US3278274A - Method of pulling monocrystalline silicon carbide - Google Patents

Method of pulling monocrystalline silicon carbide Download PDF

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US3278274A
US3278274A US411067A US41106764A US3278274A US 3278274 A US3278274 A US 3278274A US 411067 A US411067 A US 411067A US 41106764 A US41106764 A US 41106764A US 3278274 A US3278274 A US 3278274A
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sic
melt
temperature
pulling
crystallizing
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US411067A
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Liebmann Wolfgang
Werner K Spielmann
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International Business Machines Corp
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    • 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
    • C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
    • C30B15/14—Heating of the melt or the crystallised materials
    • C30B15/16—Heating of the melt or the crystallised materials by irradiation or electric discharge
    • 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
    • C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski 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
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10—Inorganic compounds or compositions
    • C30B29/36—Carbides
    • 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
    • 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
    • Y10S117/00—Single-crystal, oriented-crystal, and epitaxy growth processes; non-coating apparatus therefor
    • Y10S117/90—Apparatus characterized by composition or treatment thereof, e.g. surface finish, surface coating
    • 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
    • Y10S117/00—Single-crystal, oriented-crystal, and epitaxy growth processes; non-coating apparatus therefor
    • Y10S117/903—Dendrite or web or cage technique
    • Y10S117/904—Laser beam
    • 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
    • Y10S117/00—Single-crystal, oriented-crystal, and epitaxy growth processes; non-coating apparatus therefor
    • Y10S117/905—Electron beam

Definitions

  • This invention relates to a method of pulling monocrystalline silicon carbide, and more particularly to the fabrication of semiconductor components by this method.
  • SiC has gained increasing importance in connection with the fabrication of semiconductor components in the electrical engineering art.
  • advantages of this substance which essentially reside in its high melting point and its chemical inertness, cause unfavorable efI'ects in processing.
  • SiC cannot be pulled as a bar out of the melt, as, at approximately 2300 C., SiC changes over directly out of the solid into the gaseous phase.
  • the pulling of SiC bars out of a melt containing SiC has not been possible so far since SiC dissolves only very poorly with the solvents deemed suitable until now.
  • this invention proposes a method of pulling monocrystalline SiC in which SiC dissolved in metallic chromium is locally heated to approximately 1700 C. in an SiC crucible under the action of a suitable radiation, e.g.
  • the heated region being placed into contact with an SiC seed which, preferably rotatably, is Withdrawn at such a low speed that the chromium which has been enriched by the pulling of the SiC crystal migrates in the direction of the higher temperature away from the crystallizing front and, due to the low vapor pressure caused by the high temperature prevailing there, partly separates by changing over into the gaseous phase,
  • This method has the advantage that the crucible, which consists of SiC, remains relatively cold whereas the temperature required for performing the pulling operation remains-due to the suitably controlled radiationrestricted to the inner regions of the melt directly adjacent to the crystallizing front.
  • the optimum range of temperatures that may be used for the local heating of the SiC-Cr melt is between 1650" C. and 1800 C.
  • the temperature of the crucible lies between 1550 C. and 1650 C.
  • the maximum temperature of the locally heated regions surrounding the crystallizing front lies between 1700 C. and 1800 C.
  • the temperature of the crystallizing front lies between 1650 C. and 1750 C.
  • the figure represents a sectional view of the crucible and an arrangement for carrying through the method of this invention.
  • Represented at 1 is a crucible consisting of SiC containing a melt 2 of Cr (87 percent) and SiC (13 percent), the temperature of which is approximately 1650" C.
  • This melt is heated to a little over l700 C. by two electron beams 13 and 14 produced by means of the electron sources 6 and 7. It is into this region where the SiC seed 11 is initially dipped, which is mounted in the clamp 10 at the lead screw 9 guided in 8. By turning the lead screw 9, the seed 11 is under constant rotation pulled out of the melt 2 upwardly at such a low speed that the chromium will migrate in the direction toward the region 4 of the melt which has been heated to slightly over 1700 C. by the electron beams 13 and 14 and which surrounds the crystallizing point hemispherically.
  • the bar 12 is produced which consists of monocrystalline SiC.
  • the electron beams 13 and 14 are directed to sweep a circular region on the surface of the melt.
  • the intensity of the electron beams is controlled so that, due to the heat reflection of the crucible and the heat reflection of that portion of the melt surface enclosed by said hemispherical surface, the temperature of the melt in the region of the hemisphere indicated by the dotted line 4 is at a maximum and decreases in a direction toward the hemispheres indicated by the dotted lines 3 and 5 to reach a value of approximately 1700 C. in the region of the SiC bar 12, i.e., in the crystallizing region.
  • the Cr which has been enriched by the pulling process migrates in the direction of the higher temperature, i.e., into the region of the hemisphere indicated by the dotted line 4, and in doing so partly changes over into the gaseous phase since at the indicated temperature the vapor pressure of the Cr is only approximately 2 millimeters Hg.
  • the temperature of the crucible 1 and of the lower parts of the melt 2 is controlled by means of the induction furnace 15 in such a manner that sufficient SiC will be transferred into the melt for keeping the latters SiC content constant.
  • Method of pulling monocrystalline SiC from a melt at a crystallizing front therebetween comprising the steps of:

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)
  • Liquid Deposition Of Substances Of Which Semiconductor Devices Are Composed (AREA)

Description

1966 w. LIEBMANN ETAL 3,278,274
METHOD OF PULLING MONOCRYSTALLINE SILICON CARBIDE Filed NOV. 13, 1964 ELECTRON 13- ELECTRON BEAM BEAM INVENTORS WERNER K. SPIELMANN WOLFGANG LIEBMANN ATTORNEY 1 mwm nu LIN-" United States Patent 3,278,274 METHOD OF PULLING MONOCRYSTALLINE SILICON CARBIDE Wolfgang Liebmann, Schoneberger Weg, and Werner K.
Spielmann, Post Deufringen, Germany, assignors to International Business Machines Corporation, New York, N.Y., a corporation of New York Filed Nov. 13, 1964, Ser. No. 411,067 Claims priority, application Germany, Dec. 17, 1963,
8 Claims. (c1. 23-301 This invention relates to a method of pulling monocrystalline silicon carbide, and more particularly to the fabrication of semiconductor components by this method.
More recently, SiC has gained increasing importance in connection with the fabrication of semiconductor components in the electrical engineering art. However, the advantages of this substance, which essentially reside in its high melting point and its chemical inertness, cause unfavorable efI'ects in processing. Especially aggravating is the fact that, unlike other known semiconductor materials, SiC cannot be pulled as a bar out of the melt, as, at approximately 2300 C., SiC changes over directly out of the solid into the gaseous phase. Also, the pulling of SiC bars out of a melt containing SiC has not been possible so far since SiC dissolves only very poorly with the solvents deemed suitable until now. Thus, it has not yet been possible to pull conocrystalline bars out of a melt consisting of Si and SiC since even at 1700 C. the solubility of SiC in Si amounts only to approximately 2 percent. It has only been possible to obtain small SiC crystallites as inclusions in Si. Such crystallites are, however, only conditionally useful in fabricating semiconductor components.
In order to enable the production of the relatively large and homogenous SiC monocrystals required for the economic fabrication of semiconductor elements, this invention proposes a method of pulling monocrystalline SiC in which SiC dissolved in metallic chromium is locally heated to approximately 1700 C. in an SiC crucible under the action of a suitable radiation, e.g. under the action of a laser or an electron beam, the heated region being placed into contact with an SiC seed which, preferably rotatably, is Withdrawn at such a low speed that the chromium which has been enriched by the pulling of the SiC crystal migrates in the direction of the higher temperature away from the crystallizing front and, due to the low vapor pressure caused by the high temperature prevailing there, partly separates by changing over into the gaseous phase,
This method has the advantage that the crucible, which consists of SiC, remains relatively cold whereas the temperature required for performing the pulling operation remains-due to the suitably controlled radiationrestricted to the inner regions of the melt directly adjacent to the crystallizing front. The optimum range of temperatures that may be used for the local heating of the SiC-Cr melt is between 1650" C. and 1800 C. In accordance with a particularly advantageous embodiment of the invention, the temperature of the crucible lies between 1550 C. and 1650 C., the maximum temperature of the locally heated regions surrounding the crystallizing front lies between 1700 C. and 1800 C., and the temperature of the crystallizing front lies between 1650 C. and 1750 C. It has proved to be of particular advantage to carry out the method with the crucible having a temperature of 1600 C., with the maximum temperature of the locally heated region surrounding the crystallizing front at 1700 C. The pulling rate is appropriately 1 millimeter per hour. By a suitable additional heating of the SiC crucible it is possible to keep the SiC content of the SiC-Cr melt constant by the SiC of the crucible changing over into the SiC-Cr melt to such an extent that the SiC-Cr ratio remains constant.
The foregoing and other objects, features and advantages of the invention will be apparent from the following more particular description of preferred embodiments of the invention, as illustrated in the accompanying drawing.
In the drawing:
The figure represents a sectional view of the crucible and an arrangement for carrying through the method of this invention.
Represented at 1 is a crucible consisting of SiC containing a melt 2 of Cr (87 percent) and SiC (13 percent), the temperature of which is approximately 1650" C. This melt is heated to a little over l700 C. by two electron beams 13 and 14 produced by means of the electron sources 6 and 7. It is into this region where the SiC seed 11 is initially dipped, which is mounted in the clamp 10 at the lead screw 9 guided in 8. By turning the lead screw 9, the seed 11 is under constant rotation pulled out of the melt 2 upwardly at such a low speed that the chromium will migrate in the direction toward the region 4 of the melt which has been heated to slightly over 1700 C. by the electron beams 13 and 14 and which surrounds the crystallizing point hemispherically. Thereby, the bar 12 is produced which consists of monocrystalline SiC. The electron beams 13 and 14 are directed to sweep a circular region on the surface of the melt. The intensity of the electron beams is controlled so that, due to the heat reflection of the crucible and the heat reflection of that portion of the melt surface enclosed by said hemispherical surface, the temperature of the melt in the region of the hemisphere indicated by the dotted line 4 is at a maximum and decreases in a direction toward the hemispheres indicated by the dotted lines 3 and 5 to reach a value of approximately 1700 C. in the region of the SiC bar 12, i.e., in the crystallizing region. The Cr which has been enriched by the pulling process migrates in the direction of the higher temperature, i.e., into the region of the hemisphere indicated by the dotted line 4, and in doing so partly changes over into the gaseous phase since at the indicated temperature the vapor pressure of the Cr is only approximately 2 millimeters Hg. The temperature of the crucible 1 and of the lower parts of the melt 2 is controlled by means of the induction furnace 15 in such a manner that sufficient SiC will be transferred into the melt for keeping the latters SiC content constant.
While the invention has been particularly shown and described with reference to preferred embodiments thereof, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention.
What is claimed is:
1. Method of pulling monocrystalline SiC from a melt at a crystallizing front therebetween comprising the steps of:
pulling a seed of monocrystalline SiC from a melt of Cr and SiC, said melt being heated by a first external heating means to form a hemispherical Zone of high Cr concentration in the region of said crystallizing front; and
heating the region of the outer surface of said hemispherical zone by a second external radiation heating means to a temperature ranging between 1650 C. and 1800 C. to partially vaporize the Cr thereat and to cause said high concentration of Cr in said region of said crystallizing front to migrate to said region of said latter heating.
2. Method according to claim 1 wherein said second external radiation heating means includes an electron beam.
3. Method according to claim 1 wherein said second external radiation heating means includes a laser.
4. Method according to claim 1 wherein said pulling is at a rate of 1 millimeter per hour.
5. Method according to claim 1 wherein said temperature of heating is approximately 1700 C.
6. Method according to claim 1 wherein said melt is established in an SiC crucible, said first external heating means heats said crucible to a temperature which lies between 1550 C. and 1650 C., the maximum temperature of the heated area of the outer surface of said hemispherical zone lies between 1700 C. and 1800 C., and the temperature of said crystallizing front lies between 1650 C. and 1750 C.
7. Method according to claim 6 wherein said crucible temperature is 1600 C., said temperature of said region 4- maximum of 1750 C., and said temperature of said crystallizing front is 1700 C.
8. Method according to claim 6 wherein said temperature of said crucible of SiC is so controlled that the transfor of the SiC into the melt of SiC and Cr takes place in such a manner that the Cr-SiC ratio remains constant.
References Cited by the Examiner UNITED STATES PATENTS 2,858,199 10/1958 Larson 148-1.6 2,968,723 1/1961 Steigerwald. 3,053,635 9/1962 Shockley 23-301 NORMAN YUDKOFF, Primary Examiner.
of the outer surface of said hemispherical zone being a 15 G. P. HINES, Assistant Examiner.

Claims (1)

1. METHOD OF PULLING MONOCRYSTALLINE SIC FROM A MELT AT A CRYSTALLIZING FRONT THEREBETWEEN COMPRISING THE STEPS OF: PULLING A SEED OF MONOCRYSTALLINE SIC FROM A MELT OF CR AND SIC, SAID MELT BEING HEATED BY A FIRST EXTERNAL HEATING MEANS TO FORM A HEMISPHERICAL ZONE OF HIGH CR CONCENTRATION IN THE REGION OF SAID CRYSTALLIZING FRONT; AND
US411067A 1963-12-17 1964-11-13 Method of pulling monocrystalline silicon carbide Expired - Lifetime US3278274A (en)

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Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3494804A (en) * 1968-07-15 1970-02-10 Air Reduction Method for growing crystals
US3607139A (en) * 1968-05-02 1971-09-21 Air Reduction Single crystal growth and diameter control by magnetic melt agitation
US3660044A (en) * 1965-06-10 1972-05-02 Siemens Ag Apparatus for crucible-free zone melting of crystalline rods
US3897590A (en) * 1968-05-18 1975-07-29 Battelle Development Corp Method and apparatus for making monocrystals
US3943324A (en) * 1970-12-14 1976-03-09 Arthur D. Little, Inc. Apparatus for forming refractory tubing
US4012213A (en) * 1973-06-14 1977-03-15 Arthur D. Little, Inc. Apparatus for forming refractory fibers
US4349407A (en) * 1979-05-09 1982-09-14 The United States Of America As Represented By The United States Department Of Energy Method of forming single crystals of beta silicon carbide using liquid lithium as a solvent
US4971650A (en) * 1989-09-22 1990-11-20 Westinghouse Electric Corp. Method of inhibiting dislocation generation in silicon dendritic webs
JP2015110496A (en) * 2013-12-06 2015-06-18 信越化学工業株式会社 Silicon carbide crystal growth method
JP2015110495A (en) * 2013-12-06 2015-06-18 信越化学工業株式会社 Silicon carbide crystal growth method
US9945047B2 (en) 2013-12-06 2018-04-17 Shin-Etsu Chemical Co., Ltd. Method for growing silicon carbide crystal
US11440849B2 (en) 2015-08-06 2022-09-13 Shin-Etsu Chemical Co., Ltd. SiC crucible, SiC sintered body, and method of producing SiC single crystal

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP4450075B2 (en) * 2008-01-15 2010-04-14 トヨタ自動車株式会社 Method for growing silicon carbide single crystal
CN106482514A (en) * 2016-12-09 2017-03-08 永平县泰达废渣开发利用有限公司 A kind of induction furnace based on electron beam gun melts silicon and plays furnace apparatus and technique

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2858199A (en) * 1954-10-15 1958-10-28 Itt Crystal production
US2968723A (en) * 1957-04-11 1961-01-17 Zeiss Carl Means for controlling crystal structure of materials
US3053635A (en) * 1960-09-26 1962-09-11 Clevite Corp Method of growing silicon carbide crystals

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2858199A (en) * 1954-10-15 1958-10-28 Itt Crystal production
US2968723A (en) * 1957-04-11 1961-01-17 Zeiss Carl Means for controlling crystal structure of materials
US3053635A (en) * 1960-09-26 1962-09-11 Clevite Corp Method of growing silicon carbide crystals

Cited By (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3660044A (en) * 1965-06-10 1972-05-02 Siemens Ag Apparatus for crucible-free zone melting of crystalline rods
US3607139A (en) * 1968-05-02 1971-09-21 Air Reduction Single crystal growth and diameter control by magnetic melt agitation
US3897590A (en) * 1968-05-18 1975-07-29 Battelle Development Corp Method and apparatus for making monocrystals
US3494804A (en) * 1968-07-15 1970-02-10 Air Reduction Method for growing crystals
US3943324A (en) * 1970-12-14 1976-03-09 Arthur D. Little, Inc. Apparatus for forming refractory tubing
US4012213A (en) * 1973-06-14 1977-03-15 Arthur D. Little, Inc. Apparatus for forming refractory fibers
US4349407A (en) * 1979-05-09 1982-09-14 The United States Of America As Represented By The United States Department Of Energy Method of forming single crystals of beta silicon carbide using liquid lithium as a solvent
US4971650A (en) * 1989-09-22 1990-11-20 Westinghouse Electric Corp. Method of inhibiting dislocation generation in silicon dendritic webs
JP2015110496A (en) * 2013-12-06 2015-06-18 信越化学工業株式会社 Silicon carbide crystal growth method
JP2015110495A (en) * 2013-12-06 2015-06-18 信越化学工業株式会社 Silicon carbide crystal growth method
US9945047B2 (en) 2013-12-06 2018-04-17 Shin-Etsu Chemical Co., Ltd. Method for growing silicon carbide crystal
US9951439B2 (en) 2013-12-06 2018-04-24 Shin-Etsu Chemical Co., Ltd. Method for growing silicon carbide crystal
EP2881499B1 (en) * 2013-12-06 2020-03-11 Shin-Etsu Chemical Co., Ltd. Method for growing silicon carbide crystal
EP2881498B1 (en) * 2013-12-06 2020-03-11 Shin-Etsu Chemical Co., Ltd. Method for growing silicon carbide crystal
US11440849B2 (en) 2015-08-06 2022-09-13 Shin-Etsu Chemical Co., Ltd. SiC crucible, SiC sintered body, and method of producing SiC single crystal

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GB1031136A (en) 1966-05-25
DE1208739B (en) 1966-01-13

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