CN106282915A - A kind of preparation method of AlN thin film - Google Patents

A kind of preparation method of AlN thin film Download PDF

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CN106282915A
CN106282915A CN201610841499.8A CN201610841499A CN106282915A CN 106282915 A CN106282915 A CN 106282915A CN 201610841499 A CN201610841499 A CN 201610841499A CN 106282915 A CN106282915 A CN 106282915A
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thin film
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aln thin
ion beam
aln
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CN106282915B (en
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王文庆
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Yuncheng, Kunshan Su Ye Co., Ltd
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Dongguan Lianzhou Intellectual Property Operation and Management Co Ltd
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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
    • C23C14/02Pretreatment of the material to be coated
    • C23C14/021Cleaning or etching treatments
    • C23C14/022Cleaning or etching treatments by means of bombardment with energetic particles or 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
    • C23C14/06Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/0641Nitrides
    • 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
    • C23C14/34Sputtering
    • C23C14/35Sputtering by application of a magnetic field, e.g. magnetron sputtering

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  • Chemical Kinetics & Catalysis (AREA)
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  • Recrystallisation Techniques (AREA)
  • Physical Vapour Deposition (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

The present invention relates to the preparation field of wide bandgap semiconductor, particularly to the preparation method of the AlN thin film of a kind of (100) preferred orientation, comprise the following steps: (1) substrate pre-treatment;(2) target pretreatment;(3) ion beam assisted deposition, Ar are used+Ion beam sputter depositing Al film, N+Ion beam bombardment Al film, forms AlN cushion on substrate;(4)N2, Ar and NH3Under mixed gas, use magnetron sputtered deposition technology, AlN cushion is formed AlN thin film.Thin film (100) the preferred orientation growth that the method prepares, and film quality is excellent.

Description

A kind of preparation method of AlN thin film
Technical field
The present invention relates to the preparation field of wide bandgap semiconductor, particularly to the AlN thin film of a kind of (100) preferred orientation Preparation method.
Background technology
AlN thin-film material, as a kind of important broad stopband direct band-gap semicondictor material, has many most excellent Physical and chemical performance, such as: excellent table acoustic wave velocity, low thermal coefficient of expansion, high chemical stability, high resistivity, highly thermally conductive Rate, high rigidity, high-melting-point, broad stopband, big disruptive field intensity, low-dielectric loss etc..
The AlN thin film of different preferred orientations has different character, and for polymorph A lN thin film, thin film was growing Easily forming (002) preferred orientation in journey, its preparation is easier to.The thin film of prior art multipair (002) preferred orientation is visited Rope, and less to the AlN thin film study of (100) preferred orientation, and the present invention provides the AlN thin film of a kind of (100) preferred orientation Preparation method, provides condition for widening the application of AlN thin film.
Summary of the invention
It is an object of the invention to provide the preparation method of a kind of AlN thin film so that the thin film (100) that the method prepares is preferentially Oriented growth, and film quality is excellent.
For achieving the above object, the present invention uses techniques below means:
The preparation method of a kind of AlN thin film, comprises the following steps:
(1) substrate pre-treatment;
(2) target pretreatment;
(3) ion beam assisted deposition, Ar are used+Ion beam sputter depositing Al film, N+Ion beam bombardment Al film, at lining AlN cushion is formed at the end;
(4)N2, Ar and NH3Under mixed gas, use magnetron sputtered deposition technology, AlN cushion forms AlN thin Film.
Preferably, substrate pre-treatment includes that wet-cleaning is cleaned with dry etching.
Alternatively, dry etching cleans as to arrange ion source in magnetic control sputtering system, is served as a contrast by ion source Bombardment and cleaning The end.
More preferably, N is used+Ion beam and Ar+Substrate dry etching is cleaned by ion beam jointly.
Preferably, target pretreatment includes logical Ar target pre-sputtering and logical N2Target pre-sputtering.
Preferably, ion beam assisted depositing device is set in magnetic control sputtering system, in magnetic control sputtering system, carries out ion Bundle assistant depositing.
Preferably, NH during magnetron sputtering deposition AlN thin film3Content accounts for 2%~5%.
Preferably, magnetron sputtering deposition AlN thin film is carried out by several times, NH3Content the most gradually increases.
Preferably, magnetron sputtering shielding power supply uses the pulse power.
Preferably, Ar and N during magnetron sputtering2The ratio of volume is 1:1.
Compared with prior art, the invention have the advantages that introducing NH when the present invention sputters3,NH3Under high voltage electric field Ionizing out cation and the electronics of N and H, the cation of N goes down to assist bombardment target at electric field action, the cation induction AlN of H At (100) crystal face preferential growth, it is prepared for the AlN thin film of (100) preferred orientation;And the life of ion beam assisted depositing cushion Long so that while forming Al-N key, REINFORCED Al, N mix with substrate surface atom, make thin film strong with substrate adhesion;And The existence of cushion make after AlN thin film can homogenous growth, thin film crystallization quality is good, lattice defect is few.
Detailed description of the invention
In order to be better understood from the present invention, below by embodiment, the present invention is further described, and embodiment is served only for solving Release the present invention, the present invention will not be constituted any restriction.
Magnetic control sputtering system used by the embodiment of the present invention is composite film coating system, including ion source purging system, ion beam Assisted deposition system and magnetron sputtering coating system.By the cleaning further to substrate of ion source purging system;Pass through ion Bundle assisted deposition system forms AlN cushion;By magnetron sputtering coating system growing AIN thin film.
The present invention uses D/MAX-2200 type X-ray diffractometer (XRD) of science to characterize the structure of AlN thin film;Use middle section CSPM-3100 type atomic force microscope (AFM) that basis nanometer instrument company of chemistry institute of institute produces carrys out the shape on viewing film surface Looks, granular size and surface roughness;Thin film tack is characterized by cold cycling method, keeps 5 points in 0 ° of mixture of ice and water Clock, puts into immediately after in 100 ° of boiling water and keeps 5 minutes, several cycles of such cold cycling.
Comparative example
The preparation method of a kind of AlN thin film, comprises the following steps:
(1) substrate pre-treatment;
Substrate pre-treatment includes that substrate pre-treatment includes wet-cleaning and ion source Bombardment and cleaning.
Substrate selects the single crystalline Si (100) of finishing polish;
Wet-cleaning: the single crystalline Si (100) of polishing is immersed in acetone soln and carries out ultrasonic Treatment 15 minutes, then by essence Mixed liquor 1 (deionized water: hydrogen peroxide: fluorine water=5:2:l) boils 5 minutes, then with mixed liquor 2 (deionized water: peroxide Change hydrogen: hydrochloric acid=7:2:1) boil 5 minutes, carry out ultrasonic Treatment the most in deionized water 20 minutes, to remove silicon chip table Face Organic substance that may be present, puts into after taking-up and is filled with pure N2Drying baker in be heated to 100 DEG C dry 1 hour.
Ion source Bombardment and cleaning: cleaned single crystalline Si (100) substrate is positioned over the ion of magnetron sputtering hybrid system On the purging system sample stage of source, close cavity;Ar+Substrate dry etching is cleaned 15min by ion beam.
(2) target pretreatment;
Al target is arranged in magnetron sputtering hybrid system, normally starts magnetron sputtering apparatus, cavity is evacuated to 1 × 10-5Pa, first blocks baffle plate before deposition, is filled with Ar gas, by Al target elder generation pre-sputtering 15min, to remove the Al of target surface2O3Layer.
(3)N2, under Ar mixed gas, use pulse reaction magnetron sputtered deposition technology, form AlN thin film.Technological parameter Arrange: target-substrate distance is 4.5cm, and sputtering pressure is 0.5Pa, Ar and N2Content respectively accounts for 50%, and sputtering power is 150W, underlayer temperature Being 75 DEG C, pulse frequency 30kHz, dutycycle is 50%, and sedimentation time is 60min.
XRD result shows, the present embodiment AlN thin film only goes out AlN (002) crystallographic plane diffraction peak near 36 °, illustrates that thin film exists (002) face preferential growth;AFM 3-D view display film surface is coarse, and its r.m.s. roughness (RMS) is 4.7nm;Tack By starting shedding off after cold cycling 10 cycle.
Embodiment 1
The preparation method of a kind of AlN thin film, comprises the following steps:
(1) substrate pre-treatment;
Substrate pre-treatment includes that substrate pre-treatment includes wet-cleaning and ion source Bombardment and cleaning.
Substrate selects the single crystalline Si (100) of finishing polish;
Wet-cleaning: the single crystalline Si (100) of polishing is immersed in acetone soln and carries out ultrasonic Treatment 15 minutes, then by essence Mixed liquor 1 (deionized water: hydrogen peroxide: fluorine water=5:2:l) boils 5 minutes, then with mixed liquor 2 (deionized water: peroxide Change hydrogen: hydrochloric acid=7:2:1) boil 5 minutes, carry out ultrasonic Treatment the most in deionized water 20 minutes, to remove silicon chip table Face Organic substance that may be present, puts into after taking-up and is filled with pure N2Drying baker in be heated to 100 DEG C dry 1 hour.
Ion source Bombardment and cleaning: cleaned single crystalline Si (100) substrate is positioned over the ion of magnetron sputtering hybrid system On the purging system sample stage of source, close cavity;Ar+Substrate dry etching is cleaned 15min by ion beam.
(2) target pretreatment;
Al target is arranged in magnetron sputtering hybrid system, normally starts magnetron sputtering apparatus, cavity is evacuated to 1 × 10-5Pa, first blocks baffle plate before deposition, is filled with Ar gas, by Al target elder generation pre-sputtering 15min, to remove the Al of target surface2O3Layer.
(3) ion beam assisted deposition is used, with the Ar of 2500V/50mA+Ion beam sputter depositing Al film, 2500V/ The N of 10mA+Ion beam bombardment Al film, assistant depositing 30min forms AlN cushion on substrate;
(4) specimen rotating holder so that it is rotate to magnetron sputtering film location, N from ion beam assisted depositing plated film position2、 Ar and NH3Under mixed gas, use pulse reaction magnetron sputtered deposition technology, AlN cushion is formed AlN thin film.Work Skill parameter is arranged: target-substrate distance is 4.5cm, and sputtering pressure is 0.5Pa, NH3Content accounts for 4%, Ar and N2Content respectively accounts for 48%, sputtering Power is 150W, and underlayer temperature is 75 DEG C, pulse frequency 30kHz, and dutycycle is 50%, and sedimentation time is 60min.
XRD result shows, the present embodiment AlN thin film only goes out AlN (100) crystallographic plane diffraction peak near 33 °, illustrates that thin film exists (100) face preferential growth;AFM 3-D view display film surface is smooth, uniformity, its r.m.s. roughness (RMS) For 3.7nm;Tack starts shedding off by after cold cycling 13 cycle.
Embodiment 2
The preparation method of a kind of AlN thin film, comprises the following steps:
(1) substrate pre-treatment;
Substrate pre-treatment includes that substrate pre-treatment includes wet-cleaning and ion source Bombardment and cleaning.
Substrate selects the single crystalline Si (100) of finishing polish;
Wet-cleaning: the single crystalline Si (100) of polishing is immersed in acetone soln and carries out ultrasonic Treatment 15 minutes, then by essence Mixed liquor 1 (deionized water: hydrogen peroxide: fluorine water=5:2:l) boils 5 minutes, then with mixed liquor 2 (deionized water: peroxide Change hydrogen: hydrochloric acid=7:2:1) boil 5 minutes, carry out ultrasonic Treatment the most in deionized water 20 minutes, to remove silicon chip table Face Organic substance that may be present, puts into after taking-up and is filled with pure N2Drying baker in be heated to 100 DEG C dry 1 hour.
Ion source Bombardment and cleaning: cleaned single crystalline Si (100) substrate is positioned over the ion of magnetron sputtering hybrid system On the purging system sample stage of source, close cavity;N+Ion beam and Ar+Substrate dry etching is cleaned 15min by ion beam jointly.
(2) target pretreatment;
Al target is arranged in magnetron sputtering hybrid system, normally starts magnetron sputtering apparatus, cavity is evacuated to 1 × 10-5Pa, first blocks baffle plate before deposition, is filled with Ar gas, by Al target elder generation pre-sputtering 15min, to remove the Al of target surface2O3Layer, Turn off Ar gas, be passed through N2Gas, pre-sputtering 10min.
(3) ion beam assisted deposition is used, with the Ar of 2500V/50mA+Ion beam sputter depositing Al film, 2500V/ The N of 10mA+Ion beam bombardment Al film, assistant depositing 30min forms AlN cushion on substrate;
(4) specimen rotating holder so that it is rotate to magnetron sputtering film location, N from ion beam assisted depositing plated film position2、 Ar and NH3Under mixed gas, use pulse reaction magnetron sputtered deposition technology, AlN cushion is formed AlN thin film.Work Skill parameter is arranged: target-substrate distance is 4.5cm, and sputtering pressure is 0.5Pa, NH3Content accounts for 4%, Ar and N2Content respectively accounts for 48%, sputtering Power is 150W, and underlayer temperature is 75 DEG C, pulse frequency 30kHz, and dutycycle is 50%, and sedimentation time is 60min.
XRD result shows, the present embodiment AlN thin film only goes out AlN (100) crystallographic plane diffraction peak near 33 °, illustrates that thin film exists (100) face preferential growth;AFM 3-D view display film surface is smooth, uniformity, its r.m.s. roughness (RMS) For 3.5nm;Tack starts shedding off by after cold cycling 14 cycle.
Embodiment 3
The preparation method of a kind of AlN thin film, comprises the following steps:
(1) substrate pre-treatment;
Substrate pre-treatment includes that substrate pre-treatment includes wet-cleaning and ion source Bombardment and cleaning.
Substrate selects the single crystalline Si (100) of finishing polish;
Wet-cleaning: the single crystalline Si (100) of polishing is immersed in acetone soln and carries out ultrasonic Treatment 15 minutes, then by essence Mixed liquor 1 (deionized water: hydrogen peroxide: fluorine water=5:2:l) boils 5 minutes, then with mixed liquor 2 (deionized water: peroxide Change hydrogen: hydrochloric acid=7:2:1) boil 5 minutes, carry out ultrasonic Treatment the most in deionized water 20 minutes, to remove silicon chip table Face Organic substance that may be present, puts into after taking-up and is filled with pure N2Drying baker in be heated to 100 DEG C dry 1 hour.
Ion source Bombardment and cleaning: cleaned single crystalline Si (100) substrate is positioned over the ion of magnetron sputtering hybrid system On the purging system sample stage of source, close cavity;N+Ion beam and Ar+Substrate dry etching is cleaned 15min by ion beam jointly.
(2) target pretreatment;
Al target is arranged in magnetron sputtering hybrid system, normally starts magnetron sputtering apparatus, cavity is evacuated to 1 × 10-5Pa, first blocks baffle plate before deposition, is filled with Ar gas, by Al target elder generation pre-sputtering 15min, to remove the Al of target surface2O3Layer, Turn off Ar gas, be passed through N2Gas, pre-sputtering 10min.
(3) ion beam assisted deposition is used, with the Ar of 2500V/50mA+Ion beam sputter depositing Al film, 2500V/ The N of 10mA+Ion beam bombardment Al film, assistant depositing 30min forms AlN cushion on substrate;
(4) specimen rotating holder so that it is rotate to magnetron sputtering film location, N from ion beam assisted depositing plated film position2、 Ar and NH3Under mixed gas, use pulse reaction magnetron sputtered deposition technology, AlN cushion is formed AlN thin film.Work Skill parameter is arranged: target-substrate distance is 4.5cm, and sputtering pressure is 0.5Pa, NH3Content accounts for 5%, Ar and N2Content respectively accounts for 47.5%, spatters Penetrating power is 150W, and underlayer temperature is 75 DEG C, pulse frequency 30kHz, and dutycycle is 50%, and sedimentation time is 60min.
XRD result shows, the present embodiment AlN thin film only goes out AlN (100) crystallographic plane diffraction peak near 33 °, illustrates that thin film exists (100) face preferential growth;AFM 3-D view display film surface is smooth, uniformity, its r.m.s. roughness (RMS) For 3.3nm;Tack starts shedding off by after cold cycling 15 cycle.
Embodiment 4
The preparation method of a kind of AlN thin film, comprises the following steps:
(1) substrate pre-treatment;
Substrate pre-treatment includes that substrate pre-treatment includes wet-cleaning and ion source Bombardment and cleaning.
Substrate selects the single crystalline Si (100) of finishing polish;
Wet-cleaning: the single crystalline Si (100) of polishing is immersed in acetone soln and carries out ultrasonic Treatment 15 minutes, then by essence Mixed liquor 1 (deionized water: hydrogen peroxide: fluorine water=5:2:l) boils 5 minutes, then with mixed liquor 2 (deionized water: peroxide Change hydrogen: hydrochloric acid=7:2:1) boil 5 minutes, carry out ultrasonic Treatment the most in deionized water 20 minutes, to remove silicon chip table Face Organic substance that may be present, puts into after taking-up and is filled with pure N2Drying baker in be heated to 100 DEG C dry 1 hour.
Ion source Bombardment and cleaning: cleaned single crystalline Si (100) substrate is positioned over the ion of magnetron sputtering hybrid system On the purging system sample stage of source, close cavity;N+Ion beam and Ar+Substrate dry etching is cleaned 15min by ion beam jointly.
(2) target pretreatment;
Al target is arranged in magnetron sputtering hybrid system, normally starts magnetron sputtering apparatus, cavity is evacuated to 1 × 10-5Pa, first blocks baffle plate before deposition, is filled with Ar gas, by Al target elder generation pre-sputtering 15min, to remove the Al of target surface2O3Layer, Turn off Ar gas, be passed through N2Gas, pre-sputtering 10min.
(3) ion beam assisted deposition is used, with the Ar of 2500V/50mA+Ion beam sputter depositing Al film, 2500V/ The N of 10mA+Ion beam bombardment Al film, assistant depositing 30min forms AlN cushion on substrate;
(4) specimen rotating holder so that it is rotate to magnetron sputtering film location, N from ion beam assisted depositing plated film position2、 Ar and NH3Under mixed gas, use pulse reaction magnetron sputtered deposition technology, AlN cushion is formed AlN thin film.Work Skill parameter is arranged: target-substrate distance is 4.5cm, and sputtering pressure is 0.5Pa, NH3Content accounts for 6%, Ar and N2Content respectively accounts for 47%, sputtering Power is 150W, and underlayer temperature is 75 DEG C, pulse frequency 30kHz, and dutycycle is 50%, and sedimentation time is 60min.
XRD result shows, the present embodiment AlN thin film only goes out AlN (100) crystallographic plane diffraction peak near 33 °, illustrates that thin film exists (100) face preferential growth;AFM 3-D view display film surface is smooth, uniformity, its r.m.s. roughness (RMS) For 3.3nm;Tack starts shedding off by after cold cycling 14 cycle.
Embodiment 5
The preparation method of a kind of AlN thin film, comprises the following steps:
(1) substrate pre-treatment;
Substrate pre-treatment includes that substrate pre-treatment includes wet-cleaning and ion source Bombardment and cleaning.
Substrate selects the single crystalline Si (100) of finishing polish;
Wet-cleaning: the single crystalline Si (100) of polishing is immersed in acetone soln and carries out ultrasonic Treatment 15 minutes, then by essence Mixed liquor 1 (deionized water: hydrogen peroxide: fluorine water=5:2:l) boils 5 minutes, then with mixed liquor 2 (deionized water: peroxide Change hydrogen: hydrochloric acid=7:2:1) boil 5 minutes, carry out ultrasonic Treatment the most in deionized water 20 minutes, to remove silicon chip table Face Organic substance that may be present, puts into after taking-up and is filled with pure N2Drying baker in be heated to 100 DEG C dry 1 hour.
Ion source Bombardment and cleaning: cleaned single crystalline Si (100) substrate is positioned over the ion of magnetron sputtering hybrid system On the purging system sample stage of source, close cavity;N+Ion beam and Ar+Substrate dry etching is cleaned 15min by ion beam jointly.
(2) target pretreatment;
Al target is arranged in magnetron sputtering hybrid system, normally starts magnetron sputtering apparatus, cavity is evacuated to 1 × 10-5Pa, first blocks baffle plate before deposition, is filled with Ar gas, by Al target elder generation pre-sputtering 15min, to remove the Al of target surface2O3Layer, Turn off Ar gas, be passed through N2Gas, pre-sputtering 10min.
(3) ion beam assisted deposition is used, with the Ar of 2500V/50mA+Ion beam sputter depositing Al film, 2500V/ The N of 10mA+Ion beam bombardment Al film, assistant depositing 30min forms AlN cushion on substrate;
(4) specimen rotating holder so that it is rotate to magnetron sputtering film location, N from ion beam assisted depositing plated film position2、 Ar and NH3Under mixed gas, use pulse reaction magnetron sputtered deposition technology, AlN cushion is formed AlN thin film.Work Skill parameter is arranged: target-substrate distance is 4.5cm, and sputtering pressure is 0.5Pa, and sputtering power is 150W, and underlayer temperature is 75 DEG C, pulse frequency Rate 30kHz, dutycycle is 50%.NH for the first time3Content accounts for 3%, Ar and N2Content respectively accounts for 48.5%, and sedimentation time is 10min; Other conditions are constant, adjust NH3Content accounts for 4%, Ar and N2Content respectively accounts for 48%, and sedimentation time is 10min for the second time;Other Part is constant, adjusts NH3Content accounts for 5%, Ar and N2Content respectively accounts for 47.5%, and sedimentation time is 40min for the third time.
XRD result shows, the present embodiment AlN thin film only goes out AlN (100) crystallographic plane diffraction peak near 33 °, illustrates that thin film exists (100) face preferential growth;AFM 3-D view display film surface is smooth, uniformity, its r.m.s. roughness (RMS) For 3.1nm;Tack starts shedding off by after cold cycling 15 cycle.

Claims (10)

1. the preparation method of an AlN thin film, it is characterised in that comprise the following steps:
(1) substrate pre-treatment;
(2) target pretreatment;
(3) ion beam assisted deposition, Ar are used+Ion beam sputter depositing Al film, N+Ion beam bombardment Al film, on substrate Form AlN cushion;
(4)N2, Ar and NH3Under mixed gas, use magnetron sputtered deposition technology, AlN cushion is formed AlN thin film.
The preparation method of AlN thin film the most according to claim 1, it is characterised in that: substrate pre-treatment include wet-cleaning with Dry etching cleans.
The preparation method of AlN thin film the most according to claim 2, it is characterised in that: dry etching cleans as at magnetron sputtering Ion source is set in system, by ion source Bombardment and cleaning substrate.
The preparation method of AlN thin film the most according to claim 3, it is characterised in that: use N+Ion beam and Ar+Ion beam is altogether Clean with to substrate dry etching.
The preparation method of AlN thin film the most according to claim 1, it is characterised in that: target pretreatment includes that logical Ar target is pre- Sputtering and logical N2Target pre-sputtering.
The preparation method of AlN thin film the most according to claim 1, it is characterised in that: ion beam is set in magnetic control sputtering system Assistant depositing device, carries out ion beam assisted depositing in magnetic control sputtering system.
The preparation method of AlN thin film the most according to claim 1, it is characterised in that: NH during magnetron sputtering deposition AlN thin film3Contain Amount accounts for 2%~5%.
The preparation method of AlN thin film the most according to claim 1, it is characterised in that: magnetron sputtering deposition AlN thin film enters by several times OK, NH3Content the most gradually increases.
The preparation method of AlN thin film the most according to claim 1, it is characterised in that: magnetron sputtering shielding power supply uses pulse Power supply.
The preparation method of AlN thin film the most according to claim 1, it is characterised in that: Ar and N during magnetron sputtering2The ratio of volume For 1:1.
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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108922946A (en) * 2018-07-16 2018-11-30 厦门乾照光电股份有限公司 A kind of LED structure and preparation method thereof
CN112877657A (en) * 2021-01-12 2021-06-01 有研工程技术研究院有限公司 Preparation method of AlN thin film
CN114231933A (en) * 2021-12-23 2022-03-25 江苏籽硕科技有限公司 Method for preparing film by ion beam sputtering deposition
CN118147578A (en) * 2023-12-28 2024-06-07 华南理工大学 Aluminum nitride coating containing different preferred orientations and preparation method thereof

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5270263A (en) * 1991-12-20 1993-12-14 Micron Technology, Inc. Process for depositing aluminum nitride (AlN) using nitrogen plasma sputtering
CN101824592A (en) * 2010-05-26 2010-09-08 湖南大学 Deposition method capable of enhancing preferred orientation growth of AlN film

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5270263A (en) * 1991-12-20 1993-12-14 Micron Technology, Inc. Process for depositing aluminum nitride (AlN) using nitrogen plasma sputtering
CN101824592A (en) * 2010-05-26 2010-09-08 湖南大学 Deposition method capable of enhancing preferred orientation growth of AlN film

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
沃森等: "《薄膜加工工艺》", 31 March 1987 *
胡丽君等: "氨化时间和膜厚对Si(Ⅲ)上AlN薄膜生长取向的影响", 《山东师范大学学报(自然科学版)》 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108922946A (en) * 2018-07-16 2018-11-30 厦门乾照光电股份有限公司 A kind of LED structure and preparation method thereof
CN112877657A (en) * 2021-01-12 2021-06-01 有研工程技术研究院有限公司 Preparation method of AlN thin film
CN114231933A (en) * 2021-12-23 2022-03-25 江苏籽硕科技有限公司 Method for preparing film by ion beam sputtering deposition
CN118147578A (en) * 2023-12-28 2024-06-07 华南理工大学 Aluminum nitride coating containing different preferred orientations and preparation method thereof

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