CN107620034A - One kind prepares transparent Bi2Se3The method of film - Google Patents
One kind prepares transparent Bi2Se3The method of film Download PDFInfo
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Abstract
One kind prepares transparent Bi2Se3The method of film, comprises the following steps:A, sputtering sedimentation：Choose quartz (SiO2) substrate or sapphire (Al2O3) substrate of the substrate as magnetron sputtering, choose the Bi that purity is 99.999%2Se3Target of the material as magnetron sputtering, one layer of Bi of sputtering sedimentation on substrate2Se3Film；B, after annealing is handled：A step depositions there is into Bi2Se3The selenium grain ball that the substrate and particle diameter of film are 0.6mm 1.2mm encloses air pressure less than 1 × 10 together‑2In Pa vitreosil pipe, then vitreosil pipe is placed in tube furnace, after annealing processing is carried out under argon atmosphere, produces transparent Bi2Se3Film.This method can prepare the good Bi of light transmission of large area2Se3Film, preparation process is simple, and energy consumption is small, and cost is low, efficiency high, favorable repeatability, is suitable for industrialized production.
Description
Technical field
The present invention relates to one kind to prepare transparent Bi2Se3The method of film, more particularly to magnetron sputtering method prepare it is transparent
Bi2Se3The method of film.
Background technology
Bi2Se3Transparent membrane belongs to VA-VIA races direct band gap inorganic semiconductor, and its energy gap is narrow, stable performance, light
Electric conversion performance is good, and it has significant Third-order Nonlinear Optical Properties, shorter response time and larger non-linear
Optical coefficient, it can be used as device for non-linear optical.Transparent Bi2Se3Film is in high-performance optical electrical part (all-optical switch, light
Detector, thz laser, ripple guiding, transparency electrode) and the field such as light processing have a wide range of applications.People have used
Various methods prepare transparent Bi2Se3Film, such as：Molecular beam epitaxy (MBE) and chemical vapour deposition technique (CVD).But MBE skills
Art needs high-precision vavuum pump, and equipment is expensive, energy expenditure is big, cost is high.And the sedimentation rate of CVD technology is relatively low, participate in
The residual air of deposition is inflammable, explosive or poisonous, it is necessary to take antipollution measure；And there is corrosion resistant want to equipment
Ask.
The content of the invention
It is an object of the invention to provide one kind to prepare transparent Bi2Se3The method of film, this method can prepare the saturating of large area
Bright Bi2Se3Monocrystal thin films, obtained Film Optics performance are good；And its preparation process is simple, energy consumption is small, and cost is low, and efficiency high can
It is reproducible, it is suitable for industrialized production.
The technical scheme adopted by the invention for realizing the object of the invention is that one kind prepares transparent Bi2Se3The method of film, bag
Include following steps:
A, sputtering sedimentation：Choose quartz (SiO2) substrate or sapphire (Al2O3) substrate of the substrate as magnetron sputtering, choosing
Take the Bi that purity is 99.999%2Se3Target of the material as magnetron sputtering, one layer of Bi of sputtering sedimentation on substrate2Se3Film；
B, after annealing is handled：A step depositions there is into Bi2Se3The substrate and particle diameter of film are 0.6mm-1.2mm selenium grain ball one
Rise and enclose air pressure less than 1 × 10-2In Pa vitreosil pipe, then vitreosil pipe is placed in tube furnace, protected in argon gas
After annealing processing is carried out under atmosphere, produces transparent Bi2Se3Film；
The concrete operations of described after annealing processing are：Tube furnace is risen to 300 DEG C with 2 DEG C/min programming rate, protected
Warm 2-5h, then vitreosil pipe is pushed into cold quenching-in water.
The present invention principle be：One layer of Bi is deposited on quartz or sapphire substrate by magnetron sputtering2Se3Film, then will
The substrate and selenium grain ball of deposition film enclose progress after annealing processing in vitreosil pipe together, make atom raw in selenium-rich environment
Length, rearrange to obtain the good transparent single crystal Bi of crystal property2Se3Film.
Compared with prior art, the beneficial effects of the invention are as follows：
First, by the method for magnetron sputtering in substrate deposition film, then handled by the after annealing of specified conditions into one
Step obtains the Bi of well-crystallized2Se3Monocrystal thin films.Magnetron sputtering efficiency high, it is reproducible, large area, uniform, purity can be prepared
The strong film of adhesive force between high and substrate；And this method can be by controlling sputtering time to control film thickness.
2nd, highest vacuum requirement of the present invention is only 10-4The Pa orders of magnitude, required equipment are conventional magnetron sputtering apparatus
And tube furnace, preparation cost is low, favorable repeatability, is suitable for industrialized production.
Further, the process conditions of step a of the present invention sputtering sedimentation are：The distance of target to substrate is 5-7cm, sputtering
Before make vacuum chamber air pressure be less than 2 × 10-4Pa, then be passed through purity be 99.995% argon gas as working gas；During sputtering
Air pressure is 0.3-0.5Pa, underlayer temperature is 300-400 DEG C, and sputtering power 50-70W, sputtering time are the 1-10 seconds.
So, can be obtained with sputtering sedimentation surfacing, densification, with substrate adhesion is strong and purity is high transparent membrane.
Further, the quality of selenium grain ball and the Bi of deposition on substrate in step b of the present invention2Se3Mass ratio 0.1-0.2：
1。
So, the after annealing processing both ensured is carried out in selenium-rich environment, generates Bi of good performance2Se3Film,
The waste of selenium grain ball is avoided, reduces preparation cost.
The present invention is described in further detail with reference to the accompanying drawings and detailed description.
Brief description of the drawings
Fig. 1 is Bi prepared by the embodiment of the present invention one2Se3The X ray diffracting spectrum of film.
Fig. 2 is Bi prepared by the embodiment of the present invention one2Se330000 times of electron scanning micrographs of film.
Fig. 3 is Bi prepared by the embodiment of the present invention one2Se3The translucency experiment curv of film.
Fig. 4 is Bi prepared by the embodiment of the present invention two2Se3The X ray diffracting spectrum of film.
Fig. 5 is Bi prepared by the embodiment of the present invention two2Se330000 times of electron scanning micrographs of film.
Fig. 6 is Bi prepared by the embodiment of the present invention two2Se3The translucency experiment curv of film.
Fig. 1,4 ordinate are diffracted intensity (Intensity), arbitrary unit (a.u.)；Abscissa is the θ of the angle of diffraction 2, single
Position is degree (degree).Fig. 3,6 ordinate are light transmittance；Abscissa is wave number.
Embodiment
Embodiment one
One kind prepares transparent Bi2Se3The method of film, comprises the following steps:
A, sputtering sedimentation：Choose quartz (SiO2) substrate or sapphire (Al2O3) substrate of the substrate as magnetron sputtering, choosing
Take the Bi that purity is 99.999%2Se3Target of the material as magnetron sputtering, one layer of Bi of sputtering sedimentation on substrate2Se3Film；
The process conditions of sputtering sedimentation are：The distance of target to substrate is 7cm, the air pressure of vacuum chamber is less than 2 before sputtering
×10-4Pa, then be passed through purity be 99.995% argon gas as working gas；Air pressure during sputtering is 0.5Pa, underlayer temperature is
330 DEG C, sputtering power 70W, sputtering time are 3 seconds.
B, after annealing is handled：A step depositions there is into Bi2Se3The substrate and particle diameter of film are 0.6mm-1.2mm selenium grain ball one
Rise and enclose air pressure less than 1 × 10-2In Pa vitreosil pipe, then vitreosil pipe is placed in tube furnace, protected in argon gas
After annealing processing is carried out under atmosphere, produces transparent Bi2Se3Film；
The described quality of selenium grain ball and the Bi of deposition on substrate2Se3Mass ratio 0.1-0.2：1.
The concrete operations of described after annealing processing are：Tube furnace is risen to 300 DEG C with 2 DEG C/min programming rate, protected
Warm 2.5h, then vitreosil pipe is pushed into cold quenching-in water.
Fig. 1 is Bi made from this example2Se3The X-ray diffractogram spectrogram of film.From figure 1 it appears that remove base ceramic
Diffraction maximum outside, all Bi2Se3The characteristic peak of film is (00L) diffraction maximum, has no other miscellaneous peaks, shows on quartz substrate
The Bi of growth2Se3Film has very strong c-axis orientation and periodicity.
Fig. 2 is Bi made from this example2Se330000 times of electron scanning micrographs of film.It can be seen from the figure that film
The surfacing of sample, densification, without hole, it can thus be appreciated that this embodiment has been prepared, texture is good, the smooth Bi of surface compact2Se3
Film.
Fig. 3 is Bi made from this example2Se3The translucency experiment curv of film, as can be seen from the figure film sample is in the area
The translucency in domain is higher than 90%.
Embodiment two
One kind prepares transparent Bi2Se3The method of film, comprises the following steps:
A, sputtering sedimentation：Choose sapphire (Al2O3) substrate of the substrate as magnetron sputtering, it is 99.999% to choose purity
Bi2Se3Target of the material as magnetron sputtering, one layer of Bi of sputtering sedimentation on substrate2Se3Film；
The process conditions of sputtering sedimentation are：The distance of target to substrate is 5cm, the air pressure of vacuum chamber is less than 2 before sputtering
×10-4Pa, then be passed through purity be 99.995% argon gas as working gas；Air pressure during sputtering is 0.45Pa, underlayer temperature
For 350 DEG C, sputtering power 60W, sputtering time are 5 seconds.
B, after annealing is handled：A step depositions there is into Bi2Se3The substrate and particle diameter of film are that 0.9mm selenium grain ball is enclosed together
Air pressure is less than 1 × 10-2In Pa vitreosil pipe, then vitreosil pipe is placed in tube furnace, under argon atmosphere
After annealing processing is carried out, produces transparent Bi2Se3Film；
The described quality of selenium grain ball and the Bi of deposition on substrate2Se3Mass ratio 0.1-0.2：1.
The concrete operations of described after annealing processing are：Tube furnace is risen to 300 DEG C with 2 DEG C/min programming rate, protected
Warm 4h, then vitreosil pipe is pushed into cold quenching-in water.
Fig. 4 is Bi made from this example2Se3The X-ray diffractogram spectrogram of film.From figure 1 it appears that except substrate is blue precious
Outside the diffraction maximum of stone, all Bi2Se3The characteristic peak of film is (00L) diffraction maximum, has no other miscellaneous peaks, shows in process for sapphire-based
The Bi grown on piece2Se3Film has very strong c-axis orientation and periodicity.
Fig. 5 is Bi made from this example2Se330000 times of electron scanning micrographs of film.It can be seen from the figure that film
The surfacing of sample, densification, without hole, it can thus be appreciated that this embodiment has been prepared, texture is good, the smooth Bi of surface compact2Se3
Film.
Fig. 6 is Bi made from this example2Se3The translucency experiment curv of film, as can be seen from the figure film sample is in the area
The translucency in domain is higher than 90%.
Embodiment three
One kind prepares transparent Bi2Se3The method of film, comprises the following steps:
A, sputtering sedimentation：Choose quartz (SiO2) substrate of the substrate as magnetron sputtering, it is 99.999% to choose purity
Bi2Se3Target of the material as magnetron sputtering, one layer of Bi of sputtering sedimentation on substrate2Se3Film；
The process conditions of sputtering sedimentation are：The distance of target to substrate is 6cm, the air pressure of vacuum chamber is less than 2 before sputtering
×10-4Pa, then be passed through purity be 99.995% argon gas as working gas；Air pressure during sputtering is 0.35Pa, underlayer temperature
For 380 DEG C, sputtering power 55W, sputtering time are 10 seconds.
B, after annealing is handled：A step depositions there is into Bi2Se3The substrate and particle diameter of film are that 1.0mm selenium grain ball is enclosed together
Air pressure is less than 1 × 10-2In Pa vitreosil pipe, then vitreosil pipe is placed in tube furnace, under argon atmosphere
After annealing processing is carried out, produces transparent Bi2Se3Film；
The described quality of selenium grain ball and the Bi of deposition on substrate2Se3Mass ratio 0.1-0.2：1.
The concrete operations of described after annealing processing are：Tube furnace is risen to 300 DEG C with 2 DEG C/min programming rate, protected
Warm 3.5h, then vitreosil pipe is pushed into cold quenching-in water.
Example IV
One kind prepares transparent Bi2Se3The method of film, comprises the following steps:
A, sputtering sedimentation：Choose sapphire (Al2O3) substrate of the substrate as magnetron sputtering, it is 99.999% to choose purity
Bi2Se3Target of the material as magnetron sputtering, one layer of Bi of sputtering sedimentation on substrate2Se3Film；
The process conditions of sputtering sedimentation are：The distance of target to substrate is 6cm, the air pressure of vacuum chamber is less than 2 before sputtering
×10-4Pa, then be passed through purity be 99.995% argon gas as working gas；Air pressure during sputtering is 0.45Pa, underlayer temperature
For 400 DEG C, sputtering power 60W, sputtering time are 1 second.
B, after annealing is handled：A step depositions there is into Bi2Se3The substrate and particle diameter of film are that 0.7mm selenium grain ball is enclosed together
Air pressure is less than 1 × 10-2In Pa vitreosil pipe, then vitreosil pipe is placed in tube furnace, under argon atmosphere
After annealing processing is carried out, produces transparent Bi2Se3Film；
The described quality of selenium grain ball and the Bi of deposition on substrate2Se3Mass ratio 0.1-0.2：1.
The concrete operations of described after annealing processing are：Tube furnace is risen to 300 DEG C with 2 DEG C/min programming rate, protected
Warm 3.5h, then vitreosil pipe is pushed into cold quenching-in water.
Claims (3)
1. one kind prepares transparent Bi2Se3The method of film, comprises the following steps:
A, sputtering sedimentation：Choose quartz (SiO2) substrate or sapphire (Al2O3) substrate of the substrate as magnetron sputtering, choose pure
Spend the Bi for 99.999%2Se3Target of the material as magnetron sputtering, one layer of Bi of sputtering sedimentation on substrate2Se3Film；
B, after annealing is handled：A step depositions there is into Bi2Se3The substrate and particle diameter of film are that 0.6mm-1.2mm selenium grain ball seals together
Enter air pressure less than 1 × 10-2In Pa vitreosil pipe, then vitreosil pipe is placed in tube furnace, in argon atmosphere
Lower progress after annealing processing, produces transparent Bi2Se3Film；
The concrete operations of described after annealing processing are：Tube furnace is risen to 300 DEG C with 2 DEG C/min programming rate, is incubated 2-
5h, then vitreosil pipe is pushed into cold quenching-in water.
2. one kind according to claim 1 prepares transparent Bi2Se3The method of film, it is characterised in that：The step a's splashes
The process conditions for penetrating deposition are：The distance of target to substrate is 5-7cm, the air pressure of vacuum chamber is less than 2 × 10 before sputtering-4Pa,
Be passed through again purity be 99.995% argon gas as working gas；Air pressure during sputtering is 0.3-0.5Pa, underlayer temperature 300-
400 DEG C, sputtering power 50-70W, sputtering time are the 1-10 seconds.
3. one kind according to claim 1 prepares transparent Bi2Se3The method of film, it is characterised in that：Selenium in the step c
The grain quality of ball and the Bi of deposition on substrate2Se3Mass ratio 0.1-0.2：1.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108277466A (en) * | 2018-02-07 | 2018-07-13 | 西南交通大学 | Topological insulator heterojunction structure film Bi2Se3The preparation method of/C |
| US20190143661A1 (en) * | 2017-11-16 | 2019-05-16 | The Boeing Company | Methods of and systems for forming coatings that comprise non-carbon-based topological insulators |
| US10887996B2 (en) | 2017-11-16 | 2021-01-05 | The Boeing Company | Electronic components coated with a topological insulator |
| CN114051371A (en) * | 2021-11-01 | 2022-02-15 | 吉林大学 | Far infrared transparent electromagnetic shielding coating and preparation method thereof |
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| CN102867906A (en) * | 2012-09-21 | 2013-01-09 | 上海大学 | Method for electrochemically preparing thermoelectric film by using seeding layer |
| CN103526297A (en) * | 2013-10-17 | 2014-01-22 | 西南交通大学 | Method for preparing topological insulator Bi2Se3 film |
| CN104152856A (en) * | 2014-07-11 | 2014-11-19 | 西南交通大学 | Method for preparing Bi2Se3 thin film by virtue of magnetron sputtering process |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2010051351A2 (en) * | 2008-10-31 | 2010-05-06 | Applied Quantum Technology, Llc | Chalcogenide alloy sputter targets for photovoltaic applications and methods of manufacturing the same |
| CN102867906A (en) * | 2012-09-21 | 2013-01-09 | 上海大学 | Method for electrochemically preparing thermoelectric film by using seeding layer |
| CN103526297A (en) * | 2013-10-17 | 2014-01-22 | 西南交通大学 | Method for preparing topological insulator Bi2Se3 film |
| CN104152856A (en) * | 2014-07-11 | 2014-11-19 | 西南交通大学 | Method for preparing Bi2Se3 thin film by virtue of magnetron sputtering process |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20190143661A1 (en) * | 2017-11-16 | 2019-05-16 | The Boeing Company | Methods of and systems for forming coatings that comprise non-carbon-based topological insulators |
| US10814600B2 (en) * | 2017-11-16 | 2020-10-27 | The Boeing Company | Methods of and systems for forming coatings that comprise non-carbon-based topological insulators |
| US10887996B2 (en) | 2017-11-16 | 2021-01-05 | The Boeing Company | Electronic components coated with a topological insulator |
| CN108277466A (en) * | 2018-02-07 | 2018-07-13 | 西南交通大学 | Topological insulator heterojunction structure film Bi2Se3The preparation method of/C |
| CN108277466B (en) * | 2018-02-07 | 2019-08-20 | 西南交通大学 | Topological insulator heterojunction structure film Bi2Se3The preparation method of/C |
| CN114051371A (en) * | 2021-11-01 | 2022-02-15 | 吉林大学 | Far infrared transparent electromagnetic shielding coating and preparation method thereof |
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