US20080075838A1 - Oxidation apparatus and method for semiconductor process - Google Patents

Oxidation apparatus and method for semiconductor process Download PDF

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Publication number
US20080075838A1
US20080075838A1 US11/902,180 US90218007A US2008075838A1 US 20080075838 A1 US20080075838 A1 US 20080075838A1 US 90218007 A US90218007 A US 90218007A US 2008075838 A1 US2008075838 A1 US 2008075838A1
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Prior art keywords
gas
deoxidizing
process field
oxidation
oxidizing gas
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US11/902,180
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Inventor
Hisashi Inoue
Masataka Toiya
Yoshikatsu Mizuno
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Tokyo Electron Ltd
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Tokyo Electron Ltd
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Assigned to TOKYO ELECTRON LIMITED reassignment TOKYO ELECTRON LIMITED ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: MIZUNO, YOSHIKATSU, TOIYA, MASATAKA, INOUE, HISASHI
Publication of US20080075838A1 publication Critical patent/US20080075838A1/en
Priority to US13/025,738 priority Critical patent/US8153534B2/en
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    • 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
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • 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
    • C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
    • C23C8/08—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases only one element being applied
    • C23C8/10—Oxidising
    • 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
    • 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
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02104—Forming layers
    • H01L21/02107—Forming insulating materials on a substrate
    • H01L21/02225—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer
    • H01L21/02227—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a process other than a deposition process
    • H01L21/0223—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a process other than a deposition process formation by oxidation, e.g. oxidation of the substrate
    • H01L21/02233—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a process other than a deposition process formation by oxidation, e.g. oxidation of the substrate of the semiconductor substrate or a semiconductor layer
    • H01L21/02236—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a process other than a deposition process formation by oxidation, e.g. oxidation of the substrate of the semiconductor substrate or a semiconductor layer group IV semiconductor
    • H01L21/02238—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a process other than a deposition process formation by oxidation, e.g. oxidation of the substrate of the semiconductor substrate or a semiconductor layer group IV semiconductor silicon in uncombined form, i.e. pure silicon
    • 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
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02104—Forming layers
    • H01L21/02107—Forming insulating materials on a substrate
    • H01L21/02225—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer
    • H01L21/02227—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a process other than a deposition process
    • H01L21/02255—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a process other than a deposition process formation by thermal treatment
    • 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
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
    • H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
    • H01L21/31—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to form insulating layers thereon, e.g. for masking or by using photolithographic techniques; After treatment of these layers; Selection of materials for these layers
    • H01L21/314—Inorganic layers
    • H01L21/316—Inorganic layers composed of oxides or glassy oxides or oxide based glass
    • H01L21/3165—Inorganic layers composed of oxides or glassy oxides or oxide based glass formed by oxidation
    • H01L21/31654—Inorganic layers composed of oxides or glassy oxides or oxide based glass formed by oxidation of semiconductor materials, e.g. the body itself
    • H01L21/31658—Inorganic layers composed of oxides or glassy oxides or oxide based glass formed by oxidation of semiconductor materials, e.g. the body itself by thermal oxidation, e.g. of SiGe
    • H01L21/31662—Inorganic layers composed of oxides or glassy oxides or oxide based glass formed by oxidation of semiconductor materials, e.g. the body itself by thermal oxidation, e.g. of SiGe of silicon in uncombined form
    • 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
    • H01L21/67—Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere
    • H01L21/67005—Apparatus not specifically provided for elsewhere
    • H01L21/67011—Apparatus for manufacture or treatment
    • H01L21/67098—Apparatus for thermal treatment
    • H01L21/67109—Apparatus for thermal treatment mainly by convection

Definitions

  • the present invention relates to an oxidation apparatus and method for a semiconductor process for oxidizing the surface of a target substrate, such as a semiconductor wafer.
  • semiconductor process used herein includes various kinds of processes which are performed to manufacture a semiconductor device or a structure having wiring layers, electrodes, and the like to be connected to a semiconductor device, on a target substrate, such as a semiconductor wafer or a glass substrate used for an FPD (Flat Panel Display), e.g., an LCD (Liquid Crystal Display), by forming semiconductor layers, insulating layers, and conductive layers in predetermined patterns on the target substrate.
  • FPD Fer Panel Display
  • LCD Liquid Crystal Display
  • a semiconductor substrate such as a silicon wafer
  • various processes such as film formation, etching, oxidation, diffusion, and reformation, in general.
  • oxidation includes oxidation of the surface of a mono-crystalline silicon film or a poly-crystalline silicon film, and oxidation of a metal film.
  • a silicon oxide film formed by oxidation is applied to a device isolation film, gate oxide film, capacitor insulating film, or the like.
  • oxidation can be performed by dry oxidation that employs oxygen gas, or wet oxidation that employs water vapor.
  • an oxide film formed by wet oxidation is higher in film quality than an oxide film formed by dry oxidation. Accordingly, in consideration of film properties, such as breakdown voltage, corrosion resistance, and reliability, a wet oxide film is better as an insulating film.
  • the film formation rate of an oxide film (insulating film) to be formed and the planar uniformity thereof on a wafer are also important factors.
  • a film formed by wet oxidation under a normal pressure shows a high oxidation rate, but shows poor planar uniformity of film thickness, in general.
  • a film formed by wet oxidation under a vacuum pressure shows a low oxidation rate, but shows good planar uniformity of film thickness.
  • H 2 gas and O 2 gas are caused to react with each other under a low pressure of about 1 Torr and a relatively low temperature of, e.g., lower than 900° C. to generate oxygen radicals and hydroxyl group radicals. These radicals are used to oxidize a wafer surface, so as to form, e.g., a silicon oxide film.
  • An object of the present invention is to provide an oxidation apparatus and method for a semiconductor process, which can simplify and speed up an adjustment operation for obtaining optimized process conditions, such as the flow rate of a deoxidizing gas.
  • an oxidation apparatus for a semiconductor process comprising: a process container having a process field configured to accommodate a plurality of target substrates at intervals in a vertical direction, a heater configured to heat the process field; an exhaust system configured to exhaust gas from inside the process field; an oxidizing gas supply circuit configured to supply an oxidizing gas to the process field; and a deoxidizing gas supply circuit configured to supply a deoxidizing gas to the process field, wherein the oxidizing gas supply circuit comprises an oxidizing gas nozzle extending over a vertical length corresponding to the process field, and having a plurality of gas spouting holes arrayed over the vertical length corresponding to the process field, and the deoxidizing gas supply circuit comprises a plurality of deoxidizing gas nozzles having different heights respectively corresponding to a plurality of zones of the process field arrayed vertically, and each having a gas spouting hole formed at height of a corresponding zone.
  • an oxidation method for a semiconductor process comprising: placing a plurality of target substrates at intervals in a vertical direction within a process field of a process container; respectively supplying an oxidizing gas and a deoxidizing gas to the process field, while heating the process field; causing the oxidizing gas and the deoxidizing gas to react with each other, thereby generating oxygen radicals and hydroxyl group radicals within the process field; and performing an oxidation process on a surface of the target substrates by use of the oxygen radicals and the hydroxyl group radicals, wherein the oxidizing gas is supplied from an oxidizing gas nozzle extending over a vertical length corresponding to the process field, and having a plurality of gas spouting holes arrayed over the vertical length corresponding to the process field, and the deoxidizing gas is supplied from a plurality of deoxidizing gas nozzles having different heights respectively corresponding to a plurality of zones of the process field arrayed
  • FIG. 1 is a sectional view showing a vertical heat processing apparatus (oxidation apparatus) according to an embodiment of the present invention
  • FIG. 2 is a graph for explaining the relationship in principle between the wafer position in a process container and optimized states of the film thickness of a silicon oxide film, obtained by the oxidation apparatus shown in FIG. 1 ;
  • FIG. 3 is a graph showing optimized states of the film thickness of a silicon oxide film, and actual states and planar uniformity of the film thickness of a silicon oxide film formed on product wafers, obtained by the oxidation apparatus shown in FIG. 1 and a conventional apparatus;
  • FIGS. 4A and 4B are sectional views for explaining the disposition of the thickness of a thin film formed on the surface of a semiconductor wafer
  • FIGS. 5A and 5B are views showing modifications of nozzles
  • FIG. 6A is a view showing a case where the gas spouting direction of gas spouting holes is directed to the center of a wafer;
  • FIG. 6B is a view schematically showing the relationship of an oxidizing gas nozzle and deoxidizing gas nozzles, each of which has gas spouting holes with an improved gas spouting direction, relative to the process container and wafer;
  • FIG. 6C is a view showing an alternative modification of the gas spouting direction of gas spouting holes
  • FIG. 7 is a graph showing the planar uniformity of film thickness obtained by the gas spouting holes shown in FIGS. 6A and 6B ;
  • FIGS. 8A and 8B are graphs each showing a change in the film thickness of an oxide film obtained when an oxidation process was performed on product wafers, the number of which was smaller than that in the full load state of a wafer boat;
  • FIG. 9 is a view schematically showing a conventional vertical heat processing apparatus (oxidation apparatus).
  • FIG. 10 is a graph for explaining the relationship in principle between the wafer position in a process container and optimized states of the film thickness of a silicon oxide film, obtained by the oxidation apparatus shown in FIG. 9 .
  • FIG. 9 is a view schematically showing a conventional vertical heat processing apparatus (oxidation apparatus).
  • the oxidation apparatus includes a process container 2 formed of a quartz cylinder with a ceiling, in which a wafer boat 4 made of quartz is accommodated.
  • the wafer boat 4 can support a plurality of, such as about 25 to 150, semiconductor wafers W at predetermined intervals in the vertical direction.
  • the wafer boat 4 is supported on a heat-insulating cylinder 6 , and is moved up and down by a boat elevator (not shown), so that the wafer boat 4 is loaded and unloaded into and from the process container 2 from and to a lower side.
  • the bottom port of the process container 2 is airtightly closed by a lid 8 , which is moved up and down by the boat elevator.
  • a gas nozzle 10 for supplying oxygen gas and a plurality gas nozzles 12 A to 12 E for supplying hydrogen, gas are connected to a lower side of the process container 2 .
  • An exhaust port 14 is formed at a lower side of the process container 2 to vacuum-exhaust the inner atmosphere of the process container 2 by a vacuum pump 16 .
  • the oxygen gas nozzle 10 has an L-shape and extends inside the container so that the distal end reaches near the top.
  • the nozzle 10 has a gas spouting hole 10 A formed at the distal end, from which oxygen is supplied into the process container 2 on an upstream side of the gas flow, at a flow rate controlled by a mass flow controller 10 B.
  • the hydrogen gas nozzles 12 A to 12 E respectively have L-shapes with different lengths to correspond to different zones arrayed in the vertical direction inside the process container 2 .
  • the nozzles 12 A to 12 E respectively have gas spouting holes 13 A to 13 E formed at the distal end.
  • the hydrogen gas nozzles 12 A to 12 E are configured to supply hydrogen at flow rates controlled by respective mass flow controllers 15 A to 15 E.
  • the process field inside the process container 2 is divided into five zones 17 A to 17 E, into which H 2 gas can be supplied at gas flow rates optimized respectively for the zones 17 A to 17 E.
  • a cylindrical heater 18 is disposed around the process container 2 to heat the wafers W to a predetermined temperature.
  • H 2 gas and O 2 gas supplied into the process container 2 are burnt at a low pressure of about 1 Torr. Consequently, oxygen radicals and hydroxyl group radicals are generated and oxidize the wafer surface.
  • the hydrogen gas nozzles 12 A to 12 E arrayed along the zones can respectively replenish H 2 gas, which tends to become insufficient on a downstream side of the gas flow due to consumption on the wafer surface.
  • FIG. 10 is a graph for explaining the relationship in principle between the wafer position in a process container and optimized states of the film thickness of a silicon oxide film, obtained by the oxidation apparatus shown in FIG. 9 .
  • the horizontal axis denotes the wafer position numbered in descending order of position from the upstream side of the gas flow to the downstream side. In this embodiment, a higher wafer position in the process container 2 has a smaller number.
  • a characteristic line L 0 denotes a target film thickness, which is set at 13 nm in this example.
  • the H 2 gas flow rates of the nozzles are respectively adjusted to form an oxide film with a thickness of 13 nm on all the wafers in the vertical direction. On the other hand, the O 2 gas flow rate is fixed.
  • monitor wafers consisting of bare wafers (silicon is exposed without an SiO 2 film formed on the surface) for measuring the film thickness are placed between a plurality of dummy wafers with an SiO 2 film formed on the surface, which are used to resemble product wafers. Then, the thickness of an SiO 2 film formed on the surface of the monitor wafers by oxidation is measured, and the measurement values are plotted to form characteristic lines L 3 and L 5 , as shown in FIG. 10 . H 2 gas flow rates obtained in this operation are determined as optimum values.
  • the characteristic lines L 3 and L 5 are shaped as show in FIG. 10 , because of the following reason.
  • the film thickness tend to be smaller toward the downstream side due to consumption of the process gases. Accordingly, for example, where an SiO 2 film is formed while the H 2 gas flow rates of the nozzles 12 A to 12 E are set the same, a predicted characteristic line therefrom is a lined curved downward that indicates an decrease in film thickness with an increase in the number of the wafer position in FIG. 10 . Further, this decrease in film thickness on the downstream side (with an increase in the number of the wafer position) becomes prominent as the surface area of wafers is larger.
  • each of the characteristic lines L 3 and L 5 which are used for obtaining gas flow rates optimized for product wafers having a larger surface area (due to projected and recessed portions formed on the surface), is formed as a line curved upward to be essentially line-symmetric with the predicted characteristic line curved downward described above, relative to the characteristic line L 0 , thereby compensating for consumption of the process gases.
  • the characteristic line L 3 is a characteristic line used for an oxidation process applied to wafers each having a surface area increased to be three times larger (triple) by projected and recessed portions formed on the surface, as compared with a wafer having a flat surface.
  • the characteristic line L 5 is a characteristic line used for an oxidation process applied to wafers each having a surface area increased to be five times larger (quintuple) by projected and recessed portions formed on the surface.
  • H 2 gas is supplied from the gas nozzles 12 A to 12 E at flow rates obtained in formation of the characteristic line L 3 .
  • the flow rates of the H 2 gas nozzles 12 A to 12 E are respectively adjusted while the flow rate of O 2 gas is fixed at a certain value, as described above. Then, the gas flow rates are adjusted by repeating a trial-and-error operation, so as to attain the target film thickness indicated by the characteristic line L 0 when an oxidation process is actually performed on product wafers each having a surface area correspondingly multiplied.
  • a trial-and-error operation is preformed for each of wafer sets having different surface areas multiplied by different integer numbers.
  • the characteristic lines L 3 and L 5 are shifted each other in the vertical direction as a whole by that much corresponding to the film thickness difference. In each of the lines L 3 and L 5 , the thickness is gradually increased from the upstream side to the middle of the gas flow, and then becomes almost constant.
  • FIG. 10 shows only the characteristic lines L 3 and L 5 corresponding to two types of the surface area.
  • a characteristic line is required for each of several wafer sets having different surface areas multiplied by finely classified integer numbers, to obtaine H 2 gas flow rates for adjustment for each case. Accordingly, it is very difficult and troublesome to obtain optimized process conditions, such as the gas flow rates.
  • FIG. 1 is a sectional view showing a vertical heat processing apparatus (oxidation apparatus) according to an embodiment of the present invention.
  • the oxidation apparatus 22 has a process field configured to be selectively supplied with an oxidizing gas, such as O 2 gas, a deoxidizing gas, such as H 2 gas, and an inactive gas, such as N 2 gas.
  • the oxidation apparatus 22 is configured to oxidize the surface of target substrates, such as semiconductor wafers, in the process field.
  • the oxidation apparatus 22 includes a vertical process container 24 formed of a quartz cylinder with a ceiling.
  • the process container 24 has a predetermined length to define therein a process field 25 for accommodating and processing a plurality of semiconductor wafers (target substrates) stacked at predetermined intervals in the vertical direction.
  • a wafer boat 26 made of quartz is placed to support target substrates or semiconductor wafers W at predetermined intervals in the vertical direction. The intervals may be regular or irregular depending on the wafer position.
  • the process container 24 has a bottom port provided with a seal member 28 , such as an O-ring, and configured to be airtightly closed or opened by a lid 30 .
  • a rotary shaft 34 penetrates the lid 30 with a magnetic-fluid seal 32 interposed therebetween.
  • the rotary shaft 34 is connected to a rotary table 36 at the top, on which the wafer boat 26 is mounted through a heat-insulating cylinder 38 .
  • the rotary shaft 34 is attached to an arm 40 A of a boat elevator 40 movable in the vertical direction, so that the rotary shaft 34 is moved up and down along with the lid 30 and wafer boat 26 .
  • the wafer boat 26 is loaded and unloaded into and from the process container 24 from and to a lower side.
  • the wafer boat 26 may be fixed without being rotatable.
  • a cylindrical manifold made of, e.g., stainless steel may be disposed at the bottom of the process container 24 .
  • the sidewall of the process container 24 is connected near the bottom to an oxidizing gas supply circuit 42 and a deoxidizing gas supply circuit 44 respectively for supplying an oxidizing gas and a deoxidizing gas at controlled flow rates to the process field 25 .
  • an exhaust port 46 having a large diameter is formed in the sidewall of the process container 24 near the bottom to exhaust the atmosphere of the process field 25 .
  • the oxidizing gas supply circuit 42 includes an oxidizing gas nozzle 48 that penetrates the container sidewall.
  • the nozzle 48 is connected to a gas supply passage 50 provided with a flow rate controller 50 A, such as a mass flow controller, so that an oxidizing gas, such as oxygen, can be supplied at a controlled flow rate.
  • a flow rate controller 50 A such as a mass flow controller
  • the oxidizing gas nozzle 48 comprising a first nozzle portion extending from the bottom (one end) of the process container 24 to the top (the other end), and a second nozzle portion extending from the top to the bottom, such that the first and second nozzle portions are connected through a bent portion.
  • the oxidizing gas nozzle 48 has a U-shape extending in the vertical direction inside the process container 24 .
  • the oxidizing gas nozzle 48 has a plurality of gas spouting holes 48 A and 48 B for spouting O 2 gas, which are formed at predetermined intervals over the entire length and have a diameter of, e.g., about 0.1 to 0.4 mm (the gas spouting holes 48 A and 48 B may have the same opening surface area).
  • the intervals of the gas spouting holes 48 A and 48 B are set to be, e.g., about 8 to 200 mm (the intervals may be regular).
  • Each of the gas spouting holes 48 B formed on the second nozzle portion (downstream from the bent portion) of the oxidizing gas nozzle 48 is located at the center between two adjacent gas spouting holes 48 A formed on the first nozzle portion (upstream from the bent portion). Consequently, O 2 gas is supplied from positions distributed most in the vertical direction inside the process container 24 . Further, a gas spouting holes 48 A on a more upstream side is combined in position with a gas spouting holes 48 B on a more downstream side, so O 2 gas is spouted at an almost uniform flow rate toward all the wafers W inside the process container 24 . This is so, because O 2 gas has higher pressure and is spouted more at a gas spouting hole positioned on a more upstream side of the oxidizing gas nozzle 48 .
  • the deoxidizing gas supply circuit 44 includes a plurality of, such as five, deoxidizing gas nozzles 52 , 54 , 56 , 58 , and 60 that penetrate the container sidewall.
  • the nozzles 52 to 60 respectively connected to gas supply passages 62 , 64 , 66 , 68 , and 70 respectively provided with flow rate controllers 62 A, 64 A, 66 A, 68 A, 70 A, such as mass flow controllers, so that a deoxidizing gas, such as hydrogen, can be supplied at respectively controlled flow rates.
  • the process field 25 inside the process container 24 is divided into a plurality of, such as five, zones 72 A, 72 B, 72 C, 72 D, and 72 E, arrayed in the vertical direction, to correspond to the number of deoxidizing gas nozzles 52 to 60 .
  • the process field 25 is formed of five zones 72 A to 72 E arrayed from the upstream side of the gas flow to the downstream side.
  • the five deoxidizing gas nozzles 52 to 60 have different lengths to correspond to the five zones 72 A to 72 E.
  • the deoxidizing gas nozzles 52 to 60 respectively have sets of gas spouting holes 52 A, 54 A, 56 A, 58 A, and 60 A formed at the distal end to spout H 2 gas toward respective zones 72 A to 72 E.
  • the deoxidizing gas nozzles 52 to 60 respectively have sets of three gas spouting holes 52 A to 60 A formed at predetermined intervals.
  • the number of gas spouting holes is not limited to three.
  • the gas spouting holes 52 A to 60 A have a diameter of, e.g., about 0.1 to 0.4 mm (the gas spouting holes 52 A to 60 A may have the same opening surface area).
  • the intervals of the gas spouting holes 52 A to 60 A are set to be, e.g., about 8 to 200 mm (the intervals may be regular).
  • the exhaust port 46 formed in the sidewall of the process container 24 near the bottom is connected to a vacuum exhaust system 86 including an exhaust passage 80 provided with a pressure control valve 82 and a vacuum pump 84 to vacuum-exhaust the inner atmosphere of the process container 24 .
  • the process container 24 is surrounded by a cylindrical heat-insulating layer 88 , in which a heater 90 is disposed to heat the wafers W positioned inside to a predetermined temperature.
  • the process container 24 As regards the entire size of the process container 24 , for example, where 100 wafers W of 8-inch (product wafers) are processed together, the process container 24 has a height of about 1,300 mm. Where 25 to 50 wafers W of 12-inch are processed together, the process container 24 has a height of about 1,500 mm.
  • the oxidation apparatus 22 includes a control section 92 comprising, e.g., a micro-processor configured to control the flow rate controllers 50 A and 62 A to 70 A, pressure control valve 82 , and heater 90 , so as to generate oxygen radicals and hydroxyl group radicals by a reaction of the two gases. Further, the control section 92 is used for controlling the operation of the entire oxidation apparatus 22 , so it transmits instructions to control the oxidation apparatus 22 .
  • the control section 92 includes a storage medium or media 94 , such as a floppy disk, a flash memory, and/or a hard disk, which store programs for performing control operations.
  • the oxidation apparatus 22 further includes an inactive gas supply mechanism (not shown) for supplying an inactive gas, such as N 2 gas, as needed.
  • the process container 24 is maintained at a temperature lower than the process temperature.
  • the wafer boat 26 at room temperature, which supports a number of, such as 100, wafers is loaded from below into the process field 25 (of the process container 24 in a hot wall state) heated to a predetermined temperature.
  • the bottom port of the process container 24 is closed by the lid 30 to airtightly seal the process container 24 .
  • the process field 25 is vacuum-exhausted and kept at a predetermined process pressure. Further, the process field 25 is heated and kept at a process temperature for the oxidation process by increasing the power applied to the heater 90 . Thereafter, the predetermined process gases necessary for the oxidation process, i.e., O 2 gas and H 2 gas, are respectively supplied to the process field 25 at controlled flow rates through the oxidizing gas nozzle 48 and deoxidizing gas nozzles 52 to 60 of the gas supply circuits 42 and 44 .
  • the predetermined process gases necessary for the oxidation process i.e., O 2 gas and H 2 gas
  • O 2 gas is spouted in horizontal directions from the gas spouting holes 48 A and 48 B of the oxidizing gas nozzle 48 having a U-shape.
  • H 2 gas is supplied in horizontal directions from the gas spouting holes 52 A to 60 A of the deoxidizing gas nozzles 52 to 60 at controlled flow rates for the respective zones 72 A to 72 E.
  • O 2 gas is set to be within a range of 10 to 30,000 sccm
  • H 2 gas is set to be within a range of 1 to 5,000 sccm.
  • O 2 gas and H 2 gas are respectively supplied into the process container 24 and flow downward inside the process field 25 of the process container 24 in a hot wall state.
  • these gases generate an atmosphere mainly comprising oxygen radicals (O*) and hydroxyl group radicals (OH*) by a hydrogen combustion reaction in the vicinity of the wafers W.
  • O* oxygen radicals
  • OH* hydroxyl group radicals
  • the process conditions used at this time include a wafer temperature of 450 to 1,100° C., such as 900° C., a pressure of 466 Pa (3.5 Torr) or less, and preferably of 1 Torr or less, such as 46.6 Pa (0.35 Torr).
  • the process time is set to be, e.g., about 10 to 30 minutes, although it depends on the thickness of a film to be formed. If the process temperature is lower than 450° C., the activated species (radicals) described above cannot be sufficiently generated. If the process temperature is higher than 1,100° C., it exceeds the heat-resistant temperature of the process container 24 and/or wafer boat 26 , and jeopardizes the safety of the process. If the process pressure is higher than 3.5 Torr, the radicals described above cannot be sufficiently generated.
  • each product wafer actually processed has a surface area increased to be several times larger by projected and recessed portions formed on the surface, as compared with a wafer having a flat surface. Since consumption of radicals greatly varies, depending on the multiplication of the surface area, it is necessary to optimize process conditions, such as the flow rate of a gas to be supplied, in accordance with variation in wafer surface area, before an oxidation process is performed on product wafers.
  • process conditions such as the flow rate of a gas to be supplied, in accordance with variation in wafer surface area
  • characteristic lines of the film thickness are curved, as shown by the characteristic line L 3 for the triple surface area and the characteristic line L 5 for a quintuple surface area. In this case, an adjustment operation for obtaining gas flow rates needs to be performed in a trial-and-error manner, and thus is very troublesome.
  • the oxidizing gas nozzle 48 extends in the longitudinal direction, i.e., along the process field 25 inside the process container 24 , and is provided with gas spouting holes 48 A and 48 B formed at predetermined intervals, from which the oxidizing gas or O 2 gas is supplied. Consequently, O 2 gas is supplied in horizontal directions essentially uniformly to the process field 25 and thus to the wafers W. Further, a plurality of, such as five, deoxidizing gas nozzles 52 to 60 have different lengths or heights and are provided with gas spouting holes 52 A to 60 A, from which H 2 gas is supplied in horizontal directions to the respective zones of the process field 25 .
  • O 2 gas and H 2 gas supplied into the process container 24 sequentially replenish the gases, which may become insufficient on a downstream side of the gas flow from the upper side to the lower side, due to consumption on the wafer surface
  • Such a supply system of O 2 gas and H 2 gas can simplify and speed up an adjustment operation for optimizing the gas flow rates of the deoxidizing gas nozzles 52 to 60 to improve the inter-substrate uniformity of the film thickness on the wafers.
  • the adjustment operation may be performed with reference to the thickness of the SiO 2 film formed on monitor wafers for measuring the film thickness, which are placed between a plurality of dummy wafers.
  • the dummy wafers have an SiO 2 film formed on the surface in advance and are used to resemble product wafers.
  • the gas flow rates of the deoxidizing gas nozzles 52 to 60 are respectively adjusted to set the thickness of the SiO 2 film on the monitor wafers to be essentially uniform in the vertical direction inside the process container 24 , thereby obtaining optimized gas flow rates.
  • FIG. 2 is a graph for explaining the relationship in principle between the wafer position in the process container and optimized states of the film thickness of a silicon oxide film, obtained by the oxidation apparatus shown in FIG. 1 .
  • the wafer position is numbered in descending order of position along the gas flow, such that the wafer position is given a smaller number on a more upstream side and a larger number on a more downstream side.
  • a characteristic line MO denotes a target film thickness, which is set at 13 nm in this example.
  • the H 2 gas flow rates of the nozzles are respectively adjusted to form an oxide film with a thickness of 13 nm on all the wafers in the vertical direction.
  • the O 2 gas flow rate is fixed.
  • monitor wafers consisting of bare wafers (silicon is exposed without an SiO 2 film formed on the surface) for measuring the film thickness are placed between a plurality of dummy wafers with an SiO 2 film formed on the surface, which are used to resemble product wafers. Then, the thickness of an SiO 2 film formed on the surface of the monitor wafers by oxidation is measured, and the measurement values are plotted to form characteristic lines M 3 and M 5 , as shown in FIG. 2 . H 2 gas flow rates obtained in this operation are determined as optimum values.
  • the characteristic line M 3 is a characteristic line used for an oxidation process applied to wafers each having a surface area increased to be three times larger (triple) by projected and recessed portions formed on the surface, as compared with a wafer having a flat surface.
  • the characteristic line M 5 is a characteristic line used for an oxidation process applied to wafers each having a surface area increased to be five times larger (quintuple) by projected and recessed portions formed on the surface.
  • the H 2 gas flow rates of the deoxidizing gas nozzles 52 to 60 are respectively adjusted while the flow rate of O 2 gas is fixed at a certain value, as described above. Then, the gas flow rates are adjusted, so as to attain the target film thickness indicated by the characteristic line M 0 when an oxidation process is actually performed on product wafers each having the quintuple surface area.
  • the characteristic line M 5 linearly extends in the horizontal direction in FIG. 2 and thus renders a constant film thickness in the inter-substrate direction, unlike the characteristic lines L 3 and L 5 shown in FIG. 10 .
  • the, H 2 gas flow rates of the deoxidizing gas nozzles 52 to 60 are respectively adjusted to set the film thickness on all the monitor wafers at a constant value in the inter-substrate direction. Then, the H 2 gas flow rates thus obtained are used for performing an oxidation process on actual product wafers, so that the film thickness of the SiO 2 film formed on the product wafers renders good inter-substrate uniformity.
  • each of the characteristic lines M 3 and M 5 linearly extends in the horizontal direction, the following simple adjust operation can be adopted. Specifically, one characteristic line, such as the characteristic line M 5 , is formed in advance, and then other characteristic lines for differently multiplied surface areas, such as the characteristic line M 3 , are formed by shifting the former characteristic line in parallel in the vertical direction.
  • the characteristic line MS for the quintuple surface area can be utilized as it is while merely the process time of the oxidation process is shortened or prolonged. Consequently, it is possible to simplify and speed up an adjustment operation,for obtaining optimized process conditions, such as the flow rates of H 2 gas.
  • the oxidizing gas nozzle 48 for supplying an oxidizing gas, such as O 2 has a plurality of gas spouting holes 48 A formed at predetermined intervals over the process field 25 . Further, a plurality of deoxidizing gas nozzles 52 to 60 respectively having different lengths are disposed to supply a deoxidizing gas, such as H 2 , to the different zones of the process field 25 arrayed in the vertical direction. Consequently, film thickness characteristics for different surface area wafers W are formed with good inter-substrate uniformity (i.e., to be linear), which can simplify and speed up an adjustment operation for obtaining optimized process conditions, such as the flow rates of a deoxidizing gas.
  • process conditions described above can be generalized in a method according to this embodiment, as follows. Specifically, at first, reference conditions of an oxidation process are obtained for reference substrates each having a reference surface area, while a predetermined level of inter-substrate uniformity is satisfied (preferably to form a linear characteristic, as shown in FIG. 2 ). The surface area of each of target substrates to be actually processed has a certain ratio relative to the reference surface area. Then, actual conditions of the oxidation process to be used for the target substrates are determined from the reference conditions, while adjusting essentially merely the process time thereof, as a function of the certain ratio.
  • the inter-substrate uniformity is determined with reference to the inter-substrate uniformity of the thickness of a film formed by the oxidation process.
  • the reference conditions include the flow rates of an oxidizing gas and a deoxidizing gas.
  • FIG. 3 is a graph showing optimized states of the film thickness of a silicon oxide film, and actual states and planar uniformity of the film thickness of a silicon oxide film formed on product wafers, obtained by the oxidation apparatus shown in FIG. 1 and a conventional apparatus.
  • the measurement values of a silicon oxide film formed by the conventional apparatus are used for comparison.
  • the gas nozzles of the embodiment are schematically shown above this graph.
  • a characteristic line L 5 denotes a characteristic line optimized for the quintuple surface area by the conventional apparatus.
  • the characteristic line L denotes a film thickness obtained when the oxidation process was actually performed on product wafers with the quintuple surface area in the conventional apparatus.
  • the characteristic line L 5 was obtained under the following process conditions. Specifically, the process pressure was set at 0.35 Torr, the process temperature at 900° C., and the O 2 gas flow rate at 5.0 slm. The H 2 gas flow rates of the nozzles 12 A to 12 E shown in FIG.
  • a characteristic line M 5 denotes a characteristic line optimized for the quintuple surface area by the apparatus shown in FIG. 1 .
  • the characteristic line M denotes a film thickness obtained when the oxidation process was actually performed on product wafers with the quintuple surface area in the apparatus shown in FIG. 1 .
  • the target film thickness for the product wafers was set at 13 nm.
  • the characteristic line M 5 was obtained under the following process conditions. Specifically, the process pressure was set at 0.35 Torr, the process temperature at 900° C., and the O 2 gas flow rate at 5.0 slm.
  • the H 2 gas flow rates were set at 0.2 slm for the nozzle 52 , at 0.4 slm for the nozzle 54 , 0.42 slm for the nozzle 56 , 0.45 slm for the nozzle 58 , and 0.45 slm for the nozzle 60 .
  • the process time was set at 45 minutes.
  • a characteristic line La denotes the planar uniformity of a film thickness formed on product wafers with the quintuple surface area in the conventional apparatus.
  • a characteristic line Ma denotes the planar uniformity of a film thickness formed on product wafers with the quintuple surface area in the apparatus shown in FIG. 1 .
  • the film thickness was gradually increased from the upstream side to the middle of the gas flow, and then becomes almost constant.
  • the film thickness was essentially constant at about 16.5 nm (i.e., linear).
  • the characteristic line La obtained by the conventional apparatus rendered poor planar uniformity of the film thickness, such that the planar uniformity was increased to ⁇ 1% at TOP (upstream side) and BTM (downstream side).
  • the characteristic line Ma obtained by the apparatus shown in FIG. 1 rendered better planar uniformity of the film thickness than that of the conventional apparatus, such that the planar uniformity was ⁇ 0.5% or less at all the wafer positions.
  • a plurality of gas spouting holes 48 A and 52 A to 60 A are formed on the nozzles 48 and 52 to 60 extending in the longitudinal direction of the process container 24 , so that O 2 gas and H 2 gas are respectively distributed essentially all over the process field 25 .
  • the gases (radicals) do not become insufficient even at the wafer center, which is thus oxidized almost equally to the wafer periphery. Consequently, as shown in FIG. 4B , an SiO 2 film 96 is formed with a film thickness slightly larger at the wafer center.
  • FIGS. 5A and 5B are views showing modifications of nozzles.
  • the oxidizing gas nozzle 48 is formed of a U-shaped nozzle having two nozzle portions extending in the vertical direction and connected to each other through a bent portion.
  • the oxidizing gas nozzle 48 may be formed of one linearly extending nozzle having a plurality of gas spouting holes 48 A formed at predetermined intervals.
  • the intervals of the gas spouting holes 48 A used in this case are smaller that those shown in FIG. 1 and are preferably set at, e.g., about 1 ⁇ 2 thereof.
  • the uniformity of the O 2 gas flow rate becomes slightly poorer than that of the case shown in FIG. 1 , the same effects as those of the apparatus shown in FIG. 1 can be obtained.
  • each of the deoxidizing gas nozzles 52 to 60 has a plurality of, such as three, gas spouting holes ( 52 A to 60 A) formed at the top.
  • gas spouting holes 52 A to 60 A
  • FIG. 5B only one gas spouting hole ( 52 A to 60 A) may be formed.
  • This nozzle structure is the same as that shown in FIG. 9 .
  • the nozzle 48 shown in FIG. 5A and the nozzles 52 to 60 shown in FIG. 5B may be combined. In any of the combinations of these nozzles, the same effects as those of the apparatus shown in FIG. 1 can be obtained.
  • FIG. 6A is a view showing a case where the gas spouting direction of gas spouting holes is directed to the center of a wafer.
  • FIG. 6B is a view schematically showing the relationship of an oxidizing gas nozzle 48 and deoxidizing gas nozzles 52 to 60 , each of which has gas spouting holes with an improved gas spouting direction, relative to the process container 41 and wafer W.
  • FIG. 6C is a view showing an alternative modification of the gas spouting direction of gas spouting holes.
  • FIG. 7 is a graph showing the planar uniformity of film thickness obtained by the gas spouting holes shown in FIGS. 6A and 6B .
  • the gas spouting holes 48 A and 48 B of the oxidizing gas nozzle 48 are directed to the wafers W to spout the gas directly to the wafers W.
  • the planar uniformity of film thickness became very poor at specific wafer positions, as indicated by a characteristic line X shown in FIG. 7 . As described above, this was due to the gas directly coming into contact with the wafer W from a lateral side, whereby the balance of mixture of O 2 and H 2 gases was deteriorated and the combustion reaction was hindered from properly taking place.
  • the gas spouting holes 48 A and 48 B of the oxidizing gas nozzle 48 are set to have a gas spouting direction that forms an angle ⁇ 1 of 135° relative to a line connecting the center of the gas nozzle and the center of each wafer. Further, the gas spouting holes 48 A and 48 B of the first and second nozzle portions of the oxidizing gas nozzle 48 are directed to opposite sides. On the other hand, the gas spouting holes 52 A to 60 A of the deoxidizing gas nozzles 52 to 60 are set to have a gas spouting direction that forms an angle ⁇ 2 of 90° relative to a line connecting the center of the gas nozzle and the center of each wafer.
  • the deoxidizing gas nozzles 52 to 60 are arrayed from the upstream side in decreasing order of height. Where this arrangement was used, the planar uniformity of film thickness was greatly improved as indicated by a characteristic line Y shown in FIG. 7 , as compared with the characteristic line X.
  • the gas spouting direction of the oxidizing gas nozzle 48 and deoxidizing gas nozzles 52 to 60 deviates from at least the contour of the wafers W, as shown in FIG. 6C .
  • the gas spouting direction is set to form an angle of 90° or more relative to a line connecting the center of the gas nozzle and the center of each wafer, the gas first comes into contact with the container sidewall and then diffuses, so that the gas is uniformly distributed onto the wafer surface.
  • the gas spouting direction of the oxidizing gas nozzle 48 and deoxidizing gas nozzles 52 to 60 is set in a tangential direction to the contour of the wafers or in a direction outside the tangential direction. Further, the gas spouting direction is set to form an angle preferably of 90° or more, and more preferably of 90° to 135°, relative to a line connecting the center of the gas nozzle and the center of each wafer
  • the number of product wafers to be processed may be smaller than that in the full load state of a wafer boat.
  • the number of wafers to be subjected to an oxidation process does not necessarily reach the full load state of the wafer boat 26 , so empty spaces may be partly present in the wafer boat 26 .
  • this boat 26 may be used to hold 25 or 50 product wafers along with non-product or dummy wafers to fill the empty spaces, wherein the dummy wafers have an SiO 2 film formed on the surface.
  • the product wafers W are held on the wafer boat 26 to fill the most upstream side of the gas flow on the wafer boat 26 .
  • the wafers are inserted in supporting levels in descending order from the top of wafer boat 26 .
  • FIGS. 8A and 8B are graphs each showing a change in the film thickness of an oxide film obtained when an oxidation process was performed on product wafers, the number of which was smaller than that in the full load state of a wafer boat.
  • FIG. 8A shows the results of oxidation processes performed in the conventional apparatus shown in FIG. 9 .
  • FIG. 8B shows the results of oxidation processes performed in the apparatus shown in FIG. 1 .
  • the target film thickness was set at 5.5 nm.
  • the target film thickness was set at 6.0 nm.
  • a characteristic line Y 100 denotes a characteristic obtained when 100 product wafers were loaded (full load).
  • a characteristic line Y 50 denotes a characteristic obtained when 50 product wafers were loaded (non-full load).
  • a characteristic line Y 25 denotes a characteristic obtained when 25 product wafers were loaded (non-full load).
  • a characteristic line Z 100 denotes a characteristic obtained when 100 product wafers were loaded (full load).
  • a characteristic line Z 25 denotes a characteristic obtained when 25 product wafers were loaded (non-full load).
  • the film thickness was essentially uniform over all the wafer positions, and thus the inter-substrate uniformity of the film thickness was good, as indicated by the characteristic line Y 100 .
  • the film thickness varied with an increase in the film thickness toward the downstream side of the gas flow, as indicated by the characteristic lines Y 50 and Y 25 . This result means that an adjustment operation is required to optimize the flow rates of O 2 and H 2 gases in advance, along with a change in the number of product wafers.
  • the film thickness essentially took on the target value, as indicated by the characteristic lines Z 100 and Z 25 . Further, the film thickness was essentially uniform over all the wafer positions, and thus the inter-substrate uniformity of the film thickness was excellent. This result means that the process conditions (such as the gas flow rates) optimized for the full load of wafers can be used as they are even for a non-full load of wafers. Consequently, the adjustment operation for optimizing the flow rates can be simplified.
  • the process field 25 is divided into five zones, which are respectively provided with five deoxidizing gas nozzles 52 to 60 having different lengths.
  • the number of zones can be set at any number other than five, along with the corresponding number of nozzles having different lengths.
  • the process container 24 has the exhaust port 46 near the bottom so that gas flows inside the container from the upper side to the lower side.
  • the process container 24 may have an exhaust port 46 at the top so that gas flows inside the container from the lower side to the upper side.
  • the process container 24 is not limited to a single-tube structure, and it may have a double-tube structure, which is formed of inner and outer tubes concentrically disposed.
  • the oxidizing gas is not limited to O 2 , and it may comprise one or more gases selected from the group consisting of O 2 , N 2 O, NO, NO 2 , and O 3 .
  • the deoxidizing gas is not limited to H 2 , and it may comprise one or more gases selected from the group consisting of H 2 , NH 3 , CH 4 , HCl, and deuterium.
  • the target substrate is not limited to a semiconductor wafer, and it may be another substrate, such as a glass substrate, LCD substrate, or ceramic substrate.

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