CN108987257A - Ga is grown on a si substrate using halide vapor phase epitaxy2O3The method of film - Google Patents
Ga is grown on a si substrate using halide vapor phase epitaxy2O3The method of film Download PDFInfo
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Abstract
Ga is grown on a si substrate using halide vapor phase epitaxy the invention discloses a kind of2O3The method of film, warm area I, the Si substrate that the source metal Ga is placed in reactor are placed in the warm area II of reactor, and warm area I temperature rises to 850-950 DEG C under nitrogen atmosphere, and warm area II temperature rises to 300-1100 DEG C；After temperature is stablized, while being passed through HCl and O2, start to grow Ga2O3Film layer；Cool down after growth, takes out sample.The method of the present invention can grow good Ga on a si substrate2O3Film controls warm area II temperature, the Ga of different crystal forms can be obtained2O3.Most of semiconductor devices is all based on Si substrate at present, it is easy to accomplish the electronic device of the upper gallium oxide of Si and integrating for existing device.
Description
Technical field
Ga is grown on a si substrate using halide vapor phase epitaxy the present invention relates to a kind of2O3The method of film.
Background technique
Gallium oxide single crystal is direct band gap oxide semiconductor, and forbidden bandwidth is 4.8~4.9eV, is equivalent to 4 times of silicon
More than, or even more taller than silicon carbide (3.3eV), gallium nitride (3.4eV), referred to as forth generation ultra-wide bandgap semiconductor.Oxidation
Algan single crystal has a variety of crystal forms, wherein with β-Ga2O3It is the most stable.Gallium oxide has unique UV transmission characteristic, and (ABSORPTION EDGE can
To arrive 250nm)；Breakdown field strength is up to 8MV/cm, is nearly 27 times, third generation semiconductor carbon of first generation semiconductor silicon (Si)
The 2 times or more of SiClx (SiC) and gallium nitride (GaN)；The index Bali of the low-loss of left and right power semiconductor performance adds the figure of merit
(Baliga figure-of-merit) be approximately 10 times of silicon carbide, 4 times of gallium nitride, this figure of merit is directly proportional to the cube of breakdown electric field；
Under identical breakdown voltage, Ga2O3The conducting resistance ratio SiC of base device 1 order of magnitude low with GaN base device.Comprehensive physical
The advantage of characteristic, hetero-epitaxy, energy band tailoring and device structure design etc. is pushed away with as power semiconductor material of new generation
SiC (silicon carbide) and GaN (gallium nitride) into exploitation are compared, β-Ga2O3Have become the low-loss power device of super-pressure and dark purple
One of the preferred material of outer opto-electronic device, suitable for manufacturing the high-power vertical structure power device of high current density.
β-Ga2O3Single crystalline substrate can be used czochralski method (Cz DEG C of hralski, CZ), float-zone method (floating zone, FZ) and
The melt growths methods such as guided membrane method (edge-defined film-fed growth, EFG) method.Melt growth method is easy preparation crystallization
The single crystals that defect is few, diameter is big, advantage of lower cost.But monocrystalline melt method for growing high quality β-Ga2O3, for thermal field temperature
It is very high to spend the requirements such as distribution, oxidizing atmosphere, air pressure, it is necessary to which effective accuracy controlling is carried out to growth course.Simultaneously as under high temperature
Ga2O3It is easy to decompose, generates GaO, Ga2O, the products such as Ga, volatilization is serious and corrosion noble metal crucible, and its be easy to generate it is more
The problems such as crystals growth, contraction crystalline substance, mosaic texture, helical dislocation, cracking, therefore growing large-size, high quality β-Ga2O3Monocrystalline is extremely tired
It is difficult.In addition, the gallium oxide single crystal of melt method for growing, device could be used for by needing to carry out the techniques such as crystal orientation, cutting and polishing
Extension etc., and the cutting of gallium oxide and polishing are very easy to cause chip fragmentation.
Melt method for growing gallium oxide single crystal face large scale and it is easy to crack etc. difficult in the case where, using other thick films
Growing technology prepares gallium oxide quasi- monocrystalline material and is just provided with very important meaning.Hydride vapour phase epitaxy method is for preparing
The mature technology of third generation semiconductor gallium nitride (GaN) substrate, has been used successfully to the growth of large-size high-quality GaN substrate,
Growth rate height (reachable hundreds of microns/more than hour).The major advantage of HVPE technology includes that equipment is relatively easy, working service
Convenient, the quality of materials of growth is high, and growth rate is fast, thick film is easily obtained, without grown buffer layer etc..In addition to this, HVPE
Method growth can be also used for the extension etc. of the doping regulation and power electronic device structure in situ of gallium oxide.
The invention proposes a kind of, and to grow gallium oxide on the Si substrate of various sizes using halide vapor phase epitaxy thin
The methods and techniques of film, especially direct extension gallium oxide film and the method using buffer layer technique.Using raw on Si substrate
Long gallium oxide film has the advantage that most of semiconductor devices is all based on Si substrate at present, it is easy to accomplish the upper oxygen of Si
Change the electronic device of gallium and integrating for existing device.
Summary of the invention
It is grown on the Si substrate of various sizes the purpose of the present invention is to provide a kind of using halide vapor phase epitaxy
The methods and techniques of gallium oxide film.
The purpose of the present invention is achieved through the following technical solutions:
It is a kind of to grow Ga on a si substrate using halide vapor phase epitaxy2O3The method of film, step include:
1) cleaning treatment Si substrate；
2) warm area I, the Si substrate that the source metal Ga is placed in reactor is placed in the warm area II of reactor, warm area I under nitrogen atmosphere
Temperature rises to 850-950 DEG C, and warm area II temperature rises to 300-1100 DEG C；
3) after temperature is stablized, while HCl and O being passed through2, start to grow Ga2O3Film layer；
4) cool down after growing, take out sample.
Preferably, step 1) is specially that Si substrate successively uses acetone, ethyl alcohol, deionized water ultrasonic cleaning, then High Purity Nitrogen
Air-blowing is dry.
Preferably, growth time is 30-300min in step 3).
Preferably, O in step 3)2Flow is 50sccm, O2Carrier gas flux is 500sccm, and HCl flow is 15sccm, HCl
Carrier gas flux is 200sccm, O2Carrier gas and HCl carrier gas are nitrogen, and total nitrogen flow is 10000sccm.
It is a kind of to grow Ga on a si substrate using halide vapor phase epitaxy2O3The method of film, step include:
1) cleaning treatment Si substrate；
2) warm area I, the Si substrate that the source metal Ga is placed in reactor is placed in the warm area II of reactor, warm area I under nitrogen atmosphere
Temperature rises to 850-950 DEG C, and warm area II temperature rises to 300-500 DEG C；
3) after temperature is stablized, while HCl and O being passed through2, start to grow Ga2O3Buffer layer；
4) after buffer growth, maintenance warm area I is temperature-resistant, oxygen atmosphere is constant, and warm area II temperature is increased to
500-1100 DEG C, continue to be passed through HCl and O2Grow Ga2O3Film layer；
5) cool down after growing, take out sample.
Preferably, step 1) is specially that Si substrate successively uses acetone, ethyl alcohol, deionized water ultrasonic cleaning, then High Purity Nitrogen
Air-blowing is dry.
Preferably, growth time is 50-300 seconds in step 3), O2Flow is 50sccm, O2Carrier gas flux is 500sccm,
HCl flow is 10sccm, and HCl carrier gas flux is 200sccm, O2Carrier gas and HCl carrier gas are nitrogen, and total nitrogen flow is
5000sccm。
Preferably, growth time is 30-300min, O in step 4)2Flow is 50sccm, O2Carrier gas flux is 500sccm,
HCl flow is 15sccm, and HCl carrier gas flux is 200sccm, O2Carrier gas and HCl carrier gas are nitrogen, and total nitrogen flow is
10000sccm。
Mechanism of the invention is: generating GaCl in warm area I gallium and HCl reaction, GaCl is reached under the carrying of carrier gas
Warm area II reacts with oxygen and generates Ga2O3, Ga2O3On a silicon substrate, carrier gas generally uses nitrogen to deposition.Warm area I temperature range
It is 950-850 DEG C, 300-1100 DEG C of temperature range of warm area II, warm area II temperature is at 850 DEG C or more, the Ga of growth2O3Predominantly
β-Ga2O3；500-800 DEG C of temperature, the Ga of growth2O3Predominantly ε-Ga2O3；400-500 DEG C of temperature, the Ga of growth2O3Predominantly α-
Ga2O3；300-400 DEG C of temperature, the Ga of growth2O3Predominantly γ-Ga2O3.Key reaction is as follows:
HCl+Ga→GaCl+H2Warm area I
GaCl+O2→Ga2O3+Cl2Warm area II
The method of the present invention can grow good Ga on a si substrate2O3Film controls warm area II temperature, can be obtained
The Ga of different crystal forms2O3.Most of semiconductor devices is all based on Si substrate at present, it is easy to accomplish the electronics of the upper gallium oxide of Si
Device is integrated with existing device.
Detailed description of the invention
The XRD diffraction pattern for the gallium oxide film that Fig. 1 halide gas phase epitaxy method is grown on a silicon substrate.
The Raman for the gallium oxide film that Fig. 2 halide gas phase epitaxy method is grown on a silicon substrate is composed.
Specific embodiment
Embodiment 1:
It is a kind of to grow Ga on a si substrate using halide vapor phase epitaxy2O3The method of film, step include:
1) Si substrate successively uses acetone, ethyl alcohol, deionized water ultrasonic cleaning, and then high pure nitrogen dries up；
2) warm area I, the Si substrate that the source metal Ga is placed in reactor is placed in the warm area II of reactor, warm area I under nitrogen atmosphere
Temperature rises to 850 DEG C, and warm area II temperature rises to 1050 DEG C；
3) after temperature is stablized, while HCl and O being passed through2, start to grow Ga2O3Film layer, O2Flow is 50sccm, O2It carries
Throughput is 500sccm, and HCl flow is 15sccm, and HCl carrier gas flux is 200sccm, O2Carrier gas and HCl carrier gas are nitrogen, always
Nitrogen flow is 10000sccm, growth time 30min；
4) cool down after growing, take out sample.The XRD diffraction pattern of sample is shown in Fig. 1, and Raman spectrum is shown in Fig. 2.In sample
Ga2O3Film layer crystal form is β-Ga2O3。
Embodiment 2:
It is a kind of to grow Ga on a si substrate using halide vapor phase epitaxy2O3The method of film, step include:
1) Si substrate successively uses acetone, ethyl alcohol, deionized water ultrasonic cleaning, and then high pure nitrogen dries up；
2) warm area I, the Si substrate that the source metal Ga is placed in reactor is placed in the warm area II of reactor, warm area I under nitrogen atmosphere
Temperature rises to 950 DEG C, and warm area II temperature rises to 1100 DEG C；
3) after temperature is stablized, while HCl and O being passed through2, start to grow Ga2O3Film layer, O2Flow is 50sccm, O2It carries
Throughput is 500sccm, and HCl flow is 15sccm, and HCl carrier gas flux is 200sccm, O2Carrier gas and HCl carrier gas are nitrogen, always
Nitrogen flow is 10000sccm, growth time 60min；
4) cool down after growing, take out sample.Ga in sample2O3Film layer crystal form is β-Ga2O3。
Embodiment 3:
It is a kind of to grow Ga on a si substrate using halide vapor phase epitaxy2O3The method of film, step include:
1) Si substrate successively uses acetone, ethyl alcohol, deionized water ultrasonic cleaning, and then high pure nitrogen dries up；
2) warm area I, the Si substrate that the source metal Ga is placed in reactor is placed in the warm area II of reactor, warm area I under nitrogen atmosphere
Temperature rises to 900 DEG C, and warm area II temperature rises to 700 DEG C；
3) after temperature is stablized, while HCl and O being passed through2, start to grow Ga2O3Film layer, O2Flow is 50sccm, O2It carries
Throughput is 500sccm, and HCl flow is 15sccm, and HCl carrier gas flux is 200sccm, O2Carrier gas and HCl carrier gas are nitrogen, always
Nitrogen flow is 10000sccm, growth time 300min；
4) cool down after growing, take out sample.Ga in sample2O3Film layer crystal form is ε-Ga2O3。
Embodiment 4:
It is a kind of to grow Ga on a si substrate using halide vapor phase epitaxy2O3The method of film, step include:
1) Si substrate successively uses acetone, ethyl alcohol, deionized water ultrasonic cleaning, and then high pure nitrogen dries up；
2) warm area I, the Si substrate that the source metal Ga is placed in reactor is placed in the warm area II of reactor, warm area I under nitrogen atmosphere
Temperature rises to 850 DEG C, and warm area II temperature rises to 400-500 DEG C；
3) after temperature is stablized, while HCl and O being passed through2, start to grow Ga2O3Film layer, growth time are 100 seconds, O2
Flow is 50sccm, O2Carrier gas flux is 500sccm, and HCl flow is 10sccm, and HCl carrier gas flux is 200sccm, O2Carrier gas and
HCl carrier gas is nitrogen, and total nitrogen flow is 5000sccm；
4) cool down after growing, take out sample.Ga in sample2O3Film layer crystal form is α-Ga2O3。
Embodiment 5:
It is a kind of to grow Ga on a si substrate using halide vapor phase epitaxy2O3The method of film, step include:
1) Si substrate successively uses acetone, ethyl alcohol, deionized water ultrasonic cleaning, and then high pure nitrogen dries up；
2) warm area I, the Si substrate that the source metal Ga is placed in reactor is placed in the warm area II of reactor, warm area I under nitrogen atmosphere
Temperature rises to 950 DEG C, and warm area II temperature rises to 300-400 DEG C；
3) after temperature is stablized, while HCl and O being passed through2, start to grow Ga2O3Film layer, growth time are 30 seconds, O2Stream
Amount is 50sccm, O2Carrier gas flux is 500sccm, and HCl flow is 10sccm, and HCl carrier gas flux is 200sccm, O2Carrier gas and
HCl carrier gas is nitrogen, and total nitrogen flow is 5000sccm；
4) cool down after growing, take out sample.Ga in sample2O3Film layer crystal form is γ-Ga2O3。
Embodiment 6:
It is a kind of to grow Ga on a si substrate using halide vapor phase epitaxy2O3The method of film, step include:
1) Si substrate successively uses acetone, ethyl alcohol, deionized water ultrasonic cleaning, and then high pure nitrogen dries up；
2) warm area I, the Si substrate that the source metal Ga is placed in reactor is placed in the warm area II of reactor, warm area I under nitrogen atmosphere
Temperature rises to 900 DEG C, and warm area II temperature rises to 500 DEG C；
3) after temperature is stablized, while HCl and O being passed through2, start to grow Ga2O3Buffer layer, growth time are 300 seconds, O2
Flow is 50sccm, O2Carrier gas flux is 500sccm, and HCl flow is 10sccm, and HCl carrier gas flux is 200sccm, O2Carrier gas and
HCl carrier gas is nitrogen, and total nitrogen flow is 5000sccm；
4) after buffer growth, maintenance warm area I is temperature-resistant, oxygen atmosphere is constant, and warm area II temperature is increased to
1100 DEG C, continue to be passed through HCl and O2Grow Ga2O3Film layer, growth time 300min, O2Flow is 50sccm, O2Carrier gas stream
Amount is 500sccm, and HCl flow is 15sccm, and HCl carrier gas flux is 200sccm, O2Carrier gas and HCl carrier gas are nitrogen, total nitrogen
Flow is 10000sccm；
5) cool down after growing, take out sample.Ga in sample2O3Film layer crystal form is β-Ga2O3。
Embodiment 7:
It is a kind of to grow Ga on a si substrate using halide vapor phase epitaxy2O3The method of film, step include:
1) Si substrate successively uses acetone, ethyl alcohol, deionized water ultrasonic cleaning, and then high pure nitrogen dries up；
2) warm area I, the Si substrate that the source metal Ga is placed in reactor is placed in the warm area II of reactor, warm area I under nitrogen atmosphere
Temperature rises to 850 DEG C, and warm area II temperature rises to 300-400 DEG C；
3) after temperature is stablized, while HCl and O being passed through2, start to grow Ga2O3Buffer layer, growth time are 300 seconds, O2
Flow is 50sccm, O2Carrier gas flux is 500sccm, and HCl flow is 10sccm, and HCl carrier gas flux is 200sccm, O2Carrier gas and
HCl carrier gas is nitrogen, and total nitrogen flow is 5000sccm；
4) after buffer growth, maintenance warm area I is temperature-resistant, oxygen atmosphere is constant, and warm area II temperature is increased to
500-600 DEG C, continue to be passed through HCl and O2Grow Ga2O3Film layer, growth time 300min, O2Flow is 50sccm, O2Carrier gas
Flow is 500sccm, and HCl flow is 15sccm, and HCl carrier gas flux is 200sccm, O2Carrier gas and HCl carrier gas are nitrogen, total nitrogen
Throughput is 10000sccm；
5) cool down after growing, take out sample.Ga in sample2O3Film layer crystal form is ε-Ga2O3。
Embodiment 8:
It is a kind of to grow Ga on a si substrate using halide vapor phase epitaxy2O3The method of film, step include:
1) Si substrate successively uses acetone, ethyl alcohol, deionized water ultrasonic cleaning, and then high pure nitrogen dries up；
2) warm area I, the Si substrate that the source metal Ga is placed in reactor is placed in the warm area II of reactor, warm area I under nitrogen atmosphere
Temperature rises to 950 DEG C, and warm area II temperature rises to 400-450 DEG C；
3) after temperature is stablized, while HCl and O being passed through2, start to grow Ga2O3Buffer layer, growth time are 300 seconds, O2
Flow is 50sccm, O2Carrier gas flux is 500sccm, and HCl flow is 10sccm, and HCl carrier gas flux is 200sccm, O2Carrier gas and
HCl carrier gas is nitrogen, and total nitrogen flow is 5000sccm；
4) after buffer growth, maintenance warm area I is temperature-resistant, oxygen atmosphere is constant, and warm area II temperature is increased to
850-900 DEG C, continue to be passed through HCl and O2Grow Ga2O3Film layer, growth time 300min, O2Flow is 50sccm, O2Carrier gas
Flow is 500sccm, and HCl flow is 15sccm, and HCl carrier gas flux is 200sccm, O2Carrier gas and HCl carrier gas are nitrogen, total nitrogen
Throughput is 10000sccm；
5) cool down after growing, take out sample.Ga in sample2O3Film layer crystal form is β-Ga2O3。
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (8)
1. a kind of grow Ga using halide vapor phase epitaxy on a si substrate2O3The method of film, step include:
1) cleaning treatment Si substrate；
2) warm area I, the Si substrate that the source metal Ga is placed in reactor is placed in the warm area II of reactor, warm area I temperature under nitrogen atmosphere
850-950 DEG C is risen to, warm area II temperature rises to 300-1100 DEG C；
3) after temperature is stablized, while HCl and O being passed through2, start to grow Ga2O3Film layer；
4) cool down after growing, take out sample.
2. according to claim 1 grow Ga using halide vapor phase epitaxy on a si substrate2O3The method of film,
Be characterized in that: step 1) is specially that Si substrate successively uses acetone, ethyl alcohol, deionized water ultrasonic cleaning, and then high pure nitrogen dries up.
3. according to claim 2 grow Ga using halide vapor phase epitaxy on a si substrate2O3The method of film,
Be characterized in that: growth time is 30-300min in step 3).
4. according to claim 3 grow Ga using halide vapor phase epitaxy on a si substrate2O3The method of film,
It is characterized in that: O in step 3)2Flow is 50sccm, O2Carrier gas flux is 500sccm, and HCl flow is 15sccm, HCl carrier gas stream
Amount is 200sccm, O2Carrier gas and HCl carrier gas are nitrogen, and total nitrogen flow is 10000sccm.
5. a kind of grow Ga using halide vapor phase epitaxy on a si substrate2O3The method of film, step include:
1) cleaning treatment Si substrate；
2) warm area I, the Si substrate that the source metal Ga is placed in reactor is placed in the warm area II of reactor, warm area I temperature under nitrogen atmosphere
850-950 DEG C is risen to, warm area II temperature rises to 300-500 DEG C；
3) after temperature is stablized, while HCl and O being passed through2, start to grow Ga2O3Buffer layer；
4) after buffer growth, maintenance warm area I is temperature-resistant, oxygen atmosphere is constant, and warm area II temperature is increased to 500-
1100 DEG C, continue to be passed through HCl and O2Grow Ga2O3Film layer；
5) cool down after growing, take out sample.
6. according to claim 5 grow Ga using halide vapor phase epitaxy on a si substrate2O3The method of film,
Be characterized in that: step 1) is specially that Si substrate successively uses acetone, ethyl alcohol, deionized water ultrasonic cleaning, and then high pure nitrogen dries up.
7. according to claim 6 grow Ga using halide vapor phase epitaxy on a si substrate2O3The method of film,
Be characterized in that: growth time is 50-300 seconds in step 3), O2Flow is 50sccm, O2Carrier gas flux is 500sccm, HCl flow
For 10sccm, HCl carrier gas flux is 200sccm, O2Carrier gas and HCl carrier gas are nitrogen, and total nitrogen flow is 5000sccm.
8. according to claim 7 grow Ga using halide vapor phase epitaxy on a si substrate2O3The method of film,
Be characterized in that: growth time is 30-300min, O in step 4)2Flow is 50sccm, O2Carrier gas flux is 500sccm, HCl stream
Amount is 15sccm, and HCl carrier gas flux is 200sccm, O2Carrier gas and HCl carrier gas are nitrogen, and total nitrogen flow is 10000sccm.
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| CN110085661A (en) * | 2019-04-23 | 2019-08-02 | 中山大学 | A kind of gallium oxide semiconductor laminated structure and preparation method thereof |
| CN110616456A (en) * | 2019-10-23 | 2019-12-27 | 南京大学 | Preparation method of high-quality kappa-phase gallium oxide epitaxial film |
| CN111663181A (en) * | 2020-05-20 | 2020-09-15 | 辛国庆 | Preparation method and application of gallium oxide film |
| WO2021048950A1 (en) * | 2019-09-11 | 2021-03-18 | 日本碍子株式会社 | Semiconductor film |
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