USRE40718E1 - Method for producing nitride monocrystals - Google Patents
Method for producing nitride monocrystals Download PDFInfo
- Publication number
- USRE40718E1 USRE40718E1 US11/069,936 US6993600A USRE40718E US RE40718 E1 USRE40718 E1 US RE40718E1 US 6993600 A US6993600 A US 6993600A US RE40718 E USRE40718 E US RE40718E
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- US
- United States
- Prior art keywords
- thermal energy
- nitride
- supplied
- melt
- substrate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
Links
- 150000004767 nitrides Chemical class 0.000 title claims abstract description 39
- 238000004519 manufacturing process Methods 0.000 title claims description 10
- 238000000034 method Methods 0.000 claims abstract description 52
- 239000000758 substrate Substances 0.000 claims abstract description 45
- 239000000155 melt Substances 0.000 claims abstract description 17
- 230000005855 radiation Effects 0.000 claims description 20
- 150000002894 organic compounds Chemical class 0.000 claims description 14
- 239000000463 material Substances 0.000 claims description 8
- 239000004065 semiconductor Substances 0.000 claims description 6
- 125000000026 trimethylsilyl group Chemical group [H]C([H])([H])[Si]([*])(C([H])([H])[H])C([H])([H])[H] 0.000 claims description 6
- 239000000470 constituent Substances 0.000 claims description 5
- 230000008878 coupling Effects 0.000 claims description 5
- 238000010168 coupling process Methods 0.000 claims description 5
- 238000005859 coupling reaction Methods 0.000 claims description 5
- 230000001939 inductive effect Effects 0.000 claims description 5
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 5
- 239000000126 substance Substances 0.000 abstract description 8
- 238000006243 chemical reaction Methods 0.000 abstract description 3
- 238000000354 decomposition reaction Methods 0.000 abstract description 3
- 239000013078 crystal Substances 0.000 description 14
- 229910052782 aluminium Inorganic materials 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 2
- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 238000000407 epitaxy Methods 0.000 description 2
- 229910052733 gallium Inorganic materials 0.000 description 2
- 239000013079 quasicrystal Substances 0.000 description 2
- 229910052594 sapphire Inorganic materials 0.000 description 2
- 239000010980 sapphire Substances 0.000 description 2
- 238000005979 thermal decomposition reaction Methods 0.000 description 2
- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 description 1
- 229910002601 GaN Inorganic materials 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 230000005670 electromagnetic radiation Effects 0.000 description 1
- 150000004678 hydrides Chemical class 0.000 description 1
- 230000002452 interceptive effect Effects 0.000 description 1
- 239000006193 liquid solution Substances 0.000 description 1
- 239000013081 microcrystal Substances 0.000 description 1
- 125000002524 organometallic group Chemical group 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 238000005092 sublimation method Methods 0.000 description 1
- 238000001429 visible spectrum Methods 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
- C30B7/14—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions the crystallising materials being formed by chemical reactions in the solution
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B17/00—Single-crystal growth onto a seed which remains in the melt during growth, e.g. Nacken-Kyropoulos method
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
- C30B7/005—Epitaxial layer growth
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B9/00—Single-crystal growth from melt solutions using molten solvents
Definitions
- This invention relates to a method for producing nitride monocrystals pursuant to Patent claim 1 .
- Nitride crystals have very high bond energies. To produce corresponding substrate crystals, therefore, extremely high pressure and temperatures of about 1000° C. and higher are necessary.
- the existing methods are based either on methods that enable the formation of crystals from the melt at high pressure, or on a sublimation method in which crystal growth occurs essentially from the gas phase. Quasi-crystals also lead to reduction of dislocation densities, but because of the lattice misfits physically present, they contain prestresses that can be eliminated only by the interfering dislocations. Such quasi-crystals are produced by deposition of thick nitride films on foreign substrates (like sapphire; SiC; Si; GaAs; etc.). Examples of methods used are organometallic gas phase epitaxy and hydride gas phase epitaxy.
- the underlying objective of this invention is thus to described a method for producing nitrides, especially (Ga, Al)Ni [sic] , (Ga, Al) nitride, that on the one hand is as economical as possible, and on the other hand permits the most perfect possible monocrystalline structure.
- the method pursuant to the invention for solving this problem is based on the thermal reaction and decomposition (pyrolysis) of an organic substance that contains the atomic constituents of the nitride monocrystal to be formed.
- This organic substance is contained in a solution or in a melt that is held at a first temperature.
- a substrate nucleus consisting of the nitride material to be grown or of a related type of nitride material.
- This substrate nucleus is supplied with thermal energy so that a second temperature is reached, at least on its surface in contact with the melt, that is higher than the first temperature. Because of this, nitride molecules are formed and deposited on the heated surface, and the nitride monocrystal thus grows.
- the desired material or a related type of material is made available as a “crystal nucleus.”
- the selective heating of just this surface leads to the decomposition of the organic compounds that are either in a melt or in a solution.
- Nitride molecules are formed that contain all of the atoms necessary for crystal construction. Heating the surface of the nucleus leads to the molecules formed also being able to be deposited only there, which leads to crystal growth.
- Such a method moreover, is economical and requires only small expenditures for apparatus.
- solution or melt containing the organic substance prefferably in a container, and for the crystal nucleus to be positioned along a section of the container wall, with the thermal energy being fed to the substrate nucleus through this section of the container wall.
- the thermal energy can be introduced in different ways.
- the substrate nucleus can be impacted by radiation emitted by a radiation source, particularly an infrared radiation source.
- the thermal energy can also be supplied inductively.
- Another possibility consists of introducing the thermal energy through a resistance heater. This can contain resistance wires that run in the section of the container wall and can be supplied with electrical current.
- FIG. 1 a schematic arrangement for implementing the method of the invention
- FIGS. 2A to C forms of embodiment with respect to supplying the thermal energy to the substrate nucleus.
- FIG. 1 shows a schematic arrangement for implementing the method of the invention.
- This arrangement includes a container 1 to hold a liquid solution or melt that contains an organic compound that contains the atomic constituents of the nitride monocrystal to be formed.
- the solution or melt is held at a first temperature T 1 , for example by storing the container 1 in a furnace and adjusting the temperature of the furnace to the temperature T 1 .
- a substrate nucleus 2 that consists of the nitride to be grown or a related type of nitride.
- This substrate nucleus 2 is heated by means of an energy source that is symbolized by the arrow 3 , so that at least its surface in contact with the melt reaches a temperature T 2 that is higher than T 1 .
- gallium nitride for example, is to be grown, as described in the publication by Nutt et al. cited above, (trimethylsilyl)aminogallium dichloride or methyl (trimethylsilyl)aminogallium dichloride can be used as the organic substance.
- AlN aluminum nitride
- FIGS. 2A to 2C illustrate three different types of embodiment for the energy supply.
- the arrow 3 in FIG. 1 is thus replaced in these figures by corresponding conceivable structures.
- a light source 31 preferably an infrared light source, below the container 1 , whose emitted radiation is pointed at the section of the container wall at which the substrate nucleus 2 is located. It is also theoretically conceivable for the substrate nucleus 2 to be at any position in the melt whatsoever, and for the radiation of an external light source to be focused on it by suitable optics.
- the heat energy is introduced by inductive coupling.
- the lower section of the container 1 is surrounded by a coil winding 32 that is powered with alternating current from a source of alternating voltage 32 B.
- the coil 32 and thus the substrate nucleus 2 can be positioned at any longitudinal position on the container 1 .
- the thermal energy is supplied by a resistance heater 33 .
- the resistance heater 33 has a resistance wire 33 A that is in contact with the container wall and can be powered by a direct-voltage source 33 B with direct current. This produces Joule heat that can penetrate through the container wall into the substrate nucleus 2 .
- the resistance wire 33 A preferably follows a looped or spiral-shaped path and thus covers a certain area, in order to impact it as homogeneously as possible with thermal energy. It can be embedded permanently in the container wall with connecting wires fed to the outside. However, it is also conceivable for it to be inserted into recesses provided for it on the outside of the container wall when needed.
- Heat can be supplied very selectively to the substrate nucleus 2 by this method, but the substrate nucleus 2 has to be produced on the container wall.
- a fourth possibility for energy supply consists of introducing microwave energy.
- a microwave energy source for example, a magnetron
- the microwave radiation emitted by it can be fed to the section of the container wall on which the substrate nucleus 2 is positioned, with or without the use of a microwave guide.
- Supplying the energy by means of electromagnetic radiation or inductively has the advantage over the resistance heater that the substrate nucleus 2 in principle can be located anywhere in the melt.
- the substrate nucleus 2 has to be in contact with a wall of the container.
- the melt can be agitated constantly during growth by a mechanical mixer.
- the substrate nucleus 2 can also be rotated around its cylindrical axis during growth, and/or it can be pulled through the solution at a low velocity.
- a static or likewise rotating electric field or magnetic field can also be applied.
- laminar flow can be produced in the solution, for example by having the solution flow to the substrate nucleus in a tube pointed at the substrate nucleus. All of the measures mentioned can arbitrarily be combined with one another to provide optimal growth conditions.
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
- Liquid Deposition Of Substances Of Which Semiconductor Devices Are Composed (AREA)
Abstract
Description
Claims (39)
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE19904378A DE19904378B4 (en) | 1999-02-03 | 1999-02-03 | Process for producing nitride single crystals |
PCT/DE2000/000267 WO2000046431A1 (en) | 1999-02-03 | 2000-02-01 | Method for producing nitride monocrystals |
US09/869,221 US6527853B1 (en) | 1999-02-03 | 2000-02-01 | Method for producing nitride monocrystals |
Related Parent Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
US09/869,221 Reissue US6527853B1 (en) | 1999-02-03 | 2000-02-01 | Method for producing nitride monocrystals |
Publications (1)
Publication Number | Publication Date |
---|---|
USRE40718E1 true USRE40718E1 (en) | 2009-06-09 |
Family
ID=7896324
Family Applications (2)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
US09/869,221 Ceased US6527853B1 (en) | 1999-02-03 | 2000-02-01 | Method for producing nitride monocrystals |
US11/069,936 Expired - Lifetime USRE40718E1 (en) | 1999-02-03 | 2000-02-01 | Method for producing nitride monocrystals |
Family Applications Before (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
US09/869,221 Ceased US6527853B1 (en) | 1999-02-03 | 2000-02-01 | Method for producing nitride monocrystals |
Country Status (6)
Country | Link |
---|---|
US (2) | US6527853B1 (en) |
EP (1) | EP1155170B1 (en) |
JP (1) | JP4436572B2 (en) |
DE (2) | DE19904378B4 (en) |
TW (1) | TW460638B (en) |
WO (1) | WO2000046431A1 (en) |
Families Citing this family (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE10253161B4 (en) * | 2002-09-12 | 2010-05-06 | Osram Opto Semiconductors Gmbh | Process for the production of optoelectronic semiconductor chips with improved surface properties |
JP5015417B2 (en) * | 2004-06-09 | 2012-08-29 | 住友電気工業株式会社 | GaN crystal manufacturing method |
Citations (12)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP0145773A1 (en) | 1983-06-14 | 1985-06-26 | Konrad Dr. Altmann | Water flushing tank for wc |
WO1986006361A1 (en) | 1985-04-26 | 1986-11-06 | Sri International | Preparing metal compounds, alloys and metals by pyrolysis |
JPS621874A (en) | 1985-06-26 | 1987-01-07 | Mitsubishi Electric Corp | Metallizing method |
EP0295467A2 (en) | 1987-06-16 | 1988-12-21 | EASTMAN KODAK COMPANY (a New Jersey corporation) | Process for depositing a III-V compound layer on a substrate |
EP0429272A2 (en) | 1989-11-20 | 1991-05-29 | Dow Corning Corporation | Single and multilayer coatings containing aluminum nitride |
US5087593A (en) | 1990-12-10 | 1992-02-11 | Ford Motor Company | Preparation of titanium nitride from organometallic precursors |
WO1995017019A1 (en) | 1993-12-13 | 1995-06-22 | Cree Research, Inc. | Buffer structure between silicon carbide and gallium nitride and resulting semiconductor devices |
US5523589A (en) | 1994-09-20 | 1996-06-04 | Cree Research, Inc. | Vertical geometry light emitting diode with group III nitride active layer and extended lifetime |
WO1996036080A1 (en) | 1995-05-08 | 1996-11-14 | Cree Research, Inc. | Double heterojunction light emitting diode with gallium nitride active layer |
US5767581A (en) | 1993-04-28 | 1998-06-16 | Nichia Chemical Industries, Ltd. | Gallium nitride-based III-V group compound semiconductor |
US5776603A (en) | 1994-11-21 | 1998-07-07 | Saint-Gobain Vitrage | Glazing pane equipped with at least one thin film and method of manufacturing the same |
US5905276A (en) | 1992-10-29 | 1999-05-18 | Isamu Akasaki | Light emitting semiconductor device using nitrogen-Group III compound |
Family Cites Families (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH02145773A (en) | 1988-11-25 | 1990-06-05 | Toshiba Lighting & Technol Corp | Formation of thin film |
-
1999
- 1999-02-03 DE DE19904378A patent/DE19904378B4/en not_active Expired - Fee Related
-
2000
- 2000-02-01 US US09/869,221 patent/US6527853B1/en not_active Ceased
- 2000-02-01 EP EP00908957A patent/EP1155170B1/en not_active Expired - Lifetime
- 2000-02-01 JP JP2000597487A patent/JP4436572B2/en not_active Expired - Fee Related
- 2000-02-01 US US11/069,936 patent/USRE40718E1/en not_active Expired - Lifetime
- 2000-02-01 WO PCT/DE2000/000267 patent/WO2000046431A1/en active IP Right Grant
- 2000-02-01 DE DE50000914T patent/DE50000914D1/en not_active Expired - Lifetime
- 2000-02-02 TW TW089101806A patent/TW460638B/en not_active IP Right Cessation
Patent Citations (13)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP0145773A1 (en) | 1983-06-14 | 1985-06-26 | Konrad Dr. Altmann | Water flushing tank for wc |
WO1986006361A1 (en) | 1985-04-26 | 1986-11-06 | Sri International | Preparing metal compounds, alloys and metals by pyrolysis |
JPS621874A (en) | 1985-06-26 | 1987-01-07 | Mitsubishi Electric Corp | Metallizing method |
EP0295467A2 (en) | 1987-06-16 | 1988-12-21 | EASTMAN KODAK COMPANY (a New Jersey corporation) | Process for depositing a III-V compound layer on a substrate |
US4833103A (en) | 1987-06-16 | 1989-05-23 | Eastman Kodak Company | Process for depositing a III-V compound layer on a substrate |
EP0429272A2 (en) | 1989-11-20 | 1991-05-29 | Dow Corning Corporation | Single and multilayer coatings containing aluminum nitride |
US5087593A (en) | 1990-12-10 | 1992-02-11 | Ford Motor Company | Preparation of titanium nitride from organometallic precursors |
US5905276A (en) | 1992-10-29 | 1999-05-18 | Isamu Akasaki | Light emitting semiconductor device using nitrogen-Group III compound |
US5767581A (en) | 1993-04-28 | 1998-06-16 | Nichia Chemical Industries, Ltd. | Gallium nitride-based III-V group compound semiconductor |
WO1995017019A1 (en) | 1993-12-13 | 1995-06-22 | Cree Research, Inc. | Buffer structure between silicon carbide and gallium nitride and resulting semiconductor devices |
US5523589A (en) | 1994-09-20 | 1996-06-04 | Cree Research, Inc. | Vertical geometry light emitting diode with group III nitride active layer and extended lifetime |
US5776603A (en) | 1994-11-21 | 1998-07-07 | Saint-Gobain Vitrage | Glazing pane equipped with at least one thin film and method of manufacturing the same |
WO1996036080A1 (en) | 1995-05-08 | 1996-11-14 | Cree Research, Inc. | Double heterojunction light emitting diode with gallium nitride active layer |
Non-Patent Citations (3)
Title |
---|
Nutt, Rodger W., "Synthesis and Characterization of (Trimethylsilyl)amino)-and (Methyl(trimethylsilyl)amino) gallium Dichloride", American Chemical Siciety 1985, pp. 159-164. |
Riedel, R., "Bis (dichlor-N-trimethylsilyl)cycloaminoalan Kristallstruktur und thermscher abbau zu Aluminiumnitrd", Z. anor. Allg. Chem. 603 (1991)p. 119-127 , Stuttgart. |
Riedel, R., "Bis (dichlor-N-trimethylsilyl)cycloaminoalan Kristallstruktur und thermscher abbau zu Aluminiumnitrd", Z. anor. Allg. Chem. 603 (1991)p. 119-127, Stuttgart. |
Also Published As
Publication number | Publication date |
---|---|
JP4436572B2 (en) | 2010-03-24 |
EP1155170A1 (en) | 2001-11-21 |
EP1155170B1 (en) | 2002-12-11 |
TW460638B (en) | 2001-10-21 |
DE19904378A1 (en) | 2000-08-10 |
DE50000914D1 (en) | 2003-01-23 |
JP2002536283A (en) | 2002-10-29 |
US6527853B1 (en) | 2003-03-04 |
DE19904378B4 (en) | 2006-10-05 |
WO2000046431A1 (en) | 2000-08-10 |
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