CN112853319A - Method for low-temperature epitaxial growth of high-quality GaN film on surface of ZnO nanowire - Google Patents

Method for low-temperature epitaxial growth of high-quality GaN film on surface of ZnO nanowire Download PDF

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CN112853319A
CN112853319A CN202110025235.6A CN202110025235A CN112853319A CN 112853319 A CN112853319 A CN 112853319A CN 202110025235 A CN202110025235 A CN 202110025235A CN 112853319 A CN112853319 A CN 112853319A
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gan film
reaction chamber
tmg
plasma
precursor
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马宏平
侯欣蓝
张园览
吴帆正树
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Fudan University
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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
    • 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
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
    • C23C16/45523—Pulsed gas flow or change of composition over time
    • C23C16/45525—Atomic layer deposition [ALD]
    • 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
    • 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
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
    • C23C16/34—Nitrides
    • 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
    • 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
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/4417—Methods specially adapted for coating powder

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Abstract

The invention belongs to the technical field of semiconductor device preparation, and particularly relates to a method for low-temperature epitaxial growth of a high-quality GaN film on the surface of a ZnO nanowire. The method adopts a plasma enhanced atomic layer deposition technology, utilizes the advantage that the growth temperature can be greatly reduced by utilizing the plasma enhanced atomic layer deposition, and uses a precursor trimethyl gallium as a gallium source and ammonia as a nitrogen source; and the controllable growth of the high-quality GaN film is realized by adjusting the plasma power and the precursor pulse time process parameters. The method successfully realizes the low-temperature hetero-epitaxial growth of the GaN film, has good crystallinity and crystal orientation perfectly matched with the ZnO nanowire, and the thickness of the epitaxial layer can be accurately regulated and controlled at atomic level. The method plays an important scientific role in the fields of power devices, microelectronics, transistors, sensors, photoelectric detection, photoelectrocatalysis, energy sources and the like, and has wide application prospect.

Description

Method for low-temperature epitaxial growth of high-quality GaN film on surface of ZnO nanowire
Technical Field
The invention belongs to the technical field of semiconductor device preparation, and particularly relates to a method for growing a GaN film on the surface of a ZnO nanowire through low-temperature heteroepitaxy.
Background
The gallium nitride (GaN) film has a wide band gap, and belongs to the third generation wide bandgap semiconductor material with SiC and diamond. Compared with the first generation of Ge, Si and the second generation of GaAs, InP compound semiconductor materials, the method has very obvious advantages. Because of large forbidden band width and high heat conductivity, GaN can stably work at high temperature and high pressure. Meanwhile, the GaN material has high breakdown voltage, small on-resistance, high electron saturation speed and high carrier mobility, and the excellent characteristics enable the GaN to have wide prospects in the application aspects of photoelectrons, high-temperature high-power devices and high-frequency microwave devices. In particular, GaN is an excellent material for microwave power transistors, and at the same time, it is a semiconductor having important application value in blue light emitting devices.
GaN is a semiconductor material that has been put into use, and is widely used in the field of LED lighting and increasingly important wireless fields. With the progress of the process and the improvement of the failure rate, GaN provides a lot of advantages in the applications of alternating current and direct current power conversion, level conversion and the like. GaN-based switching power transistors can operate at high voltages, with higher performance and lower losses than previously used silicon (Si) transistors. GaN has a more important advantage than silicon for power switching applications because GaN can provide lower losses at higher voltages and use less energy for switching. Si switches have improved significantly over many years, but GaN has superior performance to Si devices under the same size and voltage conditions.
The preparation of the high-quality GaN film is the premise and the foundation of a GaN-based device, the high-quality GaN film is prepared, the advantages of the material in all aspects are expected to be fully exerted, and a semiconductor functional device with higher performance is manufactured. At present, the GaN preparation method mainly includes Molecular Beam Epitaxy (MBE), chloride vapor phase epitaxy (HVPE), Metal Organic Chemical Vapor Deposition (MOCVD), and the like. In the epitaxial growth, epitaxial growth is generally selected on a sapphire substrate. These fabrication techniques and methods commonly used generally require higher growth temperatures during the fabrication of high quality, high crystalline quality GaN films. The compatibility of the GaN film and the preparation process of the semiconductor device is severely limited, and the application of the GaN film in various fields, such as flexible electronic devices and other fields which cannot resist high temperature, is greatly reduced due to the high growth temperature. Therefore, if the low-temperature epitaxial growth of the GaN film can be realized, the high crystallization of the film and the growth of the high-quality film can be ensured, the preparation process of the GaN film is compatible with the preparation process of the semiconductor device in temperature, and the application field of the GaN film can be greatly expanded. Meanwhile, the unique advantages of the GaN material are brought into play, the preparation cost of the film is greatly reduced in various fields of GaN application, and the research and application of the GaN are promoted.
Disclosure of Invention
The invention aims to provide a method for low-temperature epitaxial growth of a GaN film on a ZnO surface, which has the advantages of simple process, low preparation cost and adjustable film thickness, so as to obtain the heteroepitaxial growth of a high-quality GaN film.
The method for epitaxially growing the high-quality GaN film on the surface of the ZnO nanowire at low temperature adopts a Plasma Enhanced Atomic Layer Deposition (PEALD) technology, and utilizes the advantage that the growth temperature can be greatly reduced by the plasma enhanced atomic layer deposition to form precursors TMG (trimethylgallium) and NH3(ammonia) is used as a gallium source and a nitrogen source, and the controllable growth of the high-quality GaN film is realized by adjusting the process parameters such as plasma power, precursor pulse time and the like; the method comprises the following specific steps:
a. putting a substrate into an ALD reaction chamber which takes inert gas as carrier gas;
b. introducing a precursor TMG into the reaction chamber, and adsorbing on the surface of the ZnO nanowire;
c. purging the surface of the ZnO nanowire sample by using inert gas, and blowing away redundant precursor TMG and reaction byproducts;
d. NH is introduced into the reaction chamber3The plasma source reacts with the precursor TMG adsorbed on the surface of the ZnO nanowire;
e. purging the surface of the substrate with an inert gas to purge excess NH3And reaction by-products;
f. the steps b, c, d, e are circularly executed for a plurality of times in sequence to form a GaN film with a preset thickness;
wherein, the plasma enhanced atomic deposition (PEALD) mode is low-temperature epitaxy, and the growth temperature in the reaction chamber is 100-400 ℃;
the vacuum degree of the reaction chamber is 1-5 mbar;
in the step b, the source temperature of the precursor TMG is controlled at 6-25 ℃, and the pulse time is 0.005-2 seconds; the time for introducing TMG is 0.01-2 seconds;
in step d, the plasma pulse time is 5-120 seconds, the total gas flow is 10-300 sccm, and the plasma power is 50-300W.
Preferably, in the step b, the time for introducing the TMG is 0.02-0.1 second.
Preferably, in steps a, c and e, the inert gas is argon or nitrogen.
Preferably, in step d, NH3The flow rate of (1) is 100-200 sccm.
Preferably, in step d, the plasma pulse time is 40-60 seconds.
Preferably, the growth temperature in the reaction chamber is 200-300 ℃. More preferably, the growth temperature is 200 ℃ to 250 ℃.
Preferably, the vacuum in the reaction chamber is 1-2 mbar.
Preferably, in steps c and e, the inert gas purging time is 10-15 seconds.
In the step f, the cycle execution times can be adjusted and set at will according to needs, and the thickness of the GaN film changes along with the set cycle times and corresponds to the cycle times one by one. The cycle times are reduced by preparing the ultrathin GaN film, and the cycle times are increased by preparing the thick GaN film.
In the invention, the ZnO nanowire is a nanowire material prepared by a hydrothermal method, a CVD method, a PLD method and the like.
Compared with the prior art, the invention has the beneficial effects that:
the method for growing the GaN film by utilizing the Plasma Enhanced Atomic Layer Deposition (PEALD) has the advantages that the GaN film with high crystallization characteristic can be grown at a lower temperature, meanwhile, the thickness of the film can be accurately regulated and controlled by regulating the ALD cycle number, the ultrathin GaN film (1-50 nm) can be grown, and very high uniformity can be realized. And the repeatability is strong, the yield is high, and convenience is brought to the preparation of the derivative device.
Drawings
FIG. 1 is a schematic diagram of a process for preparing a GaN thin film by Plasma Enhanced Atomic Layer Deposition (PEALD) used in the present invention.
FIG. 2 is a Transmission Electron Microscope (TEM) characterization result of the ZnO nanowires grown by the hydrothermal method in the example. Wherein, (a) a low resolution Transmission Electron Microscope (TEM) image, (b) a high resolution TEM image, and (c) a Selected Area Electron Diffraction (SAED) image.
FIG. 3 is the X-ray photoelectron spectroscopy (XPS) characterization of the ZnO nanowires grown hydrothermally in example 1.
FIG. 4 is TEM characterization of ZnO-GaN core-shell nanowire structures formed after ALD growth of 10nm GaN thin films in example 1. Wherein, (a) a low resolution Transmission Electron Microscope (TEM) image, (b) a high resolution TEM image, and (c) a Selected Area Electron Diffraction (SAED) image.
FIG. 5 is XPS characterization of ZnO-GaN core-shell nanowire structures formed after ALD growth of 10nm GaN thin films in example 1.
FIG. 6 is TEM characterization of ZnO-GaN core-shell nanowire structures formed after ALD growth of 20nm GaN thin films in example 2. Wherein, (a) a low resolution Transmission Electron Microscope (TEM) image, (b) a high resolution TEM image, and (c) a Selected Area Electron Diffraction (SAED) image.
Detailed Description
In order that the present invention may be more clearly and easily understood, the following detailed description is given with reference to specific embodiments.
The method for epitaxially growing the high-quality GaN film on the surface of the ZnO nanowire at low temperature by using ALD (atomic layer deposition) mainly comprises the steps of absorbing a reaction precursor, purging Ar and NH3Plasma processThe daughter is introduced into the cavity, Ar is used for blowing, and the process can form the high-quality GaN film through multiple cycles. Preferred examples of the present invention are described below in detail.
Example 1: and (3) epitaxially growing a 10nm GaN thin film by ALD at 200 ℃.
The first step, growing ZnO nanowires on a Si substrate by a hydrothermal method: the Si sample is a wafer with the size of 100 cm2Polishing a single surface, cleaning by a strict semiconductor RCA process to obtain the silicon nitride wafer, pre-etching, and soaking in a 5% hydrofluoric acid aqueous solution for 2 min to remove a surface oxide layer. And then depositing a ZnO thin film with the thickness of 20-40 nm on the Si substrate by using an ALD (atomic layer deposition) or a suspension coating method to be used as a seed crystal layer for growing the nanowire. Then, ZnO nanowires were grown at 80 ℃ by hydrothermal method, and hydrothermal growth was carried out for 8 hours, so as to obtain ZnO nanowires with a diameter of 40nm and a length of 800-1000 nm, as shown in FIG. 2.
A second step of epitaxially growing a GaN thin film on the surface of the ZnO nanowire, the method comprising the steps of:
a. putting a cleaned substrate on which ZnO nanowires grow into a reaction chamber with inert gas as carrier gas;
b. introducing a precursor TMG into the reaction chamber for 20 milliseconds;
c. purging the surface of the ZnO nanowire by using inert gas, and purging to remove redundant precursors for 10 seconds;
d. introducing NH into the reaction chamber3The plasma reacts with the precursor adsorbed on the surface of the ZnO nanowire within 40 seconds;
e. purging the surface of the ZnO nanowire by using inert gas to blow away redundant plasma NH3And reaction by-products, purge time 15 seconds;
the initial temperature of the reaction chamber is 200 ℃;
the vacuum degree of the reaction chamber is 1-2 mbar;
the inert gas used as the carrier gas and used for purging is Ar gas;
the precursor TMG introduced in the step b is a liquid source, and the source temperature is 10 ℃;
NH introduced in step d3The flow rate of (2) is 100 sccm, and the power of the plasma is 200W；
Steps b-e are one ALD process cycle, schematically illustrated in FIG. 1;
and (5) cycling the steps b-e 400 times to obtain a GaN film with the thickness of 8-12 nm, wherein the structure diagram of the TEM is shown in FIG. 4. Compared with ZnO nanowires, after the GaN thin film is grown by ALD, the diameter of the nanowires is increased from 40nm to 60nm, which shows that the GaN thin film with the thickness of 10nm is uniformly coated on the surfaces of the ZnO nanowires by ALD. And from the TEM characterization results, the crystal orientation of the grown GaN film is perfectly matched with that of ZnO.
The prepared ZnO nanowire and ZnO-GaN core-shell nanowire structures are measured by an X-ray photoelectron spectroscopy (XPS), the element types in the nanowire structures are represented, and the XPS spectrogram of the ZnO nanowire without growing a GaN film is shown in FIG. 3. Only Zn, O and C elements are contained, and Ga and N elements are not detected. And after the GaN film is grown by ALD, an XPS spectrogram of the ZnO-GaN core-shell nanowire structure is shown in FIG. 5, and a test result shows that elements such as Ga, N and the like are detected in the nanowire structure, which indicates that the GaN film grows to the surface of the ZnO nanowire.
Example 2: and epitaxially growing a 20nm GaN film by ALD at 200 ℃.
The first step, growing ZnO nanowires on a Si substrate by a hydrothermal method: the Si sample is a wafer with the size of 100 cm2Polishing a single surface, cleaning by a strict semiconductor RCA process to obtain the silicon nitride wafer, pre-etching, and soaking in a 5% hydrofluoric acid aqueous solution for 2 min to remove a surface oxide layer. And then depositing a ZnO thin film with the thickness of 20-40 nm on the Si substrate by using an ALD (atomic layer deposition) or a suspension coating method to be used as a seed crystal layer for growing the nanowire. Then, ZnO nanowires are grown at 80 ℃ by a hydrothermal method and hydrothermal growth is carried out for 8 hours, so that ZnO nanowires with the diameter of 40nm and the length of 800-1000 nm can be obtained.
A second step of epitaxially growing a GaN thin film on the surface of the ZnO nanowire, the method comprising the steps of:
a. putting a cleaned substrate on which ZnO nanowires grow into a reaction chamber with inert gas as carrier gas;
b. introducing a precursor TMG into the reaction chamber for 20 milliseconds;
c. purging the surface of the ZnO nanowire by using inert gas, and purging to remove redundant precursors for 10 seconds;
d. introducing NH into the reaction chamber3The plasma reacts with the precursor adsorbed on the surface of the ZnO nanowire within 40 seconds;
e. purging the surface of the ZnO nanowire by using inert gas to blow away redundant plasma NH3And reaction by-products, purge time 15 seconds;
the initial temperature of the reaction chamber is 200 ℃;
the vacuum degree of the reaction chamber is 1-2 mbar;
the inert gas used as the carrier gas and used for purging is Ar gas;
the precursor TMG introduced in the step b is a liquid source, and the source temperature is 10 ℃;
NH introduced in step d3The flow rate of (2) is 100 sccm, and the power of the plasma is 200W;
steps b-e are one ALD process cycle, schematically illustrated in FIG. 1;
and b-e 800 times of circulation steps can obtain a GaN film with the thickness of 16-24nm, and TEM is used as a microstructure and is characterized as shown in FIG. 6. Compared with ZnO nanowires, after the GaN thin film is grown by ALD, the diameter of the nanowires is increased from 40nm to 80nm, which shows that ALD uniformly coats a layer of GaN thin film with the thickness of 20nm on the surface of the ZnO nanowires. Also from the TEM characterization results, it can be seen that the crystal orientation of the grown GaN film is perfectly matched to ZnO.

Claims (8)

1. A method for epitaxially growing a high-quality GaN film on the surface of a ZnO nanowire at low temperature is characterized in that a plasma enhanced atomic layer deposition technology is adopted, and the advantage that the growth temperature can be greatly reduced by utilizing the plasma enhanced atomic layer deposition is utilized to form precursors TMG and NH3As a gallium source and a nitrogen source, the controllable growth of the high-quality GaN film is realized by adjusting the plasma power and the precursor pulse time process parameters; the method comprises the following specific steps:
a. putting a substrate into an ALD reaction chamber which takes inert gas as carrier gas;
b. introducing a precursor TMG into the reaction chamber, and adsorbing on the surface of the ZnO nanowire;
c. purging the surface of the ZnO nanowire sample by using inert gas, and blowing away redundant precursor TMG and reaction byproducts;
d. NH is introduced into the reaction chamber3The plasma source reacts with the precursor TMG adsorbed on the surface of the ZnO nanowire;
e. purging the surface of the substrate with an inert gas to purge excess NH3And reaction by-products;
f. circularly executing the steps b, c, d, e for a plurality of times to form a GaN film with a preset thickness;
the growth temperature in the reaction chamber is 100-400 ℃;
the vacuum degree of the reaction chamber is 1-5 mbar;
in the step b, the source temperature of the precursor TMG is controlled at 6-25 ℃, and the pulse time is 0.005-2 seconds; the time for introducing TMG is 0.01-2 seconds;
in step d, the plasma pulse time is 5-120 seconds, the total gas flow is 10-300 sccm, and the plasma power is 50-300W.
2. The method of claim 1, wherein the TMG is introduced in step b for 0.02 to 0.1 seconds.
3. The method of claim 1, wherein NH in step d3The flow rate of (1) is 100-200 sccm.
4. The method of claim 1 wherein the plasma pulse time in step d is 40-60 seconds.
5. The method of claim 1, wherein in steps a, c and e, the inert gas is argon or nitrogen.
6. The method of claim 1, wherein the growth temperature in the reaction chamber is 200 ℃ to 300 ℃.
7. The method according to claim 1, wherein the vacuum in the reaction chamber is 1-2 mbar.
8. The method of claim 1, wherein the inert gas purge time in steps c, e is 10-15 seconds.
CN202110025235.6A 2021-01-08 2021-01-08 Method for low-temperature epitaxial growth of high-quality GaN film on surface of ZnO nanowire Pending CN112853319A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2015042199A1 (en) * 2013-09-23 2015-03-26 Ultratech, Inc. Method and apparatus for forming device quality gallium nitride layers on silicon substrates
CN110066986A (en) * 2019-04-29 2019-07-30 复旦大学 A method of utilizing the GaON film of atomic layer deposition one-step method controllable preparation difference oxygen and nitrogen content
CN110066985A (en) * 2019-04-29 2019-07-30 复旦大学 The method for preparing GaON film coated fine structure material using atomic layer deposition

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2015042199A1 (en) * 2013-09-23 2015-03-26 Ultratech, Inc. Method and apparatus for forming device quality gallium nitride layers on silicon substrates
CN110066986A (en) * 2019-04-29 2019-07-30 复旦大学 A method of utilizing the GaON film of atomic layer deposition one-step method controllable preparation difference oxygen and nitrogen content
CN110066985A (en) * 2019-04-29 2019-07-30 复旦大学 The method for preparing GaON film coated fine structure material using atomic layer deposition

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
HONG-PING MA: "Low-temperature epitaxial growth of high-quality GaON films on ZnO nanowires for superior photoelectrochemical water splitting", 《NANO ENERGY》 *

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Application publication date: 20210528