WO2012165166A1 - 半導体装置の製造方法、基板処理方法および基板処理装置 - Google Patents
半導体装置の製造方法、基板処理方法および基板処理装置 Download PDFInfo
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- WO2012165166A1 WO2012165166A1 PCT/JP2012/062681 JP2012062681W WO2012165166A1 WO 2012165166 A1 WO2012165166 A1 WO 2012165166A1 JP 2012062681 W JP2012062681 W JP 2012062681W WO 2012165166 A1 WO2012165166 A1 WO 2012165166A1
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- H—ELECTRICITY
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- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
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- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
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- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
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- H01L21/02112—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer
- H01L21/02123—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer the material containing silicon
- H01L21/02164—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer the material containing silicon the material being a silicon oxide, e.g. SiO2
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- 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
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- C23C16/22—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 deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/40—Oxides
- C23C16/401—Oxides containing silicon
- C23C16/402—Silicon dioxide
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- 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
- C23C16/448—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 characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials
- C23C16/4488—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 characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials by in situ generation of reactive gas by chemical or electrochemical reaction
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- 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
- C23C16/455—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 characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
- C23C16/45523—Pulsed gas flow or change of composition over time
- C23C16/45525—Atomic layer deposition [ALD]
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- 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
- C23C16/455—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 characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
- C23C16/45523—Pulsed gas flow or change of composition over time
- C23C16/45525—Atomic layer deposition [ALD]
- C23C16/45544—Atomic layer deposition [ALD] characterized by the apparatus
- C23C16/45546—Atomic layer deposition [ALD] characterized by the apparatus specially adapted for a substrate stack in the ALD reactor
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- 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
- C23C16/52—Controlling or regulating the coating process
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- 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
- C23C16/56—After-treatment
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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
- H01L21/02104—Forming layers
- H01L21/02107—Forming insulating materials on a substrate
- H01L21/02109—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates
- H01L21/02205—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates the layer being characterised by the precursor material for deposition
- H01L21/02208—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates the layer being characterised by the precursor material for deposition the precursor containing a compound comprising Si
- H01L21/02211—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates the layer being characterised by the precursor material for deposition the precursor containing a compound comprising Si the compound being a silane, e.g. disilane, methylsilane or chlorosilane
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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
- 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
- H01L21/0226—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process
- H01L21/02263—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase
- H01L21/02271—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase deposition by decomposition or reaction of gaseous or vapour phase compounds, i.e. chemical vapour deposition
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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
- 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
- H01L21/0226—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process
- H01L21/02263—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase
- H01L21/02271—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase deposition by decomposition or reaction of gaseous or vapour phase compounds, i.e. chemical vapour deposition
- H01L21/0228—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase deposition by decomposition or reaction of gaseous or vapour phase compounds, i.e. chemical vapour deposition deposition by cyclic CVD, e.g. ALD, ALE, pulsed CVD
Definitions
- the present invention relates to a semiconductor device manufacturing method, a substrate processing method, and a substrate processing apparatus including a step of forming a thin film on a substrate.
- an insulating film used in a semiconductor device such as a flash memory
- a source gas for example, supply of a source gas into a processing container containing a substrate and a processing container under a heated pressure less than atmospheric pressure
- a silicon oxide film on a substrate such as a silicon wafer by alternately repeating supply of oxygen-containing gas and hydrogen-containing gas into the inside (see, for example, Patent Document 1).
- an object of the present invention is to provide a method for manufacturing a semiconductor device, a substrate processing method, and a substrate processing apparatus, which can improve the deposition rate even at low temperatures and improve the productivity.
- Forming a silicon-containing layer on the substrate by supplying a source gas containing silicon to the substrate housed in the processing chamber and heated to the first temperature; Generating a reactive species containing oxygen by reacting an oxygen-containing gas and a hydrogen-containing gas in a reaction preparatory chamber under a pressure atmosphere less than atmospheric pressure heated to a second temperature equal to or higher than the first temperature; The reactive species is supplied to the substrate heated to the first temperature in the processing chamber under a pressure atmosphere less than atmospheric pressure, thereby oxidizing the silicon-containing layer formed on the substrate. And changing to a silicon oxide layer, By alternately repeating the above, there is provided a method for manufacturing a semiconductor device including a step of forming a silicon oxide film having a predetermined thickness on the substrate.
- Forming a silicon-containing layer on the substrate by supplying a source gas containing silicon to the substrate housed in the processing chamber and heated to the first temperature; Generating a reactive species containing oxygen by reacting an oxygen-containing gas and a hydrogen-containing gas in a reaction preparatory chamber under a pressure atmosphere less than atmospheric pressure heated to a second temperature equal to or higher than the first temperature; The reactive species is supplied to the substrate heated to the first temperature in the processing chamber under a pressure atmosphere less than atmospheric pressure, thereby oxidizing the silicon-containing layer formed on the substrate. And changing to a silicon oxide layer, By alternately repeating the above, there is provided a substrate processing method including a step of forming a silicon oxide film having a predetermined thickness on the substrate.
- a processing chamber for accommodating and processing the substrate; A first heating source for heating the substrate in the processing chamber to a first temperature; A reaction preparatory chamber for reacting multiple types of gases; A second heating source for heating the preliminary reaction chamber to a second temperature not lower than the first temperature; A source gas supply system for supplying a source gas containing silicon into the processing chamber; An oxygen-containing gas supply system for supplying an oxygen-containing gas into the reaction preparatory chamber; A hydrogen-containing gas supply system for supplying a hydrogen-containing gas into the reaction preparatory chamber; A pressure adjusting unit for adjusting the pressure in the processing chamber and the reaction preparatory chamber; A process of forming a silicon-containing layer on the substrate by supplying the source gas to the substrate housed in the processing chamber and heated to the first temperature, and heated to the second temperature In the reaction preparatory chamber under a pressure atmosphere less than atmospheric pressure, an oxygen-containing gas and a hydrogen-containing gas are reacted to generate oxygen-containing reactive species, and the reactive species are subjected to
- a process of oxidizing the silicon-containing layer formed on the substrate into an oxide layer by supplying the substrate heated to the first temperature in the processing chamber.
- the first heating source, the second heating source, the source gas supply system, the oxygen-containing gas supply system, and the like so as to form a silicon oxide film having a predetermined thickness on the substrate.
- Hydrogen-containing gas supply system and the pressure A control unit for controlling the integer part, A substrate processing apparatus is provided.
- the present invention it is possible to provide a semiconductor device manufacturing method, a substrate processing method, and a substrate processing apparatus capable of improving the film formation rate and improving productivity even at low temperatures.
- FIG. 2 is a schematic configuration diagram of a vertical processing furnace of a substrate processing apparatus preferably used in the present embodiment, and is a view showing a processing furnace part by a cross-sectional view taken along line AA of FIG. It is a figure which shows the timing of the gas supply in the 1st film-forming sequence of this embodiment. It is a figure which shows the timing of the gas supply in the 2nd film-forming sequence of this embodiment.
- the relationship between the thickness of the SiO 2 film according to an embodiment of the present invention and the reaction spare room temperature is a graph showing.
- FIG. 1 is a schematic configuration diagram of a vertical processing furnace of a substrate processing apparatus suitably used in the present embodiment, and shows a processing furnace 202 portion in a vertical sectional view.
- FIG. 2 is a schematic configuration diagram of a vertical processing furnace suitably used in the present embodiment, and the processing furnace 202 portion is shown by a cross-sectional view along the line AA in FIG.
- the present invention is not limited to the substrate processing apparatus according to the present embodiment, and can be suitably applied to a substrate processing apparatus having a single wafer type, Hot Wall type, or Cold Wall type processing furnace.
- the processing furnace 202 has a first heater 207 as a first heating source (first heating means).
- the first heater 207 has a cylindrical shape and is vertically installed by being supported by a heater base (not shown) as a holding plate.
- the first heater 207 is a resistance heating type heater (heat source by resistance heating), and is configured to heat a wafer 200 in a processing chamber 201 described later to a first temperature.
- a process tube 203 as a reaction tube is disposed concentrically with the first heater 207.
- the process tube 203 is made of a heat resistant material such as quartz (SiO 2 ) or silicon carbide (SiC), and has a cylindrical shape with the upper end closed and the lower end opened.
- a process chamber (reaction chamber) 201 is formed in the cylindrical hollow portion of the process tube 203, and is configured so that wafers 200 as substrates can be accommodated in a horizontal posture and in a multi-stage aligned state in a vertical direction by a boat 217 described later. ing.
- a reaction vessel (processing vessel) is formed by the process tube 203.
- a first nozzle 233 as a first gas introduction part and a second nozzle 233a as a second gas introduction part are provided so as to penetrate the side wall at the lower part of the process tube 203.
- Each of the first nozzle 233 and the second nozzle 233 a extends in an arc-shaped space between the inner wall of the process tube 203 constituting the processing chamber 201 and the wafer 200 and extends from the lower part to the upper part of the inner wall of the process tube 203.
- the wafer 200 is provided to rise upward in the stacking direction.
- first nozzle 233 and the second nozzle 233a are respectively provided along the wafer arrangement region in a region that horizontally surrounds the wafer arrangement region on the side of the wafer arrangement region where the wafers 200 are arranged.
- the first nozzle 233 and the second nozzle 233a are each configured as an L-shaped long nozzle, the horizontal portion thereof is provided so as to penetrate the lower side wall of the reaction tube 203, and the vertical portion thereof is at least It is provided so as to rise from one end side to the other end side of the wafer arrangement region.
- Gas supply holes 248 and 248a for supplying gas are provided on the side surfaces of the first nozzle 233 and the second nozzle 233a, respectively.
- the gas supply holes 248 and 248 a are opened so as to face the center of the process tube 203, and gas can be supplied toward the wafer 200.
- the gas supply holes 248 and 248a both have the same opening area from the lower part to the upper part, and are provided at the same opening pitch.
- a source gas supply pipe 232 is connected to the first nozzle 233, and a reaction gas supply pipe 232f is connected to the second nozzle 233a.
- the gas supply method according to the present embodiment is achieved by the nozzles 233 arranged in the arc-shaped vertical space defined by the inner wall of the process tube 203 and the ends of the stacked wafers 200.
- Gas is conveyed through 233a, and gas is first ejected into the process tube 203 near the wafer 200 from the gas supply holes 248 and 248a opened in the nozzles 233 and 233a, respectively.
- the main flow is a direction parallel to the surface of the wafer 200, that is, a horizontal direction.
- a metal manifold that supports the process tube 203 is provided below the process tube 203, and the first nozzle 233 and the second nozzle 233a are provided so as to penetrate the side wall of the metal manifold. May be.
- an exhaust pipe 231 to be described later may be further provided on the metal manifold. Even in this case, the exhaust pipe 231 may be provided below the process tube 203 instead of the metal manifold.
- the furnace port part of the processing furnace may be made of metal, and a nozzle or the like may be attached to the metal furnace port part.
- the raw material gas supply pipe 232 is provided with a mass flow controller (MFC) 241 as a flow rate controller (flow rate control unit) and a valve 243 as an on-off valve in order from the upstream direction.
- MFC mass flow controller
- a first inert gas supply pipe 232e is connected to the downstream side of the valve 243 of the source gas supply pipe 232.
- the first inert gas supply pipe 232e is provided with a mass flow controller 241e that is a flow rate controller (flow rate control unit) and a valve 243e that is an on-off valve in order from the upstream direction.
- the above-described first nozzle 233 is connected to the distal end portion of the source gas supply pipe 232.
- a source gas supply system is mainly configured by the source gas supply pipe 232, the mass flow controller 241, and the valve 243.
- the first nozzle 233 may be included in the source gas supply system.
- a first inert gas supply system is mainly configured by the first inert gas supply pipe 232e, the mass flow controller 241e, and the valve 243e.
- the first inert gas supply system also functions as a purge gas supply system.
- hexachlorodisilane Si 2 Cl 6 , abbreviation: HCDS
- HCDS hexachlorodisilane
- Si silicon
- a gas is supplied into the processing chamber 201 through the mass flow controller 241, the valve 243, and the first nozzle 233. That is, the source gas supply system is configured as a silicon source gas supply system.
- the inert gas may be supplied from the first inert gas supply pipe 232e into the source gas supply pipe 232 via the mass flow controller 241e and the valve 243e.
- the inert gas supplied into the source gas supply pipe 232 is supplied into the processing chamber 201 together with the HCDS gas through the first nozzle 233.
- a liquid raw material which is a liquid state under normal temperature normal pressure like HCDS, a liquid raw material will be vaporized with vaporization systems, such as a vaporizer and a bubbler, and will be supplied as raw material gas.
- the reaction gas supply pipe 232f is provided with a valve 243f that is an on-off valve.
- a reaction preparatory container 300 constituting a reaction preparatory chamber 301 described later is connected to the upstream side of the reaction gas supply pipe 232f.
- a pressure as a pressure detector (pressure detection unit) that detects the internal pressure, that is, the pressure on the secondary side (downstream side) of the reaction preliminary chamber 301.
- a sensor 245b is provided.
- a reaction gas supply system is mainly configured by the reaction gas supply pipe 232f and the valve 243f.
- reaction gas supply pipe 232f and the second nozzle 233a connect the reaction preliminary chamber 301 and the processing chamber 201, and a pipe part (communication part) is configured as a connection part that communicates the two chambers. Then, a flow path for flowing gas from the reaction preliminary chamber 301 into the processing chamber 201 is formed.
- an oxygen-containing gas supply pipe 232a and a hydrogen-containing gas supply pipe 232b are connected to the reaction preliminary container 300.
- the pre-reaction vessel 300 is connected to a merging pipe portion where the oxygen-containing gas supply pipe 232a and the hydrogen-containing gas supply pipe 232b merge, and the oxygen-containing gas supply pipe 232a and the hydrogen-containing gas supply pipe 232b. Therefore, the oxygen-containing gas and the hydrogen-containing gas can be supplied into the reaction preparatory chamber 301 via the junction pipe portion.
- the oxygen-containing gas supply pipe 232a is provided with a mass flow controller 241a that is a flow rate controller (flow rate control unit) and a valve 243a that is an on-off valve in order from the upstream direction. Further, a second inert gas supply pipe 232c that supplies an inert gas is connected to the downstream side of the valve 243a of the oxygen-containing gas supply pipe 232a. The second inert gas supply pipe 232c is provided with a mass flow controller 241c that is a flow rate controller (flow rate control unit) and a valve 243c that is an on-off valve in order from the upstream direction.
- the preliminary reaction chamber 301 is connected to the front end portion (downstream end portion) of the oxygen-containing gas supply pipe 232a through a junction pipe portion.
- An oxygen-containing gas supply system is mainly configured by the oxygen-containing gas supply pipe 232a, the mass flow controller 241a, and the valve 243a.
- a second inert gas supply system is mainly configured by the second inert gas supply pipe 232c, the mass flow controller 241c, and the valve 243c.
- the second inert gas supply system also functions as a purge gas supply system.
- a mass flow controller 241b that is a flow rate controller (flow rate control unit) and a valve 243b that is an on-off valve are provided in order from the upstream direction.
- a third inert gas supply pipe 232d that supplies an inert gas is connected to the downstream side of the valve 243b of the hydrogen-containing gas supply pipe 232b.
- the third inert gas supply pipe 232d is provided with a mass flow controller 241d as a flow rate controller (flow rate control unit) and a valve 243d as an on-off valve in order from the upstream direction.
- the preliminary reaction chamber 301 is connected to the distal end portion (downstream end portion) of the hydrogen-containing gas supply pipe 232b through a merging pipe portion.
- a hydrogen-containing gas supply system is mainly configured by the hydrogen-containing gas supply pipe 232b, the mass flow controller 241b, and the valve 243b.
- a third inert gas supply system is mainly configured by the third inert gas supply pipe 232d, the mass flow controller 241d, and the valve 243d.
- the third inert gas supply system also functions as a purge gas supply system.
- oxygen (O 2 ) gas for example, as an oxidizing gas is supplied into the reaction preparatory chamber 301 via the mass flow controller 241a and the valve 243a. That is, the oxygen-containing gas supply system is configured as an oxidizing gas supply system.
- the inert gas may be supplied from the second inert gas supply pipe 232c into the oxygen-containing gas supply pipe 232a via the mass flow controller 241c and the valve 243c.
- hydrogen (H 2 ) gas for example, as a reducing gas
- the reaction preparatory chamber 301 is supplied into the reaction preparatory chamber 301 via the mass flow controller 241b and the valve 243b.
- the hydrogen-containing gas supply system is configured as a reducing gas supply system.
- the inert gas may be supplied from the third inert gas supply pipe 232d into the hydrogen-containing gas supply pipe 232b via the mass flow controller 241d and the valve 243d.
- the pressure sensor 245a is provided as a pressure detector (pressure detector) for detecting the pressure on the side).
- the preliminary reaction container 300 is made of a heat-resistant material such as quartz (SiO 2 ) or silicon carbide (SiC), and has a cylindrical shape.
- a reaction preparatory chamber 301 is formed in the hollow cylindrical portion of the reaction preparatory container 300, and the reaction preparatory chamber 301 is configured to react an oxygen-containing gas and a hydrogen-containing gas inside.
- the reaction preliminary container 300 is provided with one inlet and one outlet.
- the inlet of the reaction preparatory container 300 is connected to a merging pipe portion where the oxygen-containing gas supply pipe 232a and the hydrogen-containing gas supply pipe 232b are joined. And can be supplied.
- the reaction gas supply pipe 232 f described above is connected to the outlet of the reaction preliminary container 300, and atomic oxygen (O) generated by reacting the oxygen-containing gas with the hydrogen-containing gas in the reaction preliminary chamber 301 or the like. It is configured such that the reactive species containing oxygen can be supplied into the reactive gas supply pipe 232f.
- a second heater 302 as a second heating source (second heating means) is provided around the reaction preliminary container 300 so as to cover the cylindrical side surface of the reaction preliminary container 300.
- the second heater 302 has a cylindrical shape, and is provided concentrically with the reaction preliminary container 300 that is also cylindrical.
- the second heater 302 is a resistance heating type heater (heat source by resistance heating), and is configured to heat the reaction preliminary chamber 301 to a second temperature higher than the first temperature. Note that the second heater 302 is configured to be controllable independently of the first heater 207.
- a heat insulating member 303 is provided around the second heater 302 and the reaction preliminary container 300.
- pressure sensors 245a and 245b are provided in the vicinity of the reaction preparatory chamber 301 of the reaction gas supply pipe 232f and the merged pipe portion where the oxygen-containing gas supply pipe 232a and the hydrogen-containing gas supply pipe 232b merge. It has been.
- the pressure sensor 245a is configured to detect the pressure on the primary side (upstream side) of the preliminary reaction chamber 301, that is, the pressure on the inlet side of the preliminary reaction chamber 301, and the pressure sensor 245b The pressure on the secondary side (downstream side) of the preliminary reaction chamber 301, that is, the pressure on the outlet side of the preliminary reaction chamber 301 is detected.
- the pressure sensors 245a and 245b monitor the pressure on the primary side of the reaction preliminary chamber 301 and the pressure on the secondary side of the reaction preliminary chamber 301 to react. It is monitored whether the pressure in the preliminary chamber 301 is maintained at a predetermined pressure lower than atmospheric pressure. At this time, it is monitored whether the pressure in the piping section between the reaction preparatory chamber 301 and the processing chamber 201 is also maintained at a predetermined pressure lower than atmospheric pressure.
- the pressure on at least the secondary side of the reaction preparatory chamber 301 may be monitored. Monitoring of the primary side pressure is not necessarily performed. In this case, the pressure sensor 245a on the primary side of the preliminary reaction chamber 301 may be omitted. However, monitoring both the primary pressure and the secondary pressure in the preliminary reaction chamber 301 ensures that the pressure in the preliminary reaction chamber 301 is maintained at a predetermined pressure lower than atmospheric pressure. It is possible to monitor whether or not the reaction occurs, and it is possible to generate a more appropriate amount of reactive species, and it is possible to further increase safety.
- An exhaust pipe 231 for exhausting the atmosphere in the processing chamber 201 is provided below the process tube 203.
- An exhaust port is formed at a connection portion between the process tube 203 and the exhaust pipe 231.
- a vacuum pump 246 as a vacuum exhaust device is connected to the exhaust pipe 231 through a pressure sensor 245 as a pressure detector (pressure adjustment unit) and an APC (Auto Pressure Controller) valve 244 as a pressure regulator (pressure adjustment unit). Is connected.
- the APC valve 244 can open and close the vacuum pump 246 in a state where the vacuum pump 246 is operated, thereby evacuating the vacuum in the processing chamber 201 and stopping the vacuum exhaust. Further, the APC valve 244 is in a state where the vacuum pump 246 is operated.
- the valve is configured so that the pressure in the processing chamber 201 can be adjusted by adjusting the valve opening degree.
- An exhaust system is mainly configured by the exhaust pipe 231, the APC valve 244, and the pressure sensor 245.
- the vacuum pump 246 may be included in the exhaust system.
- the exhaust system operates the vacuum pump 246 and adjusts the opening degree of the APC valve 244 based on the pressure information detected by the pressure sensor 245, so that the pressure in the processing chamber 201 becomes a predetermined pressure (vacuum). It is configured so that it can be evacuated to a degree.
- the opening degree of the APC valve 244 is adjusted based on the pressure information detected by the pressure sensor 245 so that the pressure in the processing chamber 201 becomes a predetermined pressure lower than the atmospheric pressure.
- the pressure in the reaction preparatory chamber 301 is also adjusted to a predetermined pressure lower than atmospheric pressure.
- the pressure in the piping section between the reaction preparatory chamber 301 and the processing chamber 201 is also adjusted to be a predetermined pressure lower than atmospheric pressure.
- the pressure sensors 245a and 245b monitor the primary side pressure and the secondary side pressure of the reaction preparatory chamber 301, and the pressure in the reaction preparatory chamber 301 and the pressure in the piping section are less than atmospheric pressure. Is maintained at a predetermined pressure.
- the pressure in the reaction preparatory chamber 301 is maintained at a predetermined pressure lower than atmospheric pressure, that is, a pressure of 3999 Pa or lower, preferably 2666 Pa or lower, at a predetermined temperature, for example, 450 ° C. or higher, O 2 gas and H 2 gas react with each other to generate reactive species containing no H 2 O such as atomic oxygen (O).
- a predetermined pressure lower than atmospheric pressure that is, a pressure of 3999 Pa or lower, preferably 2666 Pa or lower
- a predetermined temperature for example, 450 ° C. or higher
- O 2 gas and H 2 gas react appropriately at a predetermined temperature, for example, 450 ° C. or higher, and the H 2
- An appropriate amount of reactive species such as atomic oxygen (O) can be generated without generating O.
- the generation efficiency of H 2 O-free reactive species such as atomic oxygen (O) is highest when the pressure in the reaction preparatory chamber 301 is 1333 Pa or less at the same temperature.
- the case where the pressure of 2666 Pa or less is the next highest is the next highest, and the case where the pressure in the reaction preparatory chamber 301 is 3999 Pa or less is the next highest. That is, the pressure in the reaction preparatory chamber 301 is 3999 Pa or less, preferably 2666 Pa or less, more preferably 1333 Pa or less.
- the reaction probability of O 2 gas and H 2 gas is relatively low, and the amount of heat supplied by the reaction heat necessary for the chain reaction is supplied.
- the pressure fluctuation accompanying local volume expansion is absorbed, it becomes possible to remove from the explosion range of the mixed gas of O 2 gas and H 2 gas.
- the pressure in the reaction preparatory chamber 301 when the pressure in the reaction preparatory chamber 301 is maintained at a predetermined pressure lower than atmospheric pressure, that is, a pressure of 3999 Pa (30 Torr) or less, the H 2 gas into the reaction preparatory chamber 301 is used.
- a pressure of 3999 Pa (30 Torr) or less
- the pressure in the reaction preparatory chamber 301 is not maintained at a pressure of 3999 Pa or lower, that is, when it exceeds 3999 Pa, the supply of H 2 gas into the reaction preparatory chamber 301 is impossible.
- the valve 243 b when the pressure in the reaction preparatory chamber 301 exceeds 3999 Pa, if the valve 243 b is closed, it cannot be opened, and the H 2 gas cannot be supplied into the reaction preparatory chamber 301. Like that. At this time, if the valve 243a is in a closed state, the valve 243a may not be opened, and the O 2 gas may not be supplied into the reaction preparatory chamber 301. When the pressure in the reaction preparatory chamber 301 exceeds 3999 Pa and the valve 243b is already open, this is closed and the supply of H 2 gas into the reaction preparatory chamber 301 is stopped. Then, the processing on the wafer 200 is stopped.
- valve 243a may be closed and the supply of O 2 gas into the reaction preparatory chamber 301 may be stopped.
- the timing of the stop of the supply of O 2 gas must be adjusted appropriately.
- the valve 243b can be kept open and the H 2 gas can be supplied into the reaction preparatory chamber 301. Keep it in good condition.
- the valve 243a is kept in an open state and the supply of O 2 gas into the reaction preparatory chamber 301 is maintained in a possible state.
- the pressure in the reaction preliminary chamber 301 is monitored by using the pressure sensors 245a and 245b, so that the pressure in the reaction preliminary chamber 301 is monitored.
- This interlock control is performed by a controller 280 described later.
- the APC valve 244 when the APC valve 244 is feedback controlled based on the pressure information detected by the pressure sensor 245, the pressure information detected by the pressure sensors 245a and 245b should be taken into consideration. It may be. That is, at least in the oxidation process during processing on the wafer 200, the APC valve 244 is feedback-controlled based on pressure information detected by the pressure sensors 245, 245a, 245b, and the pressure in the processing chamber 201 is less than atmospheric pressure. Control may be performed so that the pressure in the reaction preparatory chamber 301 or the pressure in the piping section becomes a predetermined pressure lower than the atmospheric pressure so as to be a predetermined pressure.
- a pressure control unit pressure adjustment unit
- a seal cap 219 is provided as a furnace opening lid capable of airtightly closing the lower end opening of the process tube 203.
- the seal cap 219 is configured to contact the lower end of the process tube 203 from the lower side in the vertical direction.
- the seal cap 219 is made of a metal such as stainless steel and has a disk shape.
- An O-ring 220 is provided on the upper surface of the seal cap 219 as a seal member that comes into contact with the lower end of the process tube 203.
- a rotation mechanism 267 for rotating a boat 217 as a substrate holder described later is installed.
- a rotation shaft 255 of the rotation mechanism 267 passes through the seal cap 219 and is connected to the boat 217.
- the rotation mechanism 267 is configured to rotate the wafer 200 by rotating the boat 217.
- the seal cap 219 is configured to be lifted and lowered in the vertical direction by a boat elevator 115 as a lifting mechanism that is vertically installed outside the process tube 203.
- the boat elevator 115 is configured such that the boat 217 can be carried into and out of the processing chamber 201 by moving the seal cap 219 up and down.
- a boat 217 as a substrate holder is made of a heat-resistant material such as quartz or silicon carbide, and holds a plurality of wafers 200 in a horizontal posture and aligned in a state where the centers are aligned with each other in multiple stages. Is configured to do.
- a heat insulating member 218 made of a heat resistant material such as quartz or silicon carbide is provided at the lower part of the boat 217 so that heat from the first heater 207 is not easily transmitted to the seal cap 219 side. Has been.
- the heat insulating member 218 may be constituted by a plurality of heat insulating plates made of a heat resistant material such as quartz or silicon carbide, and a heat insulating plate holder that supports the heat insulating plates in a horizontal posture in multiple stages.
- a temperature sensor 263 as a temperature detector is installed in the process tube 203.
- the temperature in the processing chamber 201 is configured to have a desired temperature distribution by adjusting the power supply to the first heater 207 based on the temperature information detected by the temperature sensor 263.
- the temperature sensor 263 is configured in an L shape and is provided along the inner wall of the process tube 203.
- a temperature sensor 263 a serving as a temperature detector is also installed in the reaction preliminary chamber 301.
- the temperature in the pre-reaction chamber 301 is set to a desired temperature by adjusting the power supply to the second heater 302 based on the temperature information detected by the temperature sensor 263a.
- the state of energization to the first heater 207 is adjusted based on the temperature information detected by the temperature sensor 263, and the wafer 200 in the processing chamber 201 and the processing chamber 201 has the first temperature. It is controlled to become. Further, the state of energization to the second heater 302 is adjusted based on the temperature information detected by the temperature sensor 263a, and the reaction preparatory chamber 301 is controlled to have a second temperature higher than the first temperature. .
- the controller 280 which is a control unit (control means), includes a CPU (Central Processing Unit) 280a, a RAM (Random Access Memory) 280b, a storage device 280c, and an I / O port 280d. It is configured as a computer.
- the RAM 280b, the storage device 280c, and the I / O port 280d are configured to exchange data with the CPU 280a via the internal bus 280e.
- an input / output device 281 configured as a touch panel or the like is connected to the controller 280.
- the storage device 280c includes, for example, a flash memory, a HDD (Hard Disk Drive), and the like.
- a control program that controls the operation of the substrate processing apparatus, a process recipe that describes the procedure and conditions of the substrate processing described later, and the like are stored in a readable manner.
- the process recipe is a combination of the controller 280 so that predetermined procedures can be obtained by causing the controller 280 to execute each procedure in the substrate processing process described later, and functions as a program.
- the process recipe, the control program, and the like are collectively referred to as simply a program.
- the RAM 280b is configured as a memory area (work area) in which a program, data, and the like read by the CPU 280a are temporarily stored.
- the I / O port 280d includes the aforementioned mass flow controllers 241, 241a, 241b, 241c, 241d, 241e, valves 243, 243a, 243b, 243c, 243d, 243e, 243f, pressure sensors 245, 245a, 245b, APC valve 244,
- the vacuum pump 246, the first heater 207, the second heater 302, the temperature sensors 263, 263a, the rotation mechanism 267, the boat elevator 115, and the like are connected.
- the CPU 280a is configured to read and execute a control program from the storage device 280c, and to read a process recipe from the storage device 280c in response to an operation command input from the input / output device 281 or the like. Then, the CPU 280a adjusts the flow rates of various gases by the mass flow controllers 241, 241a, 241b, 241c, 241d, 241e, and the valves 243, 243a, 243b, 243c, 243d, 243e, 243f opening / closing operation, pressure monitoring by pressure sensors 245, 245a, 245b, opening / closing operation of APC valve 244, pressure adjustment operation based on pressure sensor 245 by APC valve 244, interlock operation based on pressure sensors 245a, 245b, temperature sensor 263 Temperature adjusting operation of the first heater 207 based on the temperature sensor 263a, temperature adjusting operation of the second heater 302 based on the temperature sensor 263a, starting and stopping of the vacuum pump 246, rotation of the boat 2
- the controller 280 is not limited to being configured as a dedicated computer, and may be configured as a general-purpose computer.
- an external storage device storing the above-described program for example, magnetic tape, magnetic disk such as a flexible disk or hard disk, optical disk such as CD or DVD, magneto-optical disk such as MO, semiconductor memory such as USB memory or memory card
- the controller 280 according to the present embodiment can be configured by preparing 282 and installing a program on a general-purpose computer using the external storage device 282.
- the means for supplying the program to the computer is not limited to supplying the program via the external storage device 282.
- the program may be supplied without using the external storage device 282 by using communication means such as the Internet or a dedicated line.
- the storage device 280c and the external storage device 282 are configured as computer-readable recording media. Hereinafter, these are collectively referred to simply as a recording medium. Note that when the term “recording medium” is used in this specification, it may include only the storage device 280c alone, may include only the external storage device 282 alone, or may include both.
- FIG. 3 shows a gas supply timing chart in the first film forming sequence of the present embodiment.
- the upper diagram of FIG. 3 shows the timing of gas supply into the processing chamber, and the lower diagram shows the timing of gas supply into the reaction preparatory chamber.
- FIG. 3 shows the supply timing of main substances supplied into the processing chamber and the reaction preparatory chamber for convenience.
- a source gas containing silicon (HCDS gas) is supplied to a substrate housed in a processing chamber and heated to a first temperature, whereby silicon is formed on the substrate.
- a hydrogen-containing gas (H 2 gas) are reacted to generate a reactive species containing oxygen (atomic oxygen (O)), and the reactive species is a first in a processing chamber under a pressure atmosphere less than atmospheric pressure.
- a substrate By alternately supplying a substrate heated to a temperature of 5 to a silicon oxide layer (SiO 2 layer) by oxidizing a silicon-containing layer formed on the substrate, a substrate is obtained.
- a silicon oxide film (SiO 2 film having a predetermined thickness) ).
- HCDS gas is used as the source gas
- O 2 gas is used as the oxygen-containing gas
- H 2 gas is used as the hydrogen-containing gas.
- the processing chamber 201 is evacuated by the vacuum pump 246 so that a desired pressure (degree of vacuum) lower than the atmospheric pressure is obtained.
- a desired pressure degree of vacuum
- the inside of the reaction preparatory chamber 301 is evacuated by the vacuum pump 246 so as to have a desired pressure lower than the atmospheric pressure.
- the inside of the piping section (reaction gas supply pipe 232f and the second nozzle 233a) between the reaction preparatory chamber 301 and the processing chamber 201 is also evacuated by the vacuum pump 246 so as to have a desired pressure less than atmospheric pressure. It will be.
- the inside of the preliminary reaction chamber 301 is evacuated through the reactive gas supply pipe 232f, the second nozzle 233a, the processing chamber 201, and the exhaust pipe 231.
- the pressure in the processing chamber 201 is measured by the pressure sensor 245, and the APC valve 244 is feedback-controlled based on the measured pressure information (pressure adjustment).
- the vacuum pump 246 keeps being operated at least until the processing on the wafer 200 is completed.
- the pressure sensors 245a and 245b monitor the primary side pressure and the secondary side pressure of the reaction preparatory chamber 301, and the pressure in the reaction preparatory chamber 301 and the pressure in the piping section are predetermined pressures below atmospheric pressure. Is maintained (pressure monitoring).
- pressure monitoring when the pressure in the reaction preparatory chamber 301 is maintained at a predetermined pressure lower than atmospheric pressure, that is, a pressure of 3999 Pa (30 Torr) or less, it is possible to supply H 2 gas into the reaction preparatory chamber 301.
- the interlock is set to make it impossible to supply H 2 gas into the reaction preparatory chamber 301. Control is performed. It should be noted that interlock control may be similarly performed for the supply of O 2 gas into the reaction preparatory chamber 301.
- the APC valve 244 may be feedback-controlled based on pressure information measured by the pressure sensors 245, 245a, 245b. This pressure adjustment and pressure monitoring are continuously performed at least until the processing on the wafer 200 is completed.
- the inside of the processing chamber 201 and the wafer 200 in the processing chamber 201 are heated by the first heater 207 so as to be at the first temperature.
- the power supply to the first heater 207 is feedback-controlled based on the temperature information detected by the temperature sensor 263 so that the inside of the processing chamber 201 has a desired temperature distribution (temperature adjustment).
- the reaction preparatory chamber 301 is heated by the second heater 302 so as to be at a second temperature higher than the first temperature.
- the current supply to the second heater 302 is feedback-controlled based on the temperature information detected by the temperature sensor 263a so that the reaction preliminary chamber 301 has a desired temperature. Note that the heating in the processing chamber 201 by the first heater 207 and the heating in the reaction preliminary chamber 301 by the second heater 302 are continuously performed at least until the processing on the wafer 200 is completed.
- the wafer 200 is rotated by rotating the boat 217 by the rotation mechanism 267.
- the rotation of the wafer 200 by the rotation of the boat 217 is continuously performed at least until the processing on the wafer 200 is completed. Thereafter, the following four steps are sequentially executed.
- Step 1 (Silicon-containing layer forming step)
- the valve 243 of the source gas supply pipe 232 is opened, and HCDS gas is allowed to flow through the source gas supply pipe 232.
- the HCDS gas flows from the source gas supply pipe 232 and the flow rate is adjusted by the mass flow controller 241.
- the flow-adjusted HCDS gas is supplied from the gas supply holes 248 of the first nozzle 233 from a plurality of locations on the side of the wafer arrangement region corresponding to the wafer arrangement region in the heated processing chamber 201 in a reduced pressure state. .
- the HCDS gas supplied into the processing chamber 201 flows down in the processing chamber 201 and is exhausted from the exhaust pipe 231 through an exhaust port provided on the lower end side of the wafer arrangement region (HCDS gas supply).
- the valve 243e of the first inert gas supply pipe 232e may be opened to supply N 2 gas as an inert gas from the first inert gas supply pipe 232e.
- the flow rate of the N 2 gas is adjusted by the mass flow controller 241e and is supplied into the source gas supply pipe 232.
- the flow-adjusted N 2 gas is mixed with the flow-adjusted HCDS gas in the source gas supply pipe 232 and supplied from the gas supply hole 248 of the first nozzle 233 into the heated processing chamber 201 in a reduced pressure state.
- the exhaust pipe 231 is exhausted.
- the valves 243c and 243d are opened, and N 2 gas is introduced into the second inert gas supply pipe 232c and the third inert gas supply pipe 232d. You may make it flow.
- the N 2 gas is supplied into the processing chamber 201 through the oxygen-containing gas supply pipe 232a, the hydrogen-containing gas supply pipe 232b, the reaction gas supply pipe 232f, and the second nozzle 233a, and is exhausted from the exhaust pipe 231. .
- the APC valve 244 is appropriately adjusted to maintain the pressure in the processing chamber 201 at a pressure lower than atmospheric pressure, for example, in the range of 1 to 1333 Pa.
- the supply flow rate of the HCDS gas controlled by the mass flow controller 241 is, for example, a flow rate in the range of 10 to 2000 sccm (0.01 to 2 slm).
- the supply flow rate of the N 2 gas controlled by the mass flow controllers 241e, 241c, 241d is set to a flow rate in the range of, for example, 100 to 2000 sccm (0.1 to 2 slm).
- the time for supplying the HCDS gas to the wafer 200 is, for example, a time within the range of 1 to 120 seconds.
- the temperature of the first heater 207 is set so that the CVD reaction occurs in the processing chamber 201 in the above-described pressure band. That is, the temperature of the first heater 207 is set so that the temperature of the wafer 200 becomes a first temperature, for example, a temperature in the range of 100 to 450 ° C.
- the temperature of the wafer 200 is less than 100 ° C., the HCDS gas is difficult to be decomposed and adsorbed on the wafer 200.
- the temperature of the wafer 200 is set to 450 ° C. or lower, preferably 400 ° C. or lower. Therefore, the temperature of the wafer 200 is 100 ° C. or higher and 450 ° C. or lower, preferably 100 ° C. or higher and 400 ° C. or lower.
- the thickness of, for example, less than one atomic layer to several atomic layers is formed on the wafer 200 (surface underlayer film).
- a silicon-containing layer is formed.
- the silicon-containing layer may be an HCDS gas adsorption layer, a silicon layer (Si layer), or both of them.
- the silicon-containing layer is preferably a layer containing silicon (Si) and chlorine (Cl).
- the silicon layer is a generic name including a continuous layer composed of silicon (Si), a discontinuous layer, and a silicon thin film formed by overlapping these layers.
- a continuous layer made of Si may be referred to as a silicon thin film. Note that Si constituting the silicon layer includes those in which the bond with Cl is not completely broken.
- the HCDS gas adsorption layer includes a discontinuous chemical adsorption layer in addition to a continuous chemical adsorption layer of gas molecules of HCDS gas. That is, the adsorption layer of HCDS gas includes a single molecular layer composed of HCDS molecules or a chemical adsorption layer having a thickness less than one molecular layer.
- the HCDS (Si 2 Cl 6 ) molecules constituting the adsorption layer of HCDS gas include those in which the bond between Si and Cl is partially broken (Si x Cl y molecules). That is, the adsorption layer of HCDS gas includes a continuous chemical adsorption layer or a discontinuous chemical adsorption layer of Si 2 Cl 6 molecules and / or Si x Cl y molecules.
- a layer having a thickness of less than one atomic layer means an atomic layer formed discontinuously, and a layer having a thickness of one atomic layer means an atomic layer formed continuously.
- a layer having a thickness less than one molecular layer means a molecular layer formed discontinuously, and a layer having a thickness of one molecular layer means a molecular layer formed continuously.
- the silicon layer is formed by depositing Si on the wafer 200 under the condition that the HCDS gas is self-decomposed (thermally decomposed), that is, under the condition that the thermal decomposition reaction of HCDS occurs. Under the condition where the HCDS gas is not self-decomposed (thermally decomposed), that is, under the condition where the HCDS thermal decomposition reaction does not occur, the HCDS gas is adsorbed on the wafer 200 to form an HCDS gas adsorption layer. Note that it is preferable to form a silicon layer on the wafer 200 rather than forming an adsorption layer of HCDS gas on the wafer 200 because the deposition rate can be increased.
- the thickness of the silicon-containing layer formed on the wafer 200 exceeds several atomic layers, the oxidation action in step 3 described later does not reach the entire silicon-containing layer. Further, the minimum value of the thickness of the silicon-containing layer that can be formed on the wafer 200 is less than one atomic layer. Therefore, the thickness of the silicon-containing layer is preferably set to be less than one atomic layer to several atomic layers.
- the action of the oxidation reaction in Step 3 described later can be relatively enhanced.
- the time required for the oxidation reaction can be reduced.
- the time required for forming the silicon-containing layer in step 1 can also be shortened.
- the processing time per cycle can be shortened, and the total processing time can be shortened. That is, the film forming rate can be increased.
- by controlling the thickness of the silicon-containing layer to 1 atomic layer or less it becomes possible to improve the controllability of film thickness uniformity.
- Step 2 (Purge process) After the silicon-containing layer is formed on the wafer 200, the valve 243 of the source gas supply pipe 232 is closed to stop the supply of HCDS gas. At this time, the APC valve 244 of the exhaust pipe 231 is kept open, the inside of the processing chamber 201 is evacuated by the vacuum pump 246, and the remaining HCDS gas is removed from the processing chamber 201. At this time, the valves 243c, 243d, and 243e are opened, and N 2 gas as an inert gas is supplied into the processing chamber 201. The N 2 gas acts as a purge gas, whereby the effect of removing the HCDS gas remaining in the processing chamber 201 from the processing chamber 201 can be further enhanced (residual gas removal).
- the temperature of the first heater 207 at this time is set so that the temperature of the wafer 200 is in the range of 100 to 450 ° C. as in the supply of the HCDS gas.
- the supply flow rate of N 2 gas as the purge gas supplied from each inert gas supply system is set to a flow rate in the range of, for example, 100 to 2000 sccm (0.1 to 2 slm).
- a rare gas such as Ar, He, Ne, or Xe may be used in addition to the N 2 gas.
- the gas remaining in the processing chamber 201 may not be completely removed, and the processing chamber 201 may not be completely purged. If the amount of gas remaining in the processing chamber 201 is very small, there will be no adverse effect in the subsequent step 3.
- the flow rate of N 2 gas supplied into the process chamber 201 need not be a large flow rate, for example, by supplying an amount comparable to the volume of the process tube 203 (the processing chamber 201), adverse effect in Step 3 Purging to such an extent that no occurrence occurs can be performed.
- the purge time can be shortened and the throughput can be improved.
- consumption of N 2 gas can be minimized.
- Step 3 (Oxidation process) After the residual gas in the processing chamber 201 is removed, the valve 243a of the oxygen-containing gas supply pipe 232a is opened, and O 2 gas is allowed to flow through the oxygen-containing gas supply pipe 232a.
- the O 2 gas flows from the oxygen-containing gas supply pipe 232a, and the flow rate is adjusted by the mass flow controller 241a.
- the O 2 gas whose flow rate has been adjusted is supplied into the pre-reaction chamber 301 in a reduced pressure state heated to the second temperature.
- the valve 243b of the hydrogen-containing gas supply pipe 232b is opened, and H 2 gas flows through the hydrogen-containing gas supply pipe 232b.
- the H 2 gas flows from the hydrogen-containing gas supply pipe 232b, and the flow rate is adjusted by the mass flow controller 241b.
- the H 2 gas whose flow rate has been adjusted is supplied into the pre-reaction chamber 301 in a reduced pressure state heated to the second temperature. Note that the O 2 gas and the H 2 gas are mixed in the pre-reaction chamber 301 in a reduced pressure state heated to the second temperature (O 2 gas + H 2 gas supply).
- the valve 243c of the second inert gas supply pipe 232c may be opened to supply N 2 gas as an inert gas from the second inert gas supply pipe 232c.
- the flow rate of the N 2 gas is adjusted by the mass flow controller 241c and supplied to the oxygen-containing gas supply pipe 232a.
- a mixed gas of O 2 gas and N 2 gas is supplied from the oxygen-containing gas supply pipe 232a.
- the valve 243d of the third inert gas supply pipe 232d may be opened to supply N 2 gas as an inert gas from the third inert gas supply pipe 232d.
- the flow rate of the N 2 gas is adjusted by the mass flow controller 241d and supplied to the hydrogen-containing gas supply pipe 232b.
- a mixed gas of H 2 gas and N 2 gas is supplied from the hydrogen-containing gas supply pipe 232b.
- a rare gas such as Ar, He, Ne, or Xe may be used in addition to the N 2 gas.
- the APC valve 244 is appropriately adjusted to maintain the pressure in the reaction preparatory chamber 301 at a pressure below atmospheric pressure, for example, 1 to 3999 Pa, preferably 1 to 2666 Pa, more preferably 1 to 1333 Pa. To do. Further, the pressure in the piping section between the reaction preparatory chamber 301 and the processing chamber 201 is also maintained at a pressure lower than atmospheric pressure, for example, 1 to 3999 Pa, preferably 1 to 2666 Pa, more preferably 1 to 1333 Pa.
- the supply flow rate of the O 2 gas controlled by the mass flow controller 241a is, for example, a flow rate in the range of 100 to 10,000 sccm (0.1 to 10 slm).
- the supply flow rate of H 2 gas controlled by the mass flow controller 241b is, for example, a flow rate in the range of 100 to 10,000 sccm (0.1 to 10 slm). Also, when supplying N 2 gas, the supply flow rate of N 2 gas controlled mass flow controller 241c, in 241d, the flow rate within a range of, for example, 100 ⁇ 2000sccm (0.1 ⁇ 2slm) .
- the temperature of the second heater 302 is such that the temperature in the reaction preparatory chamber 301 is within the range of the second temperature, for example, 450 to 1200 ° C., preferably 550 to 1100 ° C., more preferably 600 to 1000 ° C. Set as follows. Note that the second temperature is set to be higher than the first temperature.
- the H 2 gas concentration (H 2 / (H 2 + O 2 )) is, for example, a concentration within the range of 5 to 50%, preferably 10 to 33%. That is, for example, a condition where the O 2 gas ratio is equal to or higher than the H 2 gas ratio, preferably a condition where the O 2 gas ratio is larger than the H 2 gas ratio, that is, an oxygen-rich condition.
- the H 2 gas concentration can be controlled by adjusting the ratio of the H 2 gas supply flow rate to the O 2 gas supply flow rate (H 2 / O 2 flow rate ratio).
- the H 2 / O 2 flow rate ratio is set to 0.05 to 1. What is necessary is just to adjust so that it may become the flow ratio within the range.
- the O 2 gas and H 2 gas are thermally activated by non-plasma in a heated reduced pressure atmosphere to react.
- reactive species oxidized species
- oxygen such as atomic oxygen (O)
- the reactive species generated in the reaction preparatory chamber 301 are heated in a reduced pressure state through the reaction gas supply pipe 232f and the second nozzle 233a together with unreacted O 2 gas and H 2 gas.
- the wafers are supplied from a plurality of locations on the side of the wafer arrangement area corresponding to the wafer arrangement area in the processing chamber 201.
- Reactive species, unreacted O 2 gas, H 2 gas and the like supplied into the processing chamber 201 flow down in the processing chamber 201 and exhaust pipe 231 through an exhaust port provided on the lower end side of the wafer arrangement region. (Reacted species supply).
- the valve 243e is opened so that N 2 gas flows through the first inert gas supply pipe 232e. Good.
- the N 2 gas is supplied into the processing chamber 201 through the source gas supply pipe 232 and the first nozzle 233 and is exhausted from the exhaust pipe 231.
- the APC valve 244 is appropriately adjusted to maintain the pressure in the processing chamber 201 at a pressure lower than atmospheric pressure, for example, in the range of 1 to 1333 Pa.
- the supply flow rate of N 2 gas controlled by the mass flow controller 241e is, for example, a flow rate in the range of 100 to 2000 sccm (0.1 to 2 slm).
- the time for supplying reactive species containing oxygen such as atomic oxygen (O) to the wafer 200, that is, the reactive species supply time (irradiation time) is, for example, a time in the range of 1 to 120 seconds.
- the temperature of the first heater 207 is set so that the temperature of the inside of the processing chamber 201 and the wafer 200 is the same temperature range as when HCDS gas is supplied, that is, the first temperature, for example, a temperature in the range of 100 to 450 ° C. Set. Note that the first temperature is lower than the second temperature. In consideration of the throughput, it is preferable to set the temperature of the first heater 207 so that the temperature of the wafer 200 is maintained in the same temperature range in step 1 and step 3 as described above. Further, it is more preferable that the temperature of the first heater 207 is set so that the temperature of the wafer 200 is maintained in a similar temperature range in steps 1 to 4 (described later). In this case, the temperature of the first heater 207 is set so that the temperature of the wafer 200 becomes a first temperature, for example, a constant temperature within a range of 100 to 450 ° C. in steps 1 to 4 (described later).
- the silicon-containing layer is a silicon oxide layer (SiO 2 layer, hereinafter also referred to simply as SiO layer.) To It can be changed (modified).
- oxygen such as atomic oxygen (O) generated in the reaction preparatory chamber 301
- unreacted O 2 gas and H 2 gas
- the reactive species mainly react with at least a part of the silicon-containing layer formed on the wafer 200. That is, mainly by the action of the reactive species, oxidation treatment to the silicon-containing layer is carried out, this oxidation process, the silicon-containing layer is a silicon oxide layer (SiO 2 layer, hereinafter also referred to simply as SiO layer.) To It can be changed (modified).
- SiO 2 layer silicon oxide layer
- the unreacted O 2 gas and H 2 gas supplied into the processing chamber 201 is thermally activated and reacted in the processing chamber 201 under a heated reduced-pressure atmosphere, and the processing chamber Also in 201, reactive species containing oxygen such as atomic oxygen (O) are generated.
- This reactive species generated in the processing chamber 201 also contributes to the oxidation treatment for the silicon-containing layer.
- the amount of reactive species that can be generated in a relatively low temperature zone (100 to 450 ° C.) as in the processing chamber 201 of this embodiment is limited to a small amount.
- the O 2 gas and the H 2 gas are not activated by plasma, but are activated by heat and reacted to generate reactive species containing oxygen such as atomic oxygen (O),
- reactive species containing oxygen such as atomic oxygen (O)
- the silicon-containing layer is thermally oxidized mainly by the action of the reactive species, whereby a soft reaction can be generated and the above-described oxidation treatment can be performed softly.
- oxygen-containing gas that is, the oxidizing gas, ozone (O 3 ) gas, nitrogen monoxide (NO) gas, nitrous oxide (N 2 O) gas, or the like may be used in addition to oxygen (O 2 ) gas.
- oxygen-containing gas that is, the oxidizing gas, ozone (O 3 ) gas, nitrogen monoxide (NO) gas, nitrous oxide (N 2 O) gas, or the like may be used in addition to oxygen (O 2 ) gas.
- a hydrogen-containing gas that is, a reducing gas, deuterium (D 2 ) gas, ammonia (NH 3 ) gas, methane (CH 4 ) gas, or the like may be used in addition to hydrogen (H 2 ) gas.
- oxygen-containing gas at least one gas selected from the group consisting of O 2 gas, O 3 gas, NO gas, and N 2 O gas can be used, and as the hydrogen-containing gas, H 2 gas, At least one gas selected from the group consisting of D 2 gas, NH 3 gas, and CH 4 gas can be used.
- Step 4 (Purge process) After changing the silicon-containing layer to the silicon oxide layer, the valves 243a and 243b of the oxygen-containing gas supply pipe 232a and the hydrogen-containing gas supply pipe 232b are closed, and the O 2 gas and H 2 gas into the reaction preparatory chamber 301 are closed. The supply is stopped, and the supply of the reactive species containing oxygen such as atomic oxygen (O) into the processing chamber 201 is stopped. At this time, the APC valve 244 of the exhaust pipe 231 is kept open, the inside of the processing chamber 201 is evacuated by the vacuum pump 246, and the remaining reaction species, gases, and reaction byproducts are removed in the reaction preliminary chamber 301 and the processing chamber 201. Eliminate from within.
- O atomic oxygen
- the valves 243 c and 243 d are opened, and N 2 gas as an inert gas is supplied from each of the second inert gas supply pipe 232 c and the third inert gas supply pipe 232 d via the reaction preliminary chamber 301.
- the air is supplied to the inside and exhausted from the exhaust pipe 231.
- the valve 243 e is opened, and N 2 gas as an inert gas is supplied into the processing chamber 201 from the first inert gas supply pipe 232 e and exhausted from the exhaust pipe 231.
- the N 2 gas acts as a purge gas, whereby the reaction preliminary chamber 301 and the processing chamber 201 are purged with an inert gas, and the reactive species and gas remaining in the reaction preliminary chamber 301 and the processing chamber 201 are removed. The effect can be further enhanced (residual gas removal).
- the temperature of the first heater 207 at this time is set so that the temperature of the wafer 200 is in the range of 100 to 450 ° C. as in the supply of the HCDS gas.
- the supply flow rate of N 2 gas as the purge gas supplied from each inert gas supply system is set to a flow rate in the range of, for example, 100 to 2000 sccm (0.1 to 2 slm).
- a rare gas such as Ar, He, Ne, or Xe may be used in addition to the N 2 gas.
- the gas remaining in the processing chamber 201 may not be completely removed, and the processing chamber 201 may not be completely purged. If the amount of gas remaining in the processing chamber 201 is very small, no adverse effect will occur in the subsequent step 1. At this time, the flow rate of the N 2 gas supplied into the processing chamber 201 does not need to be a large flow rate. Purging to such an extent that no occurrence occurs can be performed. Thus, by not completely purging the inside of the processing chamber 201, the purge time can be shortened and the throughput can be improved. In addition, consumption of N 2 gas can be minimized.
- Steps 1 to 4 described above are defined as one cycle, and this cycle is performed a predetermined number of times, preferably a plurality of times, so that a silicon oxide film (SiO 2 film, hereinafter simply referred to as an SiO film) having a predetermined thickness is formed on the wafer 200. ) Can be formed.
- the thickness of the silicon oxide film is, for example, in the range of 2 to 20 nm.
- the valves 243e, 243c, and 243d are maintained open, and the first inert gas supply pipe 232e, the second inert gas supply pipe 232c, and the third
- the supply of N 2 gas as an inert gas into the processing chamber 201 from each of the inert gas supply pipes 232d is continued, and the exhaust pipe 231 is exhausted.
- the N 2 gas acts as a purge gas, whereby the inside of the processing chamber 201 is purged with an inert gas, and the gas remaining in the processing chamber 201 is removed from the inside of the processing chamber 201 (purge). Thereafter, the atmosphere in the processing chamber 201 is replaced with an inert gas, and the pressure in the processing chamber 201 is returned to normal pressure (return to atmospheric pressure).
- the seal cap 219 is lowered by the boat elevator 115 to open the lower end of the process tube 203, and the processed wafer 200 is held by the boat 217 from the lower end of the process tube 203 to the outside of the process tube 203. Unloaded (boat unload). Thereafter, the processed wafer 200 is taken out from the boat 217 (wafer discharge). In this manner, a series of processes for forming a silicon oxide film having a predetermined thickness on the wafer 200 is completed.
- the placed 450 ° C. or more wafers preferably the oxidation step performed by supplying a direct O 2 gas and H 2 gas under a reduced pressure atmosphere of a high temperature range above 550 ° C., and O 2 gas and H 2 gas
- oxidized species oxygen
- the temperature of the wafer 200 is kept at a low temperature of, for example, 450 ° C. or lower, and the oxidation step is also performed in such a low-pressure reduced-pressure atmosphere.
- the pressure is less than atmospheric pressure heated to a second temperature (for example, 450 to 1200 ° C.) higher than the first temperature (for example, 100 to 450 ° C.).
- a second temperature for example, 450 to 1200 ° C.
- the first temperature for example, 100 to 450 ° C.
- O 2 gas and H 2 gas are reacted in advance to generate a large amount of reactive species (oxidized species) containing oxygen such as atomic oxygen (O), and the reaction generated in large amounts.
- Oxidelated species oxygen
- Silicon is formed on the wafer 200 by supplying the seed to the wafer 200 heated to a first temperature (for example, 100 to 450 ° C.) in the processing chamber 201 under a pressure atmosphere lower than atmospheric pressure.
- the containing layer is oxidized to change into a silicon oxide layer.
- the temperature in the preliminary reaction chamber 301 (second temperature) is set higher than the temperature of the wafer 200 in the processing chamber 201 (first temperature).
- the wafer 200 in which the generation amount of reactive species including oxygen such as atomic oxygen (O) obtained by reacting the O 2 gas and the H 2 gas is set to a first temperature that is relatively low is accommodated.
- the generated amount of reactive species obtained when supplying O 2 gas and H 2 gas directly into the processing chamber 201 can be increased.
- the reaction in the case of supplying the feed to the reactive species of the wafer 200 in the first process chamber 201 accommodating the wafer 200 which is set to a temperature, and a direct O 2 gas and H 2 gas
- the amount supplied to the seed wafer 200 can be increased. That is, when the temperature of the wafer 200 is maintained at the first temperature which is relatively low, the O 2 gas and the H 2 gas are supplied directly into the processing chamber 201 containing the wafer 200 maintained at the same temperature.
- the concentration of the reactive species in the processing chamber 201 can be increased, and a large amount of reactive species can be given to the wafer 200.
- the temperature in the reaction preparatory chamber 301 (second temperature) is set higher than the temperature of the wafer 200 in the processing chamber 201 (first temperature).
- a process that accommodates a wafer 200 in which the amount of reactive species containing oxygen such as atomic oxygen (O) obtained by reacting two gases with H 2 gas is set to a relatively high second temperature.
- the amount of reactive species generated when O 2 gas and H 2 gas are directly supplied into the chamber 201 can be made equal.
- the reaction in the case of supplying the feed to the reactive species of the wafer 200 in the second processing chamber 201 accommodating the wafer 200 which is set to a temperature, and a direct O 2 gas and H 2 gas
- the amount supplied to the seed wafer 200 can be made equal. That is, in a state in which the temperature of the wafer 200 is maintained at the first temperature that is relatively low, the O 2 gas and H are directly introduced into the processing chamber 201 containing the wafer 200 that is maintained at the second temperature that is relatively high. It is possible to supply the wafer 200 with the same amount of reactive species as when two gases are supplied.
- the wafer temperature is kept at a low temperature (for example, 450 ° C. or lower in the present embodiment) that is lower than a restriction temperature in various processes. It is possible to supply to the wafer 200 reactive species having the same concentration as the reactive species obtained when high-temperature processing is performed on the wafer 200. As a result, in the low temperature processing on the wafer 200, it is possible to increase the oxidizing power by the reactive species in the oxidation step, and it is possible to perform the oxidation step in the same way as the high temperature processing. In addition, by increasing the oxidizing power by the reactive species in the oxidation step, the oxidation time can be shortened, thereby improving the film formation rate and improving the productivity.
- a low temperature for example, 450 ° C. or lower in the present embodiment
- the oxidizing agent used in the present embodiment is a reactive species containing oxygen such as atomic oxygen (O).
- O atomic oxygen
- the reactive species generating unit can be installed in the substrate processing apparatus at low cost.
- the reactive species containing oxygen such as atomic oxygen (O) used as an oxidizing agent in this embodiment is generated in a temperature range of 450 ° C. or higher, that is, at least in a temperature range of 450 to 1200 ° C.
- the oxidation species It has been confirmed that the force exceeds the oxidizing power of O 3 gas and the oxidizing power of O 2 gas excited by plasma in the same temperature range. That is, according to the present embodiment, even when the temperature of the wafer 200 (first temperature) is a low temperature such as 100 to 450 ° C., the second temperature is set to a temperature of 450 ° C. or higher.
- the oxidation can be performed with an oxidizing power that exceeds the oxidizing power of the O 3 gas and the oxidizing power of the O 2 gas excited by the plasma in the same temperature range.
- the present embodiment it is possible to obtain a high oxidizing power at a lower cost than in the case of using O 3 gas or O 2 gas excited by plasma as the oxidizing agent, and shorten the oxidation time. Is possible. Accordingly, the film formation rate can be improved and productivity can be improved as compared with the case where O 3 gas or O 2 gas excited by plasma is used as the oxidizing agent.
- the pressure in the reaction preparatory chamber 301 or the pressure in the processing chamber 201 Is maintained at a pressure below atmospheric pressure. This makes it possible to introduce the reactive species containing oxygen such as atomic oxygen (O) generated in the preliminary reaction chamber 301 into the processing chamber 201 while suppressing the deactivation of the reactive species.
- oxygen atomic oxygen
- the energy of this reactive species is higher than the binding energy of Si—N, Si—Cl, Si—H, and Si—C contained in the silicon-containing layer that is the object of oxidation treatment.
- the Si—N, Si—Cl, Si—H, and Si—C bonds contained in the silicon-containing layer are cut off.
- N, separated the binding of Si, Cl, H, C is removed from the silicon-containing layer, N 2, Cl 2, H 2, HCl, is discharged as CO 2 or the like.
- the remaining Si bonds due to the disconnection of N, Cl, H, and C are combined with O contained in the reactive species to form Si—O bonds.
- the silicon-containing layer is oxidized to form a silicon oxide layer. That is, according to the film forming sequence of this embodiment, a high-quality silicon oxide film having extremely low concentrations of nitrogen, chlorine, hydrogen, and carbon in the film can be obtained.
- the wafer 200 after the film formation is removed from the processing chamber 201 in-situ in the processing chamber 201. It is also possible to perform an annealing process for the purpose of modifying the film quality of the SiO 2 film formed thereon. By this annealing treatment, impurities in the SiO 2 film can be further removed, and the impurity concentration in the film can be further reduced.
- Second deposition sequence is an example of a method of the wafer 200 and the formation of the SiO 2 film on the top and a modification by annealing of the SiO 2 film formed on the wafer 200, is carried out continuously in the same processing chamber It is.
- FIG. 4 shows a gas supply timing chart in the second film forming sequence of the present embodiment.
- the upper diagram in FIG. 4 shows the timing of gas supply into the processing chamber, and the lower diagram shows the timing of gas supply into the reaction preparatory chamber.
- FIG. 4 shows the supply timing of main substances supplied into the processing chamber and the reaction preparatory chamber for convenience.
- a source gas containing silicon (HCDS gas) is supplied to a substrate housed in a processing chamber and heated to a first temperature, whereby silicon is deposited on the substrate.
- a hydrogen-containing gas (H 2 gas) are reacted to generate a reactive species containing oxygen (atomic oxygen (O)), and the reactive species is a first in a processing chamber under a pressure atmosphere less than atmospheric pressure.
- a substrate By alternately supplying a substrate heated to a temperature of 5 to a silicon oxide layer (SiO 2 layer) by oxidizing a silicon-containing layer formed on the substrate, a substrate is obtained. A silicon oxide film (SiO 2 film having a predetermined thickness) ). After that, in a reaction preparatory chamber under a pressure atmosphere below atmospheric pressure heated to a second temperature higher than the first temperature, an oxygen-containing gas (O 2 gas) and a hydrogen-containing gas (H 2 gas) To generate a reactive species containing oxygen (atomic oxygen (O)), and the reactive species is heated to a first temperature or a third temperature in a treatment chamber under a pressure atmosphere less than atmospheric pressure. By supplying to the substrate, the silicon oxide film (SiO 2 film) having a predetermined thickness formed on the substrate is modified. Note that the third temperature is higher than the first temperature and lower than the second temperature.
- the HCDS gas as a source gas
- O 2 gas as an oxygen-containing gas
- a H 2 gas as the hydrogen-containing gas
- Fig. An example in which an SiO 2 film, which is an oxide film, is formed as an insulating film on the substrate by the film forming sequence 4 will be described.
- a process from forming a SiO 2 film having a predetermined thickness on the wafer 200 and purging the inside of the processing chamber 201 with an inert gas is performed in the same manner as in the first film forming sequence. Thereafter, the valve 243a of the oxygen-containing gas supply pipe 232a is opened, and O 2 gas is allowed to flow through the oxygen-containing gas supply pipe 232a.
- the O 2 gas flows from the oxygen-containing gas supply pipe 232a, and the flow rate is adjusted by the mass flow controller 241a.
- the O 2 gas whose flow rate has been adjusted is supplied into the pre-reaction chamber 301 in a reduced pressure state heated to the second temperature.
- the valve 243b of the hydrogen-containing gas supply pipe 232b is opened, and H 2 gas flows through the hydrogen-containing gas supply pipe 232b.
- the H 2 gas flows from the hydrogen-containing gas supply pipe 232b, and the flow rate is adjusted by the mass flow controller 241b.
- the H 2 gas whose flow rate has been adjusted is supplied into the pre-reaction chamber 301 in a reduced pressure state heated to the second temperature. Note that the O 2 gas and the H 2 gas are mixed in the pre-reaction chamber 301 in a reduced pressure state heated to the second temperature (O 2 gas + H 2 gas supply).
- valve 243c of the second inert gas supply pipe 232c may be opened to supply N 2 gas as an inert gas from the second inert gas supply pipe 232c.
- valve 243d of the third inert gas supply pipe 232d may be opened to supply N 2 gas as an inert gas from the third inert gas supply pipe 232d.
- the APC valve 244 is appropriately adjusted to maintain the pressure in the reaction preparatory chamber 301 at a pressure below atmospheric pressure, for example, 1 to 3999 Pa, preferably 1 to 2666 Pa, more preferably 1 to 1333 Pa. To do. Further, the pressure in the piping section between the reaction preparatory chamber 301 and the processing chamber 201 is also maintained at a pressure lower than atmospheric pressure, for example, 1 to 3999 Pa, preferably 1 to 2666 Pa, more preferably 1 to 1333 Pa.
- the supply flow rate of the O 2 gas controlled by the mass flow controller 241a is, for example, a flow rate in the range of 100 to 10,000 sccm (0.1 to 10 slm).
- the supply flow rate of H 2 gas controlled by the mass flow controller 241b is, for example, a flow rate in the range of 100 to 10,000 sccm (0.1 to 10 slm). Also, when supplying N 2 gas, the supply flow rate of N 2 gas controlled mass flow controller 241c, in 241d, the flow rate within a range of, for example, 100 ⁇ 2000sccm (0.1 ⁇ 2slm) .
- the temperature of the second heater 302 is such that the temperature in the reaction preparatory chamber 301 is within the range of the second temperature, for example, 450 to 1200 ° C., preferably 550 to 1100 ° C., more preferably 600 to 1000 ° C. Set as follows. Note that the second temperature is set to be higher than the first temperature.
- the H 2 gas concentration (H 2 / (H 2 + O 2 )) is, for example, 5 to 50%, preferably 10 to 33%. That is, for example, a condition where the O 2 gas ratio is equal to or higher than the H 2 gas ratio, preferably a condition where the O 2 gas ratio is larger than the H 2 gas ratio, that is, an oxygen-rich condition.
- the H 2 gas concentration can be controlled by adjusting the ratio of the H 2 gas supply flow rate to the O 2 gas supply flow rate (H 2 / O 2 flow rate ratio).
- the O 2 gas and H 2 gas are thermally activated by non-plasma in a heated reduced pressure atmosphere and reacted.
- a reactive species containing oxygen such as atomic oxygen (O) is generated (reactive species generation).
- the reactive species generated in the reaction preparatory chamber 301 are heated in a reduced pressure state through the reaction gas supply pipe 232f and the second nozzle 233a together with unreacted O 2 gas and H 2 gas.
- the wafers are supplied from a plurality of locations on the side of the wafer arrangement area corresponding to the wafer arrangement area in the processing chamber 201.
- Reactive species, unreacted O 2 gas, H 2 gas and the like supplied into the processing chamber 201 flow down in the processing chamber 201 and exhaust pipe 231 through an exhaust port provided on the lower end side of the wafer arrangement region. (Reacted species supply).
- the valve 243e is opened so that N 2 gas flows through the first inert gas supply pipe 232e. Good.
- the N 2 gas is supplied into the processing chamber 201 through the source gas supply pipe 232 and the first nozzle 233 and is exhausted from the exhaust pipe 231.
- the APC valve 244 is appropriately adjusted to maintain the pressure in the processing chamber 201 at a pressure lower than atmospheric pressure, for example, in the range of 1 to 1333 Pa.
- the supply flow rate of N 2 gas controlled by the mass flow controller 241e is, for example, a flow rate in the range of 100 to 2000 sccm (0.1 to 2 slm).
- the time for supplying reactive species containing oxygen such as atomic oxygen (O) to the wafer 200, that is, the reactive species supply time (irradiation time) is, for example, a time within the range of 1 to 600 minutes.
- the time for supplying the reactive species to the wafer 200 in the modification process by annealing is set longer than the time for supplying the reactive species to the wafer 200 in the oxidation step when forming the SiO 2 film.
- the temperature of the first heater 207 is the temperature range in which the temperature in the processing chamber 201 and the wafer 200 is the same as that when the SiO 2 film is formed, that is, the first temperature, for example, a temperature in the range of 100 to 450 ° C.
- the temperature of the wafer 200 is set to a third temperature higher than the wafer temperature at the time of forming the SiO 2 film, for example, 450 to 700 ° C., preferably 450 to 600 ° C.
- the first temperature and the third temperature are lower than the second temperature.
- the temperature of the first heater 207 is set so that the temperature of the wafer 200 becomes a first temperature, for example, a constant temperature within a range of 100 to 450 ° C., from the formation of the SiO 2 film to the modification process. .
- the unreacted O 2 gas and H 2 gas supplied into the processing chamber 201 is thermally activated and reacted in the processing chamber 201 under a heated reduced-pressure atmosphere, and the processing chamber Also in 201, reactive species containing oxygen such as atomic oxygen (O) are generated.
- This reactive species generated in the processing chamber 201 also contributes to the modification process for the SiO 2 film.
- the amount of reactive species that can be generated in a relatively low temperature zone (100 to 450 ° C.) as in the processing chamber 201 of this embodiment is limited to a small amount.
- the O 2 gas and the H 2 gas are not activated by plasma but are activated by heat to react with each other, thereby generating a reactive species containing oxygen such as atomic oxygen (O).
- the SiO 2 film is modified mainly by the action of the reactive species, so that a soft reaction can be generated, and the above-described modifying process can be performed softly.
- the SiO 2 film is reformed mainly by the action of the reactive species including oxygen such as atomic oxygen (O) generated in the reaction preparatory chamber. Is called. Then, this reforming process removes impurities in the SiO 2 film. According to this modification treatment, a significant effect of removing impurities in the film can be obtained at a lower temperature than O 2 annealing and N 2 annealing performed as a usual modification treatment.
- the film quality of a certain insulating film can be improved. Further, it is possible to shorten the reforming time by increasing the reactivity due to the reactive species in the reforming process, thereby improving the productivity. It has also been confirmed that this modification treatment has an effect of reducing (reducing) the natural oxide film that is the base of the SiO 2 film formation.
- the energy of this reactive species is higher than the binding energy of Si—N, Si—Cl, Si—H, and Si—C contained in the SiO 2 film
- the energy of this reactive species is annealed.
- the Si—N, Si—Cl, Si—H, and Si—C bonds contained in the SiO 2 film are cut off.
- N, H, Cl, and C from which the bond with Si has been removed are removed from the film and discharged as N 2 , H 2 , Cl 2 , HCl, CO 2, and the like.
- the remaining Si bonds by cutting bonds with N, H, Cl, and C are combined with O contained in the reactive species to form Si—O bonds.
- the SiO 2 film is densified. In this way, the modification process of the SiO 2 film is performed. That is, according to this annealing treatment, a high-quality SiO 2 film having extremely low nitrogen, hydrogen, chlorine, and carbon concentrations in the film can be obtained.
- purging in the processing chamber 201, return to atmospheric pressure, boat unloading, and wafer discharge are performed in the same manner as after the formation of the SiO 2 film in the first film forming sequence.
- the SiO 2 film is formed on the wafer 200, then, in succession in-situ, a series of processes for modifying the SiO 2 film formed on the wafer 200 by the annealing is completed.
- the present invention is applicable to zirconium (Zr), hafnium (Hf), titanium (Ti), aluminum (Al), niobium (Nb). ), Tantalum (Ta), molybdenum (Mo), and other metal elements.
- the present invention includes a zirconium oxide film (ZrO 2 film), a zirconium silicate film (ZrSiO film), a zirconium aluminate film (ZrAlO film), a hafnium oxide film (HfO 2 film), a hafnium silicate film (HfSiO film), and hafnium.
- Aluminate film HfAlO film
- titanium oxide film TiO 2 film
- aluminum oxide film Al 2 O 3 film
- niobium oxide film Nb 2 O 5 film
- tantalum oxide film Ta 2 O 5 film
- the present invention can also be applied when forming a molybdenum oxide film (MoO 2 film) or the like, or a metal oxide film (high dielectric constant insulating film) in which these are combined or mixed.
- tetrakisethylmethylaminozirconium Zr [N (C 2 H 5 ) (CH 3 )] 4 , abbreviation: TEMAZ)
- TEMAZ tetrakisethylmethylaminozirconium
- Organic raw materials such as dimethylaminozirconium (Zr [N (CH 3 ) 2 ] 4 , abbreviation: TDMAZ), tetrakisdiethylaminozirconium (Zr [N (C 2 H 5 ) 2 ] 4 , abbreviation: TDAZ), and tetrachlorozirconium
- TDMAZ dimethylaminozirconium
- TDAZ tetrakisdiethylaminozirconium
- TDAZ tetrachlorozirconium
- an inorganic raw material such as zirconium tetrachloride (ZrCl 4 ) can be used.
- the oxygen-containing gas and the hydrogen-containing gas the same gas as that in the above-described embodiment can be used.
- the processing conditions at this time can be the same processing conditions as those described in the above-described embodiment, for example.
- HfO 2 film tetrakisethylmethylaminohafnium (Hf [N (C 2 H 5 ) (CH 3 )] 4 , abbreviation: TEMAH) is used as a raw material containing Hf.
- Hf [N (C 2 H 5 ) (CH 3 )] 4 abbreviation: TEMAH
- Organic raw materials such as tetrakisdimethylaminohafnium (Hf [N (CH 3 ) 2 ] 4 , abbreviation: TDMAH), tetrakisdiethylaminohafnium (Hf [N (C 2 H 5 ) 2 ] 4 , abbreviation: TDEAH), and tetrachloro Inorganic raw materials such as hafnium, that is, hafnium tetrachloride (HfCl 4 ) can be used.
- the oxygen-containing gas and the hydrogen-containing gas the same gas as that in the above-described embodiment can be used.
- the processing conditions at this time can be the same processing conditions as those described in the above-described embodiment, for example.
- TiO 2 film as a film containing Ti
- tetrakisethylmethylaminotitanium Ti [N (C 2 H 5 ) (CH 3 )] 4
- TEMAT tetrakisethylmethylaminotitanium
- Organic raw materials such as tetrakisdimethylaminotitanium (Ti [N (CH 3 ) 2 ] 4 , abbreviation: TDMAT), tetrakisdiethylaminotitanium (Ti [N (C 2 H 5 ) 2 ] 4 , abbreviation: TDEAT), tetrachloro
- An inorganic raw material such as titanium, that is, titanium tetrachloride (TiCl 4 ) can be used.
- the oxygen-containing gas and the hydrogen-containing gas the same gas as that in the above-described embodiment can be used. Note that the processing conditions at this time can be the same processing conditions as those described in the above-de
- an organic raw material such as trimethylaluminum (Al (CH 3 ) 3 , abbreviation: TMA), trichloroaluminum, that is, aluminum tri- Inorganic raw materials such as chloride (AlCl 3 ) and trifluoroaluminum, that is, aluminum trifluoride (AlF 3 )
- TMA trimethylaluminum
- AlCl 3 aluminum tri- Inorganic raw materials
- AlF 3 aluminum trifluoroaluminum
- the processing conditions at this time can be the same processing conditions as those described in the above-described embodiment, for example.
- Nb 2 O 5 film is formed as a film containing Nb
- pentachloroniobium that is, niobium pentachloride (NbCl 5 ), pentafluoroniobium, that is, niobium pentafluoride (NbF 5 ), etc.
- oxygen-containing gas and the hydrogen-containing gas the same gas as that in the above-described embodiment can be used.
- processing conditions at this time can be the same processing conditions as those described in the above-described embodiment, for example.
- a Ta 2 O 5 film as a film containing Ta, as a raw material containing Ta, pentachlorotantalum, that is, tantalum pentachloride (TaCl 5 ), pentafluorotantalum, that is, tantalum pentafluoride (TaF 5 ), Pentaethoxy tantalum (Ta (OC 2 H 5 ) 5 , abbreviation: PET), trisdiethylamino tertiary butyl imino tantalum (Ta (NC (CH 3 ) 3 ) (N (C 2 H 5 ) 2 ) 3 , abbreviation: TBTDET ) Etc.
- pentachlorotantalum that is, tantalum pentachloride (TaCl 5 )
- pentafluorotantalum that is, tantalum pentafluoride (TaF 5 ), Pentaethoxy tantalum (Ta (OC 2 H 5 ) 5
- a MoO 2 film is formed as a film containing Mo
- pentachloromolybdenum that is, molybdenum pentachloride (MoCl 5 )
- pentafluoromolybdenum that is, molybdenum pentafluoride (MoF 5 )
- MoF 5 molybdenum pentafluoride
- oxygen-containing gas and the hydrogen-containing gas the same gas as that in the above-described embodiment can be used.
- the processing conditions at this time can be the same processing conditions as those described in the above-described embodiment, for example.
- the present invention it is possible to form a high-quality metal oxide film at a higher film formation rate at a lower temperature, for example, 450 ° C. or lower than conventional.
- the H concentration among the impurities in the film is particularly high.
- the H concentration, Cl concentration, C concentration and N concentration can be reduced among the impurities in the film. I confirmed that I can do it.
- the second temperature is higher than the first temperature (second temperature> first temperature)
- the second temperature is the first temperature.
- first temperature is also possible. That is, it is possible to make the temperature in the reaction preparatory chamber equal to the temperature in the processing chamber.
- the first temperature is 450 ° C. or higher (the oxygen-containing gas and the hydrogen-containing gas react to generate reactive species such as atomic oxygen (O)). This is effective when the temperature can be set to a temperature that enables
- the temperature in the reaction preparatory chamber and the temperature in the processing chamber are both set to the first temperature, and the reaction between the oxygen-containing gas and the hydrogen-containing gas in the reaction preparatory chamber under reduced pressure heated to the first temperature. And the reaction can proceed in a processing chamber under reduced pressure heated to a first temperature, and the concentration of atomic oxygen obtained at that temperature can be maximized.
- the reaction between the oxygen-containing gas and the hydrogen-containing gas is not started in the processing chamber, but in the reaction preliminary chamber, and the reaction preliminary chamber has a reaction delay time between the oxygen-containing gas and the hydrogen-containing gas. It plays a role as a buffer to be adjusted.
- examples of the first temperature include 450 to 600 ° C.
- the present invention is not limited to this, and one or a few at a time.
- the present invention can also be suitably applied to the case of forming a film using a single-wafer type substrate processing apparatus that processes a single substrate.
- the first heating source is not a resistance heater but a lamp heater, and a wafer that heats the wafer with energy from light irradiation to the wafer by the lamp, that is, light absorption of the wafer.
- the present invention can also be suitably applied to the case of forming a film using a substrate processing apparatus having a cold wall type processing furnace.
- the processing furnace 402 according to the present modification includes a processing vessel 403 that forms a processing chamber 401, a lamp 404 as a first heating source, a quartz window 406 that transmits light from the lamp 404, and a single wafer 200. And a support base 405 including a susceptor 407 supported in a posture.
- a processing furnace 402 includes a processing vessel 403 that forms a processing chamber 401, a shower head 409 that supplies gas into the processing chamber 401 in a shower shape, and a susceptor that supports a single wafer 200 in a horizontal posture. And a resistance heater 408 serving as a first heating source provided on the support base 405.
- the shower head 409 includes a reaction preliminary container 300 having a reaction preliminary chamber 301 formed therein, second heaters 302a, 302b, and 302c provided so as to surround the cylindrical side surface and the upper surface of the reaction preliminary container 300, and a reaction preliminary And a heat insulating member 303 provided around the container 300 and the second heaters 302a, 302b, and 302c.
- the inlet of the shower head 409 is connected to a merged piping portion where the oxygen-containing gas supply pipe 232a and the hydrogen-containing gas supply pipe 232b merge, and the outlet supplies gas into the processing chamber 401 in a shower shape.
- a gas dispersion plate 304 is provided.
- elements that are substantially the same as those described in FIGS. 1 and 2 are assigned the same reference numerals, and descriptions thereof are omitted.
- the reaction preparatory chamber 301 heated to a high temperature by using the reaction preparatory chamber 301 heated to a high temperature, the generation amount of reactive species such as atomic oxygen (O) can be increased, and the concentration of the reactive species can be remarkably increased. . Therefore, even when using a cold wall type chamber that heats the wafer by light irradiation, it is possible to improve the film quality in the low-temperature processing as in the high-temperature processing, and the film formation speed as in the high-temperature processing. It is also possible to improve. Moreover, according to the modification shown in FIGS. 7 and 8, the piping part connecting the reaction preliminary chamber 301 and the processing chamber 201 (401) is eliminated, and the reaction preliminary chamber 301 and the processing chamber 201 (401) are directly connected.
- the piping part connecting the reaction preliminary chamber 301 and the processing chamber 201 (401) is eliminated, and the reaction preliminary chamber 301 and the processing chamber 201 (401) are directly connected.
- reaction species such as atomic oxygen (O) generated in the reaction preparatory chamber 301 from being deactivated in the pipe portion.
- reaction species such as atomic oxygen (O) generated in the reaction preparatory chamber 301
- pressure monitoring in the piping part and pressure adjustment in the piping part become unnecessary, and the configuration of the substrate processing apparatus and the pressure control operation can be simplified.
- the present invention can be realized by changing a process recipe of an existing substrate processing apparatus, for example.
- the process recipe according to the present invention is installed in an existing substrate processing apparatus via a telecommunication line or a recording medium recording the process recipe, or input / output of the existing substrate processing apparatus It is also possible to operate the apparatus and change the process recipe itself to the process recipe according to the present invention.
- the SiO 2 film was formed by the first sequence of the above-described embodiment, and the relationship between the film thickness and the temperature in the reaction preliminary chamber (second temperature) was evaluated.
- HCDS gas was used as the silicon-containing gas
- O 2 gas was used as the oxygen-containing gas
- H 2 gas was used as the hydrogen-containing gas.
- the temperature in the preliminary reaction chamber was set to a temperature within a range from room temperature to 750 ° C.
- the other film forming conditions processing conditions at each step) were set within the processing condition range described in the above-described embodiment. The result is shown in FIG.
- FIG. 5 is a graph showing the relationship between the thickness of the SiO 2 film and the temperature in the reaction preparatory chamber according to this example.
- the horizontal axis in FIG. 5 represents the temperature (° C.) in the reaction preparatory chamber, and the vertical axis represents the thickness of the SiO 2 film (arbitrary unit (au)).
- the film thickness of the SiO 2 film is increased by increasing the temperature (second temperature) in the preliminary reaction chamber.
- the film formation rate can be greatly improved by setting the temperature (second temperature) in the preliminary reaction chamber to 450 ° C. or higher. That is, by setting the temperature in the preliminary reaction chamber (second temperature) to a temperature in the range of 450 ° C. or higher, the supply amount of the reactive species to the wafer is increased, and the wafer temperature (first temperature) is lowered ( For example, it can be seen that the film formation rate can be improved in a state maintained at 450 ° C. or lower.
- Forming a silicon-containing layer on the substrate by supplying a source gas containing silicon to the substrate housed in the processing chamber and heated to the first temperature; Generating a reactive species containing oxygen by reacting an oxygen-containing gas and a hydrogen-containing gas in a reaction preparatory chamber under a pressure atmosphere less than atmospheric pressure heated to a second temperature equal to or higher than the first temperature; The reactive species is supplied to the substrate heated to the first temperature in the processing chamber under a pressure atmosphere less than atmospheric pressure, thereby oxidizing the silicon-containing layer formed on the substrate. And changing to a silicon oxide layer, By alternately repeating the above, there is provided a method for manufacturing a semiconductor device including a step of forming a silicon oxide film having a predetermined thickness on the substrate.
- Appendix 2 A method of manufacturing a semiconductor device according to appendix 1, preferably, The reactive species is a reactive species not containing H 2 O.
- Appendix 3 A method of manufacturing a semiconductor device according to appendix 1, preferably, The reactive species is atomic oxygen.
- Appendix 4 A method of manufacturing a semiconductor device according to appendix 1, preferably, The first temperature is set to 100 ° C. to 600 ° C., and the second temperature is set to 450 ° C. to 1200 ° C.
- Appendix 5 A method of manufacturing a semiconductor device according to appendix 1, preferably, The first temperature is set to 100 ° C. or higher and 450 ° C. or lower, and the second temperature is set to 450 ° C. or higher and 1200 ° C. or lower.
- Appendix 6 A method of manufacturing a semiconductor device according to appendix 1, preferably, In the step of changing the silicon-containing layer into a silicon oxide layer, the pressure in the reaction preparatory chamber is set to 1 Pa or more and 3999 Pa or less, and the pressure in the processing chamber is set to 1 Pa or more and 1333 Pa or less.
- Appendix 7 A method of manufacturing a semiconductor device according to appendix 1, preferably, The reaction preparatory chamber is directly connected to the processing chamber.
- Appendix 8 A method of manufacturing a semiconductor device according to appendix 1, preferably, The reactive species are supplied to the substrate through a shower head, and the preliminary reaction chamber is provided in the shower head.
- Appendix 9 A method of manufacturing a semiconductor device according to appendix 1, preferably, In the step of changing the silicon-containing layer into a silicon oxide layer, each gas is supplied into the reaction preparatory chamber under conditions such that the flow rate of the oxygen-containing gas is greater than the flow rate of the hydrogen-containing gas.
- Appendix 10 A method of manufacturing a semiconductor device according to appendix 1, preferably, In the step of changing the silicon-containing layer to a silicon oxide layer, each gas is supplied into the reaction preparatory chamber under conditions rich in oxygen-containing gas.
- Appendix 11 A method of manufacturing a semiconductor device according to appendix 1, preferably, The silicon-containing layer is a silicon layer.
- Appendix 12 A method of manufacturing a semiconductor device according to appendix 1, preferably, The silicon-containing layer is a layer formed by depositing silicon on the substrate.
- Appendix 13 A method of manufacturing a semiconductor device according to appendix 1, preferably, The silicon-containing layer is an adsorption layer for the source gas.
- Appendix 14 A method of manufacturing a semiconductor device according to appendix 1, preferably, The silicon-containing layer is a layer formed by adsorbing the source gas on the substrate.
- Appendix 15 A method of manufacturing a semiconductor device according to appendix 1, preferably, In the reaction preparatory chamber under a pressure atmosphere less than atmospheric pressure heated to the second temperature, an oxygen-containing gas and a hydrogen-containing gas are reacted to generate a reactive species containing oxygen, and the reactive species is With respect to the substrate heated to the first temperature in the processing chamber under a pressure atmosphere less than atmospheric pressure or the third temperature higher than the first temperature and lower than the second temperature.
- the method further includes the step of modifying the silicon oxide film having a predetermined film thickness formed on the substrate by supplying.
- the oxygen-containing gas is at least one gas selected from the group consisting of oxygen gas, ozone gas, nitrogen monoxide gas and nitrous oxide gas
- the hydrogen-containing gas is hydrogen gas, deuterium gas, ammonia gas and methane gas At least one gas selected from the group consisting of:
- Appendix 17 A method of manufacturing a semiconductor device according to appendix 1, preferably, The oxygen-containing gas is oxygen gas, and the hydrogen-containing gas is hydrogen gas.
- a silicon-containing layer on the substrate by supplying a source gas containing silicon to the substrate housed in the processing chamber and heated to the first temperature; Generating a reactive species containing oxygen by reacting an oxygen-containing gas and a hydrogen-containing gas in a reaction preparatory chamber under a pressure atmosphere less than atmospheric pressure heated to a second temperature equal to or higher than the first temperature; The reactive species is supplied to the substrate heated to the first temperature in the processing chamber under a pressure atmosphere less than atmospheric pressure, thereby oxidizing the silicon-containing layer formed on the substrate. And changing to a silicon oxide layer, By alternately repeating the above, there is provided a substrate processing method including a step of forming a silicon oxide film having a predetermined thickness on the substrate.
- a processing chamber for accommodating and processing the substrate; A first heating source for heating the substrate in the processing chamber to a first temperature; A reaction preparatory chamber for reacting multiple types of gases; A second heating source for heating the preliminary reaction chamber to a second temperature not lower than the first temperature; A source gas supply system for supplying a source gas containing silicon into the processing chamber; An oxygen-containing gas supply system for supplying an oxygen-containing gas into the reaction preparatory chamber; A hydrogen-containing gas supply system for supplying a hydrogen-containing gas into the reaction preparatory chamber; A pressure adjusting unit for adjusting the pressure in the processing chamber and the reaction preparatory chamber; A process of forming a silicon-containing layer on the substrate by supplying the source gas to the substrate housed in the processing chamber and heated to the first temperature, and heated to the second temperature In the reaction preparatory chamber under a pressure atmosphere less than atmospheric pressure, an oxygen-containing gas and a hydrogen-containing gas are reacted to generate oxygen-containing reactive species, and the reactive species
- a process of oxidizing the silicon-containing layer formed on the substrate into an oxide layer by supplying the substrate heated to the first temperature in the processing chamber.
- the first heating source, the second heating source, the source gas supply system, the oxygen-containing gas supply system, and the like so as to form a silicon oxide film having a predetermined thickness on the substrate.
- Hydrogen-containing gas supply system and the pressure A control unit for controlling the integer part, A substrate processing apparatus is provided.
- a procedure for forming a silicon-containing layer on the substrate by supplying a source gas containing silicon to the substrate housed in the processing chamber of the substrate processing apparatus and heated to the first temperature; Generating a reactive species containing oxygen by reacting an oxygen-containing gas and a hydrogen-containing gas in a reaction preparatory chamber under a pressure atmosphere less than atmospheric pressure heated to a second temperature equal to or higher than the first temperature; The reactive species is supplied to the substrate heated to the first temperature in the processing chamber under a pressure atmosphere less than atmospheric pressure, thereby oxidizing the silicon-containing layer formed on the substrate. And changing to a silicon oxide layer, By alternately repeating the above, a program for causing a computer to execute a procedure for forming a silicon oxide film having a predetermined thickness on the substrate is provided.
- a procedure for forming a silicon-containing layer on the substrate by supplying a source gas containing silicon to the substrate housed in the processing chamber of the substrate processing apparatus and heated to the first temperature; Generating a reactive species containing oxygen by reacting an oxygen-containing gas and a hydrogen-containing gas in a reaction preparatory chamber under a pressure atmosphere less than atmospheric pressure heated to a second temperature equal to or higher than the first temperature; The reactive species is supplied to the substrate heated to the first temperature in the processing chamber under a pressure atmosphere less than atmospheric pressure, thereby oxidizing the silicon-containing layer formed on the substrate. And changing to a silicon oxide layer, By alternately repeating the above, a computer-readable recording medium recording a program for causing a computer to execute a procedure for forming a silicon oxide film having a predetermined thickness on the substrate is provided.
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Abstract
Description
処理室内に収容され、第1の温度に加熱された基板に対して、シリコンを含む原料ガスを供給することで、前記基板上にシリコン含有層を形成する工程と、
前記第1の温度以上の第2の温度に加熱された大気圧未満の圧力雰囲気下にある反応予備室内で、酸素含有ガスと水素含有ガスとを反応させて酸素を含む反応種を生成し、その反応種を、大気圧未満の圧力雰囲気下にある前記処理室内の前記第1の温度に加熱された前記基板に対して供給することで、前記基板上に形成された前記シリコン含有層を酸化してシリコン酸化層に変化させる工程と、
を交互に繰り返すことで、前記基板上に所定膜厚のシリコン酸化膜を形成する工程を有する半導体装置の製造方法が提供される。
処理室内に収容され、第1の温度に加熱された基板に対して、シリコンを含む原料ガスを供給することで、前記基板上にシリコン含有層を形成する工程と、
前記第1の温度以上の第2の温度に加熱された大気圧未満の圧力雰囲気下にある反応予備室内で、酸素含有ガスと水素含有ガスとを反応させて酸素を含む反応種を生成し、その反応種を、大気圧未満の圧力雰囲気下にある前記処理室内の前記第1の温度に加熱された前記基板に対して供給することで、前記基板上に形成された前記シリコン含有層を酸化してシリコン酸化層に変化させる工程と、
を交互に繰り返すことで、前記基板上に所定膜厚のシリコン酸化膜を形成する工程を有する基板処理方法が提供される。
基板を収容して処理する処理室と、
前記処理室内の基板を第1の温度に加熱する第1の加熱源と、
複数種類のガスを反応させる反応予備室と、
前記反応予備室内を第1の温度以上の第2の温度に加熱する第2の加熱源と、
前記処理室内にシリコンを含む原料ガスを供給する原料ガス供給系と、
前記反応予備室内に酸素含有ガスを供給する酸素含有ガス供給系と、
前記反応予備室内に水素含有ガスを供給する水素含有ガス供給系と、
前記処理室内および前記反応予備室内の圧力を調整する圧力調整部と、
前記処理室内に収容され、前記第1の温度に加熱された基板に対して、前記原料ガスを供給することで、前記基板上にシリコン含有層を形成する処理と、前記第2の温度に加熱された大気圧未満の圧力雰囲気下にある前記反応予備室内で、酸素含有ガスと水素含有ガスとを反応させて酸素を含む反応種を生成し、その反応種を、大気圧未満の圧力雰囲気下にある前記処理室内の前記第1の温度に加熱された前記基板に対して供給することで、前記基板上に形成された前記シリコン含有層を酸化して酸化層に変化させる処理と、を交互に繰り返すことで、前記基板上に所定膜厚のシリコン酸化膜を形成するように、前記第1の加熱源、前記第2の加熱源、前記原料ガス供給系、前記酸素含有ガス供給系、前記水素含有ガス供給系および前記圧力調整部を制御する制御部と、
を有する基板処理装置が提供される。
図3に、本実施形態の第1の成膜シーケンスにおけるガス供給のタイミング図を示す。図3の上側の図は処理室内へのガス供給のタイミングを示しており、下側の図は反応予備室内へのガス供給のタイミングを示している。なお図3は、便宜上、処理室内および反応予備室内へ供給する主な物質の供給タイミングを示している。
原料ガス供給管232のバルブ243を開き、原料ガス供給管232にHCDSガスを流す。HCDSガスは、原料ガス供給管232から流れ、マスフローコントローラ241により流量調整される。流量調整されたHCDSガスは、第1ノズル233のガス供給孔248から、加熱された減圧状態の処理室201内におけるウエハ配列領域に対応するウエハ配列領域側方における領域の複数箇所から供給される。処理室201内に供給されたHCDSガスは、処理室201内を流下してウエハ配列領域の下端側に設けられた排気口を介して排気管231から排気される(HCDSガス供給)。
ウエハ200上にシリコン含有層が形成された後、原料ガス供給管232のバルブ243を閉じ、HCDSガスの供給を停止する。このとき、排気管231のAPCバルブ244は開いたままとし、真空ポンプ246により処理室201内を真空排気し、残留したHCDSガスを処理室201内から排除する。このとき、バルブ243c,243d,243eを開き、不活性ガスとしてのN2ガスを処理室201内へ供給する。N2ガスはパージガスとして作用し、これにより、処理室201内に残留するHCDSガスを処理室201内から排除する効果を、更に高めることができる(残留ガス除去)。
処理室201内の残留ガスを除去した後、酸素含有ガス供給管232aのバルブ243aを開き、酸素含有ガス供給管232aにO2ガスを流す。O2ガスは酸素含有ガス供給管232aから流れ、マスフローコントローラ241aにより流量調整される。流量調整されたO2ガスは、第2の温度に加熱された減圧状態の反応予備室301内に供給される。このとき同時に、水素含有ガス供給管232bのバルブ243bを開き、水素含有ガス供給管232bにH2ガスを流す。H2ガスは水素含有ガス供給管232bから流れ、マスフローコントローラ241bにより流量調整される。流量調整されたH2ガスは第2の温度に加熱された減圧状態の反応予備室301内に供給される。なお、O2ガスとH2ガスは第2の温度に加熱された減圧状態の反応予備室301内で混合されることとなる(O2ガス+H2ガス供給)。
シリコン含有層をシリコン酸化層へと変化させた後、酸素含有ガス供給管232a、水素含有ガス供給管232bのバルブ243a,243bを閉じ、反応予備室301内へのO2ガス、H2ガスの供給を停止して、処理室201内への原子状酸素(O)等の酸素を含む反応種の供給を停止する。このとき、排気管231のAPCバルブ244は開いたままとし、真空ポンプ246により処理室201内を真空排気し、残留した反応種やガスや反応副生成物を反応予備室301内や処理室201内から排除する。このとき、バルブ243c,243dを開き、第2不活性ガス供給管232c、第3不活性ガス供給管232dのそれぞれから不活性ガスとしてのN2ガスを、反応予備室301を介して処理室201内へ供給し排気管231から排気する。また、バルブ243eを開き、第1不活性ガス供給管232eからも不活性ガスとしてのN2ガスを処理室201内へ供給し排気管231から排気する。N2ガスはパージガスとして作用し、これにより、反応予備室301内や処理室201内が不活性ガスでパージされ、反応予備室301内や処理室201内に残留する反応種やガスを排除する効果を更に高めることができる(残留ガス除去)。
第1の成膜シーケンスによりウエハ200上にSiO2膜を成膜した後、成膜後のウエハ200を処理室201内から取り出すことなく、その処理室201内にてin-situで、ウエハ200上に形成されたSiO2膜の膜質の改質を目的としたアニール処理を行うことも可能である。このアニールによる改質処理により、SiO2膜の膜中不純物を更に除去することが可能となり、膜中不純物濃度をより一層低減することが可能となる。
ものではなく、その要旨を逸脱しない範囲で種々変更可能である。
本発明の一態様によれば、
処理室内に収容され、第1の温度に加熱された基板に対して、シリコンを含む原料ガスを供給することで、前記基板上にシリコン含有層を形成する工程と、
前記第1の温度以上の第2の温度に加熱された大気圧未満の圧力雰囲気下にある反応予備室内で、酸素含有ガスと水素含有ガスとを反応させて酸素を含む反応種を生成し、その反応種を、大気圧未満の圧力雰囲気下にある前記処理室内の前記第1の温度に加熱された前記基板に対して供給することで、前記基板上に形成された前記シリコン含有層を酸化してシリコン酸化層に変化させる工程と、
を交互に繰り返すことで、前記基板上に所定膜厚のシリコン酸化膜を形成する工程を有する半導体装置の製造方法が提供される。
付記1の半導体装置の製造方法であって、好ましくは、
前記反応種は、H2O非含有の反応種である。
付記1の半導体装置の製造方法であって、好ましくは、
前記反応種は、原子状酸素である。
付記1の半導体装置の製造方法であって、好ましくは、
前記第1の温度を100℃以上600℃以下とし、前記第2の温度を450℃以上1200℃以下とする。
付記1の半導体装置の製造方法であって、好ましくは、
前記第1の温度を100℃以上450℃以下とし、前記第2の温度を450℃以上1200℃以下とする。
付記1の半導体装置の製造方法であって、好ましくは、
前記シリコン含有層をシリコン酸化層に変化させる工程では、前記反応予備室内の圧力を1Pa以上3999Pa以下とし、前記処理室内の圧力を1Pa以上1333Pa以下とする。
付記1の半導体装置の製造方法であって、好ましくは、
前記反応予備室は前記処理室に直結している。
付記1の半導体装置の製造方法であって、好ましくは、
前記反応種はシャワーヘッドを介して前記基板に対して供給され、前記反応予備室は、前記シャワーヘッド内に設けられる。
付記1の半導体装置の製造方法であって、好ましくは、
前記シリコン含有層をシリコン酸化層に変化させる工程では、前記反応予備室内に各ガスを、酸素含有ガスの流量が水素含有ガスの流量よりも大きくなるような条件にて供給する。
付記1の半導体装置の製造方法であって、好ましくは、
前記シリコン含有層をシリコン酸化層に変化させる工程では、前記反応予備室内に各ガスを酸素含有ガスリッチな条件にて供給する。
付記1の半導体装置の製造方法であって、好ましくは、
前記シリコン含有層はシリコン層である。
付記1の半導体装置の製造方法であって、好ましくは、
前記シリコン含有層はシリコンが前記基板上に堆積することで形成される層である。
付記1の半導体装置の製造方法であって、好ましくは、
前記シリコン含有層は前記原料ガスの吸着層である。
付記1の半導体装置の製造方法であって、好ましくは、
前記シリコン含有層は前記原料ガスが前記基板上に吸着することで形成される層である。
付記1の半導体装置の製造方法であって、好ましくは、
前記第2の温度に加熱された大気圧未満の圧力雰囲気下にある前記反応予備室内で、酸素含有ガスと水素含有ガスとを反応させて酸素を含む反応種を生成し、その反応種を、大気圧未満の圧力雰囲気下にある前記処理室内の前記第1の温度、または、前記第1の温度よりも高く前記第2の温度よりも低い第3の温度に加熱された前記基板に対して供給することで、前記基板上に形成された所定膜厚の前記シリコン酸化膜を改質する工程をさらに有する。
付記1の半導体装置の製造方法であって、好ましくは、
前記酸素含有ガスが、酸素ガス、オゾンガス、一酸化窒素ガスおよび亜酸化窒素ガスよりなる群から選択される少なくとも一つのガスであり、前記水素含有ガスが水素ガス、重水素ガス、アンモニアガスおよびメタンガスよりなる群から選択される少なくとも一つのガスである。
付記1の半導体装置の製造方法であって、好ましくは、
前記酸素含有ガスが酸素ガスであり、前記水素含有ガスが水素ガスである。
本発明の他の態様によれば、
処理室内に収容され、第1の温度に加熱された基板に対して、シリコンを含む原料ガスを供給することで、前記基板上にシリコン含有層を形成する工程と、
前記第1の温度以上の第2の温度に加熱された大気圧未満の圧力雰囲気下にある反応予備室内で、酸素含有ガスと水素含有ガスとを反応させて酸素を含む反応種を生成し、その反応種を、大気圧未満の圧力雰囲気下にある前記処理室内の前記第1の温度に加熱された前記基板に対して供給することで、前記基板上に形成された前記シリコン含有層を酸化してシリコン酸化層に変化させる工程と、
を交互に繰り返すことで、前記基板上に所定膜厚のシリコン酸化膜を形成する工程を有する基板処理方法が提供される。
本発明のさらに他の態様によれば、
基板を収容して処理する処理室と、
前記処理室内の基板を第1の温度に加熱する第1の加熱源と、
複数種類のガスを反応させる反応予備室と、
前記反応予備室内を第1の温度以上の第2の温度に加熱する第2の加熱源と、
前記処理室内にシリコンを含む原料ガスを供給する原料ガス供給系と、
前記反応予備室内に酸素含有ガスを供給する酸素含有ガス供給系と、
前記反応予備室内に水素含有ガスを供給する水素含有ガス供給系と、
前記処理室内および前記反応予備室内の圧力を調整する圧力調整部と、
前記処理室内に収容され、前記第1の温度に加熱された基板に対して、前記原料ガスを供給することで、前記基板上にシリコン含有層を形成する処理と、前記第2の温度に加熱された大気圧未満の圧力雰囲気下にある前記反応予備室内で、酸素含有ガスと水素含有ガスとを反応させて酸素を含む反応種を生成し、その反応種を、大気圧未満の圧力雰囲気下にある前記処理室内の前記第1の温度に加熱された前記基板に対して供給することで、前記基板上に形成された前記シリコン含有層を酸化して酸化層に変化させる処理と、を交互に繰り返すことで、前記基板上に所定膜厚のシリコン酸化膜を形成するように、前記第1の加熱源、前記第2の加熱源、前記原料ガス供給系、前記酸素含有ガス供給系、前記水素含有ガス供給系および前記圧力調整部を制御する制御部と、
を有する基板処理装置が提供される。
本発明のさらに他の態様によれば、
基板処理装置の処理室内に収容され、第1の温度に加熱された基板に対して、シリコンを含む原料ガスを供給することで、前記基板上にシリコン含有層を形成する手順と、
前記第1の温度以上の第2の温度に加熱された大気圧未満の圧力雰囲気下にある反応予備室内で、酸素含有ガスと水素含有ガスとを反応させて酸素を含む反応種を生成し、その反応種を、大気圧未満の圧力雰囲気下にある前記処理室内の前記第1の温度に加熱された前記基板に対して供給することで、前記基板上に形成された前記シリコン含有層を酸化してシリコン酸化層に変化させる手順と、
を交互に繰り返すことで、前記基板上に所定膜厚のシリコン酸化膜を形成する手順をコンピュータに実行させるためのプログラムが提供される。
本発明のさらに他の態様によれば、
基板処理装置の処理室内に収容され、第1の温度に加熱された基板に対して、シリコンを含む原料ガスを供給することで、前記基板上にシリコン含有層を形成する手順と、
前記第1の温度以上の第2の温度に加熱された大気圧未満の圧力雰囲気下にある反応予備室内で、酸素含有ガスと水素含有ガスとを反応させて酸素を含む反応種を生成し、その反応種を、大気圧未満の圧力雰囲気下にある前記処理室内の前記第1の温度に加熱された前記基板に対して供給することで、前記基板上に形成された前記シリコン含有層を酸化してシリコン酸化層に変化させる手順と、
を交互に繰り返すことで、前記基板上に所定膜厚のシリコン酸化膜を形成する手順をコンピュータに実行させるためのプログラムを記録したコンピュータ読み取り可能な記録媒体が提供される。
201 処理室
202 処理炉
203 プロセスチューブ
207 第1のヒータ
231 排気管
232 原料ガス供給管
232a 酸素含有ガス供給管
232b 水素含有ガス供給管
232f 反応ガス供給管
244 APCバルブ
245 圧力センサ
245a 圧力センサ
245b 圧力センサ
246 真空ポンプ
263 温度センサ
263a 温度センサ
280 コントローラ
300 反応予備容器
301 反応予備室
302 第2のヒータ
Claims (10)
- 処理室内に収容され、第1の温度に加熱された基板に対して、シリコンを含む原料ガスを供給することで、前記基板上にシリコン含有層を形成する工程と、
前記第1の温度以上の第2の温度に加熱された大気圧未満の圧力雰囲気下にある反応予備室内で、酸素含有ガスと水素含有ガスとを反応させて酸素を含む反応種を生成し、その反応種を、大気圧未満の圧力雰囲気下にある前記処理室内の前記第1の温度に加熱された前記基板に対して供給することで、前記基板上に形成された前記シリコン含有層を酸化してシリコン酸化層に変化させる工程と、
を交互に繰り返すことで、前記基板上に所定膜厚のシリコン酸化膜を形成する工程を有する半導体装置の製造方法。 - 前記反応種は、H2O非含有の反応種である請求項1記載の半導体装置の製造方法。
- 前記反応種は、原子状酸素である請求項1記載の半導体装置の製造方法。
- 前記第1の温度を100℃以上600℃以下とし、前記第2の温度を450℃以上1200℃以下とする請求項1記載の半導体装置の製造方法。
- 前記第1の温度を100℃以上450℃以下とし、前記第2の温度を450℃以上1200℃以下とする請求項1記載の半導体装置の製造方法。
- 前記シリコン含有層をシリコン酸化層に変化させる工程では、前記反応予備室内の圧力を1Pa以上3999Pa以下とし、前記処理室内の圧力を1Pa以上1333Pa以下とする請求項1記載の半導体装置の製造方法。
- 前記反応予備室は前記処理室に直結している請求項1記載の半導体装置の製造方法。
- 前記反応種はシャワーヘッドを介して前記基板に対して供給され、前記反応予備室は、前記シャワーヘッド内に設けられる請求項1記載の半導体装置の製造方法。
- 処理室内に収容され、第1の温度に加熱された基板に対して、シリコンを含む原料ガスを供給することで、前記基板上にシリコン含有層を形成する工程と、
前記第1の温度以上の第2の温度に加熱された大気圧未満の圧力雰囲気下にある反応予備室内で、酸素含有ガスと水素含有ガスとを反応させて酸素を含む反応種を生成し、その反応種を、大気圧未満の圧力雰囲気下にある前記処理室内の前記第1の温度に加熱された前記基板に対して供給することで、前記基板上に形成された前記シリコン含有層を酸化してシリコン酸化層に変化させる工程と、
を交互に繰り返すことで、前記基板上に所定膜厚のシリコン酸化膜を形成する工程を有する基板処理方法。 - 基板を収容して処理する処理室と、
前記処理室内の基板を第1の温度に加熱する第1の加熱源と、
複数種類のガスを反応させる反応予備室と、
前記反応予備室内を第1の温度以上の第2の温度に加熱する第2の加熱源と、
前記処理室内にシリコンを含む原料ガスを供給する原料ガス供給系と、
前記反応予備室内に酸素含有ガスを供給する酸素含有ガス供給系と、
前記反応予備室内に水素含有ガスを供給する水素含有ガス供給系と、
前記処理室内および前記反応予備室内の圧力を調整する圧力調整部と、
前記処理室内に収容され、前記第1の温度に加熱された基板に対して、前記原料ガスを供給することで、前記基板上にシリコン含有層を形成する処理と、前記第2の温度に加熱された大気圧未満の圧力雰囲気下にある前記反応予備室内で、酸素含有ガスと水素含有ガスとを反応させて酸素を含む反応種を生成し、その反応種を、大気圧未満の圧力雰囲気下にある前記処理室内の前記第1の温度に加熱された前記基板に対して供給することで、前記基板上に形成された前記シリコン含有層を酸化して酸化層に変化させる処理と、を交互に繰り返すことで、前記基板上に所定膜厚のシリコン酸化膜を形成するように、前記第1の加熱源、前記第2の加熱源、前記原料ガス供給系、前記酸素含有ガス供給系、前記水素含有ガス供給系および前記圧力調整部を制御する制御部と、
を有する基板処理装置。
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