CN105118851A - Sapphire substrate-based multilayer gallium oxide thin film and growing method thereof - Google Patents
Sapphire substrate-based multilayer gallium oxide thin film and growing method thereof Download PDFInfo
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- CN105118851A CN105118851A CN201510396978.9A CN201510396978A CN105118851A CN 105118851 A CN105118851 A CN 105118851A CN 201510396978 A CN201510396978 A CN 201510396978A CN 105118851 A CN105118851 A CN 105118851A
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- gallium oxide
- sapphire substrate
- epitaxial loayer
- resilient coating
- multilayer
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- AJNVQOSZGJRYEI-UHFFFAOYSA-N digallium;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Ga+3].[Ga+3] AJNVQOSZGJRYEI-UHFFFAOYSA-N 0.000 title claims abstract description 154
- 229910001195 gallium oxide Inorganic materials 0.000 title claims abstract description 154
- 239000000758 substrate Substances 0.000 title claims abstract description 63
- 229910052594 sapphire Inorganic materials 0.000 title claims abstract description 47
- 239000010980 sapphire Substances 0.000 title claims abstract description 47
- 238000000034 method Methods 0.000 title claims abstract description 21
- 239000010409 thin film Substances 0.000 title abstract description 8
- 239000002131 composite material Substances 0.000 claims abstract description 35
- 239000011248 coating agent Substances 0.000 claims description 65
- 238000000576 coating method Methods 0.000 claims description 65
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 21
- 239000001301 oxygen Substances 0.000 claims description 21
- 229910052760 oxygen Inorganic materials 0.000 claims description 21
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 8
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 6
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 238000010276 construction Methods 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims 2
- 238000000407 epitaxy Methods 0.000 claims 1
- 230000002000 scavenging effect Effects 0.000 claims 1
- QZQVBEXLDFYHSR-UHFFFAOYSA-N gallium(III) oxide Inorganic materials O=[Ga]O[Ga]=O QZQVBEXLDFYHSR-UHFFFAOYSA-N 0.000 abstract description 36
- 239000004065 semiconductor Substances 0.000 abstract description 9
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 239000013078 crystal Substances 0.000 abstract description 4
- 230000003746 surface roughness Effects 0.000 abstract 1
- 238000004549 pulsed laser deposition Methods 0.000 description 55
- 239000010408 film Substances 0.000 description 35
- 239000000463 material Substances 0.000 description 20
- 238000010586 diagram Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 230000026267 regulation of growth Effects 0.000 description 2
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N ferric oxide Chemical compound O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- 238000001534 heteroepitaxy Methods 0.000 description 1
- 238000001657 homoepitaxy Methods 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 230000000873 masking effect Effects 0.000 description 1
- 238000002488 metal-organic chemical vapour deposition Methods 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000013077 target material Substances 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
- 230000005533 two-dimensional electron gas Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L29/00—Semiconductor devices adapted for rectifying, amplifying, oscillating or switching, or capacitors or resistors with at least one potential-jump barrier or surface barrier, e.g. PN junction depletion layer or carrier concentration layer; Details of semiconductor bodies or of electrodes thereof ; Multistep manufacturing processes therefor
- H01L29/02—Semiconductor bodies ; Multistep manufacturing processes therefor
- H01L29/06—Semiconductor bodies ; Multistep manufacturing processes therefor characterised by their shape; characterised by the shapes, relative sizes, or dispositions of the semiconductor regions ; characterised by the concentration or distribution of impurities within semiconductor regions
- H01L29/0684—Semiconductor bodies ; Multistep manufacturing processes therefor characterised by their shape; characterised by the shapes, relative sizes, or dispositions of the semiconductor regions ; characterised by the concentration or distribution of impurities within semiconductor regions characterised by the shape, relative sizes or dispositions of the semiconductor regions or junctions between the regions
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02367—Substrates
- H01L21/0237—Materials
- H01L21/0242—Crystalline insulating materials
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02436—Intermediate layers between substrates and deposited layers
- H01L21/02439—Materials
- H01L21/02483—Oxide semiconducting materials not being Group 12/16 materials, e.g. ternary compounds
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02518—Deposited layers
- H01L21/02521—Materials
- H01L21/02565—Oxide semiconducting materials not being Group 12/16 materials, e.g. ternary compounds
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02612—Formation types
- H01L21/02617—Deposition types
- H01L21/02631—Physical deposition at reduced pressure, e.g. MBE, sputtering, evaporation
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L29/00—Semiconductor devices adapted for rectifying, amplifying, oscillating or switching, or capacitors or resistors with at least one potential-jump barrier or surface barrier, e.g. PN junction depletion layer or carrier concentration layer; Details of semiconductor bodies or of electrodes thereof ; Multistep manufacturing processes therefor
- H01L29/02—Semiconductor bodies ; Multistep manufacturing processes therefor
- H01L29/12—Semiconductor bodies ; Multistep manufacturing processes therefor characterised by the materials of which they are formed
- H01L29/24—Semiconductor bodies ; Multistep manufacturing processes therefor characterised by the materials of which they are formed including, apart from doping materials or other impurities, only semiconductor materials not provided for in groups H01L29/16, H01L29/18, H01L29/20, H01L29/22
Abstract
The invention discloses a sapphire substrate-based multilayer gallium oxide thin film and the growing method thereof, and mainly solves the problem of poor appearance and small crystal grain size of conventional gallium oxide thin films. The gallium oxide thin film comprises a sapphire substrate and gallium oxide epitaxial layers. and is characterized in that a plurality of epitaxial layers are provided, a 8-12nm of gallium oxide buffer layer is arranged under each gallium oxide epitaxial layer from top to bottom, and a composite structure of buffer layers and epitaxial layers alternatively formed is formed on the substrate. The surface roughness of a Ga2O3 is reduced, the surface appearance of the Ga2O3 is improved, and the crystal grain size of the Ga2O3 is increased. The sapphire substrate-based multilayer gallium oxide thin film can be used to manufacture a semiconductor power device.
Description
Technical field
The invention belongs to microelectronics technology, relate to the growing method of semi-conducting 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 semiconductor 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 semi-conducting material of material property can make up above-mentioned bi-material, and simultaneously wider, the disruptive field intensity of energy gap is suitable for more greatly manufacturing power device.
Ga2O3 semi-conducting material especially causes the interest of people, and Ga2O3 semi-conducting material energy gap is large, and disruptive field intensity is high, conducting resistance is little, can carry out homoepitaxy, be that the optimal material 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, lattice structure 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 physicochemical 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 better utilize the advantage of material, people have carried out large quantifier elimination to the growth of Ga2O3 film.The growing method adopted mainly contains: pulsed laser deposition PLD, sol-gel process, chemical vapour deposition technique CVD, metal organic chemical vapor deposition MOCVD and magnetron sputtering method etc.
Pulsed laser deposition PLD is that the scope of application 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 object.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 proportion.4. deposition rate is high, and the test period is short, and underlayer temperature requires low.5. technological 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 growth course, identical technological parameter is adopted, comprise oxygen pressure, laser energy, underlayer temperature etc. to grow, Ga2O3 film surface appearance that heteroepitaxy obtains is poor, crystallite dimension 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 multilayer gallium oxide film based on Sapphire Substrate and growing method thereof are proposed, to reduce roughness of film, improve Ga2O3 film surface appearance, increase Ga2O3 crystallite dimension, obtain high-quality Ga2O3 semiconductor material with wide forbidden band.
For achieving the above object, multilayer gallium oxide film based on Sapphire Substrate of the present invention, comprise substrate and gallium oxide epitaxial loayer, it is characterized in that: gallium oxide epitaxial loayer is set to multilayer, and be provided with the thick gallium oxide resilient coating of 8 ~ 12nm, to form resilient coating and the alternatively distributed composite construction of epitaxial loayer on substrate below every layer of gallium oxide epitaxial loayer from bottom to top.
For achieving the above object, the present invention is based on the manufacture method of the multilayer gallium oxide film of Sapphire Substrate, comprise the steps:
(1) Sapphire Substrate is cleaned, and dry up with nitrogen;
(2) utilize PLD equipment on a sapphire substrate growth thickness be the first gallium oxide resilient coating of 8 ~ 12nm;
(3) at the first gallium oxide resilient coating Epitaxial growth thickness be the first gallium oxide epitaxial loayer of 15-25nm, form first composite bed;
(4) on the first gallium oxide epitaxial loayer, growth thickness is the second gallium oxide resilient coating of 8 ~ 12nm;
(5) at the second gallium oxide resilient coating Epitaxial growth thickness be the second gallium oxide epitaxial loayer of 15-25nm, form second composite bed;
(6) the like, carry out the repeatedly alternating growth of gallium oxide resilient coating and gallium oxide epitaxial loayer, form multiple composite bed, complete the making of multilayer gallium oxide film on a sapphire substrate.
The present invention is owing to being provided with multilayer Ga2O3 resilient coating, and when improve Ga2O3 film initial growth, the coverage rate of reactant atom on substrate, adds seed crystal Enhancing Nucleation Density; Carrying out the growth of Ga2O3 epitaxial loayer by adjusting epitaxially grown technological parameter, not only increasing Ga2O3 crystallite dimension, reduce roughness of film, and improve the surface topography of whole Ga2O3 film.
Accompanying drawing explanation
Fig. 1 is the cross-sectional view of the embodiment of the present invention 1;
Fig. 2 is the Making programme schematic diagram of the embodiment of the present invention 1;
Fig. 3 is the cross-sectional view of the embodiment of the present invention 2;
Fig. 4 is the Making programme schematic diagram of the embodiment of the present invention 2;
Fig. 5 is the cross-sectional view of the embodiment of the present invention 3;
Fig. 6 is the Making programme schematic diagram of the embodiment of the present invention 3.
Embodiment
Embodiment 1, makes the multilayer gallium oxide film containing three composite beds on a sapphire substrate.
With reference to Fig. 1, the multilayer gallium oxide film of the present embodiment comprises Sapphire Substrate 1, first gallium oxide resilient coating 2, first gallium oxide epitaxial loayer 3, second gallium oxide resilient coating 4, second gallium oxide epitaxial loayer 5, the 3rd gallium oxide resilient coating 6 and the 3rd gallium oxide epitaxial loayer 7 from bottom to top.Wherein substrate 1 is the sapphire substrate of (0001) orientation, 3rd gallium oxide epitaxial loayer 7 adopts thickness to be the Ga2O3 material of 25nm, first gallium oxide resilient coating 2, second gallium oxide resilient coating 4 and the 3rd gallium oxide resilient coating 6 adopt thickness to be the Ga2O3 material of 8nm, first gallium oxide epitaxial loayer 3 adopts thickness to be the Ga2O3 material of 15nm, and the second gallium oxide epitaxial loayer 5 adopts thickness to be the Ga2O3 material of 20nm.
Described first gallium oxide resilient coating 2 forms first composite bed with described first gallium oxide epitaxial loayer 3;
Described second gallium oxide resilient coating 4 forms second composite bed with described second gallium oxide epitaxial loayer 5;
Described 3rd gallium oxide resilient coating 6 forms the 3rd composite bed with described 3rd gallium oxide epitaxial loayer 7.
With reference to Fig. 2, the step making the multilayer gallium oxide film containing three composite beds is on a sapphire substrate as follows:
Step 1, cleaning Sapphire Substrate.
(1a) mixed liquor 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 5min is used respectively;
(1c) use rinsed with deionized water Sapphire Substrate, and dry up with nitrogen.
Step 2, growth thickness is the first gallium oxide resilient coating of 8nm.
(2a) Sapphire Substrate after cleaning is put into pulsed laser deposition PLD chamber, the vacuum degree 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 550 DEG C, in adjustment pulsed laser deposition PLD chamber, partial pressure of oxygen is 0.009mbar, and arranging laser energy is 420mJ, and laser frequency is 2Hz, and pulse number is 800, at Grown the one Ga2O3 resilient coating.
Step 3, growth thickness is the first gallium oxide epitaxial loayer of 15nm.
The epitaxially grown technological parameter of pulsed laser deposition PLD is set: underlayer temperature 650 DEG C, partial pressure of oxygen 0.045mbar, laser energy 320mJ, laser frequency 3Hz, the pulse number of laser 3000 times, at the first gallium oxide resilient coating Epitaxial growth first gallium oxide epitaxial loayer, forms first composite bed.
Step 4, growth thickness is the second gallium oxide resilient coating of 8nm.
The technological parameter that pulsed laser deposition PLD grows is set: underlayer temperature 550 DEG C, partial pressure of oxygen 0.009mbar, laser energy 420mJ, laser frequency 2Hz, the pulse number of laser 800 times, on the first epitaxial layer growth regulation titanium dioxide gallium resilient coating.
Step 5, growth thickness is the second gallium oxide epitaxial loayer of 20nm.
The epitaxially grown technological parameter of pulsed laser deposition PLD is set: underlayer temperature 650 DEG C, partial pressure of oxygen 0.045mbar, laser energy 320mJ, laser frequency 3Hz, the pulse number of laser 4000 times, at the second gallium oxide resilient coating Epitaxial growth second gallium oxide epitaxial loayer, forms second composite bed.
Step 6, growth thickness is the 3rd gallium oxide resilient coating of 8nm.
The technological parameter that pulsed laser deposition PLD grows is set: underlayer temperature 550 DEG C, partial pressure of oxygen 0.009mbar, laser energy 420mJ, laser frequency 2Hz, the pulse number of laser 800 times, growth regulation three gallium oxide resilient coating on the second epitaxial loayer.
Step 7, growth thickness is the 3rd gallium oxide epitaxial loayer of 25nm.
(7a) the epitaxially grown technological parameter of pulsed laser deposition PLD is set: underlayer temperature 650 DEG C, partial pressure of oxygen 0.045mbar, laser energy 320mJ, laser frequency 3Hz, the pulse number of laser is 5000, at the 3rd gallium oxide resilient coating Epitaxial growth the 3rd gallium oxide epitaxial loayer, form the 3rd composite bed;
(7b) after the 3rd gallium oxide epitaxial loayer epitaxial growth terminates, be filled with the oxygen of 200mbar in chamber, then allow gallium oxide epitaxial loayer film naturally cool, the multilayer gallium oxide film completed containing three composite beds makes.
Embodiment 2, makes the multilayer gallium oxide film containing two composite beds on a sapphire substrate.
With reference to Fig. 3, the multilayer gallium oxide film of the present embodiment comprises Sapphire Substrate 1, first gallium oxide resilient coating 2, first gallium oxide epitaxial loayer 3, second gallium oxide resilient coating 4 and the second gallium oxide epitaxial loayer 5 from bottom to top.Wherein substrate 1 is the sapphire substrate of (0001) orientation, first gallium oxide resilient coating 2 and the second gallium oxide resilient coating 4 adopt thickness to be the Ga2O3 material of 12nm, and this first gallium oxide resilient coating 2 and the first gallium oxide epitaxial loayer 3 form first composite bed; Described; First gallium oxide epitaxial loayer 3 adopts thickness to be the Ga2O3 material of 20nm, and the second gallium oxide epitaxial loayer 5 adopts thickness to be the Ga2O3 material of 25nm, and this second gallium oxide resilient coating 4 and the second gallium oxide epitaxial loayer 5 form second composite bed.
With reference to Fig. 4, the step making the multilayer gallium oxide film containing two composite beds is on a sapphire substrate as follows:
The first step, cleaning Sapphire Substrate.
This step is identical with the step 1 of embodiment 1.
Second step, growth thickness is the first gallium oxide resilient coating of 12nm.
2.1) Sapphire Substrate after cleaning is put into pulsed laser deposition PLD chamber, the vacuum degree 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) adjusting partial pressure of oxygen in pulsed laser deposition PLD chamber is 0.01mbar, and Sapphire Substrate is heated to 570 DEG C, arranging laser energy is 450mJ, and laser frequency is 3Hz, and pulse number is 1500, at Grown the one Ga2O3 resilient coating.
3rd step, employing pulsed laser deposition PLD method is the first gallium oxide epitaxial loayer of 20nm at the first gallium oxide resilient coating Epitaxial growth thickness, and form first composite bed, its epitaxially grown technological parameter is:
Underlayer temperature 675 DEG C,
Partial pressure of oxygen 0.05mbar,
Laser energy 340mJ,
Laser frequency 3Hz,
The pulse number of laser 4000 times;
4th step, in adjustment pulsed laser deposition PLD chamber, partial pressure of oxygen is 0.01mbar, sapphire substrate temperature is reduced to 570 DEG C, arranging laser energy is 450mJ, laser frequency is 3Hz, and pulse number is 1500, and on the first gallium oxide epitaxial loayer, growth thickness is the 2nd Ga2O3 resilient coating of 12nm.
5th step, growth thickness is the second gallium oxide epitaxial loayer of 25nm.
5.1) adopt pulsed laser deposition PLD method at the second gallium oxide resilient coating Epitaxial growth second gallium oxide epitaxial loayer film, form second composite bed, its epitaxially grown technological parameter is:
Underlayer temperature 675 DEG C,
Partial pressure of oxygen 0.05mbar,
Laser energy 340mJ,
Laser frequency 3Hz,
The pulse number of laser 5000 times;
5.2) be filled with the oxygen of 200mbar in the backward chamber that the second gallium oxide outer layer growth terminates, then allow gallium oxide epitaxial loayer film naturally cool, the gallium oxide film completed containing two composite beds makes.
Embodiment 3, makes the gallium oxide film containing four layers of composite bed on a sapphire substrate.
With reference to Fig. 5, the multilayer gallium oxide film of the present embodiment comprises Sapphire Substrate 1, first gallium oxide resilient coating 2, first gallium oxide epitaxial loayer 3, second gallium oxide resilient coating 4, second gallium oxide epitaxial loayer 5, the 3rd gallium oxide resilient coating 6, the 3rd gallium oxide epitaxial loayer 7, the 4th gallium oxide resilient coating 8 and the 4th gallium oxide epitaxial loayer 9 from bottom to top.Wherein substrate 1 is the sapphire substrate of (0001) orientation, 4th gallium oxide epitaxial loayer 9 adopts thickness to be the Ga2O3 material of 25nm, first gallium oxide resilient coating 2, second gallium oxide resilient coating 4, the 3rd gallium oxide resilient coating 6 and the 4th gallium oxide resilient coating 8 adopt thickness to be the Ga2O3 material of 10nm, first gallium oxide epitaxial loayer 3 adopts thickness to be the Ga2O3 material of 15nm, and the second gallium oxide epitaxial loayer 5 and the 3rd gallium oxide epitaxial loayer 7 adopt thickness to be the Ga2O3 material of 20nm.This first gallium oxide resilient coating 2 and the first gallium oxide epitaxial loayer 3 form first composite bed; This second gallium oxide resilient coating 4 and the second gallium oxide epitaxial loayer 5 form second composite bed; 3rd gallium oxide resilient coating 6 and the 3rd gallium oxide epitaxial loayer 7 form the 3rd composite bed; 4th gallium oxide resilient coating 8 and the 4th gallium oxide epitaxial loayer 9 form the 4th composite bed.
With reference to Fig. 6, the step making the gallium oxide film containing four composite beds is on a sapphire substrate as follows:
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 first gallium oxide resilient coating of 10nm.
(B1) Sapphire Substrate after cleaning is put into pulsed laser deposition PLD chamber, the vacuum degree 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 610 DEG C, arrange pulsed laser deposition PLD technological parameter, in chamber, partial pressure of oxygen is 0.015mbar, and arranging laser energy is 470mJ, and laser frequency is 2Hz, pulse number 1200, at Grown the one Ga2O3 resilient coating.
Step C, the technological parameter of adjustment pulsed laser deposition PLD, is the first gallium oxide epitaxial loayer film of 15nm at the first gallium oxide resilient coating Epitaxial growth thickness, forms first composite bed; Epitaxially grown technological parameter is: underlayer temperature 710 DEG C, partial pressure of oxygen 0.055mbar, laser energy 350mJ, laser frequency 2Hz, the pulse number of laser 3000 times.
In step D, adjustment pulsed laser deposition PLD chamber, partial pressure of oxygen is 0.015mbar, underlayer temperature is adjusted to 610 DEG C, arranging laser energy is 470mJ, laser frequency is 2Hz, and pulse number is 1200, is the second gallium oxide resilient coating of 10nm at the first gallium oxide outer layer growth thickness.
Step e, arranges the technological parameter of pulsed laser deposition PLD, is the second gallium oxide epitaxial loayer of 20nm, forms second composite bed at the second gallium oxide resilient coating Epitaxial growth thickness; Epitaxially grown technological parameter is: underlayer temperature 710 DEG C, partial pressure of oxygen 0.055mbar, laser energy 350mJ, laser frequency 2Hz, the pulse number of laser 4000 times.
Step F, according to process conditions growth regulation three gallium oxide resilient coating on the second gallium oxide epitaxial loayer of step D.
Step G, according to the process conditions of step e at the 3rd gallium oxide resilient coating Epitaxial growth the 3rd gallium oxide epitaxial loayer, forms the 3rd composite bed.
Step H, according to process conditions growth regulation four gallium oxide resilient coating on the 3rd gallium oxide epitaxial loayer of step D.
Step I, arranges the technological parameter of pulsed laser deposition PLD, is the 4th gallium oxide epitaxial loayer of 25nm, forms the 4th composite bed at the 4th gallium oxide resilient coating Epitaxial growth thickness; Epitaxially grown technological parameter is: underlayer temperature 700 DEG C, partial pressure of oxygen 0.055mbar, laser energy 350mJ, laser frequency 2Hz, the pulse number of laser 5000 times.
After the 4th gallium oxide epitaxial loayer epitaxial growth terminates, be filled with the oxygen of 200mbar in chamber, then allow gallium oxide epitaxial loayer film naturally cool, the gallium oxide film completed containing four composite beds makes.
More than describing is only three instantiations 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 (7)
1. based on the multilayer gallium oxide film of Sapphire Substrate, comprise substrate and gallium oxide epitaxial loayer, it is characterized in that: gallium oxide epitaxial loayer is set to multilayer, and be provided with the thick gallium oxide resilient coating of 8 ~ 12nm, to form resilient coating and the alternatively distributed composite construction of epitaxial loayer on substrate below every layer of gallium oxide epitaxial loayer from bottom to top.
2. the multilayer gallium oxide film based on Sapphire Substrate according to claim 1, is characterized in that: each layer gallium oxide epitaxy layer thickness is 15 ~ 25nm.
3. the multilayer gallium oxide film based on Sapphire Substrate according to claim 1, is characterized in that: substrate is the sapphire substrate of (0001) orientation.
4., based on the growing method of the multilayer gallium oxide film of Sapphire Substrate, comprise the steps:
(1) Sapphire Substrate is cleaned, and dry up with nitrogen;
(2) utilize PLD equipment on a sapphire substrate growth thickness be the first gallium oxide resilient coating of 8 ~ 12nm;
(3) at the first gallium oxide resilient coating Epitaxial growth thickness be the first gallium oxide epitaxial loayer of 15 ~ 25nm, form first composite bed;
(4) on the first gallium oxide epitaxial loayer, growth thickness is the second gallium oxide resilient coating of 8 ~ 12nm;
(5) at the second gallium oxide resilient coating Epitaxial growth thickness be the second gallium oxide epitaxial loayer of 15 ~ 25nm, form second composite bed;
(6) the like, carry out the repeatedly alternating growth of gallium oxide resilient coating and gallium oxide epitaxial loayer, form multiple composite bed, complete the making of multilayer gallium oxide film on a sapphire substrate.
5. the growing method of the multilayer gallium oxide film based on Sapphire Substrate according to claim 4, it is characterized in that: to the cleaning of Sapphire Substrate, be carry out in the mixed solution of sulfuric acid and phosphoric acid, in mixed solution, the ratio of sulfuric acid and phosphoric acid is 3:1, scavenging period 30min.
6. the growing method of the multilayer gallium oxide film based on Sapphire Substrate according to claim 4, is characterized in that: the process conditions growing each layer gallium oxide resilient coating are:
Underlayer temperature 550 DEG C ~ 610 DEG C,
Partial pressure of oxygen 0.009mbar ~ 0.015mbar,
Laser energy 420mJ ~ 470mJ,
Pulse number 800 ~ 1500,
Laser frequency 2Hz ~ 3Hz.
7. the growing method of the multilayer gallium oxide film based on Sapphire Substrate according to claim 4, is characterized in that: the technological parameter growing each layer gallium oxide epitaxial loayer is:
Underlayer temperature 650 DEG C ~ 710 DEG C,
Partial pressure of oxygen 0.045mbar ~ 0.055mbar,
Laser energy 320mJ ~ 350mJ,
Pulse number 3000 ~ 5000,
Laser frequency 2Hz ~ 3Hz.
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| KR102509541B1 (en) | 2021-01-08 | 2023-03-14 | 한국세라믹기술원 | Gallium oxide thin film using phase-transition domain alignment buffer layer and method of manufacturing the same |
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