films is annealed 5～10 minutes at 400～600 DEG C through rapid thermal processing system.
As it is shown in figure 1, in the present embodiment, described WO3A diameter of 50mm of ceramic target 12, thickness is 3mm；Described
Substrate 7 may select quartz glass plate, (100) oriented single crystal Si, lucite or PET film, also may select all kinds of optical transmission unit
Part and the light entrance face of all kinds of electrooptical device；Described shielding power supply is unipolar pulse DC source；Described one pole
The adjustable parameter scope of pulse dc power be respectively as follows: sputtering voltage 350～400V, sputtering current 0.2～0.5A, frequency 30～
50kHz, dutycycle 60～80%, buffer gas He throughput is 30～60sccm, sputter gas Ar throughput be 60～
100sccm；The cooling length set point of described cluster source chamber 2 lateral compartments is 60～90mm；Described annealing process be
N2Atmosphere completes.
Above-mentioned utilize WO3Cluster-beam deposition system prepares WO3Thin film the operation principle of method be: when experiment starts
Time, use WO3Ceramic target is as sputtering target material rather than metal W target, and the voltage of unipolar pulse DC source is applied directly to WO3Pottery
Between porcelain target 12 and shielded target lid 13, sputter gas Ar gas is ionized to plasma by glow discharge after entering this working region
Body Ar+, Ar+Under orthogonal electric field and the action of a magnetic field, with higher energy bombardment WO3Ceramic target 12, by W and O atom/ion
Get from target, form high density W and the plasma of O, subsequently enter outside the cluster source chamber 2 of full noble gas He gas
Chamber.The wall of cluster source chamber 2 lateral compartments liquid nitrogen cools down, when He gas and the wall collision of cluster source chamber 2 lateral compartments, and He gas
Cool off.In cluster source chamber 2 lateral compartments, by air accumulation method, collide with each other between W and O and they are with He gas
Body molecular collision, causes W and O effectively to assemble growth, forms WO3Cluster.By the electric current, frequently of regulation shielding power supply in experiment
Rate, dutycycle, and sputter gas Ar gas and buffer gas He throughput, condensation length etc., thus control WO3The size of cluster
With distribution of sizes.WO3Cluster buffered gas He gas is carried through first order difference vacuum chamber 3, second level difference vacuum chamber 31
And spray through aerodynamics nozzle 9 and form the orientation Cluster Beam of collimation, the substrate 7 being finally deposited in settling chamber 4 it
Upper formation WO3Thin film.
The present invention utilizes cluster-beam deposition system to prepare WO3Thin film, is because in view of cluster-beam deposition system tool
Have the advantage that one be Cluster deposition be low-down to energy during substrate 7, be far smaller than the combination energy of atom, therefore roll into a ball
Bunch line is to be deposited in the way of " soft landing " on substrate 7, depositing ions and substrate collision will not occur and be crashed to pieces or instead
Being emitted back towards the situation of chamber, cluster incides substrate 7 and can firmly be adsorbed by substrate 7 immediately；Two is that clustered particles is difficult on substrate 7 surface
In migrating, Cluster deposition can regard the process of a kind of random stacking as, and this random stacking makes to be less likely to occur between granule
Reactive polymeric so that the structure of thin film is easily controllable, thus form a kind of cluster with good dispersion assembled by cluster
Particle film, and the size uniform of clustered particles, for nanoscale.So, the WO prepared3Thin film is strong with substrate 7 tack, cluster
Even particle distribution.And WO prepared by other deposition process3Thin film, it is difficult to ensure that be that structure is smooth, size in microstructure
Uniform nanometer particle film.WO prepared by such as magnetron sputtering method3Thin film, needs to pass through the annealing up to several hours
To become phase, and growing up of crystal grain can be caused in this course, cause crystallite dimension wayward so that particle size is from tens
Nanometer has to hundreds of nanometer, thus the WO formed3Film surface is uneven.
Embodiment 1:
Utilize WO3Cluster-beam deposition system prepares WO3The method of thin film, in conjunction with Fig. 1, its preparation methods steps is as follows:
1) totally and N will be used with ethanol, acetone and deionized water ultrasonic cleaning successively2The 10mm*10mm*0.5mm dried up
Quartz glass, be fixed on substrate pedestal 5, make quartz glass substrate 7 be positioned at the center of Cluster Beam, then by substrate
7 are sealed in settling chamber 4；
2) unload sputtering target head screening cover 13 in cluster source chamber 2, be the WO of 3mm by a diameter of 50mm, thickness3Ceramic target 12
It is arranged on target head screening cover 13 position, tightens target head screening cover 13, note controlling target head screening cover 13 and WO3Ceramic target 12 target surface
Spacing prevent electric current from puncturing, regulation condense a length of 90mm；
3) open main power and mechanical pump 10, to each vacuum chamber evacuation, when Pi Lani reading is a few Pa, open each
Molecular pump 8, continues evacuation, when the vacuum pressure of settling chamber is less than or equal to 1 × 10-5During Pa, start outside cluster source chamber 2
Chamber leads to liquid nitrogen；
4) open the valve on buffer gas entrance 14 and sputter gas entrance 15, open quality stream interconnective with it
Gauge, adjusting gas flow makes sputter gas Ar throughput be 60sccm, buffer gas He throughput is also 60sccm, is filled with lazy
After property gas, the pressure of cluster source chamber 2 is 150Pa；
5) open unipolar pulse DC power supply switch, regulate sputtering voltage, electric current, frequency, dutycycle, when sputtering voltage is
When 360V, sputtering current are 0.3A, frequency is 37.647kHz, dutycycle is 60%, it is possible to produce stable Cluster Beam, line
Arrive on settling chamber 4 quartz glass substrate 7 through first order difference vacuum chamber 3 and second level difference vacuum chamber 31, pass through crystal
Agitator 6 can detect that sedimentation rate is 0.4/s；Crystal oscillator 6 is used for detecting WO3Cluster-beam deposition speed, exists subsequently
In deposition process, it is moved upward 50cm until not affecting WO3Cluster Beam deposition on substrate 7.
6) setting sedimentation time as 10 minutes, deposition closes shielding power supply immediately after terminating, close molecular pump 8 the most successively
With mechanical pump 10, taking out deposition has WO3The quartz glass substrate 7 of cluster, in N2Under atmosphere
Anneal 10 minutes at 600 DEG C, obtain WO3Thin film.
As in figure 2 it is shown, X-ray diffractogram show prepared by the WO that thin film is well-crystallized3Monocline crystalline phase, does not has impurity
Peak.
As it is shown on figure 3, the stereoscan photograph of prepared thin film shows, WO3Thin film is by the cluster of even size distribution
Granule assembles, and the average-size of granule is 80～100 nanometers.
As shown in Figure 4, the atomic force microscopy of prepared thin film shows, WO3Film surface distribution is more smooth, equal
Even, thickness about 100 nanometer.
Embodiment 2: the present embodiment is similar to Example 1, difference is, in step 1), substrate 7 changes specification into and is
The single crystalline Si sheet that (100) of 10mm*10mm*0.5mm are orientated, is not required to through ultrasonic cleaning with the thin monocrystalline in tamper-proof Si sheet surface
Film, only need to use N2Blow surface dust that may be present impurity off.
Embodiment 3: the present embodiment is similar to Example 1, difference is, in step 1), substrate 7 changes specification into and is
The lucite of 10mm*10mm*2mm, is not required to through ultrasonic cleaning in ethanol and acetone, and only need are the most ultrasonic clearly
Wash, use N subsequently2Dry up.
Embodiment 4: the present embodiment is similar to Example 1, difference is, in step 1), substrate 7 changes specification into and is
The PET film of 10mm*10mm*1mm, is not required to through ultrasonic cleaning in ethanol and acetone, only needs ultrasonic cleaning in deionized water,
Use N subsequently2Dry up.
(Rockwell type diamond penetrator, radius of curvature is 5 μm, and loading range is to use Switzerland CSM nanometer scratching instrument
0.5～1000mN, load mode is linear stepping, and loading velocity is 1999mN/min, cut
A length of 3mm) testing example 1, embodiment 2, embodiment 3 and the WO prepared by embodiment 43Thin film is attached with substrate
Put forth effort.Film surface cut optical CCD image method is utilized to obtain the critical load numerical value (table 1) of each thin film, and critical load number
The size of value reflects the size of thin film and substrate adhesive force.As it can be seen from table 1 WO3Thin film is either deposited on quartz glass
On glass, single crystalline Si sheet, lucite or PET film, all show bigger critical normal direction load value, much larger than common sol-
The thin film critical load value (about 3～5mN) that gel method prepares, shows the WO that cluster-beam deposition system prepares3Thin film and substrate
Between there is good tack.The most also find, WO3When thin film deposition is on quartz glass, critical normal load is maximum, also
I.e. WO3Thin film is maximum with the adhesive force of quartz glass；And WO3Thin film deposition on a pet film time, critical normal load is minimum, namely
WO3Thin film is minimum with the adhesive force of quartz glass.
Table 1 embodiment 1, example 2, example 3 and the WO3 thin film critical normal load Fn of example 4 preparation3
| Example | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 |
| Critical normal load Fn(mN) | 35.22 | 26.34 | 32.63 | 15.38 |
Claims (2)
1.WO3Cluster-beam deposition system, it is characterised in that: including: housing (1), in described housing (1) the most successively
It is provided with cluster source chamber (2), first order difference vacuum chamber (3), second level difference vacuum chamber (31) and settling chamber (4), described
The inside of settling chamber (4) is respectively arranged with substrate pedestal (5) and crystal oscillator (6), and described crystal oscillator (6) is arranged on lining
The front end of bottom susceptor (5), substrate (7) is arranged on described substrate pedestal (5), described first order difference vacuum chamber (3), second
Be connected to molecular pump (8) in level difference vacuum chamber (3) and settling chamber (4), described first order difference vacuum chamber (3), the
It is respectively arranged with aerodynamics nozzle (9), in described cluster inside the front end of two grades of difference vacuum chambers (31) and settling chamber (4)
The upper connection of source chamber (2) has mechanical pump (10), and the front end of described cluster source chamber (2) is provided with atomizer (11), WO3Ceramic target
(12) it is arranged on the rear end of described atomizer (11), at described atomizer (11) rear end WO3The outside of ceramic target (12)
Be provided with target head screening cover (13) cooperated with it, the upper connection of described cluster source chamber (2) have buffer gas entrance (14),
Sputter gas entrance (15) and liquid nitrogen entrance (16).
2. utilize WO3Cluster-beam deposition system prepares WO3Thin film method, it is characterised in that: comprise the steps: 1), choosing
Select WO3Ceramic target (12) is as sputtering target material；2) the substrate base of fine vacuum settling chamber (4) it is fixed on after, being cleaned by substrate (7)
On seat (5)；3), utilize mechanical pump (10) and molecular pump (8) forvacuum, make the vacuum pressure of settling chamber (4) less than or equal to 1
×10-5Pa；4), in cluster source chamber (2) sidewall pipeline, it is passed through liquid nitrogen, after the cooling fully of cluster source chamber (2) lateral compartments,
It is passed through noble gas Ar gas and He gas, respectively as sputtering respectively by sputter gas entrance (15) and buffer gas entrance (14)
Gas and buffer gas, makes the pressure of cluster source chamber (2) reach 100 ~ 500Pa, under this air pressure, uses shielding power supply, makes
It sputters, and the W ion sputtered and O ion are constantly touched with He atom in cluster source chamber (2) by air accumulation method
Hit and gradually grow into WO3Cluster, the WO of formation3Cluster buffered gas He gas be carried through first order difference vacuum chamber (3),
The aerodynamics nozzle (9) of second level difference vacuum chamber (31) and settling chamber (4) sprays and forms the WO of collimation3Orientation cluster
Line；5) WO formed3Orientation Cluster Beam aligning substrate (7) starts deposition, and sedimentation rate is 0.1～0.5/s, during deposition
Between be 10～30 minutes, form the WO that thickness is 100～200 nanometers substrate (7) is upper3Clusters Films；6) WO obtained3Cluster
Thin film is annealed 5～10 minutes at 400～600 DEG C through rapid thermal processing system；Described WO3Ceramic target (12) a diameter of
50mm, thickness is 3mm；Described substrate (7) may select quartz glass plate, (100) oriented single crystal Si, lucite or PET film；
Described shielding power supply is unipolar pulse DC source；The adjustable parameter scope of described unipolar pulse DC source is respectively as follows:
Sputtering voltage 350～400V, sputtering current 0.2～0.5A, frequency 30～50kHz, dutycycle 60～80%, buffer gas He gas
Flow is 30～60sccm, sputter gas Ar throughput is 60～100sccm；The cooling of described cluster source chamber (2) lateral compartments
Length set point is 60～90mm；Described annealing process is at N2Atmosphere completes.
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| CN106048533B (en) * | 2016-06-27 | 2019-01-15 | 内蒙古大学 | A kind of preparation method of SmCo alloy magnetostriction film |
| CN106435509B (en) * | 2016-12-14 | 2019-03-15 | 盐城工学院 | A kind of ultrahigh vacuum catalytic unit and Cluster deposition equipment |
| CN107694478B (en) * | 2017-09-25 | 2020-08-28 | 复旦大学 | Ultrasonic gas beam device |
| CN109115660A (en) * | 2018-08-23 | 2019-01-01 | 金华职业技术学院 | A kind of particle imaging method |
| JP7179083B2 (en) * | 2018-11-30 | 2022-11-28 | 東京エレクトロン株式会社 | SUBSTRATE CLEANING METHOD, PROCESS CONTAINER CLEANING METHOD, AND SUBSTRATE PROCESSING APPARATUS |
| CN110480025B (en) * | 2019-09-06 | 2020-12-08 | 陕西师范大学 | Gas phase preparation method of high-density nano material |
| CN110642526A (en) * | 2019-09-16 | 2020-01-03 | 中国科学院宁波材料技术与工程研究所 | Preparation method of tungsten oxide electrochromic film |
| CN111575652A (en) * | 2020-04-02 | 2020-08-25 | 上海大学 | Vacuum coating equipment and vacuum coating method |
| CN113278930B (en) * | 2021-04-25 | 2023-04-18 | 北京航空航天大学合肥创新研究院(北京航空航天大学合肥研究生院) | Nanocluster beam density control device and application method thereof |
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