US3152932A - Reduction in situ of a dipolar molecular gas adhering to a substrate - Google Patents

Reduction in situ of a dipolar molecular gas adhering to a substrate Download PDF

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US3152932A
US3152932A US169276A US16927662A US3152932A US 3152932 A US3152932 A US 3152932A US 169276 A US169276 A US 169276A US 16927662 A US16927662 A US 16927662A US 3152932 A US3152932 A US 3152932A
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Prior art keywords
gas
hydrogen
germanium
substrate
film
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US169276A
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Matovich Edwin
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Raytheon Co
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Hughes Aircraft Co
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Priority to US169276A priority Critical patent/US3152932A/en
Priority to GB496/63A priority patent/GB998211A/en
Priority to DEH47983A priority patent/DE1244112B/de
Priority to FR922094A priority patent/FR1345944A/fr
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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
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F23—COMBUSTION APPARATUS; COMBUSTION PROCESSES
    • F23N—REGULATING OR CONTROLLING COMBUSTION
    • F23N2225/00—Measuring
    • F23N2225/02—Measuring filling height in burners
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F23—COMBUSTION APPARATUS; COMBUSTION PROCESSES
    • F23N—REGULATING OR CONTROLLING COMBUSTION
    • F23N2235/00—Valves, nozzles or pumps
    • F23N2235/02—Air or combustion gas valves or dampers
    • F23N2235/06—Air or combustion gas valves or dampers at the air intake
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F23—COMBUSTION APPARATUS; COMBUSTION PROCESSES
    • F23N—REGULATING OR CONTROLLING COMBUSTION
    • F23N2235/00—Valves, nozzles or pumps
    • F23N2235/12—Fuel valves
    • 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
    • Y10S148/122—Polycrystalline
    • 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

  • United States l atent C) 3 152 as: REnUcrroN IN sun or A nn'nrxn MOLECU- ran GAS ADHERHNG TO A sunsraaru V EdwinMatovich, Costa Mesa, Calif 'assignor to Hughes-
  • This invention relates to deposition of crystal mate rial on substrates, and is particularly directed to nonepitaxial growth, or deposit, of semiconductor crystal material as abase for subsequent epitaxial growth.
  • Epitaxial growth of crystal material is the growth of a new crystal material upon a base in a manner to duplicate andextendthe crystal system of the base.
  • Single crystal material may be produced upon single crystal base material, and poly-crystalline material'may be grown on polycrystalline base materials.
  • Epitaxial deposit of crystalline material has been much used insemiconductor device manufacture to deposit high resistivity material upon low resistivity material for subsequent processing in the high resistivity region. Mechanisms for epitaxial deposit include disproportionation, as
  • FIGS; 1, 2'and3 are respectively a diagram of equipment'use'd 'andii'ow diagrams of processes according tothis invention. 7
  • FIG. 4' is a schematic sketch ofchemical reactiorisQ l andidipole arrangements at a material surface which is if. proposed to explain the process'illustratedin FIGS. 1-3.
  • P16. '1 schematically illustrates equipment used for growing single crystal germanium on substrates ofquartz, anodized metals. and alumina ceramlcs.
  • a flowing gas system is illustrated containing, in success on, a gas purication train, a metering and evaporation section, a mixing, and reaction section, and termination.
  • a source of pure hydrogen gas isprovided .by delivery of hydrogen gas through a valve 11 in pipe 12 and through 'acatalytic reactor 13 to react'any oxygen present to wathen through a liquid nitrogen cold trap 19 to remove residual water vapor and oxygen.
  • the H gas is next metered through'valve 15 to bubbler 16 where it passes through liquid germanium tetrachloride (GeCl the vapor, of which is entrained in a volume proportional to the vapor pressure of liquid, and the GeCL, rich H gas is mixed in mixer 17 with pure carrier H gas from valve 18 and passed through a gas mixing chamber 20 into a furnace or reaction chamber 21.
  • Mixer 17 and mixing chamber 20 are designed to avoid stratification of light H gas from the heavier gases.
  • a quartz boat 22 carriessubstrates 23 upon which germanium is tobe deposited, at least one surface thereof being preferablysubstantially masked at' vents through an oil bubbler 25 to prevent back diifusion of atmospheric air into the system, and the exhaust from bubbler 25 is a flare burner 26.
  • a source 27 of argon (A) gas for dilution or purging is connected ahead of'the desiccant chamber 14 and sources of other gases for doping the growing deposit of crystal material are provided in bubblers 31 and 32 which are connected to the hydrogen gas train in parallel with the germanium v tetrachloride bubbler.
  • Phosphorus trichlo-ride is supplied through bubbler 31 subject to control of valve 34', and boron tribromide is supplied through bubbler 32 subject'to control of valve 35.
  • the'conductivity type of the growth and its doping level may be controlled by alternate flow of enriching boron tribromide and phosphorous trichloride, to produce in turn P and N-type layers of germanium crystal material. Any of the haldies may be used so long as suitable temperatures are maintained for vapor pressure control.
  • the substrate 23 here taken to be anodized metal such as tantalum or quartz
  • the reaction train is then purged with purified hydrogen gas.
  • the sample 23 in chamber 21 is then heated to between 420 C. and 590 C., and the valve 15 is opened to'entrain GeCli, fromthe bubbler 16.
  • the valve 15 is opened to'entrain GeCli, fromthe bubbler 16.
  • HGeClg is a polar, or dipole; molecule, the negative pole beingthe Cl-rich end'. Since any solid heated in the flowing gas system becomes positively charged by thermi'onic emission and adsorbs H gas, and the H side of the HGeCl molecule is positive, the HGeCl molecule attaches to the solid by electrostatic attractions. These surface molecules, deposited between 420 Clandf 590 C., aare o'riented" because of their dipole structure. The at tachrnent and orientation of the HGeCl molecule to the material surface after reaction (4) is illustratedby FIG. 4(a), the hydrogen atom being presumably aligned with an oxygen atom of the surface.
  • the temperature may now be r'a'isedto over 600 C. in flowing H or about, 6509 C., to 700 C., at which temperatures the surface. will be hydrogen-reduced to germanium without disorienting.
  • This hydrogen reduction may be a two step process by-which the aligned hydrogen and oxygen atoms of FIG. 4(a) are first removed in a water-forming'reaction to associate the germanium directly onto the surface Patented Get. 1'3, 1964- the reduced Ge film.
  • the germanium is further reduced to the form shown in FIG. 4(0).
  • the temperature is then reduced to 420 C..to 590 C., and the germanium tetrachloride turned on again to begin epitaxial growth on the first-deposited Ge surface as illustrated in FIG. 4(d).
  • GeCL concentrations of less than 0.1 mole percent in H should be used to avoid an etching reaction. Growth rates of 12 microns per hour may be obtained with total gas flow of 250 cm. per minute in laboratory furnace chambers.
  • the reduction step may also be done below 600 C. in reducing hydrogen gas.
  • the initial coating of the surface with the dipolar molecules may take place in a different temperature range, but it will be below the complete reduction temperature for reduction to pure metal in hydrogen gas, so that the process steps are similar in first coating the surface with the dipolar, metal-containing molecule below the reduction temperature, then heating in pure hydrogen gas to complete the reduction of the molecule, followed next by further metal deposit by one of the epitaxial growth processes.
  • the word metal includes semiconductor materials.
  • a mixture of SiCl and hydrogen gas may be delivered to the chamber 21 at a substrate temperature between 730 and 910 C. to coat the substrate surface with the dipolar molecules SiHCl Which may then be reduced to a silicon coating by very reducing hydrogen gas or by heating in hydrogen gas to over 910 C.
  • chloride gases are preferred for formation of the polar molecules, and are sufficiently polar to produce highly oriented films and large areas of single crystal semiconductor material upon completion of the epitaxial growing process
  • other halogens may be used, namely bromides and iodides, and the reaction temperatures may be adjusted accordingly.
  • the process ofcoating a substrate with an adherent molecular film of a semiconductor-material-containing dipole molecule may be used to produce epitaxial films for semiconductor device manufacture.
  • a quartz substrate 41 shown in FIG. 2a, is coated with an adherent film 42 of GeHCl shown in FIG. 2b, by the process heretofore described.
  • the film 42 is next reduced to a germanium film 43, shown in FIG. 20, in dry, deoxidized hydrogen, preferably at 650 C. to accelerate the reaction.
  • the quartz surface is then exposed to a stream of germanium tetrachloride in hydrogen as before, together with a small percentage of boron tribromide in about .001 mole percent, at 500 C., to deposit P-type conductivity germanium on the germanium coated quartz surface epitaxially as shown in FIG. 2d.
  • the flow of boron tribromide is interrupted and a stream of phosphorus trichloride is substituted, growing an additional epitaxial layer 44 of N-type germanium.
  • the resulting product as shown in FIG.
  • etching reaction tends to dissolve the surface, including the dopant impurity material, which is in turn redeposited. By reducing the etching portion of the reaction, sharper changes in resistivity in the epitaxial material are obtainable.
  • dopant source compounds may be used, as for example AsCl or AsBr for P-type dopants.
  • FIG. 3 illustrates the production of a device utilizing the intermediate oxidation step discussed in the process in connection with FIG. 1. Selective area growth of epitaxial material is thus obtained.
  • FIG. 3a shows an anodizedmetal substrate 50 such as anodized molybdenum or tantalum, the surface film 51 being an electrically insulating oxide film.
  • a polar gas film 52 in FIG. 3b is produced by exposure to SiCL; gas in hydrogen at about 800 C., or between about 730 and 910 C.
  • the polar gas of film 52 is next reduced to silicon in a hydrogen stream at 950 C., producing a sili con film 49 on the anodized surface film 51 as shown in FIG. 30.
  • This silicon film or coating is believed to be monomolecular.
  • the surface film 49 is then oxidized, as by exposure to water vapor, or oxygen, in a hydrogen gas stream to produce a silicon oxide film 53 (believed to .be largely SiO on film 51, as shown in FIG. 3d.
  • a mask 54- against a silicon oxide etchant is next placed on the film 53 where subsequent epitaxial growth is desired, and the exposed portion of the SiO film is removed.
  • An HF etch is preferred, and polymerizable photosensitive materials, such as Kodak Photo Resist, of Eastman Kodak Company, may be used to produce the mask 54.
  • FIG. 3e shows the masked film 53 prior to etching
  • FIG. 3 1 shows the etched film with the mask 54.
  • the mask 54 is then removed as shown in FIG. 3g.
  • the remaining SiO film 53 isexposed to reducing H gas to convert the same to a silicon film 55 as shown in FIG. 3h.
  • the surface of the substrate is then again exposed to the mixture of reducing hydrogen and SiCL, to deposit an adherent film 56 of SiHCl over theanodized oxide film 51, and to epitaxially grow additional silicon over the reduced silicon film 55 while inhibiting further growth over the balance of the surface.
  • a growth of the film 55 a
  • Germanium tetrachloride in a dry, deoxidizedhydrogen I stream in a concentration of about 0.1 mole'percent is passed over the substrate at 500 C., producing Gel- C1 P-type impurity producing material such as BBr is added to the silicon haloform gas in an amount of about 0.001
  • PN junction containing semiconductor crystal remains upon removal of the mask 63, as shown in FIG. 3 j, and suitable metal connectors 65 and 66 may be deposited connecting to the respective P and N-type film portions as shown in FIG. 3k. Since the film 55 is deposited on the electrically insulating layer or film 51, the resulting device is a diode. Similar techniques may be used toproduce transistors and other devices" upon noncrystalline sub strates by the process herein disclosed.
  • a method of growing a crystalline layer on a refractory material substrate surface which method comprises:
  • a method of growing a crystalline layer on a substrate surface of material of the class consisting of metals, quantz, ceramics, oxides and oxidized metals which method comprises:
  • fractory material substrate surface which method comprises:
  • a method of growing a crystalline layer on a refractory material substrate surface which method comprises:
  • A" method of growing a germanium semiconductor layer on a surface of a refractory substrate which comprises:
  • a method of growing a crystalline layer on a refractory material substrate surface which method comprises:
  • a method of growing a crystalline layer on a refractory material substrate surface which method comprises:
  • exposing the surface to a haloform gas of the material to .be grown at a temperature, below the decomposition temperature of the gas, at which the molecules on a surface of a refractory substrate which comprises: exposing the surface to an effective mixture of silicon tetrahalide and hydrogen at a temperature between 730 C. and 910 C. to coat the surface with a film of reduciblesilicon compound; exposing the coated surface to hydrogen-containing reducing gas at a temperature sufficient to reduce the silicon surface compound to metallic silicon; and subjecting the silicon coated surface to additional reducible silicon compound in a hydrogen carrier gas stream and at a temperature to deposit additional silicon on said surface.
  • a method of growing a semiconductor layer of material of the class consisting of germanium and silicon on a surface of a refractory substrate which comprises: exposing the surface to a mixture of a haloform gas of said classwith a reducible compound of said material 11'.
  • oxides and oxidized metals which comprises: exposing the surface to a mixture of a haloform gas of said material and hydrogen at a temperature suf- 'ficient to coat said surface with a reducible ,com-
  • a method of growing a layer of semiconductor material of the class consisting of silicon and germanium selectively on a refractory surface which comprises:
  • a method of growing a layer of semiconductor material of the class consisting of silicon and germanium selectively on a refractory surface which comprises:

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  • Crystallography & Structural Chemistry (AREA)
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US169276A 1962-01-29 1962-01-29 Reduction in situ of a dipolar molecular gas adhering to a substrate Expired - Lifetime US3152932A (en)

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Application Number Priority Date Filing Date Title
US169276A US3152932A (en) 1962-01-29 1962-01-29 Reduction in situ of a dipolar molecular gas adhering to a substrate
GB496/63A GB998211A (en) 1962-01-29 1963-01-04 Method of producing monocrystalline semiconductor material
DEH47983A DE1244112B (de) 1962-01-29 1963-01-17 Verfahren zur Erzeugung einer Germanium- oder Siliciumschicht auf einer erhitzten Flaeche eines Substrats
FR922094A FR1345944A (fr) 1962-01-29 1963-01-21 Procédé de fabrication d'une matière semi-conductrice monocristalline

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3345223A (en) * 1965-09-28 1967-10-03 Ibm Epitaxial deposition of semiconductor materials
US3354004A (en) * 1964-11-17 1967-11-21 Ibm Method for enhancing efficiency of recovery of semi-conductor material in perturbable disproportionation systems
US3361600A (en) * 1965-08-09 1968-01-02 Ibm Method of doping epitaxially grown semiconductor material
US3645785A (en) * 1969-11-12 1972-02-29 Texas Instruments Inc Ohmic contact system
CN116397115A (zh) * 2023-03-23 2023-07-07 山东有研国晶辉新材料有限公司 一种金属锗的制备方法

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CA1280055C (fr) * 1985-10-24 1991-02-12 Ronald Edward Enstrom Dispositif de deposition en phase vapeur

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2692839A (en) * 1951-03-07 1954-10-26 Bell Telephone Labor Inc Method of fabricating germanium bodies
US2880117A (en) * 1956-01-20 1959-03-31 Electronique & Automatisme Sa Method of manufacturing semiconducting materials
US2910394A (en) * 1953-10-02 1959-10-27 Int Standard Electric Corp Production of semi-conductor material for rectifiers

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE883784C (de) * 1949-04-06 1953-06-03 Sueddeutsche App Fabrik G M B Verfahren zur Herstellung von Flaechengleichrichtern und Kristallverstaerkerschichten aus Elementen
DE885756C (de) * 1951-10-08 1953-06-25 Telefunken Gmbh Verfahren zur Herstellung von p- oder n-leitenden Schichten
NL130620C (fr) * 1954-05-18 1900-01-01

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2692839A (en) * 1951-03-07 1954-10-26 Bell Telephone Labor Inc Method of fabricating germanium bodies
US2910394A (en) * 1953-10-02 1959-10-27 Int Standard Electric Corp Production of semi-conductor material for rectifiers
US2880117A (en) * 1956-01-20 1959-03-31 Electronique & Automatisme Sa Method of manufacturing semiconducting materials

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3354004A (en) * 1964-11-17 1967-11-21 Ibm Method for enhancing efficiency of recovery of semi-conductor material in perturbable disproportionation systems
US3361600A (en) * 1965-08-09 1968-01-02 Ibm Method of doping epitaxially grown semiconductor material
US3345223A (en) * 1965-09-28 1967-10-03 Ibm Epitaxial deposition of semiconductor materials
US3645785A (en) * 1969-11-12 1972-02-29 Texas Instruments Inc Ohmic contact system
CN116397115A (zh) * 2023-03-23 2023-07-07 山东有研国晶辉新材料有限公司 一种金属锗的制备方法

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GB998211A (en) 1965-07-14
FR1345944A (fr) 1963-12-13
DE1244112B (de) 1967-07-13

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