US3790404A - Continuous vapor processing apparatus and method - Google Patents

Continuous vapor processing apparatus and method Download PDF

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Publication number
US3790404A
US3790404A US00263915A US3790404DA US3790404A US 3790404 A US3790404 A US 3790404A US 00263915 A US00263915 A US 00263915A US 3790404D A US3790404D A US 3790404DA US 3790404 A US3790404 A US 3790404A
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United States
Prior art keywords
zone
gas
reaction zone
gaseous reactant
exit
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Expired - Lifetime
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US00263915A
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English (en)
Inventor
R Garnache
A Ghatalia
R Michaud
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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
    • C30B31/00—Diffusion or doping processes for single crystals or homogeneous polycrystalline material with defined structure; Apparatus therefor
    • C30B31/06—Diffusion or doping processes for single crystals or homogeneous polycrystalline material with defined structure; Apparatus therefor by contacting with diffusion material in the gaseous state
    • C30B31/10—Reaction chambers; Selection of materials therefor
    • C30B31/106—Continuous processes
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/54—Apparatus specially adapted for continuous coating
    • 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
    • C30B31/00—Diffusion or doping processes for single crystals or homogeneous polycrystalline material with defined structure; Apparatus therefor
    • C30B31/06—Diffusion or doping processes for single crystals or homogeneous polycrystalline material with defined structure; Apparatus therefor by contacting with diffusion material in the gaseous state
    • C30B31/16—Feed and outlet means for the gases; Modifying the flow of the gases
    • 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
    • Y10S438/935—Gas flow control

Definitions

  • lntematiqnal Business Machines Apparatus for effecting uniform and continuous mass col'lml'imon, Armonk, transport reactions, such as oxidation, diffusion, etch- [22] Filed. June 19 1972 ing, etc., between a gaseous phase reactant and semiconductor substrates.
  • the apparatus comprises a lon- PP N04 263,915 gitudinal process tube, which includes a reaction zone flanked on either side by a combination entrance- [52] us C
  • 11/08 gas is P the reaction Zone at a fixed [58] Field of Searchl 17/106 A, 106 R, 1071 1072 rate and allowed to escape from the reaction zone axi- 1 17/54. 118/48 49 d ally through the two exhaust zones.
  • This invention relates to the processing of semiconductor devices and more particularly to apparatus for continuously carrying out mass transfer operations between gaseous phase materials and solid substrate surfaces.
  • the basic aspects of the instant invention provide for substantial improvement in the quality of mass produced articles through the use of a process tube of simplified construction and operation.
  • the process tube essentially comprises a centralized reaction zone flanked on either side by a multi-functional region formed by a simple longitudinal partition dividing that portion of the tube into two isolated chambers. On one side of the reaction zone there is provided an exhaust and an entrance zone and on the other side an exhaust and an exit zone. Reactant gas is provided to the reaction zone at a constant flow rate.
  • the structure of the process tube causes the reacting gas to flow axially through the reaction zone and out both ends.
  • a flow of purge gas, or other compatible gas, is provided to both the entrance and exit zones at a rate sufficient to cause some gas to flow into the reaction zone where it immediately is swept out through its associated exhaust zone by the axially flowing reactant gas. Substrates are passed sequentially through the entrance, reaction and exit zones and are exposed to the reactant for a precisely predetermined time which provides extremely uniform processing.
  • FIG. 1 is an isometric view of the preferred embodiment of the invention showing the general layout and structure of the process tube.
  • FIG. 2 is a partial sectional view of a preferred embodiment of the invention showing the required gas flow patterns in the vicinity of the reaction zone.
  • FIG. 3 is a partial isometric view of one end of a second embodiment of the invention showing the structure of a modified partition used to isolate the exit zone from one of the exhaust zones.
  • FIG. 4 is a plot of the effect of a reaction parameter versus the flow rate of gas in the entrance/exit zones showing the independence of the reaction parameter to flow rate above a critical flow rate.
  • FIG. I there is shown an isometric view of the preferred embodiment of process tube 10.
  • the basic supporting structure for process tube 10 is a commercially procured rectangular quartz tube nominally measuring W1 inch high, 2 r inches wide, and 72 inches long.
  • a flat tube is preferred as it facilitates stacking of multiple tubes in a standard furnace thereby increasing throughput.
  • the central portion, between partitions 12 and 14, defines the reaction zone, as indicated in FIG. 1.
  • a second portion of tube 10 contains partition 12 defining an substrate entrance region, a third portion defines a gas exit region. These last mentioned portions are described more fully in connection with FIG. 2.
  • Mounted on the side of tube 10 there is provided two gas inlet tubes 16 and 18 through which gases may be passed into the entrance and exit zones.
  • a gaseous reactant inlet tube 20 In order to supply a gaseous reactant to the reaction zone there is provided a gaseous reactant inlet tube 20.
  • Representative substrate carriers 22 and semiconductor wafers 24 are shown at the exit end of tube and normally would be moved either continuously or incrementally through tube 10 during processing.
  • FIG. 2 there is shown a partial sectional view of process tube 10 mounted inside a commercial furnace consisting of heating blocks 26 and elements 28.
  • the gaseous reactant introduced through inlet 20 is supplied at a fixed volumetric rate to the reaction zone, defined by the ends of partitions l2 and 14, and allowed to pass freely out both exhaust zones.
  • a non-reactant, or purge gas is applied to inlets l6 and 18 of entrance zone 34 and exit zone 36.
  • This purge gas may conveniently be an inert gas or may be any other reactant compatible with the primary reactant supplied to the reactant zone.
  • FIG. 2 also shows the gas flow pattern necessary to isolate the reactant gas without a need for complicated pressure regulating or metering devices.
  • Reactant gas flow is indicated by long-short dashed lines 38 and purge gas flow by dashed lines 40 and 40.
  • FIG. 3 there is shown a partial isometric view of one end of a modified process tube.
  • a second extension 46 to partitions l2 and 14.
  • an exhaust port 48 which allows for more convenient removal of exhaust and purge gases through an overhead hood. It is not normally necessary to provide for further isolation of exhausted gases as the ambient temperature at the ends of the process tube is usually not sufiiciently high to support a reaction. In situations where low temperature reactions are utilized further isolation is necessary.
  • process tube 10 is placed in a furnace in which a desired temperature profile may be maintained throughout the length of the tube.
  • a reactantgas supply 15 connected through a control-valve to gaseous reactant inlet tube 20.
  • a supply of purge, or other desired gas, is connected to gas inlet tubes 16 and 18.
  • Semiconductor wafers 24 are placed on carriers 22 and passed at a constant rate through process tube 10. Reactant gas is passed into the reaction zone at a fixed rate allowing it to pass into both exhaust zones as well as the entrance and exit zones.
  • Purge gas is then passed into, for example the entrance zone at a relatively high but carefully regulated flow rate, not exceeding that of the reactant gas.
  • the flow rate of purge gas into the exit zone is then incrementally increased from zero, allowing sufficient time between changes to allow sample wafers to pass completely through the reaction zone.
  • Processed semiconductor wafers are examined to determine the conditions at which the purge gas flow rate no longer influences the reaction product. For example, such parameters as oxide thickness, diffusion depth or flatband voltage may be measured.
  • FIG. 4 there is shown a plot of a typical reaction parameter versus entrance/exit flow rate for a fixed reactant flow in a symmetrical process tube. Curve 50 initially shows a linear dependence on purge gas flow rate.
  • the reaction parameter is no longer dependent upon purge gas flow rate.
  • An operating point such as point 52 should be chosen such that expected variations in purge gas flow rate will not effect the reaction. If the process tube is symmetrical, in that both entrance and exit zones are of identical construction, the above determined operating point may be used to determine the proper flow rate in both the entrance and exit zones as they will be equal. If, however, structural variations exist between entrance and exit zones, it is preferable to repeat the above procedure by varying the entrance flow rate and monitoring reactant parameters. Alternately, both entrance and exit purge gas flow rates may be varied simultaneously to establish an operating point.
  • a process tube constructed in accordance with the above description and having a reaction zone measuring 26 A inches between partitions was mounted in a commercial diffusion furnace.
  • a flat temperature profile of 1 C was maintained over about 28 inches, including all of the reaction zone.
  • Partially processed semiconductor wafers were placed on quartz carriers and passed incrementally at 120 second intervals, 1 A inch at a time, through the process tube.
  • Dry oxygen was supplied to both the entrance zone inlet and reaction zone inlet at a flow rate of 2000 cubic centimeters per minute.
  • the nitrogen supply was connected to the exit zone inlet, but no nitrogen flow was initially supplied. This condition allowed oxygen to pass into the exit zone creating an extended oxidation zone.
  • An initial oxide thickness of 870 angstrom units was obtained.
  • said first region including a longitudinal partition dividing said first region into a gas exhaust zone and a substrate inlet zone, said third region also having a longitudinal partition dividing said third region into a gas exhaust zone and a substrate exit zone, said second region being a reaction zone;
  • a process tube having a longitudinal axis a longitudinal first portion of said tube defining a reaction zone
  • first partition means mounted adjacent to one end of said process zone, said first partition means dividing a longitudinal second portion of said process tube into an upper first gas exhaust zone and a lower substrate entrance zone,
  • a gas inlet means in said reaction zone for providing a continuous flow of a first gaseous reactant through said reaction zone and said first and second exhaust zones; gas means in said entrance zone for continuously providing a first gas, other than said gaseous reactant, to said entrance zone at a rate sufficient to cause at least some of said first gas to flow into said reaction zone and said first exhaust zone; and gas inlet means in said exit zone for continuously providing a second gas, other than said gaseous reactant, to said exit zone at a rate sufficient to cause at least some of said second gas to flow into said reaction zone and said second exhaust zone.
  • both said first and second gases comprise a second and third gaseous reactant.
  • the apparatus of claim 2 including heating means to maintain said reaction zone at a predetermined temperature.
  • ends of said partitions adjacent to said reaction zone include means to restrict the flow of said first and second gases between said entrance and exit zones and said reaction zone.

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  • Chemical & Material Sciences (AREA)
  • Metallurgy (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Mechanical Engineering (AREA)
  • General Chemical & Material Sciences (AREA)
  • Drying Of Semiconductors (AREA)
  • ing And Chemical Polishing (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)
  • Chemical Vapour Deposition (AREA)
US00263915A 1972-06-19 1972-06-19 Continuous vapor processing apparatus and method Expired - Lifetime US3790404A (en)

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US26391572A 1972-06-19 1972-06-19

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US (1) US3790404A (en:Method)
JP (1) JPS5551331B2 (en:Method)
DE (1) DE2327351A1 (en:Method)
FR (1) FR2189874B1 (en:Method)
GB (1) GB1380511A (en:Method)

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4504526A (en) * 1983-09-26 1985-03-12 Libbey-Owens-Ford Company Apparatus and method for producing a laminar flow of constant velocity fluid along a substrate
US4662981A (en) * 1983-02-23 1987-05-05 Koito Seisakusho Co., Ltd. Method and apparatus for forming crystalline films of compounds
US4807561A (en) * 1986-05-19 1989-02-28 Toshiba Machine Co., Ltd. Semiconductor vapor phase growth apparatus
US5393563A (en) * 1991-10-29 1995-02-28 Ellis, Jr.; Frank B. Formation of tin oxide films on glass substrates
US5563095A (en) * 1994-12-01 1996-10-08 Frey; Jeffrey Method for manufacturing semiconductor devices
US5620932A (en) * 1993-07-06 1997-04-15 Shin-Etsu Handotai Co., Ltd. Method of oxidizing a semiconductor wafer
US5920078A (en) * 1996-06-20 1999-07-06 Frey; Jeffrey Optoelectronic device using indirect-bandgap semiconductor material
WO2007033832A3 (de) * 2005-09-23 2007-06-14 Fraunhofer Ges Forschung Vorrichtung und verfahren zur kontinuierlichen gasphasenabscheidung unter atmosphärendruck und deren verwendung

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2718184C2 (de) * 1977-04-23 1982-10-14 Philips Patentverwaltung Gmbh, 2000 Hamburg Verfahren und Vorrichtung zum kontinuierlichen Beschichten eines langgestreckten Körpers
JPS5862489A (ja) * 1981-10-07 1983-04-13 株式会社日立製作所 ソフトランデイング装置
US5364007A (en) * 1993-10-12 1994-11-15 Air Products And Chemicals, Inc. Inert gas delivery for reflow solder furnaces

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3623854A (en) * 1968-08-28 1971-11-30 Owens Illinois Inc Vapor treatment of containers with finish air barrier
US3672948A (en) * 1970-01-02 1972-06-27 Ibm Method for diffusion limited mass transport
US3689304A (en) * 1969-04-23 1972-09-05 Pilkington Brothers Ltd Treating glass
US3688737A (en) * 1969-11-04 1972-09-05 Glass Container Mfg Inst Inc Vapor deposition apparatus including air mask

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3623854A (en) * 1968-08-28 1971-11-30 Owens Illinois Inc Vapor treatment of containers with finish air barrier
US3689304A (en) * 1969-04-23 1972-09-05 Pilkington Brothers Ltd Treating glass
US3688737A (en) * 1969-11-04 1972-09-05 Glass Container Mfg Inst Inc Vapor deposition apparatus including air mask
US3672948A (en) * 1970-01-02 1972-06-27 Ibm Method for diffusion limited mass transport

Cited By (17)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4662981A (en) * 1983-02-23 1987-05-05 Koito Seisakusho Co., Ltd. Method and apparatus for forming crystalline films of compounds
US4668480A (en) * 1983-02-23 1987-05-26 Koito Seisakusho Co., Ltd. 7C apparatus for forming crystalline films of compounds
WO1985001522A1 (en) * 1983-09-26 1985-04-11 Libbey-Owens-Ford Company Method and apparatus for coating a substrate
AU575349B2 (en) * 1983-09-26 1988-07-28 Libbey-Owens-Ford Company Method and apparatus for coating a substrate
US4504526A (en) * 1983-09-26 1985-03-12 Libbey-Owens-Ford Company Apparatus and method for producing a laminar flow of constant velocity fluid along a substrate
US4807561A (en) * 1986-05-19 1989-02-28 Toshiba Machine Co., Ltd. Semiconductor vapor phase growth apparatus
US5393563A (en) * 1991-10-29 1995-02-28 Ellis, Jr.; Frank B. Formation of tin oxide films on glass substrates
US5487784A (en) * 1991-10-29 1996-01-30 Ellis, Jr.; Frank B. Formation of tin oxide films on glass substrates
US5620932A (en) * 1993-07-06 1997-04-15 Shin-Etsu Handotai Co., Ltd. Method of oxidizing a semiconductor wafer
US5563095A (en) * 1994-12-01 1996-10-08 Frey; Jeffrey Method for manufacturing semiconductor devices
US5753531A (en) * 1994-12-01 1998-05-19 The University Of Maryland At College Park Method for continuously making a semiconductor device
US6019850A (en) * 1994-12-01 2000-02-01 Frey; Jeffrey Apparatus for making a semiconductor device in a continuous manner
US5920078A (en) * 1996-06-20 1999-07-06 Frey; Jeffrey Optoelectronic device using indirect-bandgap semiconductor material
WO2007033832A3 (de) * 2005-09-23 2007-06-14 Fraunhofer Ges Forschung Vorrichtung und verfahren zur kontinuierlichen gasphasenabscheidung unter atmosphärendruck und deren verwendung
US20080317956A1 (en) * 2005-09-23 2008-12-25 Fraunhofer-Gesellschaft Zur Forderung Der Angewandten Forschung E.V. Device and Method for Continuous Chemical Vapour Deposition Under Atmospheric Pressure and Use Thereof
US8900368B2 (en) * 2005-09-23 2014-12-02 Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. Device and method for continuous chemical vapour deposition under atmospheric pressure and use thereof
US9683289B2 (en) 2005-09-23 2017-06-20 Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. Device and method for continuous chemical vapour deposition under atmospheric pressure and use thereof

Also Published As

Publication number Publication date
FR2189874B1 (en:Method) 1977-09-02
JPS5551331B2 (en:Method) 1980-12-23
DE2327351A1 (de) 1974-01-03
FR2189874A1 (en:Method) 1974-01-25
JPS4944668A (en:Method) 1974-04-26
GB1380511A (en) 1975-01-15

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