WO1998047185A1 - Recovery of surface-ready silicon carbide substrates - Google Patents
Recovery of surface-ready silicon carbide substrates Download PDFInfo
- Publication number
- WO1998047185A1 WO1998047185A1 PCT/US1998/006836 US9806836W WO9847185A1 WO 1998047185 A1 WO1998047185 A1 WO 1998047185A1 US 9806836 W US9806836 W US 9806836W WO 9847185 A1 WO9847185 A1 WO 9847185A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- group iii
- silicon carbide
- epitaxial layer
- layer
- iii nitride
- Prior art date
Links
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices with at least one potential-jump barrier or surface barrier 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
- H01L33/0066—Processes for devices with an active region comprising only III-V compounds with a substrate not being a III-V compound
- H01L33/007—Processes for devices with an active region comprising only III-V compounds with a substrate not being a III-V compound comprising nitride compounds
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10S438/00—Semiconductor device manufacturing: process
- Y10S438/931—Silicon carbide semiconductor
Definitions
- the present invention relates to the manufacture of semiconductor devices from wide-bandgap materials, and in particular relates to a method of recovering silicon carbide substrates from composite structures of such substrates with Group III nitride epitaxial layers .
- the present invention relates to the recent increase in the research, development, manufacture and use of electronic devices made from wide-bandgap semiconductors, specifically including silicon carbide (SiC) and Group III nitrides (i.e., Group III of the Periodic Table: B, Al , Ga, In, Tl) such as gallium nitride (GaN) . Both of these materials have generated such interest for several reasons. Silicon carbide is an attractive candidate material for semiconductor applications because of its wide bandgap (2.99 eV for alpha-SiC at 300K) and its other exceptional electronic, physical, thermal and chemical properties.
- SiC silicon carbide
- Group III nitrides i.e., Group III of the Periodic Table: B, Al , Ga, In, Tl
- GaN gallium nitride
- Gallium nitride although not sharing all of the same physical properties as silicon carbide offers the electronic advantage of being a wide-bandgap (3.36 eV at 300K) directtransition emitter. Stated somewhat differently, both silicon carbide and gallium nitride are ideal candidate materials for producing light emitting diodes (EDs) that because of their wide bandgaps, are capable of emitting at higher energies. In terms of the characteristics of light, higher energy represents higher frequencies and longer wavelengths.
- EDs light emitting diodes
- gallium nitride and silicon carbide have bandgaps sufficiently wide to allow them to emit light in the blue portion of the visible spectrum (i.e., wavelengths of between about 455 and 492 nanometers, nm) , a color that cannot be directly produced by most other semiconductor materials.
- a thorough discussion of optoelectronic devices, and their design, the theory behind their operation, is set forth in Sze, Physics of Semiconductor Devices, (1981) , and particularly in Chapter 12, pages 681-742, with related discussions of photodetectors in Chapter 13 (page 743 ) and solar cells in Chapter 14 (page 790 ) . Such background and theory will not be discussed further herein other than as necessary to describe the present invention.
- gallium nitride is a direct emitter in which all of the energy generated by a transition is emitted as light.
- gallium nitride offers the possibility for more efficient LEDs, than does silicon carbide.
- gallium nitride has not been produced in bulk crystal form, and thus in order to form an LED or other optoelectronic device from gallium nitride, epitaxial layers of gallium nitride must be formed on some suitable substrate material .
- sapphire has been the preferred substrate material for gallium nitride because of its physical properties and because of the generally satisfactory crystal lattice match between gallium nitride and sapphire (A1 2 0 3 ) .
- Sapphire cannot be made electronically conductive, however, and thus the physical geometry of LEDs formed from gallium nitride epitaxial layers on sapphire substrates are typically of the "same side" variety rather than the generally more preferred “vertical” LED geometry.
- the term “vertical” refers to an LED in which the ohmic contacts can be placed on opposite faces of the device rather than on a common face .
- silicon carbide provides an excellent substrate material for gallium nitride and other Group III nitride devices. Accordingly, many recent advances in the production of blue LEDs have been based upon a combination of such gallium nitride epitaxial layers on silicon carbide substrates .
- GaN-SiC devices Although the manufacture of such GaN-SiC devices has progressed rapidly, epitaxial growth of such materials such as gallium nitride on silicon carbide continues to represent a complex process, and one in which a substantial proportion of attempts produce device precursors that are unsatisfactory for one or more reasons .
- a GaN on SiC LED typically consists of an SiC substrate with a back ohmic contact, one or more buffer layers on the SiC substrate that provide a crystal lattice transition between the SiC and the GaN, and at least two epitaxial layers of gallium nitride on the buffer layer.
- the gallium nitride layers include at least one p-type layer and one n-type layer adjacent one another to form the p-n junction of the device.
- a top ohmic contact is usually made to the top layer of gallium nitride, or in some cases to another material that for some other desired reason forms the top layer of the device.
- wafers semiconductor substrates are typically sliced from bulk crystals in the form of circular disks, generally referred to as "wafers," upon which various other layers, such as epitaxial layers of GaN, are formed. Because the bulk growth of silicon carbide and the preparation of silicon carbide wafers are both processes which represent significant technical challenge and economic investment, the wafers are in turn quite valuable. If, however, after the gallium nitride epitaxial layers are grown on the SiC wafer, they are found to be defective, or simply unsatisfactory from a desired quality standpoint, the entire wafer becomes a waste product. Thus, a need exists for removing gallium nitride from silicon carbide in a manner that preserves the silicon carbide wafer.
- gallium nitride (and other Group III nitride) epitaxial layers required to produce appropriate LEDs are similarly much more resistant to the normal techniques (typically wet or dry etching) used to remove unwanted material in conventional semiconductor processes.
- the invention meets this object with the method of recovering such substrates by subjecting a Group III nitride epitaxial layer on a silicon carbide substrate to a stress that sufficiently increases the number of dislocations in the epitaxial layer to make the epitaxial layer subject to attack and dissolution in a mineral acid, but that otherwise does not affect the silicon carbide substrate, and thereafter contacting the epitaxial layer with a mineral acid to remove the Group III nitride while leaving the silicon carbide substrate unaffected.
- the invention is a method of recovering surface-ready silicon carbide substrates from heteroepitaxial structures of Group III nitrides on silicon carbide substrates.
- the method comprises subjecting the Group III nitride epitaxial layer on a silicon carbide substrate to a stress that sufficiently increases the number of dislocations in the epitaxial layer to make the epitaxial layer subject to attack and dissolution in a mineral acid, but that otherwise does not affect the silicon carbide substrate. Thereafter, the epitaxial layer is contacted with a mineral acid to remove the Group III nitride while leaving the silicon carbide substrate unaffected.
- gallium nitride is the most commonly used Group III nitride for LEDs, the specification will often refer to gallium nitride. It will be understood, however, that the invention embraces all of the Group III nitrides described above, including binary, ternary, and tertiary nitrides. Such binary nitrides also include aluminum nitride (AlN) and indium nitride (InN) . Ternary nitrides include those often referred to as "aluminum gallium nitride," and which are typically designated by the empirical formula Al x Ga 1-x N.
- Tertiary Group III nitrides refer for example to indium aluminum gallium nitride, which is similarly designated In x Al y Ga 1 . x _ y N.
- the reasons for using gallium nitride, aluminum, Y gallium nitride, or other ternary or tertiary nitrides are set forth in exemplary, but certainly not limiting, fashion in U.S. Patent No. 5,523,589; 5,592,501; and 5,739,554; all of which are commonly assigned with the present invention.
- crystal defects referred to herein, although frequently labeled as “dislocations,” include, but are not limited to, slips, edge dislocations, and screw dislocations.
- a first technique is to raise the temperature of the substrate and the epitaxial layers to a temperature sufficient to dissociate the gallium nitride.
- this technique comprises heating the substrate and epitaxial layers to temperatures of about 1000°C in the presence of oxygen or argon.
- the equipment used for these heating steps is otherwise conventional in this art, and can be used to practice the invention without undue experimentation.
- the stress step comprises exposing the substrate and epitaxial layers to rapid thermal annealing (RTA) .
- RTA rapid thermal annealing
- rapid thermal annealing refers to the technique generally well understood in the semiconductor arts in which an item such as a semiconductor material is placed in a device that, because of its physical capabilities, can raise the temperature of the semiconductor material very quickly; i.e., on the order of about 10°C per second.
- the lattice mismatch between the gallium nitride and silicon carbide even in the presence of a buffer layer
- the mismatch creates or increases the number of defects in the crystal, particularly dislocation defects, that permit the mineral acid to attack and remove the Group III nitride.
- the rapid thermal annealing is carried out at relatively low pressure (e.g., about 10 " ⁇ torr) , while in other circumstances, the rapid thermal annealing can be carried out in an ambient atmosphere (air) at high temperatures (e.g., 1050°C) .
- the step of subjecting the Group III nitride layer to stress can comprise physically abrading the layer, for example by bombarding it with silicon carbide or aluminum oxide powders. It presently appears, however, that such physical abrasion methods may cause underlying damage to the silicon carbide substrate as well, which is a less desirable result.
- the step of contacting the epitaxial layer with a mineral acid comprises contacting the layer with phosphoric acid (H 3 P0 4 ) .
- H 3 P0 4 phosphoric acid
- the etching apparatus comprises a quartz beaker and a ollam condenser. The condenser keeps the H 3 P0 4 solution at 85% by preventing water from evaporating.
- the difficulty in removing the gallium nitride from the substrate relates back to the quality of the gallium nitride epitaxial layer, which in turn relates back to the method by which it is produced.
- the invention comprises the step of depositing the Group III nitride epitaxial layer on the substrate prior to the step of subjecting the layer to stress. More particularly, it has been found that electronically high quality Group III nitride epitaxial layers, and thus those hardest to remove, tend to be produced by metal organic chemical vapor deposition (MOCVD) , and are typically of higher quality than those produced by vapor phase epitaxy (VPE) .
- MOCVD metal organic chemical vapor deposition
- VPE vapor phase epitaxy
- vapor phase epitaxy refers to processes such as those in which a gas (such as a blend of hydrogen chloride and hydrogen) is bubbled through liquid gallium to produce a gallium chloride vapor, which is then directed to react with a nitrogen containing gas, typically ammonia (NH 3 ) , to form gallium nitride.
- a gas such as a blend of hydrogen chloride and hydrogen
- a nitrogen containing gas typically ammonia (NH 3 )
- MOCVD uses a metal organic compound (in which the Group III element is the metal) in the vapor phase.
- the vapor phase compound will dissociate to form metal radicals. These radicals in turn react with the nitrogen containing gas (again typically ammonia) to form the Group III nitride.
- Trimethyl gallium (TMG,” (CH 3 ) 3 Ga) is a preferred metal organic source for gallium.
- the step of depositing the Group III nitride epitaxial layer on the silicon carbide substrate preferably comprises MOCVD.
- the MOCVD is preferably carried out from a vapor phase reaction between an organic Group III compound such as TMG, and ammonia (NH 3 ) .
- the invention is not limited by the method in which the Group III nitride layers are deposited.
- Other appropriate methods can include (but are not limited to) molecular beam epitaxy (MBE) , the aforementioned VPE, and liquid phase epitaxy (LPE) .
- a preferred embodiment of the present invention further comprises depositing such a buffer layer on the silicon carbide substrate prior to the step of depositing the Group III nitride epitaxial layers.
- Appropriate buffer layers are described in several of the patents already cited as well in U.S. Patent No. 5,393,993, which is commonly assigned with the present invention, and which is incorporated entirely herein by reference. The method of the invention removes these buffer layers as well.
- the invention produces a silicon carbide wafer that is otherwise indistinguishable from wafers that have never carried Group III nitride epitaxial layers .
- Such recovered wafers can accordingly be used or processed in the same manner as "new" wafers, thus offering significant gains in the efficiency and economy of wafer and device production.
Abstract
Description
Claims
Priority Applications (7)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE69830788T DE69830788T2 (en) | 1997-04-17 | 1998-04-07 | RECOVERY OF SILICON CARBIDE SUBSTRATE WITH USEFUL SURFACE |
AT98914546T ATE299296T1 (en) | 1997-04-17 | 1998-04-07 | RECOVERY OF SILICON CARBIDE SUBSTRATES WITH USABLE SURFACE |
AU68874/98A AU6887498A (en) | 1997-04-17 | 1998-04-07 | Recovery of surface-ready silicon carbide substrates |
JP54398498A JP4063336B2 (en) | 1997-04-17 | 1998-04-07 | Recovery of surface-conditioned silicon carbide substrates |
KR1019997009641A KR100569796B1 (en) | 1997-04-17 | 1998-04-07 | Recovery of surface-ready silicon carbide substrates |
CA002286019A CA2286019C (en) | 1997-04-17 | 1998-04-07 | Recovery of surface-ready silicon carbide substrates |
EP98914546A EP0976162B1 (en) | 1997-04-17 | 1998-04-07 | Recovery of surface-ready silicon carbide substrates |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US08/840,961 US5923946A (en) | 1997-04-17 | 1997-04-17 | Recovery of surface-ready silicon carbide substrates |
US08/840,961 | 1997-04-17 |
Publications (1)
Publication Number | Publication Date |
---|---|
WO1998047185A1 true WO1998047185A1 (en) | 1998-10-22 |
Family
ID=25283677
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/US1998/006836 WO1998047185A1 (en) | 1997-04-17 | 1998-04-07 | Recovery of surface-ready silicon carbide substrates |
Country Status (12)
Country | Link |
---|---|
US (1) | US5923946A (en) |
EP (1) | EP0976162B1 (en) |
JP (1) | JP4063336B2 (en) |
KR (1) | KR100569796B1 (en) |
CN (1) | CN1123073C (en) |
AT (1) | ATE299296T1 (en) |
AU (1) | AU6887498A (en) |
CA (1) | CA2286019C (en) |
DE (1) | DE69830788T2 (en) |
ES (1) | ES2244055T3 (en) |
TW (1) | TW385487B (en) |
WO (1) | WO1998047185A1 (en) |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US6711191B1 (en) | 1999-03-04 | 2004-03-23 | Nichia Corporation | Nitride semiconductor laser device |
US6835956B1 (en) | 1999-02-09 | 2004-12-28 | Nichia Corporation | Nitride semiconductor device and manufacturing method thereof |
US7977687B2 (en) | 2008-05-09 | 2011-07-12 | National Chiao Tung University | Light emitter device |
US8592841B2 (en) | 1997-07-25 | 2013-11-26 | Nichia Corporation | Nitride semiconductor device |
Families Citing this family (16)
Publication number | Priority date | Publication date | Assignee | Title |
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US5679152A (en) * | 1994-01-27 | 1997-10-21 | Advanced Technology Materials, Inc. | Method of making a single crystals Ga*N article |
US6533874B1 (en) | 1996-12-03 | 2003-03-18 | Advanced Technology Materials, Inc. | GaN-based devices using thick (Ga, Al, In)N base layers |
US6459100B1 (en) * | 1998-09-16 | 2002-10-01 | Cree, Inc. | Vertical geometry ingan LED |
US6503769B2 (en) * | 1998-10-26 | 2003-01-07 | Matsushita Electronics Corporation | Semiconductor device and method for fabricating the same |
US6995032B2 (en) * | 2002-07-19 | 2006-02-07 | Cree, Inc. | Trench cut light emitting diodes and methods of fabricating same |
KR101045160B1 (en) * | 2002-12-20 | 2011-06-30 | 크리 인코포레이티드 | Methods of forming semiconductor devices having self aligned semiconductor mesas and contact layers and related devices |
US20050079642A1 (en) * | 2003-10-14 | 2005-04-14 | Matsushita Elec. Ind. Co. Ltd. | Manufacturing method of nitride semiconductor device |
US7008861B2 (en) * | 2003-12-11 | 2006-03-07 | Cree, Inc. | Semiconductor substrate assemblies and methods for preparing and dicing the same |
JP2006253172A (en) * | 2005-03-08 | 2006-09-21 | Toshiba Corp | Semiconductor light emitting element, semiconductor light emitting apparatus and method of manufacturing semiconductor light emitting element |
US20060267043A1 (en) * | 2005-05-27 | 2006-11-30 | Emerson David T | Deep ultraviolet light emitting devices and methods of fabricating deep ultraviolet light emitting devices |
TW201310692A (en) * | 2011-08-31 | 2013-03-01 | Solution Chemicals Inc | Reproducing method of LED substrate |
CN102593285B (en) * | 2012-03-06 | 2014-07-09 | 华灿光电股份有限公司 | Method for recovering pattern sapphire substrate |
KR101226904B1 (en) * | 2012-07-31 | 2013-01-29 | 주식회사 세미콘라이트 | Method of recycling a substrate used for depositng iii-nitride semiconductor thereon |
KR101226905B1 (en) * | 2012-07-31 | 2013-01-29 | 주식회사 세미콘라이트 | Method of recycling a substrate used for depositng iii-nitride semiconductor thereon |
CN103730548B (en) * | 2013-12-28 | 2016-07-06 | 福建省诺希新材料科技有限公司 | A kind of method utilizing high temperature oxidation stability gas to reclaim patterned sapphire substrate |
TWI737610B (en) | 2015-05-20 | 2021-09-01 | 美商納諾光子公司 | Processes for improving efficiency of light emitting diodes |
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US5030536A (en) * | 1989-12-26 | 1991-07-09 | Xerox Corporation | Processes for restoring amorphous silicon imaging members |
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US5393993A (en) * | 1993-12-13 | 1995-02-28 | Cree Research, Inc. | Buffer structure between silicon carbide and gallium nitride and resulting semiconductor devices |
EP0668611A1 (en) * | 1994-02-22 | 1995-08-23 | International Business Machines Corporation | Method for recovering bare semiconductor chips from plastic packaged modules |
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-
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- 1998-04-07 JP JP54398498A patent/JP4063336B2/en not_active Expired - Lifetime
- 1998-04-07 EP EP98914546A patent/EP0976162B1/en not_active Expired - Lifetime
- 1998-04-07 CN CN98804197A patent/CN1123073C/en not_active Expired - Lifetime
- 1998-04-07 AT AT98914546T patent/ATE299296T1/en not_active IP Right Cessation
- 1998-04-07 ES ES98914546T patent/ES2244055T3/en not_active Expired - Lifetime
- 1998-04-07 KR KR1019997009641A patent/KR100569796B1/en not_active IP Right Cessation
- 1998-04-07 DE DE69830788T patent/DE69830788T2/en not_active Expired - Lifetime
- 1998-04-07 AU AU68874/98A patent/AU6887498A/en not_active Abandoned
- 1998-04-07 CA CA002286019A patent/CA2286019C/en not_active Expired - Fee Related
- 1998-04-07 WO PCT/US1998/006836 patent/WO1998047185A1/en active IP Right Grant
- 1998-04-17 TW TW087105882A patent/TW385487B/en not_active IP Right Cessation
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US8592841B2 (en) | 1997-07-25 | 2013-11-26 | Nichia Corporation | Nitride semiconductor device |
US6835956B1 (en) | 1999-02-09 | 2004-12-28 | Nichia Corporation | Nitride semiconductor device and manufacturing method thereof |
US6711191B1 (en) | 1999-03-04 | 2004-03-23 | Nichia Corporation | Nitride semiconductor laser device |
US7977687B2 (en) | 2008-05-09 | 2011-07-12 | National Chiao Tung University | Light emitter device |
Also Published As
Publication number | Publication date |
---|---|
ATE299296T1 (en) | 2005-07-15 |
EP0976162A1 (en) | 2000-02-02 |
KR20010006551A (en) | 2001-01-26 |
ES2244055T3 (en) | 2005-12-01 |
CN1123073C (en) | 2003-10-01 |
JP4063336B2 (en) | 2008-03-19 |
CN1252895A (en) | 2000-05-10 |
DE69830788D1 (en) | 2005-08-11 |
JP2001525121A (en) | 2001-12-04 |
TW385487B (en) | 2000-03-21 |
CA2286019A1 (en) | 1998-10-22 |
EP0976162B1 (en) | 2005-07-06 |
US5923946A (en) | 1999-07-13 |
KR100569796B1 (en) | 2006-04-10 |
DE69830788T2 (en) | 2006-05-04 |
AU6887498A (en) | 1998-11-11 |
CA2286019C (en) | 2003-10-07 |
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