US3619282A - Method for vapor growing ternary compounds - Google Patents

Method for vapor growing ternary compounds Download PDF

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Publication number
US3619282A
US3619282A US763147A US3619282DA US3619282A US 3619282 A US3619282 A US 3619282A US 763147 A US763147 A US 763147A US 3619282D A US3619282D A US 3619282DA US 3619282 A US3619282 A US 3619282A
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substrate
growth
epitaxial films
temperature
source
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Gerald W Manley
Philip S Mcdermott
Edward S Pan
Ralph J Riley
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International Business Machines Corp
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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
    • C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition 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
    • C30B23/00—Single-crystal growth by condensing evaporated or sublimed materials
    • C30B23/02—Epitaxial-layer growth
    • G—PHYSICS
    • G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03B—APPARATUS OR ARRANGEMENTS FOR TAKING PHOTOGRAPHS OR FOR PROJECTING OR VIEWING THEM; APPARATUS OR ARRANGEMENTS EMPLOYING ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ACCESSORIES THEREFOR
    • G03B21/00—Projectors or projection-type viewers; Accessories therefor
    • G03B21/54—Accessories
    • G03B21/64—Means for mounting individual pictures to be projected, e.g. frame for transparency
    • 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
    • Y10S148/064—Gp II-VI compounds

Definitions

  • the broad object of this invention is to provide a method and apparatus capable of vapor growing ternary epitaxial films at larger production rates.
  • a gaseous mixture consisting of growth reactant gases from elements of the Il-VI valence groups and an inert transport gas such as hydrogen, argon, and mixtures thereof.
  • the constituent gases are added separately to individual streams of the carrier gas, after which the individual streams are combined and mixed to form a uniform distribution of the ternary elements and the carrier gas.
  • heat is applied to set a temperature level high enough to prevent binary reactions to occur.
  • the mixture is then rapidly cooled to simultaneously supersaturate each of the growth constituents forcing them to condense simultaneously on the growth surface of a seed crystal substrate. It is a feature of this invention that the rapid cooling is effected by passing the ternary gas and carrier mixture through a thermal gradient having equithermal lines substantially parallel with the growth surface of the substrate.
  • the apparatus for practicing the present invention is of the open tube type, that is, the maximum pressure within the apparatus does not exceed a pressure much above atmospheric.
  • the apparatus comprises plural source furnaces connected in parallel to a common carrier gas source. Source materials volatilized to the appropriate temperature and pressures are added to the gas streams of the carrier gas in the source furnaces.
  • a mixing furnace having a common input from the source furnaces provides a uniform distribution of the reactant gases and the carrier gas for feeding to a reaction furnace.
  • the mixing furnace comprises heating means operable simultaneously with the mixing action to maintain the temperature of the mixture at a level which inhibits binary reactions within the mixing chamber.
  • a growth substrate is mounted on a pedestal adjustably movable within the reaction chamber.
  • a cooling means supplies air coolant to the substrate.
  • Heating coils one of which is movable, surrounds the reaction chamber to produce high temperatures necessary to maintain the ternary mixture in its vapor phase until it is very close to the substrate growth surface.
  • a flat equithermal profile is achieved by separating the coils to provide a heating gap along the reaction chamber in the region of the deposition substrate. Unreacted gases pass from the reaction chamber, are condensed and the carrier gas passed into the atmosphere.
  • FIG. 1 is a cross-sectional schematic of a vapor growing apparatus for practicing the present invention
  • FIG. 2 is a sectional view of a mixing chamber used in the apparatus of FIG. 1;
  • FIG. 3 is a sectional detail of the reaction chamber of the apparatus of FIG. 1 illustrating a thermal map for the reaction chamber for a particular setting of heating coils for the reaction chamber;
  • FIG. 4 is a graph of a thermal profile of the thermal gradient of FIG. 3 taken along a center line 44 shown in FIG. 3.
  • the improved vapor growing apparatus comprises source furnaces 10, I1, and 12 connected in parallel between a source 13 of an inert carrier gas and a mixing furnace 14, which in turn is connected to a reaction furnace 15 connected to apparatus 16 for venting the inert gas to the atmosphere.
  • Source furnace 10 comprises a quartz chamber 17 wound with a heating coil 18.
  • a current supply and regulating means of suitable type (not shown) which is independently operable, is connected to heating coil 18 to maintain temperature levels to effect volatilizing of the elemental cadmium into the hydrogen gas stream as it flows through chamber 17.
  • the channel for supplying hydrogen gas to chamber 17 comprises tube 20 connected to chamber 17 via airtight seal 21, and through flow meter 22 and flow valve 23 to a common flow line 24.
  • Source furnace 11 comprises a quartz chamber 25 wound with heating coil 26 electrically connected and controlled in essentially the same manner as coil 18 of furnace 10.
  • a supply 27 of elemental tellurium, preferably in pellet form in a quartz boat. or the like, is located within the heating zone of coil 26 to be volatilized and added to a hydrogen gas stream flowing through chamber 25.
  • the carrier gas channel to furnace 11 comprises a tube 28 connected by an airtight seal 29 to chamber and through flow meter 30 and flow valve 31 to supply line 24.
  • Source furnace 12 comprises a T-shaped quartz tube 32 having one branch connected by an airtight seal 33 to tube 34 and through flow meter 35 and valve 36 to supply line 24.
  • the second branch of chamber 32 is connected to a mercury supply well 37.
  • Liquid mercury 38 is fed by gravity from an external reservoir 39 through connecting tube 40 to well 37.
  • An electrical coil 41 which is wound entirely around the well 37 as well as the entire junction area of tube 32 is electrically connected to current source and regulating means of a suitable type for vaporizing the mercury at predetermined temperature and pressure levels for addition to a hydrogen gas stream flowing through tube 32.
  • the connection of tube 32 to well 37 is preferably made long and the winding of coil 41 is such as to allow a measure of preheating of the mercury vapors prior to their addition to the hydrogen gas stream in tube 32.
  • the flow of hydrogen gas from source 13 is suitably measured for regulation means such as bubble column 42, or the like, connected to supply line 24.
  • the mixing furnace 14 comprises a cylindrical quartz chamber 43 entirely wound with a heating coil 44 which is electrically connected to suitable current source and regulating means (not shown) which maybe independently operable to maintain temperature of the mixing chamber 43 at levels to assure proper constituent control.
  • the mixing chamber 41 has s single tube input 45 connected in common with the outputs of chamber 17, 25 and tube 32 of source furnaces 10, 11, and 12, respectively.
  • mixing chamber 43 is provided with a series of baffles 46-49 arranged to produce eddying within the hydrogen stream as it leaves tube 45. While various types of baffling can be provided and while the number of baffle elements may vary, the baffles 46-49, as seen in FIG.
  • baffles 46 and 47 are opposed at spaced longitudinal positions.
  • Baffles 48 and 49 are similarly constructed and shaped except that they are oriented 90 from the positions of baffles 46 and 47.
  • the longitudinal spacing of the baffles is a function of rate of gas flow, but is in the preferred case set to produce eddying in 3 dimensions thereby assuring complete and thorough mixing to effect uniform distribution of the constituent gases throughout the carrier gas stream.
  • the reaction furnace 15 comprises a cylindrical quartz reaction chamber 50, a pair of coaxial heating coils 51 and 52 wound thereon, and a means for supporting a growth substrate 55 at a selectable growth site position within the chamber relative to the heating coils.
  • the reaction chamber 50 is preferably designed with a removable cylindrical section 53 which is provided with a central opening and joins with the rest of the reaction chamber at airtight seal 54.
  • the substrate support comprises a cylindrical pedestal tube 56 which is inserted through the central opening of bottom section 53. Seal ing means, such as O-rings 57, are provided between pedestal tube 56 and chamber section 53.
  • a growth substrate 58 is attached by suitable mans such as spring clip 59.
  • Cooling means comprises a silver heat sink cylinder 60 inserted within pedestal tube 56, and tube 6], connected through flow meter 62 to an air coolant source. Both the heat sink 60 and spring clip 59 structures may be other than the type shown in the above-mentioned copending application.
  • a viewing port 63 is provided in reaction chamber 50 in the general area of the desired growth site. Venting of the carrier gas from the system is provided by tube 64 connected through valve 65 to a cold trap 66. if the carrier gas is to be burned when vented, as in the case where hydrogen gas is used, an ignition device, such as coil 67, may be used.
  • the system is also connected to a vacuum pump from tube 64 through tube 68 and valve 69.
  • the heating coils 51 and 52 are connected to separate current source and regulator means. This permits flexibility in controlling the heating effects necessary to control the thermal gradients essential for vapor growing ternary compounds.
  • heating coil 52 is wound in such a manner that it is movable longitudinally along reaction chamber 50. By the movement of coil 52, a separation 70 is provided which produces a thermal gap in the heating field of the coils 51 and 52. By varying this gap, the thermal gradient profile, and thus the composition control of film grown on substrate 58 is obtained.
  • Substrate 58 is selected to have the desired crystal structure then polished and cleaned.
  • a suitable crystal would be a monocrystal of Cd Te of a nominal thickness of 10 mils cut from an ingot along the crystallographic plane. Cleaning and polishing may be performed as described in the abovementioned copending application.
  • the selected crystal 58 is then attached to the end of pedestal 56 by spring clip 59 and inserted within reaction chamber 50 through the opening in bottom section 53 (which has been assembled and sealed at 54) using O-rings 57 to effect reaction chamber sealing.
  • source materials 19 and 27 of cadmium and tellurium, respectively are placed in heating zone position within source furnaces l0 and 11 and liquid mercury 38 adjusted to the desired level within furnace 12 after which the reservoir 39 is blocked to close the mercury feed system.
  • the system is evacuated to an initial pumpdown level through valve 69 to eliminate oxidizing gases and impurities.
  • Hydrogen gas which flows from source 13 is then turned on and vented through the apparatus to atmosphere where it is ignited by coil 67.
  • the vacuum pump is stopped and valve 69 closed.
  • a back-etch operation of substrate 58 may then be performed according to well-known techniques to further polish the growth surface of substrate 58. This may be done in the apparatus of FIG. I by turning on the reaction furnace 15, mixing furnace 14, and the cadmium and mercury source furnaces l0 and 12. Source furnace ll is not turned on.
  • coil 52 is moved virtually adjacent the coil 51, thereby eliminating gap 70, and both are energized to a common temperature level.
  • furnace 12 has a temperature of 300 C. and mixing furnace l4, and source furnaces l0 and 12 have temperature settings of 850 C., 370 C., and 315 C., respectively. Heating takes place for a period of 15-20 minutes, or until the substrate surface 58 is observed through aperture 63 to take on a glossy appearance.
  • coil 52 of reaction furnace 15 is moved along chamber 50 to the desired separation of gap 70 and coils 51 and 52 energized to the desired operating temperature levels for vapor growing.
  • streams of hydrogen gas enriched with cadmium gas and mercury vapor, flow through the system, are mixed in furnaces l4 and passed through to the reaction chamber 50. Since a growth reaction does not yet take place, mercury and cadmium will condense in the lower portion of chamber 50 and collect in bottom section 53.
  • the source furnace ll is now turned on to volatilize tellurium from source 27 into the hydrogen gas stream flowing in chamber 25.
  • cooling air is supplied to heat sink 60 to drop the temperature of substrate 58 to the desired film growing level.
  • a crystaline ternary epitaxial film becomes deposited on the upper surface of the substrate 58.
  • the source furnaces and 11, and the mixing and reaction furnaces l4 and are turned off.
  • the source furnace 12 is allowed to remain on after all the other parts of the system are turned off to allow the mercury vapor pressure to remain within prescribed levels in reaction chamber 50 to prevent mercury from being volatilized from the grown film after air to heat sink 60 is cutoff.
  • Furnace 12 continues to operate until the reaction chamber 50 reaches a temperature of approximately 100 C. for Hg Cd Te films, then it is shut off and the system opened to the atmosphere.
  • Source Furnace l0 (cadmium) 305 C.
  • Source Furnace ll (tellurium) 430 C.
  • Source Furnace l2 (mercury) 3l0 C.
  • Mixing Furnace l4 850 C.
  • Reaction Furnace l5 (coil 5]) 800 C.
  • Reaction Furnace l5 (coil S2) 530 C, Substrate 480 C.
  • a minimum substrate temperature must be maintained to promote epitaxy or single crystal growth and prevent dendrite growth which can be a problem at substrate temperatures much below 450 C. and the source temperatures mentioned above.
  • stoichiometry is controlled in the growing layer by fixing the cadmium source temperature and, thus, its overpressure and then varying the amount of tellurium in the gas stream.
  • the amount of tellurium is the same as cadmium due to the relatively low substrate temperature, just Cd Te would be formed and there is very little Te available for reaction with Hg.
  • Te in excess of the cadmium present some free Te is available to react and incorporate Hg in the growing crystal lattice.
  • the growth of ternary Hg Cd Te epitaxial films requires cooling the substrate 58 at the minimum temperature and yet locating it as close to the mixing temperature (800 C.) to thereby produce a very sharptemperature gradient as close to the substrate as possible. This prevents depletion of Cd and Te by spontaneous nucleation prior to arrival at the substrate.
  • An example of a thermal profile for a gap setting of 1 cm. with temperatures of coils 51 and 52 set at 800 C. and 530 C. respectively, and a substrate temperature of 480 C. and a flow rate of cc./min. is shown in FIGS. 3 and 4.
  • Curve 71 illustrates the thermal profile taken along the center line through reaction chamber 50 through heating zone of coil 51 to the growth surface of substrate 58.
  • the temperature of the gas mixture changes from over 600 C. to below 500 C. within a space of approximately 1 cm. to a point of about 0.5 cm. from the substrate surface.
  • vapors of cadmium, tellurium, and mercury become supersaturated and, since they are very proximate the growth surface of substrate 58, condensation occurs thereon.
  • the equithermal lines above the growth surface of substrate 58 are substantially parallel with the growth surface which is preferably flat and the temperature across the growth surface is uniform over substantially the entire surface. Since film growth is a function of substrate temperature, uniformity of substrate temperature assures uniformity of composition over the growth surface.
  • This type of thermal profile is achievable by adjusting the separation 70 between coils 51 and 52 to effectively produce a gap in the thermal field in the region of the substrate 58.
  • the thermal profile would have equithermal lines of curvilinear shape of substantially larger radius extending from end to end of the substrate surface. Thus, a temperature gradient exists across the growth surface. Thus, composition would vary in the film grown on the substrate surface.
  • Detector crystals cut from such film would be of variable semiconductive properties and their use in a multiple detector configuration presents substantial performance and circuit design problems.
  • films of up to /2 square inches have been grown from which a plurality of crystals may be out having substantially the same semiconductor properties.
  • the substrate was a Cd Te monocrystal of a nominal thickness of 10 mils out along the crystallographic plane
  • the carrier gas was hydrogen
  • the source materials were 99.9999 percent purity cadmium and tellurium.
  • the growth times were 2 hours in all cases with a 60 cc./min. flow rate through each of the source furnaces 10, 11, and 12.
  • the films produced having substantially uniform composition were produced in sizes from V4 to 9% square inches. By making the growth apparatus longer, larger size crystals are obtainable.
  • a method for vapor growing ternary epitaxial films on a substrate comprising the steps of:
  • a method for vapor growing ternary epitaxial films in accordance with claim 1 in which said gaseous mixture is formed by adding each growth reactant gas to separate streams of said transport agent, followed by combining said streams into a common stream and flowing said stream through a mixing device to produce uniform distribution of said reactants in said transport agent.
  • a method for vapor growing ternary epitaxial films in accordance with claim 2 in which said heating to prevent binary combinations of said reactant gases is done concurrently with said mixing of said separate gas streams.
  • a method for vapor growing ternary epitaxial films in accordance with claim 1 in which the cooling of said substrate and the heating of the region surrounding said substrate is done in a manner which produces a thermal gradient immediately above the growth surface of said substrate having equithermal lines substantially parallel with said growth surface.

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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)
  • Physics & Mathematics (AREA)
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  • Crystals, And After-Treatments Of Crystals (AREA)
US763147A 1968-09-27 1968-09-27 Method for vapor growing ternary compounds Expired - Lifetime US3619282A (en)

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JP (1) JPS4949310B1 (fr)
CA (1) CA918548A (fr)
FR (1) FR2018988A1 (fr)
GB (1) GB1282168A (fr)

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3779803A (en) * 1969-11-17 1973-12-18 Ibm Infrared sensitive semiconductor device and method of manufacture
US3884788A (en) * 1973-08-30 1975-05-20 Honeywell Inc Substrate preparation for liquid phase epitaxy of mercury cadmium telluride
US4115163A (en) * 1976-01-08 1978-09-19 Yulia Ivanovna Gorina Method of growing epitaxial semiconductor films utilizing radiant heating
US4568397A (en) * 1984-09-12 1986-02-04 Raytheon Company Metalorganic vapor phase epitaxial growth of group II-VI semiconductor materials
US4748135A (en) * 1986-05-27 1988-05-31 U.S. Philips Corp. Method of manufacturing a semiconductor device by vapor phase deposition using multiple inlet flow control
US4886683A (en) * 1986-06-20 1989-12-12 Raytheon Company Low temperature metalorganic chemical vapor depostion growth of group II-VI semiconductor materials
US4950358A (en) * 1986-07-07 1990-08-21 Santa Barbara Research Center Vapor phase epitaxy of semiconductor material in a quasi-open system

Families Citing this family (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS512828A (fr) * 1974-06-26 1976-01-10 Matsushita Electric Ind Co Ltd
US3987772A (en) * 1975-03-10 1976-10-26 Texas Instruments Incorporated Self-regulating heater
US4107515A (en) * 1976-09-09 1978-08-15 Texas Instruments Incorporated Compact PTC resistor
JPS5541505U (fr) * 1978-09-08 1980-03-17
JPS5954739U (ja) * 1982-10-01 1984-04-10 トヨタ自動車株式会社 内燃機関の吸気加熱装置

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3178313A (en) * 1961-07-05 1965-04-13 Bell Telephone Labor Inc Epitaxial growth of binary semiconductors
US3210149A (en) * 1961-03-27 1965-10-05 Philips Corp Method of producing monocrystals of a semiconductor via the vapor phase
US3420704A (en) * 1966-08-19 1969-01-07 Nasa Depositing semiconductor films utilizing a thermal gradient
US3462323A (en) * 1966-12-05 1969-08-19 Monsanto Co Process for the preparation of compound semiconductors
US3472685A (en) * 1965-05-25 1969-10-14 Centre Nat Rech Scient Methods of depositing a volatile material on a solid support

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3210149A (en) * 1961-03-27 1965-10-05 Philips Corp Method of producing monocrystals of a semiconductor via the vapor phase
US3178313A (en) * 1961-07-05 1965-04-13 Bell Telephone Labor Inc Epitaxial growth of binary semiconductors
US3472685A (en) * 1965-05-25 1969-10-14 Centre Nat Rech Scient Methods of depositing a volatile material on a solid support
US3420704A (en) * 1966-08-19 1969-01-07 Nasa Depositing semiconductor films utilizing a thermal gradient
US3462323A (en) * 1966-12-05 1969-08-19 Monsanto Co Process for the preparation of compound semiconductors

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3779803A (en) * 1969-11-17 1973-12-18 Ibm Infrared sensitive semiconductor device and method of manufacture
US3884788A (en) * 1973-08-30 1975-05-20 Honeywell Inc Substrate preparation for liquid phase epitaxy of mercury cadmium telluride
US4115163A (en) * 1976-01-08 1978-09-19 Yulia Ivanovna Gorina Method of growing epitaxial semiconductor films utilizing radiant heating
US4568397A (en) * 1984-09-12 1986-02-04 Raytheon Company Metalorganic vapor phase epitaxial growth of group II-VI semiconductor materials
US4748135A (en) * 1986-05-27 1988-05-31 U.S. Philips Corp. Method of manufacturing a semiconductor device by vapor phase deposition using multiple inlet flow control
US4886683A (en) * 1986-06-20 1989-12-12 Raytheon Company Low temperature metalorganic chemical vapor depostion growth of group II-VI semiconductor materials
US4950358A (en) * 1986-07-07 1990-08-21 Santa Barbara Research Center Vapor phase epitaxy of semiconductor material in a quasi-open system

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CA918548A (en) 1973-01-09
DE1944985A1 (de) 1970-05-27
JPS4949310B1 (fr) 1974-12-26
DE1944985B2 (de) 1972-10-26
FR2018988A1 (fr) 1970-06-26
GB1282168A (en) 1972-07-19

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