CN103361629B - The preparation method of ECR-PEMOCVD low temperature depositing InN film on GaN buffer layer/diamond thin/Si multi-layer film structure substrate - Google Patents
The preparation method of ECR-PEMOCVD low temperature depositing InN film on GaN buffer layer/diamond thin/Si multi-layer film structure substrate Download PDFInfo
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Abstract
<b>the invention belongs to technical field of novel photoelectric material sediment preparation, it is provided that a kind of to prepare electric property good</b><b>inN</b><b>optoelectronic film and cost are low</b><b>eCR-PEMOCVD</b><b> </b><b>gaN</b><b>buffer layer</b><b>/</b><b>diamond thin</b><b>/ Si</b><b>low temperature depositing on multi-layer film structure substrate</b><b>inN</b><b>the preparation method of film. The present invention comprises the following steps:</b><b>1</b><b>) will</b><b>si</b><b>substrate is successively with, after acetone, ethanol and deionized water ultrasonic cleaning, blowing dry feeding reaction chamber with nitrogen;</b><b>2</b><b>) use heated filament</b><b>cVD</b><b>system, vacuumizes reaction chamber, will</b><b>si</b><b>substrate heating, leads to into hydrogen and methane gas in reaction chamber,</b><b>si</b><b>substrate base obtains diamond thin.</b><b>3</b><b>) adopt</b><b>eCR-PEMOCVD</b><b>(electron cyclotron resonace</b><b>-</b><b>plasma reinforcing and metal organic chemical vapor deposition) system, reaction chamber is vacuumized, by substrate heating extremely</b><b>200</b><b>~</b><b>600</b><b>dEG C, lead in reaction chamber carry into hydrogen trimethyl-gallium, nitrogen.</b>
Description
Technical field
The invention belongs to technical field of novel photoelectric material sediment preparation, particularly relate to the preparation method of a kind of ECR-PEMOCVD low temperature depositing InN film on GaN buffer layer/diamond thin/Si multi-layer film structure substrate.
Background technology
Nitrogenize indium (InN) is the important member in III group-III nitride, compares with GaN with AlN, and the mobility of InN and point peak speed etc. are all the highest, have unique advantage in the application of the electron devices such as high-speed high frequency transistor; Its band gap at room temperature is positioned at near-infrared region, is also suitable for preparing the photoelectric devices such as high efficiency solar cell, semiconductor light-emitting-diode and optical communication device. But owing to InN decomposition temperature is low, it is desired to low growth temperature, and nitrogenous source decomposition temperature height, so general InN film all grows on some substrates such as sapphire. It is well known that the price of sapphire substrate is higher, use it as the substrate of InN material, make the cost of the device of InN material base be difficult to lower, seriously hinder the development of InN material devices.
Summary of the invention
The present invention is exactly for the problems referred to above, it is provided that a kind of prepare the good InN optoelectronic film of electric property and the preparation method of the low ECR-PEMOCVD low temperature depositing InN film on GaN buffer layer/diamond thin/Si multi-layer film structure substrate of cost.
For achieving the above object, the present invention adopts following technical scheme, and the present invention comprises the following steps.
1) by Si substrate successively with, after acetone, ethanol and deionized water ultrasonic cleaning, blowing dry feeding reaction chamber with nitrogen.
2) use HF CVD system, reaction chamber is vacuumized, by Si substrate heating, lead in reaction chamber into hydrogen and methane gas, Si substrate base obtains diamond thin.
3) adopt ECR-PEMOCVD(electron cyclotron resonace-plasma reinforcing and metal organic chemical vapor deposition) system, reaction chamber is vacuumized, by substrate heating to 200��600 DEG C, lead in reaction chamber carry into hydrogen trimethyl-gallium, nitrogen; The control total pressure of gas, electron cyclotron resonace reacts, and obtains the GaN buffer layer thin film on the Si substrate of gold-plated diamond thin film.
4) continue to adopt ECR-PEMOCVD system, reaction chamber vacuumized, by substrate heating to 300��700 DEG C, lead in reaction chamber carry into hydrogen trimethyl indium, nitrogen, throughput ratio both it is (4��5): (100��180); The control total pressure of gas is 1.5��1.8Pa; Electron cyclotron resonace reaction 30min��3h, obtains the InN optoelectronic film on GaN buffer layer/diamond thin/Si structure substrate.
As a kind of preferred version, the purity of the purity of trimethyl indium of the present invention, the purity of trimethyl-gallium and nitrogen is 99.99%.
As another kind of preferred version, the thickness of diamond thin of the present invention is 300nm.
As another kind of preferred version, step 1) ultrasonic cleaning of the present invention 5 minutes; Step 2) it is evacuated to 1.0 �� 10
-2
Pa; Substrate heating to 800 DEG C; Hydrogen and methane gas flow are respectively 200sccm and 4sccm, by mass flowmeter control; Heated filament voltage is 10V, and heater current is 50A, reaction 30min.
As another kind of preferred version, step 3) of the present invention is evacuated to 8.0 �� 10
-4
Pa; The flow of trimethyl-gallium and nitrogen is respectively 0.5sccm and 100sccm, by mass flowmeter control; The control total pressure of gas is 1.2Pa; Electron cyclotron resonace power is 650W, reaction 60min; Step 4) reaction chamber is evacuated to 9.0 �� 10
-4
Pa; The flow of trimethyl indium, nitrogen is by mass flowmeter control; Electron cyclotron resonace power is 650W.
As another kind of preferred version, step 3) substrate heating to 400 DEG C of the present invention; Step 4) substrate heating to 600 DEG C; The throughput ratio of trimethyl indium and nitrogen is 4:180; The control total pressure of gas is 1.5Pa; Electron cyclotron resonace reaction 3h.
As another kind of preferred version, step 3) substrate heating to 200 DEG C of the present invention; Step 4) substrate heating to 300 DEG C; The throughput ratio of trimethyl indium and nitrogen is 4:100; The control total pressure of gas is 1.8Pa; Electron cyclotron resonace reaction 30min.
As another kind of preferred version, step 3) substrate heating to 300 DEG C of the present invention; Step 4) substrate heating to 500 DEG C; The throughput ratio of trimethyl indium and nitrogen is 5:180; The control total pressure of gas is 1.6Pa; Electron cyclotron resonace reaction 60min.
Secondly, step 3) substrate heating to 500 DEG C of the present invention; Step 4) substrate heating to 600 DEG C; The throughput ratio of trimethyl indium and nitrogen is 4:120; The control total pressure of gas is 1.5Pa; Electron cyclotron resonace reaction 70min.
In addition, step 3) substrate heating to 600 DEG C of the present invention; Step 4) substrate heating to 700 DEG C; The throughput ratio of trimethyl indium and nitrogen is 4:150; The control total pressure of gas is 1.8Pa; Electron cyclotron resonace reaction 90min.
The useful effect of the present invention.
The present invention deposited on Si by HF CVD system before this and prepared diamond (diamond possesses very high thermal conductivity and excellent thermotolerance) thick film, recycling can accurately control the ECR-PEMOCVD technology of low temperature depositing, and the correlation parameter in reaction process and material are selected, set, thus low temperature depositing prepares high-quality InN optoelectronic film on GaN buffer layer/diamond thin/Si multi-layer film structure substrate, cost is very low. In addition, the InN optoelectronic film product on GaN buffer layer/diamond thin/Si multi-layer film structure substrate of the present invention has good electric property and heat dispersion after tested, is easy to prepare the high-power device of high frequency. Secondly, GaN and InN has similar crystalline structure, as the buffer layer between InN and diamond, well solves between InN epitaxial film and glass substrate the lattice mismatch issue existed.
Accompanying drawing explanation
Below in conjunction with the drawings and specific embodiments, the present invention will be further described. Protection domain of the present invention is not only confined to the statement of following content.
Fig. 1 is the X ray diffracting spectrum of GaN/ diamond thin/Si multi-layer film structure.
Fig. 2 is the image of the atomic force microscope (AFM) of example 1 film sample.
Fig. 3 is the XRD analysis collection of illustrative plates of InN/GaN/ diamond thin/Si multi-layer film structure.
Fig. 4 is InN/GaN buffer layer/diamond thin/Si structural membrane schematic diagram that the inventive method obtains.
In Fig. 4,1 is Si substrate, and 2 is diamond thin, and 3 is GaN buffer layer thin film, and 4 is InN sample thin film.
Embodiment
The present invention comprises the following steps.
1) by Si substrate successively with, after acetone, ethanol and deionized water ultrasonic cleaning, blowing dry feeding reaction chamber with nitrogen.
2) use HF CVD system, reaction chamber is vacuumized, by Si substrate heating, lead in reaction chamber into hydrogen and methane gas, Si substrate base obtains diamond thin.
3) adopt ECR-PEMOCVD(electron cyclotron resonace-plasma reinforcing and metal organic chemical vapor deposition) system, reaction chamber is vacuumized, by substrate heating to 200��600 DEG C, lead in reaction chamber carry into hydrogen trimethyl-gallium, nitrogen; The control total pressure of gas, electron cyclotron resonace reacts, and obtains the GaN buffer layer thin film on the Si substrate of gold-plated diamond thin film.
4) continue to adopt ECR-PEMOCVD system, reaction chamber vacuumized, by substrate heating to 300��700 DEG C, lead in reaction chamber carry into hydrogen trimethyl indium, nitrogen, throughput ratio both it is (4��5): (100��180); The control total pressure of gas is 1.5��1.8Pa; Electron cyclotron resonace reaction 30min��3h, obtains the InN optoelectronic film on GaN buffer layer/diamond thin/Si structure substrate.
The purity of the purity of described trimethyl indium, the purity of trimethyl-gallium and nitrogen is 99.99%.
The thickness (free standing diamond thickness) of described diamond thin is 300nm.
Described step 1) ultrasonic cleaning 5 minutes; Step 2) it is evacuated to 1.0 �� 10
-2
Pa; Substrate heating to 800 DEG C; Hydrogen and methane gas flow are respectively 200sccm and 4sccm, by mass flowmeter control; Heated filament voltage is 10V, and heater current is 50A, reaction 30min.
Described step 3) is evacuated to 8.0 �� 10
-4
Pa; The flow of trimethyl-gallium and nitrogen is respectively 0.5sccm and 100sccm, by mass flowmeter control; The control total pressure of gas is 1.2Pa; Electron cyclotron resonace power is 650W, reaction 60min; Step 4) reaction chamber is evacuated to 9.0 �� 10
-4
Pa; The flow of trimethyl indium, nitrogen is by mass flowmeter control; Electron cyclotron resonace power is 650W.
Described step 3) substrate heating to 400 DEG C; Step 4) substrate heating to 600 DEG C; The throughput ratio of trimethyl indium and nitrogen is 4:180; The control total pressure of gas is 1.5Pa; Electron cyclotron resonace reaction 3h.
Described step 3) substrate heating to 200 DEG C; Step 4) substrate heating to 300 DEG C; The throughput ratio of trimethyl indium and nitrogen is 4:100; The control total pressure of gas is 1.8Pa; Electron cyclotron resonace reaction 30min.
Described step 3) substrate heating to 300 DEG C; Step 4) substrate heating to 500 DEG C; The throughput ratio of trimethyl indium and nitrogen is 5:180; The control total pressure of gas is 1.6Pa; Electron cyclotron resonace reaction 60min.
Described step 3) substrate heating to 500 DEG C; Step 4) substrate heating to 600 DEG C; The throughput ratio of trimethyl indium and nitrogen is 4:120; The control total pressure of gas is 1.5Pa; Electron cyclotron resonace reaction 70min.
Described step 3) substrate heating to 600 DEG C; Step 4) substrate heating to 700 DEG C; The throughput ratio of trimethyl indium and nitrogen is 4:150; The control total pressure of gas is 1.8Pa; Electron cyclotron resonace reaction 90min.
Embodiment 1.
Si substrate after 5 minutes, is blown dry feeding reaction chamber with nitrogen by acetone, ethanol and deionized water ultrasonic cleaning successively; Use HF CVD system, reaction chamber is evacuated to 1.0 �� 10
-2
Pa, by substrate heating to 800 DEG C, leads to into hydrogen and methane gas in reaction chamber, and flow both it is hydrogen be 200sccm and methane is 4sccm, by mass flowmeter control; Heated filament voltage is 10V, and heater current is 50A, and reaction 30min, obtains diamond thin on Si substrate base. Adopt ECR-PEMOCVD system, reaction chamber is evacuated to 8.0 �� 10
-4
Pa, by substrate heating to 400 DEG C, lead in reaction chamber carry into hydrogen trimethyl-gallium, nitrogen, both it, flow is respectively 0.5sccm and 100sccm, by mass flowmeter control; The control total pressure of gas is 1.2Pa; Being 650W in electron cyclotron resonance frequency, reaction 60min, obtains the GaN buffer layer thin film on the Si substrate of gold-plated diamond thin film. Continue to adopt ECR-PEMOCVD system, reaction chamber is evacuated to 9.0 �� 10
-4
Pa, by substrate heating to 600 DEG C, lead in reaction chamber carry into hydrogen trimethyl indium, nitrogen, throughput ratio both it is 4:180, by mass flowmeter control; The control total pressure of gas is 1.5Pa; Being 650W in electron cyclotron resonance frequency, reaction 3h, obtains the InN optoelectronic film on GaN buffer layer/diamond thin/Si structure substrate.
Sample thin film has been carried out as atomic force microscope detection is analyzed after terminating by experiment, and Fig. 2 is analytical test result, shows that InN film has good surface topography, and surfaceness is lower. As shown in Figure 3, its result shows that InN optoelectronic film prepared by reactive deposition has good preferred orientation structure, and InN film has good crystalline quality in the analysis of X-ray diffraction. Test result illustrates that its InN film sample meets high frequency, and high power device is to the requirement of film quality.
Embodiment 2.
Si substrate after 5 minutes, is blown dry feeding reaction chamber with nitrogen by acetone, ethanol and deionized water ultrasonic cleaning successively; Use HF CVD system, reaction chamber is evacuated to 1.0 �� 10
-2
Pa, by substrate heating to 800 DEG C, leads to into hydrogen and methane gas in reaction chamber, and flow both it is hydrogen be 200sccm and methane is 4sccm, by mass flowmeter control; Heated filament voltage is 10V, and heater current is 50A, and reaction 30min, obtains diamond thin on Si substrate base. Adopt ECR-PEMOCVD system, reaction chamber is evacuated to 8.0 �� 10
-4
Pa, by substrate heating to 200 DEG C, lead in reaction chamber carry into hydrogen trimethyl-gallium, nitrogen, both it, flow is respectively 0.5sccm and 100sccm, by mass flowmeter control; The control total pressure of gas is 1.2Pa; Being 650W in electron cyclotron resonance frequency, reaction 60min, obtains the GaN buffer layer thin film on the Si substrate of gold-plated diamond thin film. Continue to adopt ECR-PEMOCVD system, reaction chamber is evacuated to 9.0 �� 10
-4
Pa, by substrate heating to 300 DEG C, lead in reaction chamber carry into hydrogen trimethyl indium, nitrogen, throughput ratio both it is 4:100, by mass flowmeter control; The control total pressure of gas is 1.8Pa; Being 650W in electron cyclotron resonance frequency, reaction 30min, obtains the InN optoelectronic film on GaN buffer layer/diamond thin/Si structure substrate. Sample thin film is carried out test analysis after terminating by experiment, and analytical test result shows that InN film has excellent performance, meets high frequency, and high power device is to the requirement of film quality.
Embodiment 3.
Si substrate after 5 minutes, is blown dry feeding reaction chamber with nitrogen by acetone, ethanol and deionized water ultrasonic cleaning successively; Use HF CVD system, reaction chamber is evacuated to 1.0 �� 10
-2
Pa, by substrate heating to 800 DEG C, leads to into hydrogen and methane gas in reaction chamber, and flow both it is hydrogen be 200sccm and methane is 4sccm, by mass flowmeter control; Heated filament voltage is 10V, and heater current is 50A, and reaction 30min, obtains diamond thin on Si substrate base. Adopt ECR-PEMOCVD system, reaction chamber is evacuated to 8.0 �� 10
-4
Pa, by substrate heating to 300 DEG C, lead in reaction chamber carry into hydrogen trimethyl-gallium, nitrogen, both it, flow is respectively 0.5sccm and 100sccm, by mass flowmeter control; The control total pressure of gas is 1.2Pa; Being 650W in electron cyclotron resonance frequency, reaction 60min, obtains the GaN buffer layer thin film on the Si substrate of gold-plated diamond thin film. Continue to adopt ECR-PEMOCVD system, reaction chamber is evacuated to 9.0 �� 10
-4
Pa, by substrate heating to 500 DEG C, lead in reaction chamber carry into hydrogen trimethyl indium, nitrogen, throughput ratio both it is 5:180, by mass flowmeter control; The control total pressure of gas is 1.6Pa; Being 650W in electron cyclotron resonance frequency, reaction 60min, obtains the InN optoelectronic film on GaN buffer layer/diamond thin/Si structure substrate. Sample thin film is carried out test analysis after terminating by experiment, and analytical test result shows that InN film has excellent performance, meets high frequency, and high power device is to the requirement of film quality.
Embodiment 4.
Si substrate after 5 minutes, is blown dry feeding reaction chamber with nitrogen by acetone, ethanol and deionized water ultrasonic cleaning successively; Use HF CVD system, reaction chamber is evacuated to 1.0 �� 10
-2
Pa, by substrate heating to 800 DEG C, leads to into hydrogen and methane gas in reaction chamber, and flow both it is hydrogen be 200sccm and methane is 4sccm, by mass flowmeter control; Heated filament voltage is 10V, and heater current is 50A, and reaction 30min, obtains diamond thin on Si substrate base. Adopt ECR-PEMOCVD system, reaction chamber is evacuated to 8.0 �� 10
-4
Pa, by substrate heating to 500 DEG C, lead in reaction chamber carry into hydrogen trimethyl-gallium, nitrogen, both it, flow is respectively 0.5sccm and 100sccm, by mass flowmeter control; The control total pressure of gas is 1.2Pa; Being 650W in electron cyclotron resonance frequency, reaction 60min, obtains the GaN buffer layer thin film on the Si substrate of gold-plated diamond thin film. Continue to adopt ECR-PEMOCVD system, reaction chamber is evacuated to 9.0 �� 10
-4
Pa, by substrate heating to 600 DEG C, lead in reaction chamber carry into hydrogen trimethyl indium, nitrogen, throughput ratio both it is 4:120, by mass flowmeter control; The control total pressure of gas is 1.5Pa; Being 650W in electron cyclotron resonance frequency, reaction 70min, obtains the InN optoelectronic film on GaN buffer layer/diamond thin/Si structure substrate. Sample thin film is carried out test analysis after terminating by experiment, and analytical test result shows that InN film has excellent performance, meets high frequency, and high power device is to the requirement of film quality.
Embodiment 5.
Si substrate after 5 minutes, is blown dry feeding reaction chamber with nitrogen by acetone, ethanol and deionized water ultrasonic cleaning successively; Use HF CVD system, reaction chamber is evacuated to 1.0 �� 10
-2
Pa, by substrate heating to 800 DEG C, leads to into hydrogen and methane gas in reaction chamber, and flow both it is hydrogen be 200sccm and methane is 4sccm, by mass flowmeter control; Heated filament voltage is 10V, and heater current is 50A, and reaction 30min, obtains diamond thin on Si substrate base. Adopt ECR-PEMOCVD system, reaction chamber is evacuated to 8.0 �� 10
-4
Pa, by substrate heating to 600 DEG C, lead in reaction chamber carry into hydrogen trimethyl-gallium, nitrogen, both it, flow is respectively 0.5sccm and 100sccm, by mass flowmeter control; The control total pressure of gas is 1.2Pa; Being 650W in electron cyclotron resonance frequency, reaction 60min, obtains the GaN buffer layer thin film on the Si substrate of gold-plated diamond thin film. Continue to adopt ECR-PEMOCVD system, reaction chamber is evacuated to 9.0 �� 10
-4
Pa, by substrate heating to 700 DEG C, lead in reaction chamber carry into hydrogen trimethyl indium, nitrogen, throughput ratio both it is 4:150, by mass flowmeter control; The control total pressure of gas is 1.8Pa; Being 650W in electron cyclotron resonance frequency, reaction 90min, obtains the InN optoelectronic film on GaN buffer layer/diamond thin/Si structure substrate. Sample thin film is carried out test analysis after terminating by experiment, and analytical test result shows that InN film has excellent performance, meets high frequency, and high power device is to the requirement of film quality.
As shown in Figure 1, diamond thin is polycrystalline, has preferred orientation, and quality is good, and GaN buffer layer crystal property is good, meet InN film to the requirement of diamond thin thermal diffusivity and lattice match.
The model of X-ray diffraction analysis instrument used is: model BrukerAXSD8.
The model of the atomic force microscope (AFM) that the present invention utilizes is Picoscan2500, originates in Agilent company. Under the test condition of normal room temperature, the shape looks of film sample are carried out testing and analyzing. The test analysis region of sample is
��
It is understandable that, above about the specific descriptions of the present invention, the technical scheme described by the embodiment of the present invention only not it is limited to for illustration of the present invention, it will be understood by those within the art that, still the present invention can be modified or equivalent replace, to reach identical technique effect; Needs are used, all within protection scope of the present invention as long as meeting.
Claims (1)
- The preparation method of 1.ECR-PEMOCVD low temperature depositing InN film on GaN buffer layer/diamond thin/Si multi-layer film structure substrate, it is characterised in that comprise the following steps:1) by Si substrate successively with, after acetone, ethanol and deionized water ultrasonic cleaning, blowing dry feeding reaction chamber with nitrogen;2) use HF CVD system, reaction chamber is vacuumized, by Si substrate heating, lead in reaction chamber into hydrogen and methane gas, Si substrate base obtains diamond thin;3) adopt ECR-PEMOCVD system, reaction chamber vacuumized, by substrate heating to 400 DEG C, lead in reaction chamber carry into hydrogen trimethyl-gallium, nitrogen; The control total pressure of gas, electron cyclotron resonace reacts, and obtains the GaN buffer layer thin film on the Si substrate of gold-plated diamond thin film;4) continue to adopt ECR-PEMOCVD system, reaction chamber vacuumized, by substrate heating to 600 DEG C, lead in reaction chamber carry into hydrogen trimethyl indium, nitrogen, throughput ratio both it is 4:180; The control total pressure of gas is 1.5Pa; Electron cyclotron resonace reaction 3h, obtains the InN optoelectronic film on GaN buffer layer/diamond thin/Si structure substrate;The purity of the purity of described trimethyl indium, the purity of trimethyl-gallium and nitrogen is 99.99%;The thickness of described diamond thin is 300nm;Described step 3) is evacuated to 8.0 �� 10-4Pa; The flow of trimethyl-gallium and nitrogen is respectively 0.5sccm and 100sccm, by mass flowmeter control; The control total pressure of gas is 1.2Pa; Electron cyclotron resonace power is 650W, reaction 60min; Step 4) reaction chamber is evacuated to 9.0 �� 10-4Pa; The flow of trimethyl indium, nitrogen is by mass flowmeter control; Electron cyclotron resonace power is 650W;Described step 1) ultrasonic cleaning 5 minutes; Step 2) it is evacuated to 1.0 �� 10-2Pa; Substrate heating to 800 DEG C; Hydrogen and methane gas flow are respectively 200sccm and 4sccm, by mass flowmeter control; Heated filament voltage is 10V, and heater current is 50A, reaction 30min.
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| "GaN薄膜低温外延的ECR-PAMOCVD技术";徐茵等;《半导体技术》;19980228;第23卷(第1期);第37-39页 * |
| "基于ECR-PEMOCVD技术在蓝宝石衬底上高C轴择优的InN薄膜的制备及表征";周志峰;《中国优秀硕士学位论文全文数据库 信息科技辑》;20120715(第7期);第1、8、9、22、23、30和37页 * |
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Inventor after: Zhang Dong Inventor after: Wang Cunxu Inventor after: Song Shiwei Inventor after: Wang Jian Inventor after: Wang Gang Inventor after: Li Yucai Inventor before: Wang Cunxu Inventor before: Wang Shenghui Inventor before: Sun Xiaoyu Inventor before: Zhang Hongli Inventor before: Wang Xiaowen Inventor before: Xu Jian Inventor before: Li Naizhong Inventor before: Zhang Yuyan Inventor before: Wang Gang Inventor before: Du Shipeng |
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Effective date of registration: 20170303 Address after: 114017 Tiexi, Liaoning Province, South Road, prosperity in the south of the road,, 29 Patentee after: Liaoning Zhongcheng New Energy Development Co. Ltd. Address before: Shenbei New Area Puchang road Shenyang City, Liaoning province 110136 No. 18 Patentee before: Shenyang Engineering College |