US3508962A - Epitaxial growth process - Google Patents

Epitaxial growth process Download PDF

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Publication number
US3508962A
US3508962A US524765A US3508962DA US3508962A US 3508962 A US3508962 A US 3508962A US 524765 A US524765 A US 524765A US 3508962D A US3508962D A US 3508962DA US 3508962 A US3508962 A US 3508962A
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substrate
film
silicon
films
single crystal
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Expired - Lifetime
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US524765A
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English (en)
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Harold M Manasevit
William I Simpson
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Boeing North American Inc
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North American Rockwell 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
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/02—Elements
    • C30B29/06—Silicon
    • 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
    • C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
    • C30B25/02—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
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/02—Elements
    • C30B29/08—Germanium
    • 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
    • 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
    • Y10S148/00—Metal treatment
    • Y10S148/025—Deposition multi-step
    • 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
    • Y10S148/00—Metal treatment
    • Y10S148/113—Nitrides of boron or aluminum or gallium
    • 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
    • Y10S148/00—Metal treatment
    • Y10S148/15—Silicon on sapphire SOS
    • 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
    • Y10S438/967—Semiconductor on specified insulator

Definitions

  • the invention is directed to a process for growing an epitaxial film on a single crystal substrate comprising the steps of forming initially an extremely thin film of semiconductor material on a desired substrate or surface by thermal decomposition of a hydride. Subsequently, a thicker film is deposited or grown on the thin film by thermally decomposing a halide in a hydrogen atmosphere or a mixture of halides and hydrides in a hydrogen atmosphere.
  • This invention relates to a process for improving the quality of a single crystal films grown on single crystal substrates.
  • Vapor deposition processes for depositing single crystal films on single crystal substrates often produce films of low quality. Defects in the substrate surface have a tendency to produce depositions with imperfections. The defects are more noticeable when thicker films are produced. Twinning in the deposited films also occurs more frequently when using existing deposition processes.
  • a process is needed whereby certain substrate surface defects can be tolerated and thick, high quality films can be produced with a minimum of twinning. Such a process would permit greater latitude in techniques of crystal growth when forming epitaxial films.
  • the improved process could also be useful in the formation of composites useful in the technology of translating devices, e.g. lasers, transistors, rectifiers, diodes, and other materials and devices associated with the field of microelectronics.
  • Another object of this invention is to produce single crystalline films on single crystalline substrates with-a minimum of twin densities.
  • the invention in a particular embodiment may be characterized as a process for growing an epitaxial film on a single crystal substrate comprising the steps of forming initially an extremely thin film of semiconductor material on a desired substrate or surface by the pyrolysis (thermal decomposition) of a hydride. This step may be called the nucleation step. Subsequently, a thicker film is deposited or grown on the thin film by thermally decomposing a halide in a hydrogen atmosphere or a mixture of halides and hydrides in a hydrogen atmosphere. The materials are decomposed on the thin surface for such a period of time as required to produce a desired film thickness.
  • Each of the process steps has particular merits which when combined, results in producing a thick, high quality semiconducting film on a substrate.
  • the first step provides an extremely high density of discrete semiconductor nuclei which tend to agglomerate such that many surface defects, for example dirt, fine scratches, small substrate defects, etc. are eventually overcome by the rapidly growing film. Films thus nucleated have displayed twinned densities much less than films formed by halide nucleation. After the nucleation step, the remainder of the film is produced by thermal decomposition of materials exemplified herein.
  • the figure is an illustraiton of the apparatus used in depositing the films on the substrate.
  • the system includes flow meters 5, 6, 7, 8 and 9 including valves 10 1-1, 12, 13, 14, 15, 16, 17, 18, 19, 20, 21, 22, 23, 24 and 33 for controlling the flow of material into and out of reactor 2.
  • the system may also include deoxidizer 25, molecular sieves 26, and traps of liquid nitrogen 27.
  • Other material sources such as a hydrogen source 28, silicon tetrachloride (SiCl source 29, silane (SiH source 30, germane (Gel-I source 31, diborane (B H in H source 32 are also shown. Some of the materials may not be used in every process.
  • halides such as trichlorosilane, silicon tetrabromide, and silicon tetraiodide may be used as alternate silicon sources for the second step of the process.
  • Higher hydrides of silicon such as Si H may also be considered for use in the nucleation step 1.
  • germane In depositing single crystal germanium, germane (GeH and germanium hydrides followed by germanium tetrahalides or trichloro germane in hydrogen may be used.
  • Substrate materials such as sapphire, beryllium oxide, magnesium oxide, silicon, germanium, chrysoberyl, calcium fluoride, Group IIV compounds, Group II'-VI compounds, and others may be considered for single crystal deposits.
  • the thickness of the film deposited in the nucleation step should be at least from 500 A. to 1,000 A. in thickness, whereas the total film deposited by thermal decomposition need only be limited by the thickness desired for use in a particular device. It was also observed in films investigated that the degree of microtwinning is related to the nucleation step and is relatively unaffected by the second step.
  • EXAMPLE I The sapphire substrate was placed on a pedestal inside a vertical reactor and heated by radio frequency to a temperature of approximately 1150 C.
  • a silicon film was nucleated by 15-30 second pyrolysis of a 0.3 mole percent silane concentration in hydrogen flowing at about 3 liters per minute over the substrate.
  • valves 21 and 24 were activated to cut off the silane source; and silicon tetrahalide was introduced into the hydrogen stream by manipulating valves 10, 11, 12 and 33 so that enough hydrogen was diverted through the SiSl, bubbler kept at a temperature of approximately 0 so that about 0.3 mole percent SiCL, passed into the reaction zone containing the substrate.
  • a silicon growth rate of about 0.3 micron per minute resulted.
  • the substrate material does not necessarily have to be identical to the deposited semiconductor material, for example, germanium on silicon, boron on silicon, silicon on beryllium and other combinations may be used.
  • a process for improving the quality of semiconductor epitaxial layers grown on single crystal substrates EXAMPLE II
  • two polished sapphire (alpha-alumina) substrates cut from the same boule were placed individually in the vertical reactor 2 and heated as before.
  • Two 6.6 micron films of silicon were grown; one by the use of silane and one by the improved two step process.
  • the film formed by the two step process was more uniform in thickness and had the physical appearance of a better quality film.
  • the two step process film had better reflectivity, surface structure, etc. as determined by test.
  • Substrate materials as beryllium oxide, magnesium oxide, silicon, chrysoberyl, calcium fluoride, Group 1IIV compounds, Group II-VI compounds may also be used as substrate materials under proper substrate temperature conditions.
  • semiconductor devices are fabricated in the films. 'It was determined by measuring characteristics of the produced semiconductor devices that the devices produced in films formed by the two step process have relatively improved characteristics over those produced in films from the one step process.
  • said substrate is selected from the class consisting of sapphire, beryllium oxide, chrysoberyl and silicon.
  • a process for improving the quality of semiconductor epitaxial layers grown on single crystal substrates comprising the steps of forming a nucleation film of semiconductor material on a single crystal substrate by thermally decomposing a germane and depositing on said film a relatively thicker layer of germanium by thermally decomposing a germanium halide in a hydrogen atmosphere.
  • said substrate is selected from the class consisting of sapphire, beryllium oxide, chrysoberyl, silicon and germanium.
  • a process for improving the quality of epitaxial layers grown on single crystal substrates comprising the steps of forming a nucleation film of semiconductor material on a single crystal substrate by thermally decomposing a boron hydride and depositing on said film a relatively thicker layer of boron by thermally decomposing a boron halide in a hydrogen atmosphere.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Physics & Mathematics (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Manufacturing & Machinery (AREA)
  • Computer Hardware Design (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Power Engineering (AREA)
  • Recrystallisation Techniques (AREA)
US524765A 1966-02-03 1966-02-03 Epitaxial growth process Expired - Lifetime US3508962A (en)

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Cited By (21)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3645230A (en) * 1970-03-05 1972-02-29 Hugle Ind Inc Chemical deposition apparatus
US3765960A (en) * 1970-11-02 1973-10-16 Ibm Method for minimizing autodoping in epitaxial deposition
US3847686A (en) * 1970-05-27 1974-11-12 Gen Electric Method of forming silicon epitaxial layers
US3930067A (en) * 1966-04-16 1975-12-30 Philips Corp Method of providing polycrystalline layers of elementtary substances on substrates
US3941647A (en) * 1973-03-08 1976-03-02 Siemens Aktiengesellschaft Method of producing epitaxially semiconductor layers
US3963539A (en) * 1974-12-17 1976-06-15 International Business Machines Corporation Two stage heteroepitaxial deposition process for GaAsP/Si LED's
US3963538A (en) * 1974-12-17 1976-06-15 International Business Machines Corporation Two stage heteroepitaxial deposition process for GaP/Si
US4087571A (en) * 1971-05-28 1978-05-02 Fairchild Camera And Instrument Corporation Controlled temperature polycrystalline silicon nucleation
US4180618A (en) * 1977-07-27 1979-12-25 Corning Glass Works Thin silicon film electronic device
US4279688A (en) * 1980-03-17 1981-07-21 Rca Corporation Method of improving silicon crystal perfection in silicon on sapphire devices
US4309241A (en) * 1980-07-28 1982-01-05 Monsanto Company Gas curtain continuous chemical vapor deposition production of semiconductor bodies
US4311545A (en) * 1979-03-30 1982-01-19 Wacker-Chemitronic Gesellschaft Fur Elektronik-Grundstoffe Mbh Method for the deposition of pure semiconductor material
US4368098A (en) * 1969-10-01 1983-01-11 Rockwell International Corporation Epitaxial composite and method of making
US4404265A (en) * 1969-10-01 1983-09-13 Rockwell International Corporation Epitaxial composite and method of making
US4464222A (en) * 1980-07-28 1984-08-07 Monsanto Company Process for increasing silicon thermal decomposition deposition rates from silicon halide-hydrogen reaction gases
US4509990A (en) * 1982-11-15 1985-04-09 Hughes Aircraft Company Solid phase epitaxy and regrowth process with controlled defect density profiling for heteroepitaxial semiconductor on insulator composite substrates
US4753895A (en) * 1987-02-24 1988-06-28 Hughes Aircraft Company Method of forming low leakage CMOS device on insulating substrate
US4826300A (en) * 1987-07-30 1989-05-02 Hughes Aircraft Company Silicon-on-sapphire liquid crystal light valve and method
US5431733A (en) * 1992-06-29 1995-07-11 Matsushita Electric Industrial Co., Ltd. Low vapor-pressure material feeding apparatus
US5690736A (en) * 1987-08-24 1997-11-25 Canon Kabushiki Kaisha Method of forming crystal
US20100117131A1 (en) * 2008-11-12 2010-05-13 Hynix Semiconductor Inc. Transistor for Preventing or Reducing Short Channel Effect and Method for Manufacturing the Same

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS58500360A (ja) * 1981-03-11 1983-03-10 クロ−ナ−・コ−ポレイション 非晶質半導体の方法及び装置
FR3101782B1 (fr) 2019-10-09 2021-09-24 Pierre Chovrelat Barre de Suspension en Bois Télescopique

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3160521A (en) * 1960-11-30 1964-12-08 Siemens Ag Method for producing monocrystalline layers of semiconductor material
US3192072A (en) * 1960-12-08 1965-06-29 Slemens & Halske Ag Method of pulling a dendritic crystal from a vapor atmosphere
US3312572A (en) * 1963-06-07 1967-04-04 Barnes Eng Co Process of preparing thin film semiconductor thermistor bolometers and articles
US3341376A (en) * 1960-04-02 1967-09-12 Siemens Ag Method of producing crystalline semiconductor material on a dendritic substrate

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3341376A (en) * 1960-04-02 1967-09-12 Siemens Ag Method of producing crystalline semiconductor material on a dendritic substrate
US3160521A (en) * 1960-11-30 1964-12-08 Siemens Ag Method for producing monocrystalline layers of semiconductor material
US3192072A (en) * 1960-12-08 1965-06-29 Slemens & Halske Ag Method of pulling a dendritic crystal from a vapor atmosphere
US3312572A (en) * 1963-06-07 1967-04-04 Barnes Eng Co Process of preparing thin film semiconductor thermistor bolometers and articles

Cited By (22)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3930067A (en) * 1966-04-16 1975-12-30 Philips Corp Method of providing polycrystalline layers of elementtary substances on substrates
US4368098A (en) * 1969-10-01 1983-01-11 Rockwell International Corporation Epitaxial composite and method of making
US4404265A (en) * 1969-10-01 1983-09-13 Rockwell International Corporation Epitaxial composite and method of making
US3645230A (en) * 1970-03-05 1972-02-29 Hugle Ind Inc Chemical deposition apparatus
US3847686A (en) * 1970-05-27 1974-11-12 Gen Electric Method of forming silicon epitaxial layers
US3765960A (en) * 1970-11-02 1973-10-16 Ibm Method for minimizing autodoping in epitaxial deposition
US4087571A (en) * 1971-05-28 1978-05-02 Fairchild Camera And Instrument Corporation Controlled temperature polycrystalline silicon nucleation
US3941647A (en) * 1973-03-08 1976-03-02 Siemens Aktiengesellschaft Method of producing epitaxially semiconductor layers
US3963538A (en) * 1974-12-17 1976-06-15 International Business Machines Corporation Two stage heteroepitaxial deposition process for GaP/Si
US3963539A (en) * 1974-12-17 1976-06-15 International Business Machines Corporation Two stage heteroepitaxial deposition process for GaAsP/Si LED's
US4180618A (en) * 1977-07-27 1979-12-25 Corning Glass Works Thin silicon film electronic device
US4311545A (en) * 1979-03-30 1982-01-19 Wacker-Chemitronic Gesellschaft Fur Elektronik-Grundstoffe Mbh Method for the deposition of pure semiconductor material
US4279688A (en) * 1980-03-17 1981-07-21 Rca Corporation Method of improving silicon crystal perfection in silicon on sapphire devices
US4309241A (en) * 1980-07-28 1982-01-05 Monsanto Company Gas curtain continuous chemical vapor deposition production of semiconductor bodies
US4464222A (en) * 1980-07-28 1984-08-07 Monsanto Company Process for increasing silicon thermal decomposition deposition rates from silicon halide-hydrogen reaction gases
US4509990A (en) * 1982-11-15 1985-04-09 Hughes Aircraft Company Solid phase epitaxy and regrowth process with controlled defect density profiling for heteroepitaxial semiconductor on insulator composite substrates
US4753895A (en) * 1987-02-24 1988-06-28 Hughes Aircraft Company Method of forming low leakage CMOS device on insulating substrate
US4826300A (en) * 1987-07-30 1989-05-02 Hughes Aircraft Company Silicon-on-sapphire liquid crystal light valve and method
US5690736A (en) * 1987-08-24 1997-11-25 Canon Kabushiki Kaisha Method of forming crystal
US5431733A (en) * 1992-06-29 1995-07-11 Matsushita Electric Industrial Co., Ltd. Low vapor-pressure material feeding apparatus
US20100117131A1 (en) * 2008-11-12 2010-05-13 Hynix Semiconductor Inc. Transistor for Preventing or Reducing Short Channel Effect and Method for Manufacturing the Same
US8703564B2 (en) 2008-11-12 2014-04-22 SK Hynix Inc. Method for manufacturing a transistor for preventing or reducing short channel effect

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DE1619980A1 (de) 1970-04-09
DE1619980B2 (de) 1971-01-14
GB1176871A (en) 1970-01-07
FR1501313A (fr) 1967-11-10
NL6615797A (enrdf_load_html_response) 1967-08-04
USB524765I5 (enrdf_load_html_response) 1900-01-01
DE1619980C3 (de) 1975-05-28

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