US3729348A - Method for the solution growth of more perfect semiconductor crystals - Google Patents

Method for the solution growth of more perfect semiconductor crystals Download PDF

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Publication number
US3729348A
US3729348A US00076550A US3729348DA US3729348A US 3729348 A US3729348 A US 3729348A US 00076550 A US00076550 A US 00076550A US 3729348D A US3729348D A US 3729348DA US 3729348 A US3729348 A US 3729348A
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Prior art keywords
growth
halt
crystal
solution
solvent
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Expired - Lifetime
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US00076550A
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English (en)
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R Saul
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AT&T Corp
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Bell Telephone Laboratories Inc
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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
    • C30B19/00—Liquid-phase epitaxial-layer growth
    • C30B19/10—Controlling or regulating
    • 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
    • Y10S148/097—Lattice strain and defects
    • 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
    • Y10S148/107—Melt
    • 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
    • Y10S148/108—Melt back

Definitions

  • FIG. 1 is a graph which shows an exemplary temperature vs. time schedule experimentally used to illus- ICC trate the disclosed invention as applied to the liquid phase epitaxial growth of gallium phosphide.
  • a modification of this process is known as the Traveling Solvent Method.
  • This method starts with a seed crystal at the bottom, above which is a zone of solvent material typically one to several millimeters thick. Above the solvent and in contact with it is a body of polycrystalline or powdered material of the composition to be grown. A temperature gradient is maintained across the solvent zone, the polycrystalline material being maintained at a higher temperature than the single crystal material below the solvent. The temperature and the temperature gradient is adjusted so that material is dissolved at the upper end of the solvent zone. diffuses through the solvent and is deposited as a single crystal at the lower end of the solvent zone. As the single crystal grows the temperature gradient is moved upward and more of the polycrystalline or powder dissolves.
  • Crystal growth with halts In accordance with the invention disclosed here, crystal growth by methods such as the exemplary methods described above are caused to proceed with a brief halt in the growth schedule while maintaining the crystal tn contact with the solvent and adding nothing to the solvent. In uniform temperature methods, cooling is halted and in temperature gradient methods, the motion of the temperature gradient with respect to the single crystal and polycrystalline material is halted. The period of the halt can be as little as one minute and still yield discernible improvement; halts of the order of five minutes are usually to be preferred in order to assure appreciable improvement; while interruptions greater than five minutes may in some situations be desirable. However, it would usually be uneconomic to interrupt crystal growth for greater than two hours.
  • the halts can take two general forms-crystal growth can be halted and the growth face of the material held stationary during the halt period or the growth process can be reversed and some of the already deposited material dissolved. Further improvements in crystal perfection have been observed by both repeated growth and halt cycles.
  • the figure shows three exemplary cooling cycles used to exhibit the invention as applied to liquid phase epitaxial growth of gallium phosphide from gallium solution.
  • segment 11 between points A and B represent the warm up of the system to the temperature at which growth will be initiated.
  • the segments 12, 13, 14 between points B and E represent the control experiment which defines cooling cycle I.
  • This cooling cycle includes no halts.
  • Cooling cycle II includes segments 12, 13, 16, and 17 between points B, D, F, and G.
  • Cooling cycle III includes segments 12, 15 and 17 between points B, C, P, and G. In this cooling cycle the temperature is held stationary during the halt.
  • a method for growing of crystalline compound semiconductor matter of a conductivity type by epitaxial depo sition of the matter on a surface of a crystalline solid of the same conductivity type which surface is in contact With a liquid body comprising a solvent and the compound semiconductor matter in solution therein characterized in that, after the deposition has proceeded and an epitaxial layer has been produced, the deposition is halted for a time period while maintaining the surface in contact with the liquid body and maintaining the composition of the liquid body essentially constant, after which time period the deposition is resumed thereby producing an improvement in the crystalline perfection of the material deposited subsequent to the time period.
  • a method of claim in which the time period at 6. A crystalline body of a semiconducting material produced by the method of claim 1.
  • Woodall et al. Liquid Phase Epitaxial Growth of Ga A1 As, ibid., vol. 116, No. 6, June 1969, pp. 899- 903.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Liquid Deposition Of Substances Of Which Semiconductor Devices Are Composed (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)
  • Led Devices (AREA)
US00076550A 1970-09-29 1970-09-29 Method for the solution growth of more perfect semiconductor crystals Expired - Lifetime US3729348A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
US7655070A 1970-09-29 1970-09-29

Publications (1)

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US3729348A true US3729348A (en) 1973-04-24

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US00076550A Expired - Lifetime US3729348A (en) 1970-09-29 1970-09-29 Method for the solution growth of more perfect semiconductor crystals

Country Status (8)

Country Link
US (1) US3729348A (fr)
JP (1) JPS505026B1 (fr)
BE (1) BE772812A (fr)
CA (1) CA947186A (fr)
DE (1) DE2147265B2 (fr)
FR (1) FR2106326A5 (fr)
GB (1) GB1355852A (fr)
IT (1) IT939894B (fr)

Cited By (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3862859A (en) * 1972-01-10 1975-01-28 Rca Corp Method of making a semiconductor device
US3877883A (en) * 1973-07-13 1975-04-15 Rca Corp Method of growing single crystals of compounds
US3984263A (en) * 1973-10-19 1976-10-05 Matsushita Electric Industrial Co., Ltd. Method of producing defectless epitaxial layer of gallium
US4246050A (en) * 1979-07-23 1981-01-20 Varian Associates, Inc. Lattice constant grading in the Aly Ca1-y As1-x Sbx alloy system
US4421576A (en) * 1981-09-14 1983-12-20 Rca Corporation Method for forming an epitaxial compound semiconductor layer on a semi-insulating substrate
US4483736A (en) * 1981-03-24 1984-11-20 Mitsubishi Monsanto Chemical Co., Ltd. Method for producing a single crystal of a IIIb -Vb compound
US4632712A (en) * 1983-09-12 1986-12-30 Massachusetts Institute Of Technology Reducing dislocations in semiconductors utilizing repeated thermal cycling during multistage epitaxial growth
US4838988A (en) * 1986-11-05 1989-06-13 Pechiney Process for obtaining crystals of intermetallic compounds, in particular isolated monocrystals, by cooling alloys in the molten state
US4889493A (en) * 1987-08-13 1989-12-26 The Furukawa Electric Co., Ltd. Method of manufacturing the substrate of GaAs compound semiconductor
US5091333A (en) * 1983-09-12 1992-02-25 Massachusetts Institute Of Technology Reducing dislocations in semiconductors utilizing repeated thermal cycling during multistage epitaxial growth
US5209811A (en) * 1988-03-25 1993-05-11 Shin-Etsu Handotai Company Limited Of Japan Method for heat-treating gallium arsenide monocrystals
US5228927A (en) * 1988-03-25 1993-07-20 Shin-Etsu Handotai Company Limited Method for heat-treating gallium arsenide monocrystals
US5252173A (en) * 1990-11-28 1993-10-12 Fujitsu Limited Process for growing semiconductor layer on substrate
US6010937A (en) * 1995-09-05 2000-01-04 Spire Corporation Reduction of dislocations in a heteroepitaxial semiconductor structure

Cited By (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3862859A (en) * 1972-01-10 1975-01-28 Rca Corp Method of making a semiconductor device
US3877883A (en) * 1973-07-13 1975-04-15 Rca Corp Method of growing single crystals of compounds
US3984263A (en) * 1973-10-19 1976-10-05 Matsushita Electric Industrial Co., Ltd. Method of producing defectless epitaxial layer of gallium
US4246050A (en) * 1979-07-23 1981-01-20 Varian Associates, Inc. Lattice constant grading in the Aly Ca1-y As1-x Sbx alloy system
US4483736A (en) * 1981-03-24 1984-11-20 Mitsubishi Monsanto Chemical Co., Ltd. Method for producing a single crystal of a IIIb -Vb compound
US4421576A (en) * 1981-09-14 1983-12-20 Rca Corporation Method for forming an epitaxial compound semiconductor layer on a semi-insulating substrate
US4632712A (en) * 1983-09-12 1986-12-30 Massachusetts Institute Of Technology Reducing dislocations in semiconductors utilizing repeated thermal cycling during multistage epitaxial growth
US5091333A (en) * 1983-09-12 1992-02-25 Massachusetts Institute Of Technology Reducing dislocations in semiconductors utilizing repeated thermal cycling during multistage epitaxial growth
US4838988A (en) * 1986-11-05 1989-06-13 Pechiney Process for obtaining crystals of intermetallic compounds, in particular isolated monocrystals, by cooling alloys in the molten state
US4889493A (en) * 1987-08-13 1989-12-26 The Furukawa Electric Co., Ltd. Method of manufacturing the substrate of GaAs compound semiconductor
US5209811A (en) * 1988-03-25 1993-05-11 Shin-Etsu Handotai Company Limited Of Japan Method for heat-treating gallium arsenide monocrystals
US5228927A (en) * 1988-03-25 1993-07-20 Shin-Etsu Handotai Company Limited Method for heat-treating gallium arsenide monocrystals
US5252173A (en) * 1990-11-28 1993-10-12 Fujitsu Limited Process for growing semiconductor layer on substrate
US6010937A (en) * 1995-09-05 2000-01-04 Spire Corporation Reduction of dislocations in a heteroepitaxial semiconductor structure

Also Published As

Publication number Publication date
IT939894B (it) 1973-02-10
JPS505026B1 (fr) 1975-02-27
DE2147265A1 (de) 1972-03-30
CA947186A (en) 1974-05-14
BE772812A (fr) 1972-01-17
GB1355852A (en) 1974-06-05
FR2106326A5 (fr) 1972-04-28
DE2147265B2 (de) 1973-08-23

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