WO2020137528A1 - 付着物除去方法及び成膜方法 - Google Patents
付着物除去方法及び成膜方法 Download PDFInfo
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- WO2020137528A1 WO2020137528A1 PCT/JP2019/048352 JP2019048352W WO2020137528A1 WO 2020137528 A1 WO2020137528 A1 WO 2020137528A1 JP 2019048352 W JP2019048352 W JP 2019048352W WO 2020137528 A1 WO2020137528 A1 WO 2020137528A1
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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
- 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
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- 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
- H01L21/02296—Forming insulating materials on a substrate characterised by the treatment performed before or after the formation of the layer
- H01L21/02299—Forming insulating materials on a substrate characterised by the treatment performed before or after the formation of the layer pre-treatment
- H01L21/02301—Forming insulating materials on a substrate characterised by the treatment performed before or after the formation of the layer pre-treatment in-situ cleaning
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
- H01J37/32—Gas-filled discharge tubes
- H01J37/32431—Constructional details of the reactor
- H01J37/32798—Further details of plasma apparatus not provided for in groups H01J37/3244 - H01J37/32788; special provisions for cleaning or maintenance of the apparatus
- H01J37/32853—Hygiene
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B5/00—Cleaning by methods involving the use of air flow or gas flow
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B7/00—Cleaning by methods not provided for in a single other subclass or a single group in this subclass
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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
- C23C16/22—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
- C23C16/305—Sulfides, selenides, or tellurides
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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
- C23C16/22—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
- C23C16/405—Oxides of refractory metals or yttrium
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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
- C23C16/4401—Means for minimising impurities, e.g. dust, moisture or residual gas, in the reaction chamber
- C23C16/4405—Cleaning of reactor or parts inside the reactor by using reactive gases
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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
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
- C23C8/08—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases only one element being applied
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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
- H01L21/02041—Cleaning
- H01L21/02057—Cleaning during device manufacture
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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
- H01L21/02112—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
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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
- H01L21/02227—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a process other than a deposition process
Definitions
- the present invention relates to a deposit removal method and a film formation method.
- semiconductor materials containing elements other than silicon have attracted attention in the field of semiconductors.
- the semiconductor material containing an element other than silicon include a semiconductor material containing a III-V group element such as germanium (Ge) and indium gallium arsenide (InGaAs), and a semiconductor material containing a metal chalcogenide.
- these semiconductor materials have the advantage of higher mobility (mobility) than silicon materials, they may be difficult to deposit or have a high defect density at the interface between the materials. It was
- Patent Document 1 a method of forming a passivation film using a hydrogen sulfide (H 2 S) gas on a substrate such as germanium or molybdenum has been proposed (for example, Patent Document 1). See 1).
- a method for forming a metal chalcogenide a method of forming a molybdenum sulfide layer and a tungsten sulfide layer by treating a molybdenum oxide layer and a tungsten oxide layer with hydrogen sulfide gas has been proposed (for example, see Patent Document 2). ).
- Patent Document 3 discloses a technique for cleaning a substrate using a plasma cleaning device.
- sulfur derived from the sulfur hexafluoride gas used for cleaning the substrate adheres to the substrate, the adhered sulfur is removed by sputtering with argon.
- the technique disclosed in Patent Document 3 since sulfur is physically removed, the removed sulfur is redeposited to another place in the plasma cleaning apparatus or is disposed downstream of the plasma cleaning apparatus. There was a problem of reattachment to the piping.
- the present invention relates to a deposit removing method and a film forming method capable of removing deposits containing sulfur adhering to the inner surface of a chamber or the inner surface of a pipe connected to the chamber without disassembling the chamber.
- the challenge is to provide.
- the fluorine-containing compound gas is at least one selected from the group consisting of fluorine gas, nitrogen trifluoride gas, and fluorinated hydrocarbon gas, and the fluorinated hydrocarbon gas has the following formula (1).
- a deposit removing step of removing deposits containing sulfur, which are attached to at least one of the inner surface of the chamber and the inner surface of the pipe connected to the chamber Equipped with A film forming method, wherein the deposit removing step is performed by the deposit removing method according to any one of [1] to [4].
- the film forming method according to [5] wherein the sulfur-containing compound gas is hydrogen sulfide gas.
- the present invention it is possible to remove the deposit containing sulfur, which is attached to the inner surface of the chamber or the inner surface of the pipe connected to the chamber, without disassembling the chamber.
- the present embodiment shows an example of the present invention, and the present invention is not limited to this embodiment.
- various changes or improvements can be added to the present embodiment, and a mode in which such changes or improvements are added can be included in the present invention.
- the first embodiment of the present invention is an embodiment of a method for removing deposits, which is a deposit containing sulfur attached to at least one of the inner surface of the chamber and the inner surface of the pipe connected to the chamber (hereinafter, simply (Sometimes referred to as “adhesion”) is removed by reacting with a cleaning gas containing a fluorine-containing compound gas.
- a cleaning gas containing a fluorine-containing compound gas is reacting with a cleaning gas containing a fluorine-containing compound gas.
- the fluorine-containing compound gas and the cleaning gas do not contain sulfur atoms.
- the inner surface of the chamber or the pipe connected to the chamber (for example, the cleaning gas supply pipe connected to the upstream side of the chamber or the downstream side of the chamber)
- the deposit containing sulfur may adhere to the inner surface of the exhaust pipe connected to the side. Since the reaction may be adversely affected if the next reaction is carried out with the adhered substances attached, it is preferable to carry out the next reaction after removing the adhered substances.
- the deposit removing method according to the first embodiment is a method in which a cleaning gas is brought into contact with the deposit and sulfur in the deposit is reacted with a fluorine-containing compound gas in the cleaning gas to form a sulfur fluoride gas such as sulfur hexafluoride. Since the adhered matter is removed by generating, it is possible to remove the adhered matter adhered to the inner surface of the chamber and the inner surface of the pipe connected to the chamber without disassembling the chamber. Therefore, the deposit can be easily removed.
- the contact between the cleaning gas and the deposit is preferably carried out under the conditions of a temperature of 20° C. or higher and 800° C. or lower, more preferably 40° C. or higher and 600° C. or lower. If the temperature is 800° C. or lower, the fluorine-containing compound gas in the cleaning gas and the generated sulfur fluoride gas are unlikely to corrode metallic materials such as stainless steel forming the chamber and piping, and The reverse reaction in which the sulfur fluoride gas generated by the reaction between sulfur and the fluorine-containing compound gas in the cleaning gas returns to sulfur is unlikely to occur. On the other hand, if the temperature is 20° C. or higher, the reaction between the sulfur in the deposit and the fluorine-containing compound gas in the cleaning gas is likely to proceed.
- the contact between the cleaning gas and the adhered matter is preferably performed under the absolute pressure of 20 Pa or more and 101 kPa or less, more preferably 60 Pa or more and 90 kPa or less. If the pressure is 101 kPa or less, problems in the chamber and piping are unlikely to occur.
- the chamber is a reaction vessel of a film forming apparatus that reacts a substrate with a passivation gas to form a passivation film on the surface of the substrate, it is premised that the chamber is used under a reduced pressure environment. Is preferably 101 kPa or less.
- the pressure is 20 Pa or more, the reaction between the sulfur in the deposit and the fluorine-containing compound gas in the cleaning gas is likely to proceed.
- the fluorine-containing compound gas is a gas of a compound having a fluorine atom and further does not have a sulfur atom, and examples thereof include fluorine gas (F 2 ), nitrogen trifluoride gas (NF 3 ), and fluorination.
- Hydrocarbon gas may be mentioned.
- the fluorinated hydrocarbon gas include at least one gas selected from compounds represented by the following formulas (1), (2), (3), and (4).
- m in the above formula (1) is an integer of 1 or more and 4 or less
- n in the above formula (2) is an integer of 1 or more and 6 or less
- q in the above formula (3) is 1 or more and 8 or less. It is the following integers
- r in the above formula (4) is an integer of 1 or more and 10 or less.
- Examples of the compound represented by the above formula (1) include tetrafluoromethane (CF 4 ), trifluoromethane (CHF 3 ), difluoromethane (CH 2 F 2 ), and fluoromethane (CH 3 F).
- Examples of the compound represented by the above (2) include hexafluoroethane (C 2 F 6 ), pentafluoroethane (C 2 HF 5 ), tetrafluoroethane (C 2 H 2 F 4 ), trifluoroethane ( C 2 H 3 F 3 ), difluoroethane (C 2 H 4 F 2 ) and fluoroethane (C 2 H 5 F) can be mentioned.
- Examples of the compound represented by the above (3) include octafluoropropane (C 3 F 8 ), heptafluoropropane (C 3 HF 7 ), hexafluoropropane (C 3 H 2 F 6 ), pentafluoropropane ( C 3 H 3 F 5), tetrafluoropropane (C 3 H 4 F 4) , trifluoroacetic propane (C 3 H 5 F 3) , difluoropropane (C 3 H 6 F 2) , fluoropropane (C 3 H 7 F).
- Examples of the compound represented by the above (4) include decafluorobutane (C 4 F 10 ), nonafluorobutane (C 4 HF 9 ), octafluorobutane (C 4 H 2 F 8 ), and heptafluorobutane ( C 4 H 3 F 7), hexafluorobutane (C 4 H 4 F 6) , pentafluorobutane (C 4 H 5 F 5) , tetrafluoro butane (C 4 H 6 F 4) , trifluoroacetic butane (C 4 H 7 F 3), difluoro butane (C 4 H 8 F 2) , perfluorobutane (C 4 H 9 F) and the like.
- decafluorobutane C 4 F 10
- nonafluorobutane C 4 HF 9
- octafluorobutane C 4 H 2 F 8
- heptafluorobutane C 4 H
- the compounds represented by the above formulas (1), (2), (3), and (4) are not limited to the above compounds, and isomers can be included.
- fluorine-containing compound gases fluorine gas, nitrogen trifluoride gas and tetrafluoromethane are preferable, and fluorine gas is more preferable.
- Fluorine gas reacts with sulfur at a temperature of 50° C. or higher under a pressure of 101 kPa. Therefore, when the cleaning gas contains fluorine gas, the cleaning gas and sulfur (adhered substances) are removed at a temperature of 50° C. or higher and 800° C. or lower. Contact is preferred. When the cleaning gas contains fluorine gas, it is preferable to remove the adhering matter while heating the inside of the chamber or the piping in order to efficiently remove the adhering matter.
- the content ratio of the fluorine-containing compound gas in the cleaning gas is not particularly limited as long as it is an amount sufficient to remove sulfur (adhered matter), but is preferably 5% by volume or more, and 20% by volume. More preferably, it is more preferably 90% by volume or more, still more preferably 100% by volume.
- the component other than the fluorine-containing compound gas contained in the cleaning gas is not particularly limited as long as it is a compound gas having no sulfur atom, and examples thereof include an inert gas such as nitrogen gas and argon gas. You can
- the chamber is not particularly limited as long as it is formed of a material having resistance to hydrogen sulfide, but it is preferable that the chamber has a structure capable of reducing the pressure to a predetermined pressure.
- the material include, for example, aluminum whose surface is anodized.
- the pipe connected to the chamber is not particularly limited as long as it is made of a material having resistance to hydrogen sulfide, but preferably has a structure capable of withstanding a predetermined pressure.
- the deposit removal method according to the first embodiment can be preferably applied to a chamber provided as a reaction container in a semiconductor film forming apparatus and a pipe connected to the chamber.
- a second embodiment of the present invention is an embodiment of a film forming method, in which a passivation gas containing a sulfur-containing compound gas is supplied to a chamber in which a substrate is accommodated, and the substrate and the passivation gas are reacted with each other to form a substrate.
- a deposit removing step is performed by the adhering matter removing method of the first embodiment.
- the inner surface of the chamber or the pipe connected to the chamber for example, the supply of the passivation gas or the cleaning gas connected to the upstream side of the chamber.
- the deposit containing sulfur may adhere to the inner surface of the exhaust pipe or the exhaust pipe connected to the downstream side of the chamber.
- the substrate is introduced into the chamber with deposits adhering to the inner surface of the chamber and the inner surface of the pipe, sulfur particles may adhere to the substrate when the chamber is evacuated and replaced with an inert gas. Then, when the sulfur particles adhere to the substrate, the performance of the manufactured semiconductor structure may deteriorate. Further, if the next passivation step is performed while the sulfur particles remain attached to the substrate, there is a possibility that problems such as a film formation rate of the passivation film and deterioration of the film quality may occur. Therefore, it is preferable to perform the next passivation step after removing the deposits.
- a cleaning gas is brought into contact with the deposit, and the sulfur in the deposit is reacted with the fluorine-containing compound gas in the cleaning gas to generate a sulfur fluoride gas such as sulfur hexafluoride. Since the deposits are removed by the generation, it is possible to remove the deposits adhering to the inner surface of the chamber and the inner surface of the pipe connected to the chamber without disassembling the chamber. Therefore, the deposit can be easily removed. Further, according to the film forming method according to the second embodiment, it is possible to suppress the sulfur particles from adhering to the substrate due to the removal of the adhering substances, so that it is possible to manufacture a semiconductor structure having excellent performance. ..
- the deposit removal step it is not always necessary to perform the deposit removal step each time the passivation step is performed, and the deposit removal step is performed each time the passivation step is performed multiple times. Good. If the number of times the deposit removing step is performed with respect to the number of times the passivation step is performed, the utilization efficiency of the film forming apparatus can be improved.
- the type of the passivation gas containing the sulfur-containing compound gas is not particularly limited as long as it is a compound gas containing sulfur, but hydrogen sulfide gas is preferable because it has good passivation performance.
- the content ratio of the sulfur-containing compound gas in the passivation gas is not particularly limited as long as it is an amount sufficient for forming the passivation film, but it is preferably 1% by volume or more, and 2% by volume or more. Is more preferable, 10% by volume or more is further preferable, and 100% by volume is particularly preferable.
- the components other than the sulfur-containing compound gas contained in the passivation gas are not particularly limited, but examples thereof include inert gases such as nitrogen gas and argon gas.
- the type of material forming the substrate is not particularly limited as long as it is a semiconductor material, and examples thereof include materials containing elements such as silicon, germanium, III-V group compounds, molybdenum and tungsten.
- silicon silicon used for forming a semiconductor element is suitable, and examples thereof include amorphous silicon, polysilicon, and single crystal silicon.
- germanium, III-V group compounds, molybdenum, and tungsten those used for forming semiconductor elements are also suitable.
- the pressure in the chamber when forming the passivation film in the passivation step is not particularly limited, but is preferably 1 Pa or more and 101 kPa or less, more preferably 10 Pa or more and 90 kPa or less, and 100 Pa or more and 80 kPa or less. The following is more preferable.
- the temperature of the substrate at the time of reacting the substrate with the passivation gas in the passivation step is not particularly limited, but in order to obtain high in-plane uniformity of the treatment of the surface of the substrate with the passivation gas, it is 20° C. or higher.
- the temperature is preferably 1500°C or lower, more preferably 50°C or higher and 1200°C or lower, and further preferably 100°C or higher and 1000°C or lower.
- the length of the passivation time in the passivation process is not particularly limited, but it is preferably 120 minutes or less in consideration of the efficiency of the semiconductor element manufacturing process.
- the passivation time is the time from supplying the passivation gas to the chamber containing the substrate until exhausting the passivation gas in the chamber with a vacuum pump or the like to finish the treatment of the surface of the substrate with the passivation gas. Point to.
- the film forming method according to the second embodiment can be suitably applied to a semiconductor film forming apparatus that forms a passivation film on the surface of a substrate.
- the structure of the film forming apparatus is not particularly limited, and the positional relationship between the substrate housed in the chamber which is the reaction container and the pipe connected to the chamber is also not particularly limited.
- Example 1 Using the film forming apparatus 1 shown in FIG. 1, a passivation step of forming a passivation film on the surface of the substrate and an adhering matter removing step of removing an adhering matter containing sulfur were repeated.
- the film forming apparatus 1 includes a chamber 10 that performs a passivation process and an adhered substance removing process, and a temperature adjusting device (not shown) that adjusts the temperature inside the chamber 10.
- a stage 11 that supports the sample 20 is provided inside the chamber 10.
- a sample having a silicon oxide film with a thickness of 150 nm formed on a silicon substrate and further having a germanium film with a thickness of 80 nm formed thereon was used.
- a passivation gas supply pipe 12 for supplying a passivation gas containing a sulfur-containing compound gas to the chamber 10 and a cleaning for supplying a cleaning gas containing a fluorine-containing compound gas to the chamber 10.
- the gas supply pipe 13 and the inert gas supply pipe 14 for supplying the inert gas to the chamber 10 are connected via valves 32, 33 and 34, respectively.
- an exhaust pipe 15 for discharging the gas in the chamber 10 to the outside is connected to the chamber 10 on the downstream side thereof, and a vacuum pump 38 is provided on the downstream side of the exhaust pipe 15 via a valve 35. It is connected.
- the pressure inside the chamber 10 is controlled by a pressure controller 37 that controls the valve 35.
- a passivation process was performed using such a film forming apparatus 1.
- the temperature inside the chamber 10 was raised to 800°C.
- the valve 32 was opened, and hydrogen sulfide gas was supplied as a passivation gas into the chamber 10 from the passivation gas supply pipe 12 at a pressure of 101 kPa.
- the flow rate of the passivation gas at this time was 100 sccm, and the pressure in the chamber 10 when forming the passivation film on the surface of the sample 20 was 67 kPa. Note that sccm represents a flow rate (mL/min) at 0° C. and 101.3 kPa.
- the introduction of the passivation gas was carried out for 30 minutes, and after the surface of the sample 20 was sulfided under the condition of the temperature of 800° C. and the pressure of 67 kPa to form the passivation film, the introduction of the passivation gas was stopped. Then, the inside of the chamber 10 was evacuated by the vacuum pump 38, an inert gas was supplied into the chamber 10 through the inert gas supply pipe 14, and the inside of the chamber 10 was replaced with the inert gas. Then, the temperature in the chamber 10 was lowered to room temperature, and the sample 20 having the passivation film formed thereon was taken out of the chamber 10.
- the deposit removing process was performed using the film forming apparatus 1.
- the pressure inside the chamber 10 from which the sample 20 was taken out was reduced to less than 10 Pa
- the temperature inside the chamber 10 was raised to 500°C.
- the valve 33 is opened, and a mixed gas of fluorine gas and nitrogen gas as a cleaning gas from the cleaning gas supply pipe 13 to the inside of the chamber 10 and the exhaust pipe 15 (the concentration of the fluorine gas is 20% by volume, The concentration of nitrogen gas is 80% by volume).
- the flow rate of the cleaning gas at this time was 100 sccm, and the pressure in the chamber 10 at the time of removing the deposit was 67 kPa.
- the introduction of the cleaning gas was stopped. Then, the inside of the chamber 10 was evacuated by the vacuum pump 38, an inert gas was supplied into the chamber 10 through the inert gas supply pipe 14, and the inside of the chamber 10 was replaced with the inert gas.
- a passivation process was performed in the same manner as above, and a passivation film was formed on a new sample 20. Then, the attached matter removing step was performed in the same manner as above. By repeating such an operation, a total of 100 samples 20 having the passivation film formed were manufactured.
- Example 2 In the same manner as in Example 1 except that the temperature in the chamber 10 in the deposit removing step was 350° C. and the pressure was 100 Pa, 100 samples 20 having a passivation film formed were manufactured.
- Example 3 In the same manner as in Example 1 except that the temperature inside the chamber 10 in the deposit removing step was set to 20° C., 100 sheets of the sample 20 on which the passivation film was formed were manufactured.
- Example 4 In the same manner as in Example 1 except that the temperature inside the chamber 10 in the deposit removing step was set to 800° C., 100 samples 20 having a passivation film formed were manufactured.
- Example 5 In the same manner as in Example 1 except that the pressure in the chamber 10 in the deposit removing step was set to 20 Pa, 100 samples 20 having a passivation film formed were manufactured.
- Example 6 In the same manner as in Example 1 except that the pressure in the chamber 10 in the deposit removing step was set to 101 kPa, 100 samples 20 having a passivation film formed were manufactured. (Example 7) Except that the cleaning gas supplied from the cleaning gas supply pipe 13 in the deposit removing step is nitrogen trifluoride gas (not a mixed gas with nitrogen gas, but 100% by volume nitrogen trifluoride gas). In the same manner as in Example 1, 100 samples 20 each having a passivation film formed were manufactured.
- Example 8 The same as Example 1 except that the cleaning gas supplied from the cleaning gas supply pipe 13 in the deposit removing step was tetrafluoromethane gas (100% by volume of tetrafluoromethane gas, not a mixed gas with nitrogen gas). Then, 100 samples 20 having a passivation film formed were manufactured.
- Comparative Example 1 100 samples 20 each having a passivation film formed were manufactured in the same manner as in Example 1 except that only the passivation step was repeated without performing the deposit removal step.
- the number of sulfur particles adhering to the surface of the sample 20 is measured every time the passivation process of each of the first to 100th samples 20 is completed. did.
- the number of particles was measured using a wafer inspection device Surfscan (registered trademark) 6240 manufactured by KLA Tencor. The measurement results are shown in Table 1.
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Abstract
Description
これらの半導体材料は、シリコン材料と比較してモビリティ(移動度)が高いというメリットを有しているものの、成膜が困難である場合や、材料間の界面の欠陥密度が高くなる場合があった。
チャンバーの内面やチャンバーの下流側に配された配管の内面に硫黄を含有する付着物が付着した状態で、ウエハ等の基板をチャンバー内に導入すると、チャンバー内を真空にして不活性ガスで置換した際に硫黄のパーティクルがウエハ等の基板に付着するおそれがあった。そして、硫黄のパーティクルが基板に付着すると、製造された半導体構造の性能が低下するおそれがあった。
しかしながら、特許文献3に開示の技術では、硫黄を物理的に除去しているため、除去された硫黄がプラズマ洗浄装置内の別の場所に再付着したり、プラズマ洗浄装置の下流側に配された配管に再付着したりするという問題があった。
本発明は、チャンバーの内面又はチャンバーに接続された配管の内面に付着している、硫黄を含有する付着物を、チャンバーを解体することなく除去することが可能な付着物除去方法及び成膜方法を提供することを課題とする。
[1] チャンバーの内面及び前記チャンバーに接続された配管の内面の少なくとも一方に付着している、硫黄を含有する付着物を、フッ素含有化合物ガスを含有するクリーニングガスと反応させることにより除去する付着物除去方法。
[3] 前記フッ素含有化合物ガスが、フッ素ガス、三フッ化窒素ガス、及びフッ素化炭化水素ガスからなる群より選ばれる少なくとも1種であり、前記フッ素化炭化水素ガスが、下記式(1)、(2)、(3)、及び(4)で表される化合物のうちの少なくとも1種のガスである[1]又は[2]に記載の付着物除去方法。
CH4-mFm ・・・(1)
C2H6-nFn ・・・(2)
C3H8-qFq ・・・(3)
C4H10-rFr ・・・(4)
ただし、上記式(1)中のmは1以上4以下の整数であり、上記式(2)中のnは1以上6以下の整数であり、上記式(3)中のqは1以上8以下の整数であり、上記式(4)中のrは1以上10以下の整数である。
[4] 前記フッ素含有化合物ガスがフッ素ガスである[1]又は[2]に記載の付着物除去方法。
前記パッシベーション工程を行った後に、前記チャンバーの内面及び前記チャンバーに接続された配管の内面の少なくとも一方に付着している、硫黄を含有する付着物を除去する付着物除去工程と、
を備え、
前記付着物除去工程を、[1]~[4]のいずれか一項に記載の付着物除去方法によって行う成膜方法。
[6] 前記硫黄含有化合物ガスが硫化水素ガスである[5]に記載の成膜方法。
本発明の第一実施形態は、付着物除去方法の実施形態であり、チャンバーの内面及びチャンバーに接続された配管の内面の少なくとも一方に付着している、硫黄を含有する付着物(以下、単に「付着物」と記すこともある)を、フッ素含有化合物ガスを含有するクリーニングガスと反応させることにより除去する方法である。なお、フッ素含有化合物ガスとクリーニングガスは硫黄原子を含有しない。
C2H6-nFn ・・・(2)
C3H8-qFq ・・・(3)
C4H10-rFr ・・・(4)
ただし、上記式(1)中のmは1以上4以下の整数であり、上記式(2)中のnは1以上6以下の整数であり、上記式(3)中のqは1以上8以下の整数であり、上記式(4)中のrは1以上10以下の整数である。
これらのフッ素含有化合物ガスの中では、フッ素ガス、三フッ化窒素ガス、及びテトラフルオロメタンが好ましく、フッ素ガスがより好ましい。
本発明の第二実施形態は、成膜方法の実施形態であり、硫黄含有化合物ガスを含有するパッシベーションガスを、基板が収容されたチャンバーに供給し、基板とパッシベーションガスとを反応させて、基板の表面にパッシベーション膜を成膜するパッシベーション工程と、パッシベーション工程を行った後に、チャンバーの内面及びチャンバーに接続された配管の内面の少なくとも一方に付着している、硫黄を含有する付着物を除去する付着物除去工程と、を備える方法である。そして、この付着物除去工程は、第一実施形態の付着物除去方法によって行われるものである。
パッシベーションガスにおける硫黄含有化合物ガスの含有比率は、パッシベーション膜の成膜に十分な量であれば特に限定されるものではないが、1体積%以上であることが好ましく、2体積%以上であることがより好ましく、10体積%以上であることがさらに好ましく、100体積%であることが特に好ましい。パッシベーションガスに含有される硫黄含有化合物ガス以外の成分は、特に限定されるものではないが、例えば、窒素ガス、アルゴンガス等の不活性ガスを挙げることができる。
(実施例1)
図1に示す成膜装置1を用いて、基板の表面にパッシベーション膜を成膜するパッシベーション工程と、硫黄を含有する付着物を除去する付着物除去工程とを繰り返し行った。成膜装置1は、パッシベーション工程や付着物除去工程を行うチャンバー10と、チャンバー10の内部の温度を調整する温度調整装置(図示せず)と、を有する。チャンバー10の内部には、試料20を支持するステージ11が備えられている。試料20としては、シリコン基板上に厚さ150nmのシリコン酸化膜が形成され、さらにその上に厚さ80nmのゲルマニウム膜が形成されたものを使用した。
付着物除去工程におけるチャンバー10内の温度を350℃、圧力を100Paとした点以外は、実施例1と同様にして、パッシベーション膜を成膜した試料20を100枚製造した。
(実施例3)
付着物除去工程におけるチャンバー10内の温度を20℃とした点以外は、実施例1と同様にして、パッシベーション膜を成膜した試料20を100枚製造した。
付着物除去工程におけるチャンバー10内の温度を800℃とした点以外は、実施例1と同様にして、パッシベーション膜を成膜した試料20を100枚製造した。
(実施例5)
付着物除去工程におけるチャンバー10内の圧力を20Paとした点以外は、実施例1と同様にして、パッシベーション膜を成膜した試料20を100枚製造した。
付着物除去工程におけるチャンバー10内の圧力を101kPaとした点以外は、実施例1と同様にして、パッシベーション膜を成膜した試料20を100枚製造した。
(実施例7)
付着物除去工程におけるクリーニングガス給気用配管13から供給するクリーニングガスを三フッ化窒素ガス(窒素ガスとの混合ガスではなく、100体積%の三フッ化窒素ガス)とした点以外は、実施例1と同様にして、パッシベーション膜を成膜した試料20を100枚製造した。
付着物除去工程におけるクリーニングガス給気用配管13から供給するクリーニングガスをテトラフルオロメタンガス(窒素ガスとの混合ガスではなく、100体積%のテトラフルオロメタンガス)とした点以外は、実施例1と同様にして、パッシベーション膜を成膜した試料20を100枚製造した。
付着物除去工程を行わずパッシベーション工程のみを繰り返し行う点以外は、実施例1と同様にして、パッシベーション膜を成膜した試料20を100枚製造した。
実施例1~8及び比較例1の試料20について、1枚目から100枚目の各試料20のパッシベーション工程が終了するたびに、試料20の表面に付着している硫黄のパーティクルの個数を測定した。パーティクルの個数の測定は、KLAテンコール社製のウエハ検査装置サーフスキャン(登録商標)6240を用いて行った。測定結果を表1に示す。
このように、付着物除去工程を行うことにより、チャンバーを解体洗浄することなく、付着するパーティクルの個数を低く保ったままパッシベーション工程を繰り返し行うことができることが示された。
10・・・チャンバー
11・・・ステージ
12・・・パッシベーションガス給気用配管
13・・・クリーニングガス給気用配管
14・・・不活性ガス給気用配管
15・・・排気用配管
20・・・試料
Claims (6)
- チャンバーの内面及び前記チャンバーに接続された配管の内面の少なくとも一方に付着している、硫黄を含有する付着物を、フッ素含有化合物ガスを含有するクリーニングガスと反応させることにより除去する付着物除去方法。
- 温度20℃以上800℃以下、圧力20Pa以上101kPa以下の条件下で、前記クリーニングガスを前記付着物に接触させる請求項1に記載の付着物除去方法。
- 前記フッ素含有化合物ガスが、フッ素ガス、三フッ化窒素ガス、及びフッ素化炭化水素ガスからなる群より選ばれる少なくとも1種であり、前記フッ素化炭化水素ガスが、下記式(1)、(2)、(3)、及び(4)で表される化合物のうちの少なくとも1種のガスである請求項1又は請求項2に記載の付着物除去方法。
CH4-mFm ・・・(1)
C2H6-nFn ・・・(2)
C3H8-qFq ・・・(3)
C4H10-rFr ・・・(4)
ただし、上記式(1)中のmは1以上4以下の整数であり、上記式(2)中のnは1以上6以下の整数であり、上記式(3)中のqは1以上8以下の整数であり、上記式(4)中のrは1以上10以下の整数である。 - 前記フッ素含有化合物ガスがフッ素ガスである請求項1又は請求項2に記載の付着物除去方法。
- 硫黄含有化合物ガスを含有するパッシベーションガスを、基板が収容されたチャンバーに供給し、前記基板と前記パッシベーションガスとを反応させて、前記基板の表面にパッシベーション膜を成膜するパッシベーション工程と、
前記パッシベーション工程を行った後に、前記チャンバーの内面及び前記チャンバーに接続された配管の内面の少なくとも一方に付着している、硫黄を含有する付着物を除去する付着物除去工程と、
を備え、
前記付着物除去工程を、請求項1~4のいずれか一項に記載の付着物除去方法によって行う成膜方法。 - 前記硫黄含有化合物ガスが硫化水素ガスである請求項5に記載の成膜方法。
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