CN109136859A - A method of preparing high transparency gallium oxide film - Google Patents

A method of preparing high transparency gallium oxide film Download PDF

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Publication number
CN109136859A
CN109136859A CN201811228392.1A CN201811228392A CN109136859A CN 109136859 A CN109136859 A CN 109136859A CN 201811228392 A CN201811228392 A CN 201811228392A CN 109136859 A CN109136859 A CN 109136859A
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China
Prior art keywords
gallium oxide
oxide film
high transparency
buffer layer
pulse laser
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CN201811228392.1A
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Chinese (zh)
Inventor
李炳生
宋东雨
李丽
李林
余立冬
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Harbin Institute of Technology
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Harbin Institute of Technology
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    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24Vacuum evaporation
    • C23C14/28Vacuum evaporation by wave energy or particle radiation
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/02Pretreatment of the material to be coated
    • C23C14/021Cleaning or etching treatments
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/08Oxides
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/54Controlling or regulating the coating process

Abstract

The invention discloses a kind of methods for preparing high transparency gallium oxide film, are related to a kind of method that optimization technique prepares high transparency gallium oxide film.The present invention passes through optimization preparation process, hence it is evident that the optical property for improving gallium oxide film overcomes the low technical problem of light transmittance.The present invention has obtained the gallium oxide film of high transparency by the method for introducing low temperature buffer layer, and light transmittance is up to 90% or more.

Description

A method of preparing high transparency gallium oxide film
Technical field
The invention belongs to semiconductor light electro-technical fields, and in particular to a kind of side for preparing high transparency gallium oxide film Method.
Background technique
Gallium oxide thin-film material is the most stable with monoclinic form β phase, because it is monoclinic form β phase oxidation gallium thin-film material tool There is a direct band gap structure, forbidden bandwidth 4.9eV, therefore in deep-UV light-emitting, transparent conductive electrode, day blind detection and high-frequency electronic Device etc. has important application, and has become the research hotspot in wide bandgap semiconductor materials field.But existing method system Standby gallium oxide film is also difficult to reach higher light transmittance, makes it in the fields such as luminous, detection and the sub- device of transparent photoelectric Using being greatly limited.
The raising of gallium oxide film light transmittance will improve the performance of the sub- device of gallium oxide film base transparent photoelectric. Currently, it is considerably less for the research for improving gallium oxide film light transmittance, especially lack having suitable for impulse laser deposition system Efficacious prescriptions method.So far, the quality problems of gallium oxide thin-film material are still to limit the principal element of gallium oxide thin-film material application. The method that we prepare gallium oxide film by introducing two steps of low temperature buffer layer, can significantly improve the crystallization of gallium oxide film Quality finally obtains the gallium oxide film of high transparency.
The present invention is to solve the low technical problem of existing gallium oxide film light transmittance.The present invention is by increasing buffer layer Method obtained the gallium oxide film of high transparency, and light transmittance is up to 90% or more.
Summary of the invention
The purpose of the present invention is to solve the low technical problems of existing gallium oxide film light transmittance, provide a kind of increase oxygen Change the method that gallium thin film buffer layer obtains high transparency gallium oxide film, and light transmittance is up to 90% or more.
To achieve the above object, the technical solution adopted by the present invention is as follows:
Step 1: cleaning substrate: the substrate is quartz substrate;
Step 2: pulse laser deposition prepares gallium oxide buffer layer thin film:
(1), gallium oxide target is mounted on pulse laser deposition targets, then the cleaned substrate of step 1 is put into very On the console of empty room, start to vacuumize, heats substrate, be passed through sputter gas O2, so that the pressure of vacuum chamber is maintained at 1Pa;
(2), substrate is covered with baffle, deposition 10min is carried out under pulse laser, open substrate shutter, pulse laser item Film deposition is carried out under part, obtains the gallium oxide thin film buffer layer with a thickness of 1~5nm;
One, the method for preparing gallium oxide film include: magnetron sputtering deposition, pulse laser deposition, molecular beam epitaxy, etc. from The methods of chemical vapor deposition, light auxiliary or Metalorganic chemical vapor deposition of plasmaassisted of daughter enhancing come real It is existing.Wherein specific step is as follows for pulse laser depositing gallium oxide film:
(1), substrate is covered with baffle, the gallium oxide thin film buffer layer that step 2 is obtained heats, in heating process, always Being passed through for sputter gas is kept, so that the pressure of vacuum chamber remains unchanged.
(2), substrate shutter is opened, deposition 60min is carried out under pulse laser, obtains the gallium oxide film of high transparency;
The present invention has the advantage that
1, the target particle sputtered has higher energy, preferable with the adhesion of substrate, can be in lower temperature even room Crystalline membrane is formed under temperature, the deposition of film under low temperature can be realized on some specialized substrates materials.
2, by adjusting deposition parameter, thus it is possible to vary each side's surface properties of film.
Detailed description of the invention
Fig. 1 is the optical bandwidth curve graph for increasing gallium oxide thin film buffer layer and preparing gallium oxide film sample;
Fig. 2 is that increase gallium oxide thin film buffer layer prepares gallium oxide film sample and non-oxidation gallium thin film buffer layer prepares oxygen Change the XRD diagram of gallium film sample.
Specific embodiment
Following embodiment is some citings of the invention, is not construed as limitation of the invention, all to the present invention Technical solution is modified or replaced equivalently, and without departing from the spirit and scope of the technical solution of the present invention, should all be covered at this In the protection scope of invention.
Specific embodiment one: the present embodiment is the method for preparing high transparency gallium oxide film, specifically according to the following steps It carries out:
One, clean substrate: the substrate is quartz substrate;
Two, the preparation of pulse laser deposition prepares gallium oxide film damper layer film:
(1), gallium oxide target is mounted on pulse laser deposition targets, then the cleaned substrate of step 1 is put into very On the console of empty room, start to vacuumize, heats substrate to 200 DEG C, be passed through sputter gas O2, so that the pressure of vacuum chamber is kept In 1Pa;
(2), substrate is covered with baffle, deposition 10min is carried out under pulse laser, open substrate shutter, pulse laser item It is carried out pre-deposition one minute under part, obtains the gallium oxide thin film buffer layer with a thickness of 5nm;
Three, the method for preparing gallium oxide film include: magnetron sputtering deposition, pulse laser deposition, molecular beam epitaxy, etc. from The methods of chemical vapor deposition, light auxiliary or Metalorganic chemical vapor deposition of plasmaassisted of daughter enhancing come real It is existing.Wherein specific step is as follows for pulse laser depositing gallium oxide foamed film:
(1), substrate is covered with baffle, the gallium oxide thin film buffer layer that step 2 obtains is heated to 800 DEG C, heating process In, it is always maintained at being passed through for sputter gas, so that the pressure of vacuum chamber remains unchanged.
(2), substrate shutter is opened, deposition 60min is carried out under pulse laser, obtains the gallium oxide film of high transparency;
Specific embodiment two: the difference of the present embodiment and specific embodiment one is: underlayer temperature described in step 2 It is 150 DEG C.Other are identical as specific embodiment one.
Specific embodiment three: the difference of the present embodiment and specific embodiment one or two is: substrate described in step 2 Temperature is 100 DEG C.Other are identical as specific embodiment one or two.
Specific embodiment four: the difference of the present embodiment and specific embodiment one to three is: substrate described in step 2 Temperature is 50 DEG C.Other are identical as specific embodiment one to three.
Specific embodiment five: the difference of the present embodiment and specific embodiment one to four is: substrate described in step 2 Temperature is room temperature.Other are identical as specific embodiment one to four.
Specific embodiment six: the difference of the present embodiment and specific embodiment one to five is: buffering described in step 3 Layer temperature is 800 DEG C.Other are identical as specific embodiment one to five.
Specific embodiment seven: the difference of the present embodiment and specific embodiment one to six is: buffering described in step 3 Layer temperature is 700 DEG C.Other are identical as specific embodiment one to six.
Specific embodiment eight: the difference of the present embodiment and specific embodiment one to seven is: buffering described in step 3 Layer temperature is 600 DEG C.Other are identical as specific embodiment one to seven.
Specific embodiment nine: the difference of the present embodiment and specific embodiment one to eight is: buffering described in step 3 Layer temperature is 500 DEG C.Other are identical as specific embodiment one to eight
Specific embodiment ten: the difference of the present embodiment and specific embodiment one to nine is: buffering described in step 3 Layer temperature is 400 DEG C.Other are identical as specific embodiment one to nine.
Specific embodiment 11: the difference of the present embodiment and specific embodiment one to ten is: delaying described in step 3 Rushing layer temperature is 300 DEG C.Other are identical as specific embodiment one to ten.

Claims (9)

1. a kind of method for preparing high transparency gallium oxide film, it is characterised in that the method comprises the following steps:
Step 1: cleaning substrate;Step 2: prepare buffer layer, preparation method include: magnetron sputtering deposition, pulse laser deposition, Molecular beam epitaxy, the chemical vapor deposition of plasma enhancing, light assist or the Metal Organic Chemical Vapor of plasmaassisted Deposition, the methods of electron beam evaporation are realized.
Wherein pulse laser deposition prepares buffer layer specific step is as follows: (1), gallium oxide target being mounted on pulse laser sinks On product target, then the cleaned substrate of step 1 is placed on the console of vacuum chamber, starts to be evacuated to certain vacuum degree, And substrate is heated to certain temperature, it is passed through sputter gas, so that the pressure of vacuum chamber is maintained at certain pressure intensity.(2), it is hidden with baffle Firmly substrate carries out pre-deposition certain time under the conditions of the pulse laser of certain power, substrate shutter is opened, in certain power Certain time is formally deposited under the conditions of pulse laser, obtains certain thickness gallium oxide thin film buffer layer;
Step 3: the method for preparing gallium oxide film include: magnetron sputtering deposition, pulse laser deposition, molecular beam epitaxy, etc. from The chemical vapor deposition of daughter enhancing, light assist or the Metalorganic chemical vapor deposition of plasmaassisted, electron beam evaporation The methods of realize.Wherein specific step is as follows for pulse laser depositing gallium oxide film: (1), with baffle covering substrate, will walk Rapid two obtained gallium oxide thin film buffer layers are heated to certain temperature, in heating process, are always maintained at being passed through for sputter gas, make The pressure for obtaining vacuum chamber is maintained at certain pressure intensity.(2), substrate shutter is opened, is carried out under the conditions of the pulse laser of certain power Certain time is deposited, the gallium oxide film of certain thickness high transparency is obtained.
2. the method according to claim 1 for increasing buffer layer and preparing high transparency gallium oxide film, cleaning substrate Method are as follows: successively cleaned 5 minutes, acetone ultrasonic cleaning 5 minutes, deionized water cleaning 5 minutes with EtOH Sonicate.
3. the method according to claim 1 for preparing high transparency gallium oxide film is magnetron sputtering deposition, pulse laser Deposition, molecular beam epitaxy, the chemical vapor deposition of plasma enhancing, light assist or the organometallic chemistry of plasmaassisted The methods of vapor deposition is realized.
4. the method according to claim 1 for increasing buffer layer and preparing high transparency gallium oxide film, it is characterised in that step Temperature described in rapid two is certain temperature.
5. the method according to claim 1 for increasing buffer layer and preparing high transparency gallium oxide film, it is characterised in that step The pressure of vacuum chamber described in rapid two is maintained at certain pressure intensity.
6. the method according to claim 1 for increasing buffer layer and preparing high transparency gallium oxide film, it is characterised in that step Sputter gas described in rapid two is oxygen.
7. the method according to claim 1 for increasing buffer layer and preparing high transparency gallium oxide film, it is characterised in that step Certain temperature, which is heated to, in buffer layer described in rapid three carries out pulse laser depositing gallium oxide film.
8. the method according to claim 1 for increasing buffer layer and preparing high transparency gallium oxide film, it is characterised in that step The pressure of vacuum chamber described in rapid three is maintained at certain pressure intensity.
9. the method according to claim 1 for increasing buffer layer and preparing high transparency gallium oxide film, it is characterised in that step Deposition certain time is carried out under the conditions of the pulse laser of certain power described in rapid three.
CN201811228392.1A 2018-10-22 2018-10-22 A method of preparing high transparency gallium oxide film Pending CN109136859A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110854233A (en) * 2019-11-17 2020-02-28 金华紫芯科技有限公司 Ga2O3Film-based solar blind ultraviolet detector, preparation method and application
CN110993504A (en) * 2019-10-14 2020-04-10 西安电子科技大学 Ga based on SiC substrate2O3Preparation method of film and Ga based on SiC substrate2O3Film(s)
CN111048402A (en) * 2019-10-14 2020-04-21 西安电子科技大学 Based on SiC and Ga2O3And a method for manufacturing the semiconductor structure
CN112831750A (en) * 2021-01-04 2021-05-25 广东省科学院中乌焊接研究所 Method for growing gallium oxide film on substrate and gallium oxide film

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Publication number Priority date Publication date Assignee Title
EP1598450A2 (en) * 2003-02-24 2005-11-23 Waseda University B-Ga2o3 SINGLE CRYSTAL GROWING METHOD, THIN-FILM SINGLE CRYSTAL GROWING METHOD, Ga2o3 LIGHT-EMITTING DEVICE, AND ITS MANUFACTURING METHOD
CN104962858A (en) * 2015-07-08 2015-10-07 西安电子科技大学 GaAs substrate-based gallium oxide thin film and growing method thereof
CN104988579A (en) * 2015-07-08 2015-10-21 西安电子科技大学 Gallium oxide film based on sapphire substrate and growing method of gallium oxide film
CN105118853A (en) * 2015-07-08 2015-12-02 西安电子科技大学 MgO substrate-based gallium oxide thin film and growing method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1598450A2 (en) * 2003-02-24 2005-11-23 Waseda University B-Ga2o3 SINGLE CRYSTAL GROWING METHOD, THIN-FILM SINGLE CRYSTAL GROWING METHOD, Ga2o3 LIGHT-EMITTING DEVICE, AND ITS MANUFACTURING METHOD
CN104962858A (en) * 2015-07-08 2015-10-07 西安电子科技大学 GaAs substrate-based gallium oxide thin film and growing method thereof
CN104988579A (en) * 2015-07-08 2015-10-21 西安电子科技大学 Gallium oxide film based on sapphire substrate and growing method of gallium oxide film
CN105118853A (en) * 2015-07-08 2015-12-02 西安电子科技大学 MgO substrate-based gallium oxide thin film and growing method thereof

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110993504A (en) * 2019-10-14 2020-04-10 西安电子科技大学 Ga based on SiC substrate2O3Preparation method of film and Ga based on SiC substrate2O3Film(s)
CN111048402A (en) * 2019-10-14 2020-04-21 西安电子科技大学 Based on SiC and Ga2O3And a method for manufacturing the semiconductor structure
CN110854233A (en) * 2019-11-17 2020-02-28 金华紫芯科技有限公司 Ga2O3Film-based solar blind ultraviolet detector, preparation method and application
CN110854233B (en) * 2019-11-17 2021-09-07 金华紫芯科技有限公司 Ga2O3Film-based solar blind ultraviolet detector, preparation method and application
CN112831750A (en) * 2021-01-04 2021-05-25 广东省科学院中乌焊接研究所 Method for growing gallium oxide film on substrate and gallium oxide film

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Application publication date: 20190104