CN106531862B - A kind of preparation method of GaN base compound substrate - Google Patents
A kind of preparation method of GaN base compound substrate Download PDFInfo
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- CN106531862B CN106531862B CN201611184509.1A CN201611184509A CN106531862B CN 106531862 B CN106531862 B CN 106531862B CN 201611184509 A CN201611184509 A CN 201611184509A CN 106531862 B CN106531862 B CN 106531862B
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- 239000000758 substrate Substances 0.000 title claims abstract description 215
- 150000001875 compounds Chemical class 0.000 title claims abstract description 84
- 238000002360 preparation method Methods 0.000 title claims abstract description 41
- 229910052594 sapphire Inorganic materials 0.000 claims abstract description 53
- 239000010980 sapphire Substances 0.000 claims abstract description 53
- 238000000034 method Methods 0.000 claims abstract description 36
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 30
- 238000001312 dry etching Methods 0.000 claims description 21
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 19
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 16
- 229910052757 nitrogen Inorganic materials 0.000 claims description 15
- 239000011265 semifinished product Substances 0.000 claims description 15
- 238000004381 surface treatment Methods 0.000 claims description 13
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 claims description 12
- 229910052733 gallium Inorganic materials 0.000 claims description 12
- 239000007767 bonding agent Substances 0.000 claims description 11
- 238000002248 hydride vapour-phase epitaxy Methods 0.000 claims description 11
- 238000004140 cleaning Methods 0.000 claims description 10
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- 150000002576 ketones Chemical class 0.000 claims 1
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- 238000001657 homoepitaxy Methods 0.000 abstract description 9
- 238000000407 epitaxy Methods 0.000 abstract description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 35
- 239000010949 copper Substances 0.000 description 16
- 238000005516 engineering process Methods 0.000 description 16
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 16
- 238000010586 diagram Methods 0.000 description 14
- 239000010931 gold Substances 0.000 description 14
- 229910002704 AlGaN Inorganic materials 0.000 description 12
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 12
- 239000011651 chromium Substances 0.000 description 12
- 239000013078 crystal Substances 0.000 description 11
- 229910045601 alloy Inorganic materials 0.000 description 10
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- 229910052759 nickel Inorganic materials 0.000 description 10
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 9
- 229920001940 conductive polymer Polymers 0.000 description 9
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 8
- 229910052802 copper Inorganic materials 0.000 description 8
- 239000010936 titanium Substances 0.000 description 8
- 239000000463 material Substances 0.000 description 7
- 229910000789 Aluminium-silicon alloy Inorganic materials 0.000 description 6
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 6
- 108010010803 Gelatin Proteins 0.000 description 6
- 229910052782 aluminium Inorganic materials 0.000 description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 6
- 229910052804 chromium Inorganic materials 0.000 description 6
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 229910016525 CuMo Inorganic materials 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical group [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 4
- 239000004411 aluminium Substances 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 4
- 229910052737 gold Inorganic materials 0.000 description 4
- 229910002804 graphite Inorganic materials 0.000 description 4
- 239000010439 graphite Substances 0.000 description 4
- 150000002739 metals Chemical class 0.000 description 4
- 229910052750 molybdenum Inorganic materials 0.000 description 4
- 239000011733 molybdenum Substances 0.000 description 4
- 229910052763 palladium Inorganic materials 0.000 description 4
- 229910052697 platinum Inorganic materials 0.000 description 4
- 229910052710 silicon Inorganic materials 0.000 description 4
- 239000010703 silicon Substances 0.000 description 4
- JBQYATWDVHIOAR-UHFFFAOYSA-N tellanylidenegermanium Chemical compound [Te]=[Ge] JBQYATWDVHIOAR-UHFFFAOYSA-N 0.000 description 4
- 229910052719 titanium Inorganic materials 0.000 description 4
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 4
- 229910052721 tungsten Inorganic materials 0.000 description 4
- 239000010937 tungsten Substances 0.000 description 4
- 238000001039 wet etching Methods 0.000 description 4
- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
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- 238000006056 electrooxidation reaction Methods 0.000 description 3
- 238000001755 magnetron sputter deposition Methods 0.000 description 3
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- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
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- 206010040844 Skin exfoliation Diseases 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 239000012752 auxiliary agent Substances 0.000 description 2
- 229910052796 boron Inorganic materials 0.000 description 2
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 239000004332 silver Substances 0.000 description 2
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- 241001062009 Indigofera Species 0.000 description 1
- 229910000990 Ni alloy Inorganic materials 0.000 description 1
- 229910001260 Pt alloy Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
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- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
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Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/02—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies
- H01L33/26—Materials of the light emitting region
- H01L33/30—Materials of the light emitting region containing only elements of Group III and Group V of the Periodic Table
- H01L33/32—Materials of the light emitting region containing only elements of Group III and Group V of the Periodic Table containing nitrogen
-
- 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/005—Processes
- H01L33/0062—Processes for devices with an active region comprising only III-V compounds
- H01L33/0075—Processes for devices with an active region comprising only III-V compounds comprising nitride compounds
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/02—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies
- H01L33/20—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies with a particular shape, e.g. curved or truncated substrate
- H01L33/22—Roughened surfaces, e.g. at the interface between epitaxial layers
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- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Recrystallisation Techniques (AREA)
- Led Devices (AREA)
Abstract
A kind of preparation method of GaN base compound substrate, the GaN base compound substrate successively includes thermal conductivity transfer substrate, bonding medium layer and GaN base epitaxial film from lower to upper, comprising the following steps: epitaxial growth GaN base epitaxial film obtains sapphire GaN base compound substrate on a sapphire substrate；Then bonding medium layer is prepared respectively on GaN base epitaxial film surface and thermal conductivity transfer substrate, then by GaN base epitaxial film together with thermal conductivity transfer substrate bonding；Obtain GaN base compound substrate after removing Sapphire Substrate again, GaN base epitaxial film transfer before, in transfer process and transfer after be selectively surface-treated.The advantages of present invention had not only taken into account the homoepitaxy that the compound substrate that previous transfer is realized has and can directly prepare vertical structure device, but also there is low-stress state and high-temperature stability, the quality of subsequent GaN epitaxy growth and chip preparation can be effectively improved.
Description
Technical field
The invention belongs to semiconductor photoelectronic device technical field, specifically a kind of preparation of GaN base compound substrate
Method.
Background technique
Broad stopband GaN base semiconductor material have excellent photoelectric characteristic, be widely used in make light emitting diode,
Laser, ultraviolet detector and high temperature, high frequency, high power electronic device, and can apply to high-end micro- needed for preparation aerospace
Electronic device has become international photoelectron neck such as high mobility transistor (HEMT) and heterojunction transistor (HFET)
The research hotspot in domain.And for crystalline epitaxial, no matter from epitaxial growth theoretically or semiconductor epitaxial technology
Developing history, all verified homoepitaxy is optimal selection.Extremely difficult, large size single crystal is prepared due to GaN body monocrystalline
GaN is difficult to directly obtain, and expensive, and the epitaxial growth of GaN material system is mainly based upon the hetero-epitaxy skill of big mismatch
Art.With the entirety progress of technology, GaN substrate technology of preparing has large increase, so that GaN epitaxy has returned homoepitaxy,
It can effectively improve GaN later period epitaxial crystal quality, but GaN single crystal substrate holds at high price, become and limit it and answer comprehensively
Main problem.
Homoepitaxy advantage and control cost in order to balance, some research institution has begun to focus on is turned using substrate
GaN epitaxy single crystalline layer is transferred on the substrate of the high conductivity of high heat conductance by shifting technology, prepares the GaN composite lining of thermal conductivity
Bottom.Number of patent application are as follows: 201210068033.0 and number of patent application are as follows: 201210068026.0 Chinese invention patent, it is public
A kind of combination MOCVD epitaxy technology of cloth, HVPE epitaxy technology, laser lift-off technique, bonding techniques are with micro-processing technology system
Standby novel compound lining material product and preparation method.The compound substrate had both taken into account homogeneity required for GaN extension
Extension improves crystal quality, and can directly prepare vertical structure LED, currently, preparing thermally conductive lead using substrate transfer technology
There are still some problems when electric GaN compound substrate: 1) bonding bonding strength is inadequate, moves back during subsequent homoepitaxy
Bonding and bubbling phenomenon；2) in bonding process, preparation process introduces very big stress, can cause residual stress in substrate
It is larger, to influence crystal quality and subsequent homoepitaxy effect；3) in nitrogen polarity thermal conductivity GaN compound substrate, laser stripping
It is serious from surface scaling loss, it is unfavorable for homoepitaxy, to influence device performance and stability.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of preparation method of GaN base compound substrate, by before transfer,
And/or the GaN base epitaxial film surface is surface-treated in transfer process, and/or after transfer, regulate and control surface roughness,
Bonding medium layer is improved in the adhesive force and corresponding bond strength on the surface GaN, and portion of residual can be discharged by rough surface
Stress, and can improve after nitrogen polarity laser lift-off, other substrate desquamation technologies and in substrate transfer technology to surface topography
Damage improves crystal quality and subsequent homoepitaxy effect, final to improve device performance and stability.
In order to solve the above-mentioned technical problem, the present invention takes following technical scheme:
A kind of preparation method of GaN base compound substrate is used to prepare the GaN base compound substrate of nitrogen polar surface upward, the GaN
Base compound substrate successively includes thermal conductivity transfer substrate, bonding medium layer and GaN base epitaxial film, this method packet from lower to upper
Include following steps:
S11, epitaxial growth GaN base epitaxial film obtains sapphire GaN base compound substrate on a sapphire substrate；
S13 prepares bonding medium layer on GaN base epitaxial film surface and thermal conductivity transfer substrate respectively, then will
The bonding medium layer on GaN base epitaxial film surface is bonded with the bonding medium layer on thermal conductivity transfer substrate, makes GaN base
Epitaxial film is obtained comprising Sapphire Substrate, GaN base epitaxial film, bonding medium layer and is led with thermal conductivity transfer substrate bonding
The semi-finished product compound substrate of thermal conductivity electrotransfer substrate；
S14 removes the Sapphire Substrate in semi-finished product compound substrate, is obtained outside the GaN base of nitrogen polar surface upward after cleaning
Prolong finished product GaN base compound substrate of the film together with thermal conductivity transfer substrate bonding；
GaN base epitaxial film surface in sapphire GaN base compound substrate obtained in step S11 is carried out at surface
Reason, and/or the GaN base epitaxial film surface after the Sapphire Substrate in the removal semi-finished product compound substrate of step S14 is carried out
Surface treatment.
A kind of preparation method of GaN base compound substrate is used to prepare the face-up GaN base compound substrate of gallium polarity, the GaN
Base compound substrate successively includes thermal conductivity transfer substrate, bonding medium layer and GaN base epitaxial film, this method packet from lower to upper
Include following steps:
S21, epitaxial growth GaN base epitaxial film obtains sapphire GaN base compound substrate on a sapphire substrate, using viscous
It connects agent GaN base epitaxial film is connected on interim transfer substrate, removes Sapphire Substrate；
S23 prepares bonding medium layer in GaN base epitaxial film and thermal conductivity transfer substrate surface, then by GaN respectively
The bonding medium layer on base epitaxial film surface is bonded with the bonding medium layer of thermal conductivity transfer substrate surface, realizes GaN
The strong conjunction of base epitaxial film and thermal conductivity transfer substrate bonding；
S24, in bonding process, bonding agent is carbonized at high temperature, it is interim shift substrate from GaN base epitaxial film surface from
It is dynamic to fall off, GaN of the face-up GaN base epitaxial film of gallium polarity together with thermal conductivity transfer substrate bonding is obtained after cleaning
Base compound substrate；
GaN base epitaxial film surface in sapphire GaN base compound substrate in step S21 is surface-treated, and/
Or the GaN base epitaxial film being connected to using bonding agent on interim transfer substrate and after removal Sapphire Substrate in step S21
Surface be surface-treated and/or step S24 in temporarily shift substrate from the GaN after the Automatic-falling of GaN base epitaxial film surface
Base epitaxial film surface is surface-treated.
The surface treatment is in dry etching, wet etching, electrochemical corrosion, photoelectrochemical etching and electrodeless corrosion
Any one, two or more combination.
For the temperature that the step S13 and step S23 is used when being bonded for 0 DEG C -2000 DEG C, pressure is 20 kilogram/square English
It is very little to 20 tons/square inch.
The bonding medium layer with a thickness of 10 nanometers to 100 microns；Thermal conductivity shift substrate with a thickness of 10 microns
To 3000 microns.
The bonding medium layer is molybdenum (Mo), gold (Au), titanium (Ti), copper (Cu), palladium (Pd), tungsten (W), nickel (Ni), platinum
(Pt) and any one elemental metals or two or more alloy in chromium (Cr)；Or bonding medium layer is resin base
It is any in body and conducting particles silver-colored (Ag), golden (Au), copper (Cu), aluminium (Al), zinc (Zn), iron (Fe), nickel (Ni) and graphite (C)
A kind of, two or more composition conducting polymer；Or bonding medium layer is conducting particles silver (Ag), gold (Au), copper
(Cu), any one in aluminium (Al), zinc (Zn), iron (Fe), nickel (Ni) and graphite (C), two or more particle with
Adhesive, solvent, electrocondution slurry or bonding medium layer composed by auxiliary agent are silicate-base high-temperature electric conduction glue；Or bonding
Dielectric layer is the high temperature alloy slurry that nickel (Ni), chromium (Cr), silicon (Si) and boron (B) are formed.
The bonding medium layer utilizes magnetron sputtering, plating, vacuum thermal evaporation or wet processing, prepares in GaN base extension
The surface of film and thermal conductivity transfer substrate.
The thermal conductivity transfer substrate is molybdenum (Mo), titanium (Ti), palladium (Pd), copper (Cu), tungsten (W), nickel (Ni), platinum (Pt)
It is brilliant with one of chromium (Cr) elemental metals or two or more alloy or silicon (Si) crystal, silicon carbide (SiC)
Body or silicated aluminum (AlSi) crystal.
The GaN base epitaxial film with a thickness of 10 nanometers to 100 microns.
The GaN base epitaxial film be in GaN film, AlN film and InN film any one, two kinds or three kinds
Alloy firm.
The present invention is surface-treated in the preparation process of compound substrate, and the face Ga of GaN base epitaxial film is either shelled
The face N from after is surface-treated, and surface roughness is regulated and controled, and improves bonding medium layer in the adhesive force on the surface GaN and corresponding
Bond strength, and portion of residual stress can be discharged by rough surface, and nitrogen polarity laser lift-off, other substrate desquamations can be improved
To the damage of surface topography after technology and in substrate transfer technology, crystal quality and subsequent homoepitaxy effect are improved, finally
Improve device performance and stability.
Detailed description of the invention
Attached drawing 1 is the schematic diagram of the section structure for the GaN base compound substrate that the present invention is prepared；
Attached drawing 2 is the process schematic that the present invention is used to prepare the face-up GaN base compound substrate of gallium polarity；
Attached drawing 3 is the process schematic that the present invention is used to prepare the GaN base compound substrate of nitrogen polar surface upward；
Attached drawing 4 is the preparation process schematic diagram of the embodiment of the present invention one；
Attached drawing 5-1 is the preparation process schematic diagram of the embodiment of the present invention two；Attached drawing 5-2 is the preparation of the embodiment of the present invention two
Process schematic；Attached drawing 5-3 is the preparation process schematic diagram of the embodiment of the present invention two；Attached drawing 5-4 is the embodiment of the present invention two
Preparation process schematic diagram；
Attached drawing 6-1 is the preparation process schematic diagram of the embodiment of the present invention three；Attached drawing 6-2 is the preparation of the embodiment of the present invention three
Process schematic；Attached drawing 6-3 is the preparation process schematic diagram of the embodiment of the present invention three；Attached drawing 6-4 is the embodiment of the present invention three
Preparation process schematic diagram；Attached drawing 6-5 is the preparing processes schematic diagram of the embodiment of the present invention three；
Attached drawing 7-1 is the preparation process schematic diagram of the embodiment of the present invention four；Attached drawing 7-2 is the preparation of the embodiment of the present invention four
Process schematic；Attached drawing 7-3 is the preparation process schematic diagram of the embodiment of the present invention four；Attached drawing 7-4 is the embodiment of the present invention four
Preparation process schematic diagram；Attached drawing 7-5 is the preparation process schematic diagram of the embodiment of the present invention four；Attached drawing 7-6 is the embodiment of the present invention
Four preparation process schematic diagram.
Appended drawing reference
Bonding medium layer -1；GaN base epitaxial film -2；Bonding agent -3；AlGaN base epitaxial film -4.
Specific embodiment
For the ease of the understanding of those skilled in the art, the present invention is made in the following with reference to the drawings and specific embodiments further
Description.
Preparation method of the invention can be used for preparing nitrogen polar surface GaN base compound substrate upward or gallium polar surface court
On GaN base compound substrate.
As shown in attached drawing 1 and 3, a kind of preparation method of GaN base compound substrate is used to prepare the GaN of nitrogen polar surface upward
Base compound substrate, the GaN base compound substrate successively include thermal conductivity transfer substrate, bonding medium layer 1 and GaN base from lower to upper
Epitaxial film 2, method includes the following steps:
S11, epitaxial growth GaN base epitaxial film 2 obtains sapphire GaN base compound substrate on a sapphire substrate.
S13 prepares bonding medium layer 1 on 2 surface of GaN base epitaxial film and thermal conductivity transfer substrate, then respectively
The bonding medium layer 1 on 2 surface of GaN base epitaxial film is bonded with the bonding medium layer 1 on thermal conductivity transfer substrate, is made
GaN base epitaxial film 2 obtains comprising Sapphire Substrate with thermal conductivity transfer substrate bonding, GaN base epitaxial film 2, is bonded Jie
The semi-finished product compound substrate of matter layer 1 and thermal conductivity transfer substrate, the temperature that when bonding uses is 0 DEG C -2000 DEG C, pressure 20
Kilogram/square inch is to 20 tons/square inch.
S14 removes the Sapphire Substrate in semi-finished product compound substrate, is obtained outside the GaN base of nitrogen polar surface upward after cleaning
Prolong finished product GaN base compound substrate of the film together with thermal conductivity transfer substrate bonding.
GaN base epitaxial film surface in sapphire GaN base compound substrate obtained in step S11 is carried out at surface
Reason, and/or the GaN base epitaxial film surface after the Sapphire Substrate in the removal semi-finished product compound substrate of step S14 is carried out
Surface treatment.
As shown in figure 1 and 2, a kind of preparation method of GaN base compound substrate, is used to prepare the face-up GaN of gallium polarity
Base compound substrate, the GaN base compound substrate successively include thermal conductivity transfer substrate, bonding medium layer 1 and GaN base from lower to upper
Epitaxial film 2, method includes the following steps:
S21, epitaxial growth GaN base epitaxial film 2 obtains sapphire GaN base compound substrate on a sapphire substrate, uses
GaN base epitaxial film 2 is connected on interim transfer substrate by bonding agent 3, removes Sapphire Substrate.
S23 prepares bonding medium layer 1 in GaN base epitaxial film 2 and thermal conductivity transfer substrate surface respectively, then will
The bonding medium layer 1 on 2 surface of GaN base epitaxial film is bonded with the bonding medium layer 1 of thermal conductivity transfer substrate surface, real
The strong conjunction of existing GaN base epitaxial film 2 and thermal conductivity transfer substrate bonding, the temperature that when bonding uses are pressed for 0 DEG C -2000 DEG C
Power is 20 kilograms/square inch to 20 tons/square inch.
S24, in bonding process, bonding agent 3 is carbonized at high temperature, and the interim substrate that shifts is from 2 surface of GaN base epitaxial film
Automatic-falling obtains the face-up GaN base epitaxial film of gallium polarity together with thermal conductivity transfer substrate bonding after cleaning
GaN base compound substrate.
GaN base epitaxial film surface in sapphire GaN base compound substrate in step S21 is surface-treated, and/
Or the GaN base epitaxial film being connected to using bonding agent on interim transfer substrate and after removal Sapphire Substrate in step S21
Surface be surface-treated and/or step S24 in temporarily shift substrate from the GaN after the Automatic-falling of GaN base epitaxial film surface
Base epitaxial film surface is surface-treated.
The surface treatment is in dry etching, wet etching, electrochemical corrosion, photoelectrochemical etching and electrodeless corrosion
Any one, two or more combination.Wherein dry etching is carried out in the equipment such as HVPE, MOCVD, ICP,
Wet etching is carried out in the solution such as phosphoric acid, sulfuric acid, hydrochloric acid, potassium hydroxide, sodium hydroxide.Dry etching, wet process are carved
Erosion, electrochemical corrosion, photoelectrochemical etching and electrodeless corrosion concrete operations mode, be the known of those skilled in the art
Common sense, in this not go into detail.
In addition, bonding medium layer with a thickness of 10 nanometers to 100 microns；Thermal conductivity shift substrate with a thickness of 10 microns
To 3000 microns.
The bonding medium layer is molybdenum (Mo), gold (Au), titanium (Ti), copper (Cu), palladium (Pd), tungsten (W), nickel (Ni), platinum
(Pt) and any one elemental metals or two or more alloy in chromium (Cr)；Or bonding medium layer is resin base
It is any in body and conducting particles silver-colored (Ag), golden (Au), copper (Cu), aluminium (Al), zinc (Zn), iron (Fe), nickel (Ni) and graphite (C)
A kind of, two or more composition conducting polymer；Or bonding medium layer is conducting particles silver (Ag), gold (Au), copper
(Cu), any one in aluminium (Al), zinc (Zn), iron (Fe), nickel (Ni) and graphite (C), two or more particle with
Adhesive, solvent, electrocondution slurry or bonding medium layer composed by auxiliary agent are silicate-base high-temperature electric conduction glue；Or bonding
Dielectric layer is the high temperature alloy slurry that nickel (Ni), chromium (Cr), silicon (Si) and boron (B) are formed.
The bonding medium layer utilizes magnetron sputtering, plating, vacuum thermal evaporation or wet processing, prepares in GaN base extension
The surface of film and thermal conductivity transfer substrate.
The thermal conductivity transfer substrate is molybdenum (Mo), titanium (Ti), palladium (Pd), copper (Cu), tungsten (W), nickel (Ni), platinum (Pt)
It is brilliant with one of chromium (Cr) elemental metals or two or more alloy or silicon (Si) crystal, silicon carbide (SiC)
Body or silicated aluminum (AlSi) crystal.
The GaN base epitaxial film with a thickness of 10 nanometers to 100 microns.GaN base epitaxial film is GaN film, AlN thin
In film and InN film any one, the alloy firms of two kinds or three kinds.
Further illustrate is made to the present invention with preferable specific embodiment below.
Embodiment one
As shown in Fig. 4, a kind of preparation method of GaN base compound substrate, before transfer to GaN base epitaxial film surface into
Row surface treatment, the surface treatment carry out dry etching using HVPE equipment, and 1 material of bonding medium layer uses Au, thermal conductivity
Shift substrate use Si substrate, be used to prepare the GaN base compound substrate of nitrogen polar surface upward, preparation method the following steps are included:
S11, epitaxial growth GaN base epitaxial film 2 obtains sapphire GaN base compound substrate on a sapphire substrate.Specifically
First to use 4.5 microns of thick GaN bases of MOCVD technology epitaxial growth in 2 inches 430 microns thick of plate Sapphire Substrate
Epitaxial film, then grown in HVPE and thicken the GaN base epitaxial film growth to 35 microns.
The GaN base epitaxial film surface 2 of obtained sapphire GaN base compound substrate is passed through by S12 in HVPE equipment
Dry etching 2 hours at 890 DEG C of HCl gas.
S13, surface and 400 microns thick of Si substrate face after the etching of GaN base epitaxial film 2, uses magnetic control respectively
Sputtering prepares 1 micron thick of Au bonding medium layer 1, and then at 600 DEG C of temperature, pressure is to carry out bonding in 80 minutes under 4T, real
Existing GaN base epitaxial film is bonded with Si substrate, obtains semi-finished product compound substrate.
S14 removes the Sapphire Substrate in semi-finished product compound substrate, then to the semi-finished product using laser lift-off technique
Compound substrate carries out the surface cleans techniques such as hydrochloric acid, acetone, obtains AuAu bonding, device architecture is followed successively by GaN base from lower to upper
Epitaxial film/Au bonding medium layer/Au bonding medium layer/Si substrate low-stress state nitrogen polar GaN base compound substrate.
Embodiment two
A kind of preparation method of GaN base compound substrate, before transfer and transfer after the completion of to GaN base epitaxial film surface into
Row surface treatment, the surface treatment carry out dry etching using HVPE equipment and ICP equipment, and 1 material of bonding medium layer uses Ni/
Pt alloy, thermal conductivity shift substrate and use AlSi substrate, are used to prepare the GaN base compound substrate of nitrogen polar surface upward, prepare
Method the following steps are included:
S11, on a sapphire substrate epitaxial growth GaN base epitaxial film 2.Specially in 2 inches of 430 microns of thick plates
In Sapphire Substrate, GaN base epitaxial film first thick using 4.5 microns of MOCVD technology epitaxial growth, then should in HVPE
GaN base epitaxial film growth is thickeied to 30 microns.
2 surface of GaN base epitaxial film of above-mentioned sapphire GaN base compound substrate is etched 30 points by S12 in HVPE equipment
Clock, as shown in attached drawing 5-1.
S13, surface and 150 microns thick of AlSi substrate face after obtained GaN base epitaxial film 2 etches, respectively
1 micron thick Ni and 5 micron of thickness Pt conductive bond dielectric layer 1 is prepared using magnetron sputtering, then at 500 DEG C of temperature, pressure 12T
Under, bonding in 120 minutes is carried out, realization GaN base epitaxial film 2 is bonded with AlSi substrate, obtains semi-finished product compound substrate, such as
Shown in attached drawing 5-2.
(4) as shown in attached drawing 5-3 and attached drawing 5-4, using laser lift-off technique, the indigo plant removed in semi-finished product compound substrate is precious
Then stone lining bottom carries out dry etching using ICP to 2 surface of GaN base epitaxial film of the semi-finished product compound substrate, using salt
After the surface cleans technique such as acid, acetone, obtain Ni/Pt bonding, device architecture be followed successively by from top to bottom for GaN base epitaxial film/
Ni/Pt bonding medium layer/Pt/Ni bonding medium layer/AlSi substrate low-stress state nitrogen polar GaN base compound substrate.
Embodiment three
A kind of preparation method of GaN base compound substrate carries out at surface the GaN base epitaxial film surface after once inside out
Reason, using ICP equipment dry etching, 1 material of bonding medium layer uses high temperature alloy slurry NiCrSiB, thermal conductivity transfer lining
Bottom uses CuW substrate, and bonding agent 3 uses 502 quick-drying gelatins, and the interim substrate that shifts is ceramic substrate, is used to prepare gallium polar surface court
On GaN base compound substrate, preparation method the following steps are included:
S21, on a sapphire substrate epitaxial growth GaN base epitaxial film 2.Specially in 2 inches of 430 microns of thick plates
In Sapphire Substrate, GaN base epitaxial film first thick using 4.5 microns of MOCVD technology epitaxial growth then should in HVPE
GaN base epitaxial film growth is thickeied to 25 microns, and the GaN base epitaxial film 2 is then adhered to 2 inches using 502 quick-drying gelatins 3
In 300 microns thick ceramic substrates, then Sapphire Substrate is removed to get to being bonded in ceramic substrate using laser lift-off technique
On GaN base epitaxial film, as in Figure 6-1.
2 surface of GaN base epitaxial film of bonding on a ceramic substrate is carried out in ICP equipment dry etching 30 and divided by S22
Clock obtains uniform outer surface.
S23, surface and CuW substrate face after the etching of GaN base epitaxial film 2, respectively using knife coating procedure preparation 10
The NiCrSiB layer of micron, as bonding medium layer 1, then at 1300 DEG C of temperature, pressure is to carry out 60 minutes high temperature under 8T
Diffusion interlinked, realization GaN base epitaxial film is bonded with CuW substrate, as shown in attached drawing 6-2 and attached drawing 6-3.
(4) as shown in attached drawing 6-4 and attached drawing 6-5, in bonding process, 502 quick-drying gelatins 3 are carbonized at high temperature, ceramic liner
Bottom carries out the surface cleans techniques such as hydrochloric acid, acetone from 2 surface Automatic-falling of GaN base epitaxial film, to compound substrate obtained,
It is finally obtained to be due to have passed through gluing before and after GaN base epitaxial film and high temperature alloy slurry medium is overturn twice
NiCrSiB bonding, device architecture be followed successively by from top to bottom for GaN base epitaxial film/NiCrSiB bonding medium layer/
NiCrSiB bonding medium layer/CuW substrate gallium polarity up, suitable for GaN isoepitaxial growth low-stress state it is multiple
Close substrate.
Example IV
A kind of preparation method of GaN base compound substrate, while melting is used to GaN base epitaxial film surface before transfer
The ICP dry etching on GaN base epitaxial film surface and final GaN base compound substrate after the removing of KOH burn into Sapphire Substrate
The processing of surface MOCVD dry etching, 1 material of bonding medium layer use elargol Ag Paste, and thermal conductivity shifts substrate and uses
CuMo substrate, bonding agent 3 use 502 quick-drying gelatins, and the interim substrate that shifts is glass substrate, using AlGaN base epitaxial film 4, system
The standby face-up GaN base compound substrate of gallium polarity, preparation method the following steps are included:
S21 first uses 4.5 microns of MOCVD technology epitaxial growth in 2 inches 430 microns thick of plate Sapphire Substrate
Then thick AlGaN base epitaxial film 4 corrodes the AlGaN base epitaxial film 4 in melting KOH, utilizes wet etching
Processing mode processing, then reuses 502 quick-drying gelatins 3 for the AlGaN base epitaxial film 4 and is adhered to 2 inch of 500 micron thick glass
On substrate, then Sapphire Substrate is removed to get arriving outside the AlGaN base of bonding on a glass substrate using laser lift-off technique
Prolong film 4, as shown in attached drawing 7-1.
S22 carries out AlGaN base epitaxial film 4 obtained in step S21 dry etching 20 minutes in ICP equipment,
Uniform outer surface is obtained, as shown in attached drawing 7-2.
S23, surface and CuMo substrate face to AlGaN base epitaxial film 4 prepare 50 microns using spin coating method respectively
Elargol layer, as bonding medium layer 1, then at 300 DEG C of temperature, pressure is to carry out bonding in 120 minutes under 15T, is realized
AlGaN base epitaxial film 4 is bonded with CuMo substrate, as shown in attached drawing 7-3 and shown in attached drawing 7-4.
S24, as shown in attached drawing 7-5 and attached drawing 7-6, in bonding process, 502 quick-drying gelatins 3 are carbonized at high temperature, glass lined
Bottom from 4 surface Automatic-falling of AlGaN base epitaxial film, then again to 4 surface of AlGaN base epitaxial film in MOCVD device into
Row dry etching 30 minutes, after then passing through the surface cleans technique such as hydrochloric acid, acetone, finally obtained was elargol bonding, device
Structure is followed successively by AlGaN base epitaxial film/Ag Paste bonding medium layer/Ag Paste bonding medium layer/CuMo from top to bottom
The gallium polarity of substrate up, suitable for the low-stress state compound substrate of GaN isoepitaxial growth.
It should be noted that the description of the above various embodiments is not limited to the present invention, it is of the invention not departing from
Under the premise of concept, it is any obviously replace it is within the scope of the present invention.
Claims (3)
1. a kind of preparation method of GaN base compound substrate, is used to prepare the GaN of nitrogen polar surface upward
Base compound substrate, the GaN base compound substrate from lower to upper successively include thermal conductivity transfer substrate, bonding medium layer and
GaN base epitaxial film, method includes the following steps:
S11, epitaxial growth GaN base epitaxial film obtains sapphire GaN base compound substrate on a sapphire substrate；
S13 prepares bonding medium layer on GaN base epitaxial film surface and thermal conductivity transfer substrate, then by GaN base respectively
The bonding medium layer on epitaxial film surface is bonded with the bonding medium layer on thermal conductivity transfer substrate, makes GaN base extension
Film and thermal conductivity transfer substrate bonding are obtained comprising Sapphire Substrate, GaN base epitaxial film, bonding medium layer and thermally conductive are led
The semi-finished product compound substrate of electrotransfer substrate；
S14 removes the Sapphire Substrate in semi-finished product compound substrate, it is thin that the GaN base extension of nitrogen polar surface upward is obtained after cleaning
Finished product GaN base compound substrate of the film together with thermal conductivity transfer substrate bonding；
Hydrochloric acid, third are successively carried out to the GaN base epitaxial film surface in sapphire GaN base compound substrate obtained in step S11
Ketone cleaning, removes surface contaminant, dry etching surface treatment is carried out using HVPE equipment, to improve surface topography and surface
Can, metallic dielectric layer is improved in the adhesive force and corresponding bond strength of GaN base epitaxial film surface；
And/or successively to the GaN base epitaxial film surface after the Sapphire Substrate in the removal semi-finished product compound substrate of step S14
Hydrochloric acid, acetone cleaning are carried out, surface contaminant is removed, HVPE equipment is reused and ICP equipment carries out dry etching surface treatment,
It is acted on by dry etching and repairs the surface damage caused by epitaxial film when removing Sapphire Substrate, to improve GaN base epitaxial film
Surface roughness and pattern.
2. a kind of preparation method of GaN base compound substrate is used to prepare the face-up GaN base compound substrate of gallium polarity, the GaN base
Compound substrate successively includes that thermal conductivity transfer substrate, bonding medium layer and GaN base epitaxial film, this method include from lower to upper
Following steps:
S21, epitaxial growth GaN base epitaxial film obtains sapphire GaN base compound substrate on a sapphire substrate, uses bonding agent
GaN base epitaxial film is connected on interim transfer substrate, Sapphire Substrate is removed；
S23 prepares bonding medium layer in GaN base epitaxial film and thermal conductivity transfer substrate surface respectively, then will be outside GaN base
The bonding medium layer for prolonging film surface is bonded with the bonding medium layer of thermal conductivity transfer substrate surface, is realized outside GaN base
Prolong the strong conjunction of film and thermal conductivity transfer substrate bonding；
S24, in bonding process, bonding agent is carbonized at high temperature, and the interim substrate that shifts takes off automatically from GaN base epitaxial film surface
It falls, it is multiple that GaN base of the face-up GaN base epitaxial film of gallium polarity together with thermal conductivity transfer substrate bonding is obtained after cleaning
Close substrate；
To the GaN base epitaxial film surface in the sapphire GaN base compound substrate in step S21, it is clear successively to carry out hydrochloric acid, acetone
It washes, removes surface contaminant, then dry etching surface treatment is carried out using ICP equipment, to improve surface topography and surface energy, mention
The adhesive force and corresponding bond strength of high GaN base epitaxial film surface；
And/or to the GaN base being connected to using bonding agent on interim transfer substrate and after removal Sapphire Substrate in step S21
Epitaxial film surface successively carries out hydrochloric acid, acetone cleaning, removes surface contaminant, then carry out dry etching using MOCVD device
Surface treatment is acted on by dry etching and repairs the surface damage caused by epitaxial film when removing Sapphire Substrate, to improve GaN
The surface roughness and pattern of based epitaxial film improve the adhesive force and corresponding bond strength of subsequent metal dielectric layer；
And/or to temporarily shifting substrate in step S24 from the GaN base epitaxial film after the Automatic-falling of GaN base epitaxial film surface
Surface carries out inductively coupled plasma body (ICP) surface treatment, passes through when dry etching effect reparation removal Sapphire Substrate pairs
Surface damage caused by epitaxial film to improve the surface roughness and pattern of GaN base epitaxial film, then successively carries out acetone, hydrochloric acid
Cleaning, removes the pollutant on surface.
3. the preparation method of GaN base compound substrate according to claim 2, which is characterized in that
For the temperature that the step S23 is used when being bonded for 0 DEG C -2000 DEG C, pressure is 20 kilograms/square inch to 20 tons/square
Inch.
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| TWI618244B (en) | 2017-06-06 | 2018-03-11 | Huang Zhi Shu | N-face III family/nitride epitaxial structure and active element and polarity inversion manufacturing method thereof |
| CN107634104B (en) * | 2017-08-31 | 2021-06-11 | 北京世纪金光半导体有限公司 | High-heat-dissipation GaN diode structure with buried metal layer and preparation method thereof |
| US20230154785A1 (en) * | 2020-08-13 | 2023-05-18 | Enkris Semiconductor, Inc. | N-face polar gan-based device and composite substrate thereof, and method of manufacturing composite substrate |
| CN112216610A (en) * | 2020-10-10 | 2021-01-12 | 东莞市中镓半导体科技有限公司 | Preparation method of HEMT (high electron mobility transistor) based on sapphire substrate |
| CN112967992B (en) * | 2020-12-07 | 2022-09-23 | 重庆康佳光电技术研究院有限公司 | Transfer method of epitaxial structure |
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| JP2003165798A (en) * | 2001-11-28 | 2003-06-10 | Hitachi Cable Ltd | Method for producing gallium nitride single crystal substrate, free standing substrate for epitaxial growth of gallium nitride single crystal, and device element formed on the same |
| CN103305909A (en) * | 2012-03-14 | 2013-09-18 | 东莞市中镓半导体科技有限公司 | Preparation method of composite substrate for GaN growth |
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| JP2003165798A (en) * | 2001-11-28 | 2003-06-10 | Hitachi Cable Ltd | Method for producing gallium nitride single crystal substrate, free standing substrate for epitaxial growth of gallium nitride single crystal, and device element formed on the same |
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