CN104962858A - GaAs substrate-based gallium oxide thin film and growing method thereof - Google Patents
GaAs substrate-based gallium oxide thin film and growing method thereof Download PDFInfo
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Abstract
The invention discloses a GaAs substrate-based gallium oxide thin film and a growing method thereof, and mainly solves the problems of poor surface appearance and small grain size of an existing gallium oxide thin film. The gallium oxide thin film comprises a GaAs substrate (1) and a gallium oxide epitaxial layer (3), and is characterized in that a gallium oxide buffer layer (2) of 6 to 12 nm is arranged between the GaAs substrate (1) and the gallium oxide epitaxial layer (3), and the crystal quality of the gallium oxide buffer layer is improved by utilizing thermal annealing. The surface roughness of a Ga2O3 thin film is reduced, the surface appearance of the Ga2O3 thin film is improved, and the Ga2O3 grain size is increased; the GaAs substrate-based gallium oxide thin film and the growing method can be used for making semiconductor power devices.
Description
Technical field
The invention belongs to microelectronics technology, relate to the growth method of semiconductor material, specifically a kind of Ga2O3 film manufacturing method, can be used for making semiconductor power device.
Background technology
, the characteristic such as breakdown electric field high, thermal conductivity high, saturated electrons speed large and heterojunction boundary two-dimensional electron gas high large with its energy gap with SiC and the GaN third generation semi-conductor that is representative, makes it be subject to extensive concern in recent years.Although third generation semiconductor materials and devices achieves great progress, and enters practical stage, due to SiC and GaN material exist many defects make its on a large scale in application be still very restricted.For this reason, on SiC and GaN material growth, device manufacture and the basis of applying, people are also in the deficiency that continuous searching itself has homo-substrate, excellent, the low-cost semiconductor material of material property can make up above-mentioned bi-material, and simultaneously wider, the breaking down field strength of energy gap is suitable for more greatly manufacturing power device.
Ga2O3 semiconductor material especially causes the interest of people, and Ga2O3 semiconductor material energy gap is large, and breaking down field strength is high, conducting resistance is little, can carry out iso-epitaxy, be that the best materials of power device development is selected.Ga2O3 belongs to monoclinic crystal, and energy gap is about 4.8eV-4.9eV.Obtained at present the Ga2O3 single crystalline substrate of 2 inches and 4 inches by float-zone method and EFG technique, can obtain that defect dislocation is few, crystalline network is relatively complete by the method for isoepitaxial growth Ga2O3 film in Ga2O3 single crystalline substrate, carrier concentration has been 10
17cm
-3~ 10
19cm
-3continually varying high-quality thin film, has excellent optical property and stable physico-chemical property, can be used for making high performance power electronic device, Ultraviolet sensor, day blind detector etc., be with a wide range of applications.
In order to can the advantage of better utilised material, people have carried out large quantifier elimination to the growth of Ga2O3 film.The growth method adopted mainly contains: pulsed laser deposition PLD, sol-gel method, chemical Vapor deposition process CVD, metal organic chemical vapor deposition MOCVD and magnetron sputtering method etc.
Pulsed laser deposition PLD is that the use range that development in recent years is got up is the widest, most promising masking technique.In simple terms, pulsed laser deposition PLD is exactly that pulsed laser beam focuses on solid target surface, and the superpower power of laser makes target material rapid plasma, and then sputter is on target compound.It has the following advantages: 1. because laser photon energy is very high, can the coating of a lot of difficulty of Slag coating: as high-temperature superconducting thin film, ceramic oxide film, multiple layer metal film etc.; PLD can be used for synthesis of nano pipe, nanometer powder etc.2.PLD can by controlling laser energy and umber of pulse, accurate control thickness.3. easily obtain the multi-component film expecting stoichiometric ratio.4. sedimentation rate is high, and the test period is short, and underlayer temperature requires low.5. processing parameter regulates arbitrarily.6. be convenient to clean, multiple thin-film material can be prepared.
But, current employing PLD deposits Ga2O3 film and all adopts single growth method, namely in process of growth, identical processing parameter is adopted, comprise oxygen pressure, laser energy, underlayer temperature etc. to grow, Ga2O3 film surface appearance that hetero epitaxy obtains is poor, grain-size is little to make to adopt PLD technology to carry out on gaas substrates.
Summary of the invention
The object of the invention is to the deficiency for above-mentioned existing pulsed laser deposition PLD, a kind of gallium oxide film based on GaAs substrate and growth method thereof are proposed, with by the adjustment of processing parameter and optimization, reduce roughness of film, improve Ga2O3 film surface appearance, obtain high-quality Ga2O3 semiconductor material with wide forbidden band.
Technical scheme of the present invention is achieved in that
The present invention is based on the gallium oxide film of GaAs substrate, comprise GaAs substrate and gallium oxide epitaxial film, it is characterized in that: the gallium oxide buffer layer being provided with 6-12nm between GaAs substrate and gallium oxide epitaxial film.
The present invention is based on the growth method of the gallium oxide film of GaAs substrate, comprise the steps:
(1) GaAs substrate is cleaned, and dry up with nitrogen;
(2) utilize PLD equipment to grow the gallium oxide buffer layer of 6-12nm on gaas substrates, its processing parameter is:
Underlayer temperature 625 DEG C ~ 700 DEG C,
Oxygen partial pressure 0.04mbar ~ 0.06mbar,
Laser energy 310mJ ~ 360mJ,
Laser frequency 2Hz ~ 4Hz.
(3) in oxygen atmosphere, thermal annealing is carried out to gallium oxide buffer layer;
(4) on gallium oxide buffer layer, grow gallium oxide epitaxial film, its processing parameter is:
Underlayer temperature 500 DEG C ~ 600 DEG C,
Oxygen partial pressure 0.009mbar ~ 0.02mbar,
Laser energy 420mJ ~ 460mJ,
Laser frequency 2Hz ~ 3Hz;
The present invention owing to being provided with Ga2O3 buffer layer between GaAs substrate and Ga2O3 epitaxial film, the fraction of coverage of reactant atom on substrate when improve Ga2O3 film initial growth, add seed crystal Enhancing Nucleation Density, simultaneously owing to heat-treating Ga2O3 buffer layer, improve the crystalline quality of buffer layer; In addition owing to being carried out the growth of Ga2O3 epitaxial film by the epitaxially grown processing parameter of adjustment, not only increase Ga2O3 grain-size, reduce roughness of film, and improve the surface topography of whole Ga2O3 film.
Accompanying drawing explanation
Fig. 1 is cross-sectional view of the present invention;
Fig. 2 is process flow diagram of the present invention.
Embodiment
With reference to Fig. 1, the present invention includes GaAs substrate 1, buffer layer 2 and epitaxial film 3.Wherein the high preferred orientation of GaAs substrate 1 is (001), and epitaxial film 3 adopts thickness to be the Ga2O3 material of 90-150nm, and buffer layer 2 adopts thickness to be the Ga2O3 material of 6-12nm, and between GaAs substrate 1 and epitaxial film 3.
With reference to Fig. 2, making method of the present invention provides following three kinds of embodiments:
Embodiment 1, makes the gallium oxide film that buffer layer thickness is 6nm.
Step 1, cleaning GaAs substrate.
(1.1) with toluene, acetone, ethanol and deionized water ultrasonic cleaning GaAs substrate 5min successively;
(1.2) ratio GaAs substrate being put into 60-70 DEG C is the sulfuric acid of 5:1:1, the mixing solutions of hydrogen peroxide and water soaks 1min;
(1.3) with deionized water, GaAs substrate is rinsed well, and dry up with N2.
Step 2, growth thickness is the gallium oxide buffer layer of 6nm.
(2.1) the GaAs substrate after cleaning is put into pulsed laser deposition PLD chamber, the vacuum tightness of pulsed laser deposition PLD chamber is extracted into 10
-6mbar, the distance between substrate and gallium oxide target is adjusted to 50mm, and the rotating speed of target keeps 30rpm;
(2.2) by GaAs silicon to 700 DEG C, in adjustment pulsed laser deposition PLD chamber, oxygen partial pressure is 0.04mbar, and arranging laser energy is 360mJ, and laser frequency is 2Hz, and pulse number is 900 growth Ga2O3 buffer layers;
(2.3) after buffer growth terminates, in pulsed laser deposition PLD chamber, be filled with the oxygen of 200mbar, then allow growth gallium oxide buffer layer thin film naturally cooling.
Step 3, carries out thermal annealing to gallium oxide buffer layer in oxygen atmosphere, and annealing temperature is 800 DEG C, annealing time 70min.
Step 4, growth thickness is the gallium oxide epitaxial film of 90nm.
(4.1) the gallium oxide buffer layer after thermal annealing is put into pulsed laser deposition PLD chamber, the vacuum tightness of chamber is extracted into 10
-6mbar, the distance between adjustment substrate and target is 50mm, and the rotating speed of target keeps 30rpm;
(4.2) the epitaxially grown processing parameter of pulsed laser deposition PLD is set: underlayer temperature 500 DEG C, oxygen partial pressure 0.02mbar, laser energy 460mJ, laser frequency 2Hz, pulse number 9000 epitaxy gallium oxide films of laser;
(4.3) be filled with the oxygen of 200mbar in the backward chamber that outer layer growth terminates, then allow gallium oxide epitaxial film film naturally cooling, completing gallium oxide buffer layer thickness is that the gallium oxide film of 6nm makes.
Embodiment 2, makes the gallium oxide film that buffer layer thickness is 12nm.
The first step, cleaning GaAs substrate.
This step is identical with the step 1 of embodiment 1.
Second step, growth thickness is the gallium oxide buffer layer of 12nm.
2.1) the GaAs substrate after cleaning is put into pulsed laser deposition PLD chamber, the vacuum tightness of pulsed laser deposition PLD chamber is extracted into 10
-6mbar, the distance between substrate and gallium oxide target is adjusted to 50mm, and the rotating speed of target keeps 30rpm;
2.2) by GaAs silicon to 625 DEG C, in adjustment pulsed laser deposition PLD chamber, oxygen partial pressure is 0.06mbar, and arranging laser energy is 310mJ, and laser frequency is 3Hz, and pulse number is 1500 growth Ga2O3 buffer layers;
2.3) after buffer growth terminates, in pulsed laser deposition PLD chamber, be filled with the oxygen of 200mbar, then allow growth gallium oxide buffer layer thin film naturally cooling.
3rd step, to gallium oxide buffer layer thermal annealing 60min at the temperature of 950 DEG C in oxygen atmosphere.
4th step, growth thickness is the gallium oxide epitaxial film of 150nm.
4.1) the gallium oxide buffer layer after thermal annealing is put into pulsed laser deposition PLD chamber, the vacuum tightness of chamber is extracted into 10
-6mbar, the distance between adjustment substrate and target is 50mm, and the rotating speed of target keeps 30rpm;
4.2) adopt pulsed laser deposition PLD method at gallium oxide buffer layer Epitaxial growth gallium oxide film, its epitaxially grown processing parameter is:
Underlayer temperature 600 DEG C,
Oxygen partial pressure 0.009mbar,
Laser energy 420mJ,
Laser frequency 3Hz,
The pulse number of laser 13000 times;
4.3) be filled with the oxygen of 200mbar in the backward chamber that outer layer growth terminates, then allow gallium oxide epitaxial film film naturally cooling, completing gallium oxide buffer layer thickness is that the gallium oxide film of 12nm makes.
Embodiment 3, makes the gallium oxide film that buffer layer thickness is 10nm.
Steps A, cleaning GaAs substrate.
The realization of this step is identical with the step 1 in embodiment 1.
Step B, growth thickness is the gallium oxide buffer layer of 10nm.
(B1) the GaAs substrate after cleaning is put into pulsed laser deposition PLD chamber, the vacuum tightness of pulsed laser deposition PLD chamber is extracted into 10
-6mbar, the distance between substrate and gallium oxide target is adjusted to 50mm, and the rotating speed of target keeps 30rpm;
(B2) by silicon to 650 DEG C, in adjustment pulsed laser deposition PLD chamber, oxygen partial pressure is 0.05mbar, and arranging laser energy is 340mJ, and laser frequency is 4Hz, and pulse number is 1200 growth Ga2O3 buffer layers;
(B3) after buffer growth terminates, in pulsed laser deposition PLD chamber, be filled with the oxygen of 200mbar, then allow growth gallium oxide buffer layer thin film naturally cooling.
Step C, arranging annealing temperature is 750 DEG C, gallium oxide buffer layer is carried out to the thermal annealing of 80min in oxygen atmosphere.
Step D, growth thickness is the gallium oxide epitaxial film of 125nm.
(D1) the gallium oxide buffer layer after thermal annealing is put into pulsed laser deposition PLD chamber, the vacuum tightness of chamber is extracted into 10
-6mbar, the distance between adjustment substrate and target is 50mm, and the rotating speed of target keeps 30rpm;
(D2) arrange the processing parameter of pulsed laser deposition PLD, at gallium oxide buffer layer Epitaxial growth gallium oxide film, epitaxially grown processing parameter is: underlayer temperature 550 DEG C, oxygen partial pressure 0.015mbar, laser energy 450mJ, laser frequency 3Hz, the pulse number of laser 10000 times;
(D3) be filled with the oxygen of 200mbar in the backward chamber that outer layer growth terminates, then allow gallium oxide epitaxial film film naturally cooling, completing gallium oxide buffer layer thickness is that the gallium oxide film of 10nm makes.
More than describing is only three specific exampless of the present invention; do not form any limitation of the invention; obviously for the professional person of this area; after having understood content of the present invention and principle; all may when not deviating from the principle of the invention, structure; carry out the various parameters revision in form and details and change, but these based on inventive concept correction and change still within claims of the present invention.
Claims (6)
1. based on the gallium oxide film of GaAs substrate, comprise GaAs substrate (1) and gallium oxide epitaxial film (3), it is characterized in that: the gallium oxide buffer layer (2) being provided with 6-12nm between GaAs substrate (1) and gallium oxide epitaxial film (3).
2. the gallium oxide film based on GaAs substrate according to claim 1, is characterized in that: epitaxial film (3) adopts Ga2O3 material, and thickness is 90 ~ 150nm.
3. the gallium oxide film based on GaAs substrate according to claim 1, is characterized in that: the high preferred orientation of GaAs substrate (1) is (001).
4., based on the growth method of the gallium oxide film of GaAs substrate, comprise the steps:
(1) GaAs substrate is cleaned, and dry up with nitrogen;
(2) utilize pulsed laser deposition PLD equipment to grow the gallium oxide buffer layer of 6-12nm on gaas substrates, its processing parameter is:
Underlayer temperature 625 DEG C ~ 700 DEG C,
Oxygen partial pressure 0.04mbar ~ 0.06mbar,
Laser energy 310mJ ~ 360mJ,
Laser frequency 2Hz ~ 4Hz;
(3) in oxygen atmosphere, thermal annealing is carried out to gallium oxide buffer layer;
(4) gallium oxide buffer layer after annealing grows gallium oxide epitaxial film, its processing parameter is:
Underlayer temperature 500 DEG C ~ 600 DEG C,
Oxygen partial pressure 0.009mbar ~ 0.02mbar,
Laser energy 420mJ ~ 460mJ,
Laser frequency 2Hz ~ 3Hz.
5. the gallium oxide film process based on GaAs substrate according to claim 4, is characterized in that: in oxygen atmosphere, the processing condition of thermal annealing are: annealing temperature 750 DEG C ~ 950 DEG C, annealing time 60 ~ 80min.
6. the gallium oxide film process based on GaAs substrate according to claim 4, is characterized in that: to the cleaning of GaAs substrate, is be soak time 1min in the mixing solutions of the sulfuric acid of 5:1:1, hydrogen peroxide and water in ratio.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106920849A (en) * | 2017-04-21 | 2017-07-04 | 吉林大学 | Ga with good heat dissipation performance2O3Base metal oxide semiconductor field effect transistor and preparation method thereof |
| CN109136859A (en) * | 2018-10-22 | 2019-01-04 | 哈尔滨工业大学 | A method of preparing high transparency gallium oxide film |
| CN110911270A (en) * | 2019-12-11 | 2020-03-24 | 吉林大学 | High-quality gallium oxide film and homoepitaxial growth method thereof |
| CN110993504A (en) * | 2019-10-14 | 2020-04-10 | 西安电子科技大学 | Ga based on SiC substrate2O3Preparation method of film and Ga based on SiC substrate2O3Film(s) |
| CN111455324A (en) * | 2020-04-21 | 2020-07-28 | 华南理工大学 | Preparation method of crystal form and thickness controllable zirconium dioxide film |
| CN113097055A (en) * | 2021-04-02 | 2021-07-09 | 吉林大学 | High-quality p-type gallium oxide nano columnar structure film and preparation method thereof |
| CN113223928A (en) * | 2021-04-16 | 2021-08-06 | 西安电子科技大学 | Gallium oxide epitaxial growth method based on transfer bonding |
| CN113471064A (en) * | 2021-06-30 | 2021-10-01 | 中国科学技术大学 | Method for preparing III-group oxide film based on oblique-angle substrate and epitaxial wafer thereof |
| CN113517173A (en) * | 2021-06-07 | 2021-10-19 | 西安电子科技大学 | Homoepitaxy beta-Ga2O3Film and preparation method thereof |
| CN113643960A (en) * | 2021-06-07 | 2021-11-12 | 西安电子科技大学 | beta-Ga based on pulse method2O3Film and preparation method thereof |
| CN114823977A (en) * | 2022-04-25 | 2022-07-29 | 中国科学技术大学 | Preparation method of gallium oxide photoelectric detector |
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| CN106920849B (en) * | 2017-04-21 | 2019-07-02 | 吉林大学 | Ga with good heat dissipation performance2O3Base metal oxide semiconductor field effect transistor and preparation method thereof |
| CN106920849A (en) * | 2017-04-21 | 2017-07-04 | 吉林大学 | Ga with good heat dissipation performance2O3Base metal oxide semiconductor field effect transistor and preparation method thereof |
| CN109136859A (en) * | 2018-10-22 | 2019-01-04 | 哈尔滨工业大学 | A method of preparing high transparency gallium oxide film |
| CN110993504A (en) * | 2019-10-14 | 2020-04-10 | 西安电子科技大学 | Ga based on SiC substrate2O3Preparation method of film and Ga based on SiC substrate2O3Film(s) |
| CN110911270B (en) * | 2019-12-11 | 2022-03-25 | 吉林大学 | High-quality gallium oxide film and homoepitaxial growth method thereof |
| CN110911270A (en) * | 2019-12-11 | 2020-03-24 | 吉林大学 | High-quality gallium oxide film and homoepitaxial growth method thereof |
| CN111455324A (en) * | 2020-04-21 | 2020-07-28 | 华南理工大学 | Preparation method of crystal form and thickness controllable zirconium dioxide film |
| CN111455324B (en) * | 2020-04-21 | 2021-10-26 | 华南理工大学 | Preparation method of crystal form and thickness controllable zirconium dioxide film |
| CN113097055A (en) * | 2021-04-02 | 2021-07-09 | 吉林大学 | High-quality p-type gallium oxide nano columnar structure film and preparation method thereof |
| CN113097055B (en) * | 2021-04-02 | 2022-04-29 | 吉林大学 | High-quality p-type gallium oxide nano columnar structure film and preparation method thereof |
| CN113223928A (en) * | 2021-04-16 | 2021-08-06 | 西安电子科技大学 | Gallium oxide epitaxial growth method based on transfer bonding |
| CN113223928B (en) * | 2021-04-16 | 2024-01-12 | 西安电子科技大学 | Gallium oxide epitaxial growth method based on transfer bonding |
| CN113643960B (en) * | 2021-06-07 | 2024-03-19 | 西安电子科技大学 | beta-Ga based on pulse method 2 O 3 Film and method for producing the same |
| CN113517173A (en) * | 2021-06-07 | 2021-10-19 | 西安电子科技大学 | Homoepitaxy beta-Ga2O3Film and preparation method thereof |
| CN113643960A (en) * | 2021-06-07 | 2021-11-12 | 西安电子科技大学 | beta-Ga based on pulse method2O3Film and preparation method thereof |
| CN113517173B (en) * | 2021-06-07 | 2024-03-19 | 西安电子科技大学 | Homoepitaxial beta-Ga 2 O 3 Film and method for producing the same |
| CN113471064A (en) * | 2021-06-30 | 2021-10-01 | 中国科学技术大学 | Method for preparing III-group oxide film based on oblique-angle substrate and epitaxial wafer thereof |
| CN114823977B (en) * | 2022-04-25 | 2024-02-23 | 中国科学技术大学 | Preparation method of gallium oxide photoelectric detector |
| CN114823977A (en) * | 2022-04-25 | 2022-07-29 | 中国科学技术大学 | Preparation method of gallium oxide photoelectric detector |
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