CN104988579A - Gallium oxide film based on sapphire substrate and growing method of gallium oxide film - Google Patents
Gallium oxide film based on sapphire substrate and growing method of gallium oxide film Download PDFInfo
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- CN104988579A CN104988579A CN201510397660.2A CN201510397660A CN104988579A CN 104988579 A CN104988579 A CN 104988579A CN 201510397660 A CN201510397660 A CN 201510397660A CN 104988579 A CN104988579 A CN 104988579A
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Abstract
The invention discloses a gallium oxide film based on a sapphire substrate and a growing method of the gallium oxide film to mainly solve the problems that an existing gallium oxide film is poor in surface appearance and small in grain size. The gallium oxide film comprises the sapphire substrate (1) and a gallium oxide epitaxial layer (3). The gallium oxide film is characterized in that a 7-12 nm gallium oxide buffering layer (2) is arranged between the sapphire substrate (1) and the gallium oxide epitaxial layer (3), and the crystal quality of the gallium oxide buffering layer is improved through thermal annealing. The roughness of the surface of a Ga2O3 film is reduced, the surface appearance of the Ga2O3 film is improved, the grain size of Ga2O3 is increased, and the gallium oxide film can be used for manufacturing a semiconductor power device.
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.
Sapphire is a kind of insulating material, has excellent chemical stability and high physical strength, and sapphire moderate cost, manufacturing technology relative maturity, be widely used among semiconductor material growing at present simultaneously.
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 a sapphire substrate.
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 Sapphire 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 Sapphire Substrate, comprise Sapphire Substrate and gallium oxide epitaxial film, it is characterized in that: the gallium oxide buffer layer being provided with 7-12nm between Sapphire Substrate and gallium oxide epitaxial film.
The present invention is based on the growth method of the gallium oxide film of Sapphire Substrate, comprise the steps:
(1) Sapphire Substrate is cleaned, and dry up with nitrogen;
(2) utilize PLD equipment to grow the gallium oxide buffer layer of 7-12nm on a sapphire substrate, 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;
(3) in argon atmosphere, thermal annealing is carried out to gallium oxide buffer layer;
(4) processing parameter changing PLD grows gallium oxide epitaxial film on gallium oxide buffer layer.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.
The present invention owing to being provided with Ga2O3 buffer layer between Sapphire 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 Sapphire Substrate 1, buffer layer 2 and epitaxial film 3.Wherein being oriented to (0001) of Sapphire Substrate 1, epitaxial film 3 adopts thickness to be the Ga2O3 material of 90-160nm, and buffer layer 2 adopts thickness to be the Ga2O3 material of 7-12nm, and between Sapphire 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 7nm.
Step 1, cleaning Sapphire Substrate.
(1a) mixed solution Sapphire Substrate being placed in sulfuric acid and phosphoric acid soaks 30min, and the ratio of sulfuric acid and phosphoric acid is 3:1;
(1b) acetone and washes of absolute alcohol Sapphire Substrate 6min is used respectively;
(1c) use rinsed with deionized water Sapphire Substrate, and dry up with dry nitrogen.
Step 2, growth thickness is the gallium oxide buffer layer of 7nm.
(2a) Sapphire 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;
(2b) Sapphire Substrate is heated to 500 DEG C, in adjustment pulsed laser deposition PLD chamber, oxygen partial pressure is 0.009mbar, and arranging laser energy is 420mJ, and laser frequency is 2Hz, and pulse number is 900 growth Ga2O3 buffer layers;
(2c) 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 argon atmosphere, and annealing temperature is 800 DEG C, annealing time 70min.
Step 4, growth thickness is the gallium oxide epitaxial film of 90nm.
(4a) 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;
(4b) the epitaxially grown processing parameter of pulsed laser deposition PLD is set: underlayer temperature 625 DEG C, oxygen partial pressure 0.04mbar, laser energy 310mJ, laser frequency 2Hz, pulse number 7500 epitaxy gallium oxide films of laser;
(4c) 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 7nm makes.
Embodiment 2, makes the gallium oxide film that buffer layer thickness is 12nm.
The first step, cleaning Sapphire 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) Sapphire 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) Sapphire Substrate is heated to 570 DEG C, in adjustment pulsed laser deposition PLD chamber, oxygen partial pressure is 0.015mbar, and arranging laser energy is 450mJ, and laser frequency is 3Hz, and pulse number is 1600 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 850 DEG C in argon atmosphere.
4th step, growth thickness is the gallium oxide epitaxial film of 160nm.
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 675 DEG C,
Oxygen partial pressure 0.05mbar,
Laser energy 340mJ,
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 Sapphire 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) Sapphire 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 600 DEG C, in adjustment pulsed laser deposition PLD chamber, oxygen partial pressure is 0.02mbar, and arranging laser energy is 460mJ, and laser frequency is 3Hz, and pulse number is 1400 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 950 DEG C, gallium oxide buffer layer is carried out to the thermal annealing of 50min in argon 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 700 DEG C, oxygen partial pressure 0.06mbar, laser energy 360mJ, laser frequency 4Hz, 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 Sapphire Substrate, comprise Sapphire Substrate (1) and gallium oxide epitaxial film (3), it is characterized in that: the gallium oxide buffer layer (2) being provided with 7-12nm between Sapphire Substrate (1) and gallium oxide epitaxial film (3).
2. the gallium oxide film based on Sapphire Substrate according to claim 1, is characterized in that: epitaxial film (3) adopts Ga2O3 material, and thickness is 90 ~ 160nm.
3. the gallium oxide film based on Sapphire Substrate according to claim 1, is characterized in that: the high preferred orientation of Sapphire Substrate (1) is (0001).
4., based on the growth method of the gallium oxide film of Sapphire Substrate, comprise the steps:
(1) Sapphire Substrate is cleaned, and dry up with nitrogen;
(2) utilize pulsed laser deposition PLD equipment to grow the gallium oxide buffer layer of 7-12nm on a sapphire substrate, 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;
(3) in argon 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 625 DEG C ~ 700 DEG C,
Oxygen partial pressure 0.04mbar ~ 0.06mbar,
Laser energy 310mJ ~ 360mJ,
Laser frequency 2Hz ~ 4Hz.
5. the gallium oxide film process based on Sapphire Substrate according to claim 4, is characterized in that: in argon atmosphere, the processing condition of thermal annealing are: annealing temperature 800 DEG C ~ 950 DEG C, annealing time 50 ~ 70min.
6. the gallium oxide film process based on Sapphire Substrate according to claim 4, it is characterized in that: to the cleaning of Sapphire Substrate, be carry out in the mixing solutions of sulfuric acid and phosphoric acid, in mixing solutions, the ratio of sulfuric acid and phosphoric acid is 3:1, scavenging period 30min.
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| CN105624782A (en) * | 2015-12-31 | 2016-06-01 | 中国科学院半导体研究所 | Preparation method of gallium oxide thin film |
| 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 |
| CN107359122A (en) * | 2017-06-07 | 2017-11-17 | 西安电子科技大学 | Mn adulterates the preparation method of hetero-junctions spin fet |
| CN109136859A (en) * | 2018-10-22 | 2019-01-04 | 哈尔滨工业大学 | A method of preparing high transparency gallium oxide film |
| CN110534555A (en) * | 2019-08-26 | 2019-12-03 | 西安电子科技大学 | Based on the face r Al2O3β-the Ga of graph substrate2O3Film manufacturing method |
| CN110867368A (en) * | 2019-11-17 | 2020-03-06 | 金华紫芯科技有限公司 | Preparation method of gallium oxide epitaxial film |
| CN110911270A (en) * | 2019-12-11 | 2020-03-24 | 吉林大学 | High-quality gallium oxide film and homoepitaxial growth method thereof |
| CN112126897A (en) * | 2020-10-09 | 2020-12-25 | 南京信息工程大学 | Preparation method of alpha-phase gallium oxide film |
| CN112359417A (en) * | 2020-09-27 | 2021-02-12 | 南京新澳半导体科技有限公司 | Method for maskless in-situ transverse epitaxy of alpha-phase gallium oxide film |
| CN113451435A (en) * | 2021-06-30 | 2021-09-28 | 南方科技大学 | Single-crystal gallium oxide based solar blind ultraviolet photoelectric detector and preparation method and application thereof |
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| JP2021527610A (en) * | 2018-05-18 | 2021-10-14 | 中国科学院蘇州納米技術与納米▲ファン▼生研究所 | Gallium oxide thin film based on sapphire substrate, its growth method, and use |
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| CN113584587A (en) * | 2021-07-30 | 2021-11-02 | 中国科学院宁波材料技术与工程研究所 | Sn-doped metastable gallium oxide crystalline phase film and preparation method and application 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 |
| CN115000228A (en) * | 2022-05-13 | 2022-09-02 | 厦门大学 | High-performance Ga 2 O 3 Thin film active solar blind ultraviolet detector and preparation method thereof |
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| CN115838971A (en) * | 2023-02-14 | 2023-03-24 | 楚赟精工科技(上海)有限公司 | Gallium oxide film and preparation method thereof |
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| CN115029683B (en) * | 2022-06-13 | 2023-08-22 | 集美大学 | Through low bond energy N 2 Preparation of high-quality steady-state beta-Ga by O thermal oxidation 2 O 3 Method for producing thin films |
| CN115838971A (en) * | 2023-02-14 | 2023-03-24 | 楚赟精工科技(上海)有限公司 | Gallium oxide film and preparation method thereof |
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