CN115558890A - Tantalum-doped Ga 2 O 3 Controllable preparation process method of film - Google Patents

Tantalum-doped Ga 2 O 3 Controllable preparation process method of film Download PDF

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CN115558890A
CN115558890A CN202211379912.5A CN202211379912A CN115558890A CN 115558890 A CN115558890 A CN 115558890A CN 202211379912 A CN202211379912 A CN 202211379912A CN 115558890 A CN115558890 A CN 115558890A
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tantalum
film
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gallium oxide
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黄健
邓洁
黄浩斐
王梦倩
王世琳
刘尊
顾客云
李洪伟
丽娜.阿扎提
张磊
唐可
王林军
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University of Shanghai for Science and Technology
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
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    • C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
    • C23C14/352—Sputtering by application of a magnetic field, e.g. magnetron sputtering using more than one target
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    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
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    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
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    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
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Abstract

The invention discloses Ta doped Ga 2 O 3 The controllable preparation process method of the film comprises the steps of co-sputtering tantalum oxide and gallium oxide by a magnetron sputtering method to generate a tantalum-doped gallium oxide film; and annealing the tantalum-doped gallium oxide film. The tantalum-doped gallium oxide film prepared by the method has the advantages of uniform surface distribution, compact structure and controllable film thickness. The preparation method provided by the invention is simple to operate and strong in process controllability. The process has important significance for developing devices such as photoelectric detectors, high-power devices, field effect transistors and the like, and has wide application prospects in the fields of aerospace, rail traffic, energy conversion, communication and automobiles.

Description

Tantalum-doped Ga 2 O 3 Controllable preparation process method of film
Technical Field
The invention relates to a preparation method of a performance-controllable tantalum-doped gallium oxide film by a co-sputtering method, and particularly relates to the technical field of semiconductor material manufacturing processes.
Background
Gallium oxide is considered to be a semiconductor material having the maximum energy gap among transparent conductive oxides as a novel ultra-wide energy gap semiconductor (4.9 eV). It has high breakdown electric field strength, high Bari-plus-merit value, low dielectric constant, stable physical and chemical properties and high mechanical strength. These excellent characteristics make gallium oxide have great application potential in the fields of photoelectric devices and the like, and become one of the research hotspots of wide bandgap semiconductor materials in recent years. According to the characteristics, the gallium oxide is applied to ultraviolet detectors, field effect transistors, schottky diodes, high-power devices and X-ray detectors, and is suitable for national defense and military industry, aerospace, microwave communication, rail transit, high-end equipment, smart grids, energy conversion and the like.
However, it is more difficult to achieve high conductivity as the band gap of the semiconductor is wider. Intrinsic gallium oxide has high resistance, which limits its application as a transparent conductive oxide in electronic devices to some extent, and the most common way to effectively improve the electrical properties of materials is by doping the materials with different elements. For common doped gallium oxide based on Sn, ge, si and other elements, a high-quality and high-doping-content film is difficult to obtain, and a great progress space is left for the large-scale application requirement of the gallium oxide. Therefore, the current efficient doping process of gallium oxide thin film is the key of its industrial application.
The preparation method of the gallium oxide film mainly comprises Atomic Layer Deposition (ALD), molecular Beam Epitaxy (MBE), radio frequency magnetron sputtering, metal Organic Chemical Vapor Deposition (MOCVD) and the like. Aiming at the preparation of the film, the magnetron sputtering method has the advantages of good stability, good controllability, flexible selection of target materials, room-temperature processing, low cost and good operation, and particularly the magnetron co-sputtering method can realize the controllable adjustment of the doping concentration, thereby being an ideal preparation method of the gallium oxide-doped film with controllable performance.
Disclosure of Invention
In order to solve the problems of the prior art, the invention aims to overcome the defects of the prior art and provide a tantalum-doped Ga 2 O 3 The controllable preparation process method of the film, the tantalum-doped gallium oxide film prepared by the invention has the advantages of uniform surface distribution, compact structure and controllable film thickness. The preparation method provided by the invention is simple to operate and strong in process controllability. The process has important significance for developing devices such as photoelectric detectors, high-power devices, field effect transistors and the like, and has wide application prospects in the fields of aerospace, rail transit, energy conversion, communication and automobiles.
In order to achieve the purpose of the invention, the invention adopts the following technical scheme:
tantalum-doped Ga 2 O 3 The controllable preparation process method of the film comprises the following steps:
(1) Target selection
According to the calculation method of the material purity by taking the impurity concentration ratio of the material as the material purity, uniformly doped blocky gallium oxide and tantalum oxide with the purity not lower than 99.99% are selected as the target material for magnetron co-sputtering, and the target material is put into a magnetron co-sputtering chamber for standby;
(2) Substrate processing
The substrate was cleaned sequentially with acetone, methanol, ethanol and deionized water in an ultrasonic wave, and N was used 2 Atmosphere blowingDrying, namely putting the treated substrate into a magnetron co-sputtering chamber for later use;
(3) Twin target sputtering
Introducing Ar gas to generate glow plasma, and growing a doped gallium oxide film on the substrate by adopting a radio frequency magnetron sputtering method; regulating sputtering air pressure, sputtering power and substrate temperature, and preparing the tantalum-doped gallium oxide film by adopting a sputtering process method;
(4) Post annealing
And after the sputtering process is finished, putting the film into an annealing furnace for high-temperature annealing, thereby crystallizing the film and obtaining a finished product of the tantalum-doped gallium oxide film with a uniform and compact structure.
In the step (2), an inorganic material base or a semiconductor material base is used as the substrate. The substrate is further preferably made of quartz or c-plane sapphire.
As a preferable technical solution of the present invention, in the step (2), the time for ultrasonically cleaning the substrate in each reagent is not less than 5 minutes. As a further improvement of the invention, the ultrasonic cleaning time in each reagent in the step (2) is 5-30 minutes.
As a preferable technical scheme of the invention, in the step (3), the background vacuum of the magnetron co-sputtering chamber is less than or equal to 5 multiplied by 10 -4 Pa, and the working gas is argon. As a further preferable technical scheme of the invention, the argon is high-purity argon, and the flow rate is not lower than 30sccm.
As a further improvement of the invention, the sputtering pressure in the step (3) is 0.3-1.0 Pa, the power of the gallium oxide target is 50-150W, and the power of the tantalum oxide target is 3-10W.
As a further preferable technical solution of the present invention, in the step (3), during sputtering, the chamber pressure is not higher than 1.0Pa, and further preferably, the chamber pressure is not higher than 0.6 to 1.0Pa, the power of the gallium oxide target is 70 to 100W, the power of the tantalum oxide target is 5 to 8W, and the thickness of the tantalum-doped gallium oxide thin film is 200 to 500nm. As a further preferable technical proposal of the invention, the pre-sputtering time is 5 to 10 minutes.
As a preferable technical scheme, in the step (4), annealing is carried out in a vacuum environment, the annealing temperature is not lower than 900 ℃, and the heat preservation time is at least 1 hour. Annealing is carried out in a vacuum environment to avoid the introduction of impurity gases. As a further preferable technical scheme of the invention, the annealing temperature is 900-1100 ℃, and the annealing time is 1h.
As a preferable technical scheme, the temperature rising and falling rate in the annealing in the step (4) is more than or equal to 5 ℃/min, and the temperature is naturally reduced along with the furnace in a vacuum environment after being reduced to 300 ℃, so that the internal stress of the film is reduced to a certain extent.
As a further preferable technical scheme of the invention, in the step (4), the temperature rise rate of annealing is not lower than 6 ℃/min, the temperature reduction rate before the temperature reduction to 300 ℃ is not lower than 6 ℃/min, and the annealing furnace is naturally cooled along with the furnace in a vacuum environment after the temperature is lower than 300 ℃.
As a preferred technical scheme of the invention, in the step (4), the thickness of the prepared tantalum-doped gallium oxide thin film is not less than 200nm.
As a further preferable technical scheme of the invention, in the step (4), the thickness of the prepared tantalum-doped gallium oxide thin film is not less than 200-500 nm.
As a preferable technical scheme of the invention, in the step (4), the Ta/(Ta + Ga) ratio of the prepared tantalum-doped gallium oxide film is not less than 5% by mass percent.
As a further preferable technical scheme of the invention, in the step (4), the Ta/(Ta + Ga) ratio of the prepared tantalum-doped gallium oxide thin film is not less than 5-22.66%.
Compared with the prior art, the invention has the following obvious and prominent substantive characteristics and remarkable advantages:
1. in the invention, the transition metal Ta has 5 valence electrons, and compared with 4 valence electrons of Sn and Si elements, the introduction of Ta is expected to bring more electrons for a conduction band, thereby improving the carrier concentration and generating better electrical performance; compared with
Figure BDA0003927915120000031
Figure BDA0003927915120000032
Ions of doping elements are mixed in the plasma,
Figure BDA0003927915120000033
ionic radius of and
Figure BDA0003927915120000034
the ionic radius of the Ta element is closer, so that the lattice change caused by the doping of the Ta element in gallium oxide is small, and the Ta element is easier to dope;
2. aiming at the preparation of the film, the magnetron sputtering method has the advantages of good stability, good controllability, room-temperature processability, low cost and good operation;
3. the method adopts a magnetron co-sputtering method, and can conveniently regulate and control the tantalum-doped Ga by changing the technological parameters of two target positions 2 O 3 The performance of the film, and thus the film with corresponding performance can be obtained according to requirements.
Drawings
FIG. 1 is a schematic view of the manufacturing process equipment for tantalum-doped gallium oxide thin film according to the preferred embodiment of the present invention.
FIG. 2 shows doping concentration and forbidden band width of samples under different sputtering pressures, wherein A is example 1 and the sputtering pressure is 0.6Pa; b is example 2, the sputtering pressure is 0.8Pa; the sputtering pressure of C was 1.0Pa.
FIG. 3 shows the performance trend of samples at different substrate temperatures, wherein the sample at 600 ℃ corresponds to the tantalum-doped Ga prepared in example 3 2 O 3 A film.
FIG. 4 is a current-voltage characteristic curve of samples of tantalum oxide of example 4 of the present invention at different sputtering powers, wherein Ta is sputtered at 5W 2 O 5 Is example 4 sample, 8W sputtered Ta 2 O 5 Is the sample of example 1.
Detailed Description
The above-described embodiments are further illustrated below with reference to specific examples, in which preferred embodiments of the invention are detailed below:
example 1
In this example, a tantalum doped Ga 2 O 3 The controllable preparation process method of the film comprises the following steps:
(1) Substrate processing
Sequentially cleaning c-surface sapphire with acetone, methanol, ethanol and deionized water in ultrasonic wave for 5min, and cleaning with N 2 Drying the atmosphere, and putting the treated substrate into a magnetron co-sputtering chamber;
(2) Twin target sputtering
And respectively placing the target materials into two target positions of a magnetron sputtering device, introducing argon to generate glow plasma, and pre-sputtering the double targets simultaneously after glow starting, wherein the pre-sputtering time is 8min. The substrate temperature is room temperature, the sputtering pressure is adjusted to be 0.6Pa, and the sputtering powers of the gallium oxide target and the tantalum oxide target are respectively 100W and 8W. Simultaneously, the baffle is opened to start sputtering, and the sputtering time is 2 hours.
(3) Post annealing
After sputtering, the sample is put into an annealing furnace and vacuumized to 10 DEG -1 Pa, and carrying out high-temperature annealing at 900 ℃ for 1h under vacuum.
The tantalum-doped gallium oxide film prepared in the embodiment is used as a sample to be tested, and the scanning electron microscope is used for observation, so that the obtained film is uniform and compact in structure, the Ta/(Ta + Ga) ratio is 15.37% through EDS test analysis, and the thickness of the film is 500nm through a step profiler.
Example 2
This embodiment is substantially the same as embodiment 1, and is characterized in that:
in this embodiment, a tantalum-doped Ga 2 O 3 The controllable preparation process method of the film comprises the following steps:
(1) Substrate processing
Sequentially cleaning c-surface sapphire with acetone, methanol, ethanol and deionized water under ultrasonic wave for 5min, and cleaning with N 2 Drying the substrate in a dry atmosphere, and putting the treated substrate into a magnetron co-sputtering chamber;
(2) Twin target sputtering
And respectively placing the target materials into two target positions of a magnetron sputtering device, introducing argon to generate glow plasma, and pre-sputtering the double targets simultaneously after glow starting, wherein the pre-sputtering time is 8min. The substrate temperature is room temperature, the sputtering pressure is adjusted to be 0.8Pa, and the sputtering power of the gallium oxide target and the tantalum oxide target is respectively 100W and 8W. Meanwhile, the baffle is opened to start sputtering, and the sputtering time is 2 hours.
(3) Post annealing
After sputtering, the sample is put into an annealing furnace and vacuumized to 10 DEG -1 Pa, and carrying out high-temperature annealing at 900 ℃ for 1h under vacuum.
The tantalum-doped gallium oxide film prepared in the embodiment is used as a sample to be tested, and the scanning electron microscope is used for observation, so that the obtained film is uniform and compact in structure, the Ta/(Ta + Ga) ratio is 17.30% through EDS test analysis, and the thickness of the film is 485nm through a step profiler.
Example 3
This embodiment is substantially the same as the above embodiment, and is characterized in that:
in this example, a tantalum doped Ga 2 O 3 The controllable preparation process method of the film comprises the following steps:
(1) Substrate processing
Sequentially cleaning quartz substrate with acetone, methanol, ethanol and deionized water under ultrasonic wave for 5min, and cleaning with N 2 Drying the substrate in a dry atmosphere, and putting the treated substrate into a magnetron co-sputtering chamber;
(2) Twin target sputtering
Raising the temperature of the substrate to 600 ℃, preserving the heat for half an hour, and then carrying out pre-sputtering. Argon is introduced to generate glow plasma, and the double targets are simultaneously pre-sputtered after glow starting, wherein the pre-sputtering time is 8min. The sputtering pressure is adjusted to be 0.8Pa, and the powers of the gallium oxide and the tantalum oxide are respectively 100W and 8W. Meanwhile, the baffle is opened to start sputtering, and the sputtering time is 2.5 hours.
(3) Post annealing
After sputtering, the sample is put into an annealing furnace and vacuumized to 10 DEG -1 Pa, and carrying out high-temperature annealing at 900 ℃ for 1h under vacuum.
The tantalum-doped gallium oxide film prepared in the embodiment is used as a sample to be tested, and the scanning electron microscope is used for observation, so that the obtained film is uniform and compact in structure, the Ta/(Ta + Ga) ratio is 22.66% through EDS test analysis, and the thickness of the film is 510nm through a step profiler.
Example 4
This embodiment is substantially the same as the above embodiment, and is characterized in that:
in this embodiment, a tantalum-doped Ga 2 O 3 The controllable preparation process method of the film comprises the following steps:
(1) Substrate processing
Sequentially cleaning quartz with acetone, methanol, ethanol and deionized water under ultrasonic wave for 5min, and adding N 2 Drying the atmosphere, and putting the treated substrate into a magnetron co-sputtering chamber;
(2) Twin target sputtering
Argon is introduced to generate glow plasma, and the double targets are simultaneously pre-sputtered after glow starting, wherein the pre-sputtering time is 8min. The substrate temperature is room temperature, the sputtering pressure is adjusted to be 0.8Pa, and the sputtering powers of the gallium oxide target and the tantalum oxide target are respectively 100W and 5W. Meanwhile, the baffle is opened to start sputtering, and the sputtering time is 2 hours.
(3) Post annealing
After sputtering, the sample is put into an annealing furnace and vacuumized to 10 DEG -1 Pa, and carrying out high-temperature annealing at 900 ℃ for 1h under vacuum.
The tantalum-doped gallium oxide film prepared by the embodiment is used as a sample to be tested, and the scanning electron microscope is used for observation, so that the obtained film is uniform and compact in structure, the Ta/(Ta + Ga) ratio is 5% through EDS test analysis, and the thickness of the film is 320nm through a step profiler.
Test analysis and test:
FIG. 2 shows the doping concentration and the forbidden band width of the sample under different sputtering pressures, wherein A is case 1 and the sputtering pressure is 0.6Pa; b is example 2, the sputtering pressure is 0.8Pa; the sputtering pressure of C was 1.0Pa. It can be known from fig. 2 that the sputtering pressure has different degrees of influence on the forbidden bandwidth and the doping concentration of the prepared sample, and the forbidden bandwidth of the sample prepared under lower pressure is more ideal.
FIG. 3 shows the behavior trend of samples with different substrate temperatures, wherein the 600 ℃ sample is the Ta-doped Ga prepared in example 3 2 O 3 A film. It can be seen from fig. 3 that the doping concentration and the forbidden bandwidth of the sample prepared at a lower substrate temperature are more desirable.
FIG. 4 is a graph showing the current-voltage characteristics of samples of tantalum oxide sputtered at different sputtering powers in example 4 of the present invention, in which Ta is sputtered at 5W 2 O 5 Is example 4 sample, 8W sputtered Ta 2 O 5 Is the sample of example 1. As can be seen from FIG. 4, the electrical properties of the sample prepared by the higher tantalum oxide sputtering power are more ideal.
Ta-doped Ga of the above-described embodiments of the invention 2 O 3 The controllable preparation process method of the film comprises the steps of co-sputtering tantalum oxide and gallium oxide by a magnetron sputtering method to generate a tantalum-doped gallium oxide film; and annealing the tantalum-doped gallium oxide film. The tantalum-doped gallium oxide film prepared by the method has the advantages of uniform surface distribution, compact structure and controllable film thickness. The preparation method provided by the invention is simple to operate and strong in process controllability. The process has important significance for developing devices such as photoelectric detectors, high-power devices, field effect transistors and the like, and has wide application prospects in the fields of aerospace, rail transit, energy conversion, communication and automobiles.
The embodiments of the present invention have been described above with reference to the accompanying drawings, but the present invention is not limited to the above embodiments, and various changes can be made according to the purpose of the invention, and all changes, modifications, substitutions, combinations or simplifications made according to the spirit and principle of the technical solution of the present invention shall be made in the form of equivalent substitution, so long as the invention is in accordance with the purpose of the invention, and the invention shall fall within the protection scope of the present invention as long as the technical principle and the inventive concept of the present invention are not departed from the present invention.

Claims (8)

1. Tantalum-doped Ga 2 O 3 The controllable preparation process method of the film is characterized by comprising the following steps:
(1) Target selection
According to the calculation method of the material purity by taking the impurity concentration ratio of the material as the material purity, uniformly doped blocky gallium oxide and tantalum oxide with the purity not lower than 99.99% are selected as the target material for magnetron co-sputtering, and the target material is put into a magnetron co-sputtering chamber for standby;
(2) Substrate processing
The substrate was cleaned sequentially with acetone, methanol, ethanol and deionized water in an ultrasonic wave, and N was used 2 Drying the substrate in the air, and placing the treated substrate into a magnetron co-sputtering chamber for later use;
(3) Twin target sputtering
Introducing Ar gas to generate glow plasma, and growing a doped gallium oxide film on the substrate by adopting a radio frequency magnetron sputtering method; regulating sputtering air pressure, sputtering power and substrate temperature, and preparing a tantalum-doped gallium oxide film by adopting a sputtering process;
(4) Post annealing
And after the sputtering process is finished, putting the film into an annealing furnace for high-temperature annealing so as to crystallize the film and obtain a finished product of the tantalum-doped gallium oxide film with a uniform and compact structure.
2. Tantalum-doped Ga according to claim 1 2 O 3 The controllable preparation process method of the film is characterized by comprising the following steps: in the step (2), the substrate is an inorganic material base or a semiconductor material base.
3. Tantalum-doped Ga according to claim 2 2 O 3 The controllable preparation process method of the film is characterized in that: in the step (2), quartz or c-plane sapphire is used as the substrate.
4. Tantalum-doped Ga according to claim 1 2 O 3 The controllable preparation process method of the film is characterized in that: in the step (2), the substrate is ultrasonically cleaned in each reagent for not less than 5 minutes.
5. Tantalum-doped Ga according to claim 1 2 O 3 The controllable preparation process method of the film is characterized in thatThe method comprises the following steps: in the step (3), the background vacuum of the magnetron co-sputtering chamber is less than or equal to 5 x 10 -4 Pa, and the working gas is argon.
6. Tantalum-doped Ga according to claim 1 2 O 3 The controllable preparation process method of the film is characterized in that: in the step (3), during sputtering, the chamber pressure is not higher than 1.0Pa, the power of the gallium oxide target is 70-100W, the power of the tantalum oxide target is 5-8W, and the thickness of the tantalum-doped gallium oxide film is 200-500 nm.
7. Tantalum-doped Ga according to claim 1 2 O 3 The controllable preparation process method of the film is characterized by comprising the following steps: in the step (4), annealing is carried out in a vacuum environment, the annealing temperature is not lower than 900 ℃, and the heat preservation time is at least 1 hour.
8. Tantalum-doped Ga according to claim 1 2 O 3 The controllable preparation process method of the film is characterized by comprising the following steps: in the step (4), the temperature rise rate of annealing is not lower than 6 ℃/min, the temperature reduction rate before the temperature is reduced to 300 ℃ is not lower than 6 ℃/min, and the annealing furnace is naturally cooled along with the furnace in a vacuum environment after the temperature is lower than 300 ℃.
CN202211379912.5A 2022-11-04 2022-11-04 Tantalum-doped Ga 2 O 3 Controllable preparation process method of film Pending CN115558890A (en)

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