WO2011033917A1 - 成膜方法および記憶媒体 - Google Patents

成膜方法および記憶媒体 Download PDF

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WO2011033917A1
WO2011033917A1 PCT/JP2010/064573 JP2010064573W WO2011033917A1 WO 2011033917 A1 WO2011033917 A1 WO 2011033917A1 JP 2010064573 W JP2010064573 W JP 2010064573W WO 2011033917 A1 WO2011033917 A1 WO 2011033917A1
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Prior art keywords
film forming
film
forming method
reducing agent
substrate
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PCT/JP2010/064573
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English (en)
French (fr)
Japanese (ja)
Inventor
小島　康彦
秀司 東雲
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Tokyo Electron Ltd
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Tokyo Electron Ltd
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Priority to US13/054,361 priority Critical patent/US20120164328A1/en
Application filed by Tokyo Electron Ltd filed Critical Tokyo Electron Ltd
Priority to KR1020107026851A priority patent/KR101362176B1/ko
Publication of WO2011033917A1 publication Critical patent/WO2011033917A1/ja
Anticipated expiration legal-status Critical
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    • 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
    • C23C16/06—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 metallic material
    • C23C16/18—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 metallic material from metallo-organic compounds
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    • 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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    • 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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    • 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
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    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
    • C23C18/1601—Process or apparatus
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    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
    • C23C18/1601—Process or apparatus
    • C23C18/1633—Process of electroless plating
    • C23C18/1646—Characteristics of the product obtained
    • C23C18/165—Multilayered product
    • C23C18/1653—Two or more layers with at least one layer obtained by electroless plating and one layer obtained by electroplating
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    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
    • C23C18/1601—Process or apparatus
    • C23C18/1633—Process of electroless plating
    • C23C18/1655—Process features
    • C23C18/1658—Process features with two steps starting with metal deposition followed by addition of reducing agent
    • 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
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
    • C23C18/1601—Process or apparatus
    • C23C18/1633—Process of electroless plating
    • C23C18/1655—Process features
    • C23C18/166—Process features with two steps starting with addition of reducing agent followed by metal deposition
    • 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
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
    • C23C18/1601—Process or apparatus
    • C23C18/1633—Process of electroless plating
    • C23C18/1675—Process conditions
    • C23C18/1678—Heating of the substrate
    • 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
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
    • C23C18/1601—Process or apparatus
    • C23C18/1633—Process of electroless plating
    • C23C18/1689—After-treatment
    • C23C18/1692—Heat-treatment
    • C23C18/1696—Control of atmosphere
    • C—CHEMISTRY; METALLURGY
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    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
    • C23C18/31—Coating with metals
    • C23C18/32—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
    • C23C18/34—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents
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    • 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
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    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/02—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings only including layers of metallic material
    • C23C28/023—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings only including layers of metallic material only coatings of metal elements only
    • 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
    • H01L21/02365—Forming inorganic semiconducting materials on a substrate
    • H01L21/02612—Formation types
    • H01L21/02617—Deposition types
    • H01L21/0262—Reduction or decomposition of gaseous compounds, e.g. CVD
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
    • H01L21/28—Manufacture of electrodes on semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/268
    • H01L21/283—Deposition of conductive or insulating materials for electrodes conducting electric current
    • H01L21/285—Deposition of conductive or insulating materials for electrodes conducting electric current from a gas or vapour, e.g. condensation
    • H01L21/28506—Deposition of conductive or insulating materials for electrodes conducting electric current from a gas or vapour, e.g. condensation of conductive layers
    • H01L21/28512—Deposition of conductive or insulating materials for electrodes conducting electric current from a gas or vapour, e.g. condensation of conductive layers on semiconductor bodies comprising elements of Group IV of the Periodic Table
    • H01L21/28556—Deposition of conductive or insulating materials for electrodes conducting electric current from a gas or vapour, e.g. condensation of conductive layers on semiconductor bodies comprising elements of Group IV of the Periodic Table by chemical means, e.g. CVD, LPCVD, PECVD, laser CVD
    • H01L21/28562—Selective deposition
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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
    • H01L21/70—Manufacture or treatment of devices consisting of a plurality of solid state components formed in or on a common substrate or of parts thereof; Manufacture of integrated circuit devices or of parts thereof
    • H01L21/71—Manufacture of specific parts of devices defined in group H01L21/70
    • H01L21/768—Applying interconnections to be used for carrying current between separate components within a device comprising conductors and dielectrics
    • H01L21/76838—Applying interconnections to be used for carrying current between separate components within a device comprising conductors and dielectrics characterised by the formation and the after-treatment of the conductors
    • H01L21/76841—Barrier, adhesion or liner layers
    • H01L21/76843—Barrier, adhesion or liner layers formed in openings in a dielectric

Definitions

  • the present invention relates to a film forming method for forming a Co film or the like by a CVD method and a storage medium.
  • Electroplating is used for the Cu wiring, and as a seed of the Cu wiring by electrolytic plating, a change from the conventional Cu to Co is being studied from the viewpoint of improving the embedding property.
  • CoSi x or NiSi x that is silicided after a Co film or Ni film is formed is being used for contact with Si to the source / drain electrode and gate electrode in the MOS type semiconductor.
  • PVD physical vapor deposition
  • a Co film or Ni film formation method a Co film or Ni film is formed on a substrate by a thermal decomposition reaction of a source gas containing Co or Ni or a reduction reaction of the source gas with a reducing gas.
  • Chemical vapor deposition (CVD) methods are being used.
  • the Co film or Ni film formed by such a CVD method has good step coverage (step coverage) and is excellent in film formability in a long and narrow pattern. For this reason, the Co film or Ni film formed by the CVD method has high followability to a fine pattern and is suitable as a seed layer or contact layer for Cu plating.
  • CVD using cobalt amidinate and H 2 has low reactivity, and impurities in the film tend to remain, resulting in poor film quality. Further, when high-temperature film formation is performed in order to solve the problem of low reactivity, deterioration of surface properties due to Co aggregation becomes a problem. In addition, in CVD using cobalt amidinate and NH 3 , Co nitride is formed, which causes a problem that the film has high resistance.
  • the Ni film may also be formed by a CVD method using nickel amidinate and H 2 or NH 3 as a reducing agent, but the same problem occurs.
  • an object of the present invention is to provide a film forming method capable of forming a Co film having a good surface condition and film quality at a low temperature by using cobalt amidinate as a film forming raw material.
  • Another object of the present invention is to provide a film forming method capable of forming a Ni film having a good surface condition and film quality at a low temperature by using nickel amidinate as a film forming raw material.
  • Still another object of the present invention is to provide a storage medium storing a program for executing these film forming methods.
  • the present inventors have studied to achieve the above object. As a result, when cobalt amidinate or nickel amidinate is used as a film forming raw material, a Co film, Ni can be formed at a low film temperature and at a film forming speed applicable to a semiconductor process by using carboxylic acid as a reducing agent. The present inventors have found that a film can be formed and the surface properties and film quality are improved, and the present invention has been completed.
  • a substrate is carried into a processing container, and a film forming raw material containing cobalt amidinate and a reducing agent containing carboxylic acid are in a gas phase state in the processing container. Introducing and forming a Co film on a substrate is provided.
  • a substrate is carried into a processing container, and a film forming raw material containing nickel amidinate and a reducing agent containing carboxylic acid are introduced into the processing container in a gas phase state. Then, a film forming method including forming a Ni film on a substrate is provided.
  • a storage medium that operates on a computer and stores a program for controlling a film forming apparatus, and the program carries a substrate into a processing container at the time of execution. Forming a Co film on the substrate by introducing a film forming raw material containing cobalt amidinate and a reducing agent containing carboxylic acid in a gas phase state into the processing vessel.
  • a storage medium is provided that causes a computer to control the deposition apparatus.
  • a storage medium that operates on a computer and stores a program for controlling a film forming apparatus, and the program carries a substrate into a processing container at the time of execution. And forming a Ni film on the substrate by introducing a film forming raw material containing nickel amidinate and a reducing agent containing carboxylic acid into the processing container in a gas phase state.
  • a storage medium is provided that causes a computer to control the deposition apparatus.
  • FIG. 1 is a schematic cross-sectional view showing an example of a film forming apparatus for performing a film forming method of the present invention. It is a timing chart which shows an example of a film-forming sequence. It is a timing chart which shows the other example of the film-forming sequence.
  • FIG. 1 is a schematic cross section showing an example of a film forming apparatus for carrying out the film forming method of the present invention.
  • the film forming apparatus 100 includes a substantially cylindrical chamber 1 that is airtightly configured, and a susceptor 2 for horizontally supporting a semiconductor wafer W that is a substrate to be processed is provided at the lower center of the chamber. It arrange
  • the susceptor 2 is made of a ceramic such as AlN.
  • a heater 5 is embedded in the susceptor 2, and a heater power source 6 is connected to the heater 5.
  • thermocouple 7 is provided in the vicinity of the upper surface of the susceptor 2, and a signal from the thermocouple 7 is transmitted to the heater controller 8.
  • the heater controller 8 transmits a command to the heater power supply 6 in accordance with a signal from the thermocouple 7, and controls the heating of the heater 5 to control the wafer W to a predetermined temperature.
  • the susceptor 2 is provided with three wafer raising / lowering pins (not shown) so as to be able to project and retract with respect to the surface of the susceptor 2, and protrudes from the surface of the susceptor 2 when the wafer W is transferred. To be.
  • a circular hole 1 b is formed in the top wall 1 a of the chamber 1, and a shower head 10 is fitted so as to protrude into the chamber 1 from there.
  • the shower head 10 is for discharging a film-forming gas supplied from a gas supply mechanism 30 to be described later into the chamber 1, and a first introduction into which a film-forming source gas is introduced is provided above the shower head 10.
  • a passage 11 and a second introduction passage 12 through which a reducing agent is introduced into the chamber 1 are provided.
  • the first introduction path 11 and the second introduction path 12 are provided separately in the shower head 10, and the film forming source gas and the reducing agent are mixed after discharge.
  • a first introduction path 11 is connected to the upper space 13, and a first gas discharge path 15 extends from the space 13 to the bottom surface of the shower head 10.
  • a second introduction path 12 is connected to the lower space 14, and a second gas discharge path 16 extends from the space 14 to the bottom surface of the shower head 10. That is, the shower head 10 discharges the film forming raw material gas and the carboxylic acid gas as the reducing agent independently from the discharge passages 15 and 16.
  • An exhaust chamber 21 protruding downward is provided on the bottom wall of the chamber 1.
  • An exhaust pipe 22 is connected to the side surface of the exhaust chamber 21, and an exhaust device 23 having a vacuum pump, a pressure control valve, and the like is connected to the exhaust pipe 22.
  • an exhaust device 23 having a vacuum pump, a pressure control valve, and the like is connected to the exhaust pipe 22.
  • a loading / unloading port 24 for loading / unloading the wafer W to / from a wafer transfer chamber (not shown) and a gate valve G for opening / closing the loading / unloading port 24 are provided on the side wall of the chamber 1.
  • a heater 26 is provided on the wall portion of the chamber 1 so that the temperature of the inner wall of the chamber 1 can be controlled during the film forming process.
  • the gas supply mechanism 30 has a film forming material tank 31 for storing the film forming material S.
  • the film forming raw material S cobalt amidinate is used when a Co film is formed, and nickel amidinate is used when a Ni film is formed.
  • cobalt amidinate for example, bis (N-tertiarybutyl-N′-ethyl-propionamidinate) cobalt (II) (Co (tBu-Et-Et-amd) 2 ) can be used.
  • nickel amidinate for example, bis (N, N′-di-tert-butyl-acetamidinate) nickel (II) (Ni (tBu-amd) 2 ) can be used.
  • a heater 32 is provided around the film-forming raw material tank 31 so that the film-forming raw materials are heated and liquefied.
  • a carrier gas pipe 33 for supplying, for example, Ar gas as a carrier gas is inserted from the bottom of the film forming material tank 31.
  • the carrier gas pipe 33 is provided with two valves 35 sandwiching the mass flow controller 34 and the mass flow controller 34.
  • a film forming material supply pipe 36 is inserted into the film forming material tank 31 from above, and the other end of the film forming material supply pipe 36 is connected to the first introduction path 11.
  • the film forming raw material heated by the heater 32 to become a liquid is bubbled by the carrier gas supplied from the carrier gas pipe 33, becomes a gas, and passes through the film forming raw material pipe 36 and the first introduction path 11 and showers. Supplied to the head 10.
  • a heater 37 is provided around the film forming raw material supply pipe 36 so that the gaseous film forming raw material is not liquefied.
  • the film forming material supply pipe 36 is provided with a flow rate adjusting valve 38, an opening / closing valve 39 immediately downstream thereof, and an opening / closing valve 40 immediately adjacent to the first introduction path 11.
  • a reducing agent supply pipe 44 that supplies a carboxylic acid gas as a reducing agent is connected to the second introduction path 12 of the shower head 10.
  • a carboxylic acid supply source 46 that supplies carboxylic acid as a reducing agent is connected to the reducing agent supply pipe 44.
  • a valve 45 is interposed in the vicinity of the second introduction path 12 of the reducing agent supply pipe 44.
  • the reducing agent supply pipe 44 is provided with two valves 48 sandwiching the mass flow controller 47 and the mass flow controller 47.
  • a carrier gas supply pipe 44a is branched upstream of the mass flow controller 47 of the reducing agent supply pipe 44, and a carrier gas supply source 41 is connected to the carrier gas pipe 44a.
  • Gas is supplied.
  • Ar gas for example, is supplied and supplied as a carrier gas from the carrier gas supply source 41 through the carrier gas supply pipe 44a, the reducing gas supply pipe 44, and the shower head 10 into the chamber 1.
  • the carboxylic acid as the reducing agent formic acid (HCOOH) and acetic acid (CH 3 COOH) can be preferably used.
  • the film forming apparatus 100 includes a control unit 50, and the control unit 50 controls each component, for example, the heater power supply 6, the exhaust device 23, the mass flow controllers 34 and 47, the flow rate adjustment valve 38, the valves 35, 39, 40, 45, and so on. 48 and the like, temperature control of the susceptor 2 through the heater controller 8 and the like are performed.
  • the control unit 50 includes a process controller 51 including a microprocessor (computer), a user interface 52, and a storage unit 53. Each component of the film forming apparatus 100 is electrically connected to the process controller 51 and controlled.
  • the user interface 52 is connected to the process controller 51, and a keyboard on which an operator inputs commands to manage each component of the film forming apparatus 100, and operating status of each component of the film forming apparatus 100.
  • the storage unit 53 is also connected to the process controller 51, and the storage unit 53 corresponds to a control program for realizing various processes executed by the film forming apparatus 100 under the control of the process controller 51 and processing conditions.
  • a control program for causing each component of the film forming apparatus 100 to execute a predetermined process, that is, a process recipe, various databases, and the like are stored.
  • the processing recipe is stored in a storage medium (not shown) in the storage unit 53.
  • the storage medium may be a fixed medium such as a hard disk or a portable medium such as a CDROM, DVD, or flash memory. Moreover, you may make it transmit a recipe suitably from another apparatus via a dedicated line, for example.
  • a predetermined processing recipe is called from the storage unit 53 by an instruction from the user interface 52 and executed by the process controller 51, so that the film forming apparatus 100 can control the process controller 51. Desired processing is performed.
  • the gate valve G is opened, and the wafer W is introduced into the chamber 1 by a transfer device (not shown) and placed on the susceptor 2.
  • the wafer W has a SiOxCy insulating film (x and y are positive numbers) or an organic insulating film as a base on the surface. Used.
  • a wafer W having a silicon substrate surface serving as a source / drain electrode exposed on the surface or a polysilicon film formed on the surface is used.
  • the inside of the chamber 1 is evacuated by the exhaust device 23 so that the pressure in the chamber 1 is 1.33 to 1333 Pa (10 mTorr to 10 Torr), and the susceptor 2 is heated by the heater 5 so that the temperature of the susceptor 2 (wafer temperature) is 300.
  • the carrier gas supply source 41 the carrier gas supply pipe 44a, the reducing agent supply pipe 44, and the shower head 10.
  • Carrier gas is supplied for stabilization.
  • a flow rate of 100 to 1500 mL / min (sccm) of carrier gas is supplied from the pipe 33 to the film forming material tank 31 heated to, for example, 60 to 120 ° C. by the heater 32.
  • Cobalt amidinate for example, bis (N-tertiarybutyl-N′-ethyl-propionamidinate) cobalt (II) (Co (tBu-Et-Et-amd)) 2
  • gaseous carboxylic acid as a reducing agent is supplied from the carboxylic acid supply source 46 to the reducing agent supply pipe 44 and the shower head 10. Is introduced into the chamber 1 to start the formation of the Co film.
  • Cobalt amidinate has a structural formula such as the following formula (1) and is usually liquid at room temperature. As shown in the formula (1), Co atoms of cobalt amidinate are bonded to four N atoms, and a Co film is obtained by cutting this bond with carboxylic acid as a reducing agent. However, R 1, R 2, R 3, R 4, R 5, R 6 represents a hydrocarbon-based functional group.
  • Co (tBu-Et-Et-amd) 2 which is a specific example of cobalt amidinate, has a liquid vapor pressure of 3990 Pa (30 Torr) or less at 110 ° C.
  • the structural formula of Co (tBu-Et-Et-amd) 2 is shown in the following formula (2).
  • formic acid HCOOH
  • acetic acid CH 3 COOH
  • carboxylic acids these are particularly highly reducible. Of these, formic acid is more preferred.
  • the flow rate of cobalt amidinate in the film forming process under conditions of a raw material container temperature of 80 ° C. and a container pressure of 10 Torr is the same as that of the carrier gas when Co (tBu-Et-Et-amd) 2 is used. In a certain range of 100 to 1500 mL / min (sccm), it is about 2 to 30 mL / min (sccm).
  • the flow rate of the carboxylic acid as the reducing agent is about 1 to 2000 mL / min (sccm).
  • the film forming sequence as shown in FIG. 2, there can be mentioned normal CVD for simultaneously supplying a film forming raw material (in this case, cobalt amidinate) and a carboxylic acid as a reducing agent.
  • a so-called ALD method can be used in which a film forming raw material (cobalt amidinate) and a carboxylic acid as a reducing agent are alternately performed with a purge interposed therebetween. Purge can be performed by supplying a carrier gas. By this ALD method, the film forming temperature can be further lowered.
  • a purge process is performed.
  • the supply of the carrier gas to the film forming raw material tank 31 is stopped and the supply of cobalt amidinate is stopped, and then the vacuum pump of the exhaust device 23 is turned off and the carrier gas is supplied from the carrier gas supply source 41. Is purged into the chamber 1 as a purge gas to purge the chamber 1.
  • the gate valve G is opened, and the wafer W is unloaded through the loading / unloading port 24 by a transfer device (not shown). Thus, a series of steps for one wafer W is completed.
  • carboxylic acid when CVD film formation is performed using carboxylic acid as a reducing agent for cobalt amidinate, which is a film forming raw material, carboxylic acid has a high reducing ability with respect to cobalt amidinate.
  • a Co film can be formed at a practical film formation speed at a low temperature of ° C.
  • carboxylic acids when formic acid (HCOOH) or acetic acid (CH 3 COOH) is used, a particularly high reduction ability can be obtained, and impurities can be formed at a low temperature of 120 to 250 ° C. and at a practical film formation rate. It is possible to form a Co film having a small and good film quality. Further, since the Co film can be formed at such a low temperature and at a practical film formation rate, it is possible to obtain a Co film that is less likely to cause Co aggregation and that has good surface properties.
  • the Co film formed as described above is suitable as a seed film for Cu wiring formed by electrolytic plating. It can also be used as a base film for a CVD-Cu film. Furthermore, when used as a contact layer, after the Co film is formed on the surface of the silicon substrate or the polysilicon film as described above, heat treatment for silicidation is performed in an inert gas atmosphere or a reducing gas atmosphere. Do. The heat treatment temperature at this time is preferably 450 to 800 ° C.
  • the gate valve G is opened, and the wafer W is introduced into the chamber 1 by a transfer device (not shown) and placed on the susceptor 2.
  • a transfer device not shown
  • a wafer W having a silicon substrate surface serving as a source / drain electrode exposed on the surface or a polysilicon film formed on the surface is used.
  • the inside of the chamber 1 is evacuated by the exhaust device 23 so that the pressure in the chamber 1 is 1.33 to 1333 Pa (10 mTorr to 10 Torr), and the susceptor 2 is heated by the heater 5 so that the temperature of the susceptor 2 (wafer temperature) is 300.
  • the carrier gas supply source 41 the carrier gas supply pipe 44a, the reducing agent supply pipe 44, and the shower head 10.
  • Carrier gas is supplied for stabilization.
  • a flow rate of 100 to 1500 mL / min (sccm) of carrier gas is supplied from the pipe 33 to the film forming material tank 31 heated to, for example, 60 to 120 ° C. by the heater 32.
  • vaporized nickel amidinate for example bis (N, N'-di-tert-butylacetoamidinate) nickel (II) (Ni (tBu-amd) 2
  • II bis (N, N'-di-tert-butylacetoamidinate) nickel (II) (Ni (tBu-amd) 2
  • gaseous carboxylic acid as a reducing agent is supplied from the carboxylic acid supply source 46 through the reducing agent supply pipe 44 and the shower head 10. 1 is introduced to start the formation of the Ni film.
  • Nickel amidinate has a structural formula such as the following formula (3), and is usually solid at room temperature and has a melting point of 85 to 90 ° C. As shown in the formula (3), Ni atoms of nickel amidinate are bonded to four N atoms, and a Ni film is obtained by cutting this bond with carboxylic acid as a reducing agent. However, R 7, R 8, R 9, R 10, R 11, R 12 represents a hydrocarbon-based functional group.
  • Ni (tBu-amd) 2 which is a specific example of nickel amidinate, has a melting point of 87 ° C., and the vapor pressure of the liquid at 90 ° C. is 26.6 Pa (200 mTorr) or less.
  • the structural formula of Ni (tBu-amd) 2 is shown in the following formula (4).
  • formic acid HCOOH
  • acetic acid CH 3 COOH
  • carboxylic acids these are particularly highly reducible. Of these, formic acid is more preferred.
  • the flow rate of nickel amidinate in the film forming process under the conditions of a raw material container temperature of 90 ° C. and a container internal pressure of 10 Torr is 100 to 1500 mL which is the above-mentioned carrier gas flow rate when Ni (tBu-amd) 2 is used. In the range of / min (sccm), it is about 2 to 30 mL / min (sccm).
  • the flow rate of the carboxylic acid as the reducing agent is about 10 to 2000 mL / min (sccm).
  • a film forming sequence as shown in FIG. 2 described above, normal CVD for simultaneously supplying a film forming raw material (in this case, nickel amidinate) and a carboxylic acid as a reducing agent can be exemplified.
  • a so-called ALD method can be used in which a film forming raw material (nickel amidinate) and a carboxylic acid as a reducing agent are alternately performed with a purge interposed therebetween. Purge can be performed by supplying a carrier gas. By this ALD method, the film forming temperature can be further lowered.
  • a purge process is performed.
  • the supply of the carrier gas to the film forming raw material tank 31 is stopped and the supply of cobalt amidinate is stopped, and then the vacuum pump of the exhaust device 23 is turned off and the carrier gas is supplied from the carrier gas supply source 41. Is purged into the chamber 1 as a purge gas to purge the chamber 1.
  • the gate valve G is opened, and the wafer W is unloaded through the loading / unloading port 24 by a transfer device (not shown). Thus, a series of steps for one wafer W is completed.
  • carboxylic acid when performing CVD film formation using nickel carboxylic acid as a reducing agent for nickel amidinate as a film forming raw material, carboxylic acid has a high reducing ability with respect to nickel amidinate.
  • the Ni film can be formed at a practical film formation speed at a low temperature of ° C.
  • carboxylic acids when formic acid (HCOOH) or acetic acid (CH 3 COOH) is used, a particularly high reduction ability can be obtained, and impurities can be formed at a low temperature of 120 to 250 ° C. and at a practical film formation rate. It is possible to form a Ni film having a small and good film quality.
  • the Ni film since the Ni film can be formed at such a low temperature and at a practical film formation rate, it is possible to obtain a Ni film that hardly causes aggregation of Ni and has good surface properties.
  • the Ni film formed as described above is suitable as a contact layer.
  • heat treatment for silicidation is performed in an inert gas atmosphere or a reducing gas atmosphere.
  • the heat treatment temperature at this time is preferably 300 to 700 ° C.
  • carboxylic acid is used as a reducing agent for cobalt amidinate or nickel amidinate which is a film forming raw material, but since carboxylic acid has a high reducing ability for cobalt amidinate and nickel amidinate, By the CVD method, it is possible to form a Co film or a Ni film having a good film quality with few impurities at a low temperature and a practical film formation rate. Further, since the film can be formed at such a low temperature and at a practical film formation rate, it is possible to obtain a Co film and a Ni film that are less likely to cause aggregation of Co and Ni and have good surface properties.
  • the present invention can be variously modified without being limited to the above embodiment.
  • Co (tBu-Et-Et-amd) 2 is exemplified as the cobalt amidinate constituting the film forming raw material
  • Ni (tBu-amd) 2 is exemplified as the nickel amidinate.
  • the carboxylic acid constituting the reducing agent is not limited to formic acid and acetic acid, and other carboxylic acids such as propionic acid, butyric acid, and valeric acid can also be used.
  • the supply method of cobalt amidinate and nickel amidinate as film forming raw materials is not necessarily limited to the method of the above embodiment, and various methods can be applied.
  • the film forming apparatus is not limited to the one in the above embodiment, and various apparatuses such as a mechanism provided with a plasma forming mechanism for promoting the decomposition of the film forming source gas can be used.

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