WO2012114856A1 - シリコン窒化膜の成膜方法、有機電子デバイスの製造方法及びシリコン窒化膜の成膜装置 - Google Patents

シリコン窒化膜の成膜方法、有機電子デバイスの製造方法及びシリコン窒化膜の成膜装置 Download PDF

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Publication number
WO2012114856A1
WO2012114856A1 PCT/JP2012/052608 JP2012052608W WO2012114856A1 WO 2012114856 A1 WO2012114856 A1 WO 2012114856A1 JP 2012052608 W JP2012052608 W JP 2012052608W WO 2012114856 A1 WO2012114856 A1 WO 2012114856A1
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Prior art keywords
gas
plasma
silicon nitride
nitride film
processing
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PCT/JP2012/052608
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English (en)
French (fr)
Japanese (ja)
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拓 石川
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東京エレクトロン株式会社
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Priority to KR1020137022207A priority Critical patent/KR101881470B1/ko
Priority to CN2012800105318A priority patent/CN103403847A/zh
Publication of WO2012114856A1 publication Critical patent/WO2012114856A1/ja

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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
    • H01L21/02274—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 in the presence of a plasma [PECVD]
    • 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
    • C23C16/34—Nitrides
    • C23C16/345—Silicon nitride
    • 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
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/14—Metallic material, boron or silicon
    • C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
    • C23C14/165—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon by cathodic sputtering
    • 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
    • C23C16/45563—Gas nozzles
    • C23C16/45565—Shower nozzles
    • 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
    • C23C16/45563—Gas nozzles
    • C23C16/45574—Nozzles for more than one gas
    • 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
    • C23C16/50—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 using electric discharges
    • C23C16/511—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 using electric discharges using microwave discharges
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K50/00—Organic light-emitting devices
    • H10K50/80—Constructional details
    • H10K50/84—Passivation; Containers; Encapsulations
    • H10K50/844—Encapsulations
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K59/00—Integrated devices, or assemblies of multiple devices, comprising at least one organic light-emitting element covered by group H10K50/00
    • H10K59/80—Constructional details
    • H10K59/87—Passivation; Containers; Encapsulations
    • H10K59/871—Self-supporting sealing arrangements
    • H10K59/8722—Peripheral sealing arrangements, e.g. adhesives, sealants
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K59/00—Integrated devices, or assemblies of multiple devices, comprising at least one organic light-emitting element covered by group H10K50/00
    • H10K59/80—Constructional details
    • H10K59/87—Passivation; Containers; Encapsulations
    • H10K59/873—Encapsulations

Definitions

  • the present invention relates to a silicon nitride film forming method, an organic electronic device manufacturing method, and a silicon nitride film forming apparatus.
  • organic EL elements using organic electroluminescence (EL), which is a light-emitting device including an organic material layer, have been developed. Since organic EL elements emit light by themselves, they have advantages such as low power consumption and superior viewing angle as compared with liquid crystal displays (LCDs).
  • LCDs liquid crystal displays
  • the most basic structure of this organic EL element is a sandwich structure in which an anode (anode) layer, a light emitting layer, and a cathode (cathode) layer are formed on a glass substrate.
  • the light emitting layer is weak to moisture and oxygen, and when moisture and oxygen are mixed, the characteristics change and non-light emitting points (dark spots) are generated, which contributes to shortening the lifetime of the organic EL element.
  • an organic element is sealed so that external moisture and oxygen are not transmitted into the device. That is, in the manufacture of an organic electronic device, an anode layer, a light emitting layer, and a cathode layer are sequentially formed on a glass substrate, and a sealing film layer is further formed.
  • a silicon nitride film (SiN film) is used as the sealing film described above.
  • the silicon nitride film is formed by, for example, plasma CVD (Chemical Vapor Deposition). Specifically, for example, a source gas containing silane (SiH 4 ) gas or nitrogen (N 2 ) gas is excited by microwave power to generate plasma, and a silicon nitride film is formed using the generated plasma. . Further, since the organic EL element may be damaged when the temperature of the glass substrate reaches a high temperature of 100 ° C. or higher, the silicon nitride film is formed in a low temperature environment of 100 ° C. or lower (Patent Document 1).
  • the film characteristics of the silicon nitride film may be deteriorated.
  • the step coverage (step coverage) and film quality (eg, the density related to the wet etching rate for hydrofluoric acid) of the silicon nitride film may be low, and the film stress (film stress) of the silicon nitride film May not be appropriate.
  • the present invention has been made in view of such points, and in a low temperature environment where the temperature of the substrate is 100 ° C. or lower, a silicon nitride film is appropriately formed on the substrate, and the film characteristics of the silicon nitride film are improved. The purpose is to let you.
  • a silicon nitride film forming method for forming a silicon nitride film on a substrate accommodated in a processing container.
  • a processing gas containing a silane-based gas, nitrogen (N 2 ) gas and hydrogen (H 2 ) gas is supplied to the substrate, the processing gas is excited to generate plasma, and plasma processing using the plasma is performed to form silicon on the substrate.
  • a nitride film is formed.
  • the film stress of the silicon nitride film can be appropriately controlled. Therefore, according to the present invention, the controllability of the formation of the silicon nitride film formed on the substrate can be improved even in a low temperature environment where the temperature of the substrate in the processing container is 100 ° C. or less, for example. it can.
  • the fact that the controllability of the film characteristics is improved by adding hydrogen gas to the processing gas will be described in detail later.
  • a method for manufacturing an organic electronic device in which an organic element is formed on a substrate, and thereafter, a silane-based gas, a nitrogen gas, and a hydrogen gas are introduced into a processing container containing the substrate.
  • a processing gas is supplied, the processing gas is excited to generate plasma, plasma processing using the plasma is performed, and a silicon nitride film is formed as a sealing film so as to cover the organic element.
  • a silicon nitride film forming apparatus for forming a silicon nitride film on a substrate, a processing container for storing and processing the substrate, and a silane-based material in the processing container.
  • a processing gas supply unit for supplying a processing gas containing gas, nitrogen gas and hydrogen gas; a plasma excitation unit for generating plasma by exciting the processing gas; and a silicon nitride film on the substrate by performing plasma processing using the plasma
  • a control unit for controlling the plasma excitation unit.
  • the present invention it is possible to appropriately form a silicon nitride film on a substrate in a low temperature environment where the temperature of the substrate is 100 ° C. or lower, and to improve the controllability of the film characteristics of the silicon nitride film.
  • 6 is a graph showing the relationship between the supply flow rate of hydrogen gas and the film stress of a silicon nitride film when the plasma film forming method according to the present embodiment is used. 6 is a graph showing the relationship between the microwave power and the film stress of the silicon nitride film when the plasma film forming method according to the present embodiment is used.
  • a silicon nitride film is formed using a processing gas containing silane gas, nitrogen gas and hydrogen gas as in the present embodiment, and a silicon nitride film is formed using a processing gas containing silane gas and ammonia gas as in the prior art. It is explanatory drawing compared with the case where it forms into a film. It is a top view of the source gas supply structure concerning other embodiments. It is sectional drawing of the source gas supply pipe
  • FIG. 1 is an explanatory diagram showing an outline of the configuration of the substrate processing system 1.
  • FIG. 2 is an explanatory view showing a manufacturing process of the organic EL device.
  • a case where an organic EL device is manufactured as an organic electronic device will be described.
  • the cluster type substrate processing system 1 has a transfer chamber 10.
  • the transfer chamber 10 has, for example, a substantially polygonal shape (in the illustrated example, a hexagonal shape) in plan view, and is configured to be able to seal the inside.
  • a load lock chamber 11 Around the transfer chamber 10, a cleaning device 12, a vapor deposition device 13, a sputtering device 14, an etching device 15, and a plasma film forming device 16 are arranged in this order in the clockwise direction in plan view. Has been.
  • an articulated transfer arm 17 capable of bending, stretching and turning is provided inside the transfer chamber 10.
  • a glass substrate as a substrate is transferred to the load lock chamber 11 and the processing apparatuses 12 to 16 by the transfer arm 17.
  • the load lock chamber 11 is a vacuum transfer chamber in which a glass substrate transferred from the atmospheric system is held in a predetermined reduced pressure state in order to transfer the glass substrate to the transfer chamber 10 in a reduced pressure state.
  • the configuration of the plasma film forming apparatus 16 will be described in detail later. Moreover, about the washing
  • an anode (anode) layer 20 is formed on the upper surface of the glass substrate G in advance.
  • the anode layer 20 is made of a transparent conductive material such as, for example, indium tin oxide (ITO: Indium Tin Oxide).
  • ITO Indium Tin Oxide
  • the anode layer 20 is formed on the upper surface of the glass substrate G, for example, by sputtering.
  • the light emitting layer 21 has, for example, a multilayer structure in which a hole transport layer, a non-light emitting layer (electron block layer), a blue light emitting layer, a red light emitting layer, a green light emitting layer, and an electron transport layer are stacked.
  • a cathode (cathode) layer 22 made of, for example, Ag or Al is formed on the light emitting layer 21 in the sputtering apparatus 14.
  • the cathode layer 22 is formed by depositing target atoms on the light emitting layer 21 through a pattern mask by sputtering, for example.
  • the anode layer 20, the light emitting layer 21, and the cathode layer 22 constitute the organic EL element of the present invention, and may be simply referred to as “organic EL element” below.
  • the light emitting layer 21 is dry-etched in the etching apparatus 15 using the cathode layer 22 as a mask.
  • the light emitting layer 21 is patterned into a predetermined pattern.
  • the exposed portion of the organic EL element and the glass substrate G is cleaned to remove a substance adsorbed on the organic EL element, such as an organic substance, so-called precleaning. Also good.
  • precleaning for example, a silylation treatment using a coupling agent may be performed to form an extremely thin adhesion layer (not shown) on the cathode layer 22.
  • the adhesion layer and the organic EL element are firmly adhered, and the adhesion layer and a silicon nitride film 23 described later are firmly adhered.
  • silicon nitride which is a sealing film so as to cover the periphery of the light emitting layer 21 and the cathode layer 22 and the exposed portion of the anode layer 20.
  • a film (SiN film) 23 is formed.
  • the silicon nitride film 23 is formed by, for example, a microwave plasma CVD method as will be described later.
  • the organic EL device A thus manufactured can cause the light emitting layer 21 to emit light by applying a voltage between the anode layer 20 and the cathode layer 22.
  • Such an organic EL device A can be applied to a display device and a surface light emitting element (illumination, light source, etc.), and can be used for various other electronic devices.
  • FIG. 3 is a longitudinal sectional view showing an outline of the configuration of the plasma film forming apparatus 16.
  • the plasma film forming apparatus 16 of the present embodiment is a CVD apparatus that generates plasma using a radial line slot antenna.
  • the plasma film forming apparatus 16 includes, for example, a bottomed cylindrical processing container 30 having an open top surface.
  • the processing container 30 is made of, for example, an aluminum alloy.
  • the processing container 30 is grounded.
  • a mounting table 31 as a mounting unit for mounting a glass substrate G, for example, is provided at a substantially central portion of the bottom of the processing container 30.
  • the mounting table 31 includes, for example, an electrode plate 32, and the electrode plate 32 is connected to a DC power source 33 provided outside the processing container 30.
  • the DC power source 33 can generate electrostatic force on the surface of the mounting table 31 so that the glass substrate G can be electrostatically adsorbed onto the mounting table 31.
  • the electrode plate 32 may be connected to, for example, a bias high-frequency power source (not shown).
  • a dielectric window 41 is provided in the upper opening of the processing container 30 via a sealing material 40 such as an O-ring for ensuring airtightness, for example.
  • the inside of the processing container 30 is closed by the dielectric window 41.
  • a radial line slot antenna 42 is provided as a plasma excitation unit that supplies microwaves for plasma generation.
  • alumina Al 2 O 3
  • the dielectric window 41 is resistant to nitrogen trifluoride (NF 3 ) gas used in dry cleaning.
  • the surface of the alumina of the dielectric window 41 is covered with yttria (Y 2 O 3 ), spinel (MgAl 2 O 4 ), or aluminum nitride (AlN). Also good.
  • the radial line slot antenna 42 includes a substantially cylindrical antenna body 50 having an open bottom surface.
  • a disc-shaped slot plate 51 in which a large number of slots are formed is provided in the opening on the lower surface of the antenna body 50.
  • a dielectric plate 52 made of a low-loss dielectric material is provided on the upper portion of the slot plate 51 in the antenna body 50.
  • a coaxial waveguide 54 communicating with the microwave oscillating device 53 is connected to the upper surface of the antenna body 50.
  • the microwave oscillating device 53 is installed outside the processing container 30 and can oscillate a microwave having a predetermined frequency, for example, 2.45 GHz, with respect to the radial line slot antenna 42.
  • the microwave oscillated from the microwave oscillating device 53 is propagated in the radial line slot antenna 42, compressed by the dielectric plate 52 and shortened in wavelength, and then circularly polarized in the slot plate 51. And radiated from the dielectric window 41 into the processing container 30.
  • a substantially plate-shaped source gas supply structure 60 is provided between the mounting table 31 in the processing container 30 and the radial line slot antenna 42.
  • the source gas supply structure 60 is formed in a circular shape whose outer shape is at least larger than the diameter of the glass substrate G when viewed from the plane.
  • the inside of the processing vessel 30 is partitioned into a plasma generation region R1 on the radial line slot antenna 42 side and a source gas dissociation region R2 on the mounting table 31 side.
  • alumina may be used for the source gas supply structure 60. In such a case, since alumina is a ceramic, it has higher heat resistance and higher strength than a metal material such as aluminum.
  • the source gas supply structure 60 has resistance to nitrogen trifluoride gas used in dry cleaning. Furthermore, in order to improve the resistance to nitrogen trifluoride gas, the alumina surface of the raw material gas supply structure 60 may be coated with yttria, spinel or aluminum nitride.
  • the raw material gas supply structure 60 is constituted by a continuous raw material gas supply pipe 61 arranged in a substantially lattice pattern on the same plane as shown in FIG.
  • the raw material gas supply pipe 61 has a rectangular longitudinal section when viewed from the axial direction.
  • a large number of openings 62 are formed in the gaps between the source gas supply pipes 61.
  • the plasma and radicals generated in the plasma generation region R1 on the upper side of the source gas supply structure 60 can enter the source gas dissociation region R2 on the mounting table 31 side through the opening 62.
  • a large number of source gas supply ports 63 are formed on the lower surface of the source gas supply pipe 61 of the source gas supply structure 60 as shown in FIG. These source gas supply ports 63 are evenly arranged in the surface of the source gas supply structure 60.
  • a gas pipe 65 that communicates with a source gas supply source 64 installed outside the processing container 30 is connected to the source gas supply pipe 61.
  • a source gas supply source 64 for example, silane (SiH 4 ) gas and hydrogen (H 2 ) gas, which are silane-based gases, are individually sealed as source gases.
  • the gas pipe 65 is provided with a valve 66 and a mass flow controller 67.
  • a predetermined flow rate of silane gas and hydrogen gas are respectively introduced from the source gas supply source 64 into the source gas supply pipe 61 through the gas pipe 65. And these silane gas and hydrogen gas are supplied toward each lower raw material gas dissociation area
  • a first plasma excitation gas supply port 70 for supplying a plasma excitation gas serving as a plasma raw material is formed on the inner peripheral surface of the processing vessel 30 covering the outer peripheral surface of the plasma generation region R1.
  • the first plasma excitation gas supply ports 70 are formed at a plurality of locations along the inner peripheral surface of the processing container 30.
  • the first plasma excitation gas supply port 70 penetrates, for example, a side wall portion of the processing container 30 and communicates with a first plasma excitation gas supply source 71 installed outside the processing container 30.
  • a working gas supply pipe 72 is connected.
  • the first plasma excitation gas supply pipe 72 is provided with a valve 73 and a mass flow controller 74.
  • a plasma excitation gas having a predetermined flow rate can be supplied from the side into the plasma generation region R1 in the processing container 30.
  • argon (Ar) gas for example, is sealed in the first plasma excitation gas supply source 71 as the plasma excitation gas.
  • a substantially flat plasma excitation gas supply structure 80 having a configuration similar to that of the source gas supply structure 60 is laminated and disposed on the upper surface of the source gas supply structure 60.
  • the plasma excitation gas supply structure 80 includes second plasma excitation gas supply tubes 81 arranged in a lattice pattern.
  • alumina may be used for the plasma excitation gas supply structure 80. Even in such a case, since alumina is a ceramic as described above, it has higher heat resistance and higher strength than a metal material such as aluminum. Moreover, since the plasma produced
  • a dense film can be generated by sufficient ion irradiation to the film on the glass substrate.
  • the plasma excitation gas supply structure 80 is resistant to nitrogen trifluoride gas used in dry cleaning. Furthermore, in order to improve resistance to nitrogen trifluoride gas, the surface of the alumina of the plasma excitation gas supply structure 80 may be coated with yttria or spinel.
  • a plurality of second plasma excitation gas supply ports 82 are formed on the upper surface of the second plasma excitation gas supply pipe 81 as shown in FIG.
  • the plurality of second plasma excitation gas supply ports 82 are evenly arranged in the surface of the plasma excitation gas supply structure 80.
  • this plasma excitation gas is, for example, argon gas.
  • nitrogen (N 2 ) gas that is a source gas is also supplied from the plasma excitation gas supply structure 80 to the plasma generation region R1.
  • An opening 83 is formed in the gap between the lattice-shaped second plasma excitation gas supply pipes 81, and the plasma and radicals generated in the plasma generation region R ⁇ b> 1 are exchanged with the plasma excitation gas supply structure 80. It can enter the lower source gas dissociation region R2 through the source gas supply structure 60.
  • a gas pipe 85 communicating with a second plasma excitation gas supply source 84 installed outside the processing vessel 30 is connected to the second plasma excitation gas supply pipe 81.
  • the second plasma excitation gas supply source 84 for example, argon gas, which is a plasma excitation gas, and nitrogen gas, which is a source gas, are individually sealed.
  • the gas pipe 85 is provided with a valve 86 and a mass flow controller 87. With this configuration, it is possible to supply a predetermined flow rate of nitrogen gas and argon gas from the second plasma excitation gas supply port 82 to the plasma generation region R1.
  • the source gas and the plasma excitation gas described above constitute the processing gas of the present invention.
  • the source gas supply structure 60 and the plasma excitation gas supply structure 80 constitute a processing gas supply unit of the present invention.
  • the exhaust port 90 for exhausting the atmosphere in the processing container 30 is provided on both sides of the mounting table 31 at the bottom of the processing container 30.
  • An exhaust pipe 92 communicating with an exhaust device 91 such as a turbo molecular pump is connected to the exhaust port 90.
  • the control unit 100 is provided in the plasma film forming apparatus 16 described above.
  • the control unit 100 is, for example, a computer and has a program storage unit (not shown).
  • the program storage unit stores a program for controlling the film forming process of the silicon nitride film 23 on the glass substrate G in the plasma film forming apparatus 16.
  • the program storage unit controls the supply of the above-described source gas, the supply of plasma excitation gas, the emission of microwaves, the operation of the drive system, and the like, thereby realizing the film forming process in the plasma film forming apparatus 16.
  • a program is also stored.
  • the program is recorded on a computer-readable storage medium such as a computer-readable hard disk (HD), flexible disk (FD), compact disk (CD), magnetic optical desk (MO), or memory card. Or installed in the control unit 100 from the storage medium.
  • HD computer-readable hard disk
  • FD flexible disk
  • CD compact disk
  • MO magnetic optical desk
  • the supply flow rate of the argon gas supplied from the first plasma excitation gas supply port 70 and the argon gas supplied from the second plasma excitation gas supply port 82 are changed.
  • the supply flow rate is adjusted so that the concentration of the argon gas supplied into the plasma generation region R1 is uniform.
  • the exhaust device 91 is operated, and an appropriate air supply is supplied from each of the plasma excitation gas supply ports 70 and 82 in a state where an air flow similar to that in the actual film formation process is formed in the processing container 30.
  • Argon gas set at a flow rate is supplied.
  • the film forming process of the glass substrate G in the plasma film forming apparatus 16 is started.
  • the glass substrate G is carried into the processing container 30 and sucked and held on the mounting table 31.
  • the temperature of the glass substrate G is maintained at 100 ° C. or lower, for example, 50 ° C. to 100 ° C.
  • evacuation of the processing container 30 is started by the exhaust device 91, the pressure in the processing container 30 is reduced to a predetermined pressure, for example, 20 Pa to 60 Pa, and the state is maintained.
  • the temperature of the glass substrate G is not limited to 100 ° C. or lower, and may be any temperature as long as the organic EL device A is not damaged, and depends on the material of the organic EL device A and the like.
  • the pressure in the processing container 30 was lower than 20 Pa, the silicon nitride film 23 may not be properly formed on the glass substrate G. Moreover, when the pressure in the processing container 30 exceeded 60 Pa, it turned out that the reaction between the gas molecules in a gaseous phase increases, and there exists a possibility that a particle
  • argon gas is supplied from the lateral first plasma excitation gas supply port 70 into the plasma generation region R1, and a lower second plasma excitation gas supply port is provided. Nitrogen gas and argon gas are supplied from 82. At this time, the concentration of argon gas in the plasma generation region R1 is uniformly maintained in the plasma generation region R1. Nitrogen gas is supplied at a flow rate of 21 sccm, for example. From the radial line slot antenna 42, microwaves with a power of 2.5 kW to 3.0 kW, for example, are radiated at a frequency of 2.45 GHz toward the plasma generation region R1 immediately below.
  • the argon gas is turned into plasma in the plasma generation region R1, and the nitrogen gas is radicalized (or ionized). At this time, the microwave traveling downward is absorbed by the generated plasma. As a result, high-density plasma is generated in the plasma generation region R1.
  • Plasma and radicals generated in the plasma generation region R1 pass through the plasma excitation gas supply structure 80 and the raw material gas supply structure 60 and enter the lower raw material gas dissociation region R2.
  • Silane gas and hydrogen gas are supplied from the source gas supply ports 63 of the source gas supply structure 60 to the source gas dissociation region R2.
  • the silane gas is supplied at a flow rate of 18 sccm, for example
  • the hydrogen gas is supplied at a flow rate of 64 sccm, for example.
  • the supply flow rate of this hydrogen gas is set according to the film characteristics of the silicon nitride film 23 as will be described later.
  • Silane gas and hydrogen gas are dissociated by plasma entering from above. Then, the silicon nitride film 23 is deposited on the glass substrate G by these radicals and radicals of nitrogen gas supplied from the plasma generation region R1.
  • the silicon nitride film 23 is formed and the silicon nitride film 23 having a predetermined thickness is formed on the glass substrate G, the emission of microwaves and the supply of the processing gas are stopped. Thereafter, the glass substrate G is unloaded from the processing container 30 and a series of plasma film forming processes is completed.
  • FIG. 6 shows how the wet etching rate of the silicon nitride film 23 with respect to hydrofluoric acid changes when the supply flow rate of hydrogen gas in the processing gas is changed using the plasma film forming method of the above embodiment. ing. At this time, the supply flow rate of silane gas was 18 sccm, and the supply flow rate of nitrogen gas was 21 sccm. Moreover, the temperature of the glass substrate G was 100 degreeC during the plasma film-forming process.
  • the wet etching rate of the silicon nitride film 23 is reduced by adding hydrogen gas to the processing gas containing silane gas and nitrogen gas. Accordingly, the density of the silicon nitride film 23 is improved by the hydrogen gas in the processing gas, and the film quality (chemical resistance and density) of the silicon nitride film 23 is improved. Also, the step coverage of the silicon nitride film 23 is improved. Further, it has been found that the refractive index of the silicon nitride film 23 is improved to, for example, 2.0 ⁇ 0.1. Therefore, by controlling the supply flow rate of hydrogen gas, the wet etching rate of the silicon nitride film 23 can be controlled, and the film characteristics of the silicon nitride film 23 can be controlled.
  • FIG. 7 shows how the film stress of the silicon nitride film 23 changes when the supply flow rate of hydrogen gas in the processing gas is varied using the plasma film formation method of the above embodiment.
  • the supply flow rate of silane gas was 18 sccm
  • the supply flow rate of nitrogen gas was 21 sccm.
  • the temperature of the glass substrate G was 100 degreeC during the plasma film-forming process.
  • the film stress of the silicon nitride film 23 changes to the negative side (compression side) by further adding hydrogen gas to the processing gas containing silane gas and nitrogen gas. Therefore, the film stress of the silicon nitride film 23 can be controlled by controlling the supply flow rate of the hydrogen gas.
  • the film characteristics of the silicon nitride film 23 can be changed by changing the flow rate of the hydrogen gas in the processing gas. Therefore, since the silicon nitride film 23 can be appropriately formed as a sealing film in the organic EL device A, the organic EL device A can be appropriately manufactured.
  • the absolute value of the magnitude of stress in the sealing film is preferably small.
  • plasma is generated using microwaves radiated from the radial line slot antenna 42.
  • the processing gas contains silane gas, nitrogen gas, and hydrogen gas, for example, as shown in FIG. 8, the power of the microwave and the film stress of the silicon nitride film 23 are approximately proportional. I found out that there was a relationship. Therefore, according to the present embodiment, the film stress of the silicon nitride film 23 can also be controlled by controlling the microwave power. By optimizing the flow rate of hydrogen gas and optimizing the microwave power, a film having desired film characteristics can be obtained precisely. Specifically, after determining the power of the microwave, the flow rate of hydrogen gas may be optimized.
  • a processing gas containing the above-described silane gas and ammonia (NH 3 ) gas is also used.
  • a metal electrode for example, an aluminum electrode
  • the film is formed in a low temperature environment, unreacted ammonia is trapped in the silicon nitride film. If ammonia is trapped in the silicon nitride film, after performing an environmental test or the like, the ammonia may be degassed from the silicon nitride film, which may deteriorate the organic EL device.
  • nitrogen gas is used instead of ammonia gas. Therefore, the above-described corrosion of the underlying metal electrode and the deterioration of the organic EL device can be prevented.
  • the film characteristics of the silicon nitride film formed as shown in FIG. 9 are improved. Can do. That is, the film quality (density) of the silicon nitride film in the step portion can be improved.
  • 9 shows the state of the silicon nitride film when a processing gas containing silane gas and ammonia gas is used, and the lower stage shows the silicon nitride film when a processing gas containing silane gas, nitrogen gas and hydrogen gas is used. It shows a state. Further, the left column in FIG. 9 shows the state of the silicon nitride film immediately after the film formation, and the right column shows the state of the silicon nitride film after performing the wet etching with buffered hydrofluoric acid (BHF) for 120 seconds.
  • BHF buffered hydrofluoric acid
  • the silane gas and the hydrogen gas are supplied from the source gas supply structure 60 and the nitrogen gas and the argon gas are supplied from the plasma excitation gas supply structure 80.
  • the gas may be supplied from the plasma excitation gas supply structure 80.
  • the hydrogen gas may be supplied from both the source gas supply structure 60 and the plasma excitation gas supply structure 80.
  • the film characteristics of the silicon nitride film 23 can be controlled by controlling the supply flow rate of the hydrogen gas as described above.
  • the refractive index of the silicon nitride film 23 is about 2.0. I found out that Further, it was found that the refractive index is preferably 2.0 ⁇ 0.1 from the viewpoint of the barrier property (sealing property) of the silicon nitride film 23.
  • the ratio of the nitrogen gas supply flow rate to the silane gas supply flow rate is preferably set to 1 to 1.5 in the plasma film forming apparatus 16.
  • the ratio of the nitrogen gas supply flow rate to the silane gas supply flow rate is generally 10 to 50. Since a normal plasma CVD apparatus requires a large amount of nitrogen in this manner, the flow rate of silane gas is increased to increase the film formation rate, and at the same time, a nitrogen flow rate corresponding to the increase is required, which limits the exhaust system.
  • the plasma film-forming apparatus 16 of this Embodiment has an extremely excellent effect compared with a normal plasma CVD apparatus.
  • the film stress of the silicon nitride film 23 can be controlled within the range of the refractive index of 2.0 ⁇ 0.1. Specifically, the film stress can be brought close to zero. Further, this film stress can be controlled by adjusting the microwave power from the radial line slot antenna 42 and the supply flow rate of hydrogen gas.
  • the supply flow rate of nitrogen gas in the plasma film forming apparatus 16 can be reduced compared to a normal plasma CVD apparatus because the supplied nitrogen gas is easily activated and the degree of dissociation is increased. Because it can. That is, when the nitrogen gas is supplied from the plasma excitation gas supply structure 80, the second plasma excitation of the plasma excitation gas supply structure 80 is achieved by being sufficiently close to the dielectric window 41 where plasma is generated. The nitrogen gas released to the plasma generation region R1 in the processing vessel 30 in a relatively high pressure state from the gas supply port 82 is easily ionized to generate a large amount of active nitrogen radicals and the like.
  • the plasma excitation gas supply structure 80 is disposed at a position within 30 mm from the radial line slot antenna 42 (strictly, the dielectric window 41).
  • the plasma excitation gas supply structure 80 when the plasma excitation gas supply structure 80 is disposed at such a position, the plasma excitation gas supply structure 80 itself is disposed in the plasma generation region R1. For this reason, the dissociation degree of nitrogen gas can be raised.
  • the supply of the source gas may be performed simultaneously with the generation of the plasma or before the plasma generation. That is, first, silane gas and hydrogen gas (or only silane gas) are supplied from the source gas supply structure 60. At the same time as or after supplying the silane gas and hydrogen gas, argon gas and nitrogen gas (and hydrogen gas) are supplied from the plasma excitation gas supply structure 80, and microwaves are radiated from the radial line slot antenna 42. Then, plasma is generated in the plasma generation region R1.
  • a cathode layer 22 containing a metal element is formed on the glass substrate G on which the silicon nitride film 23 is formed.
  • the cathode layer 22 may be peeled off from the light emitting layer 21 and the organic EL element A may be damaged.
  • plasma is generated at the same time as or after the supply of the silane gas and the hydrogen gas, so that the formation of the silicon nitride film 23 is started simultaneously with the generation of the plasma. Therefore, the surface of the cathode layer 22 is protected, and the organic EL device A can be appropriately manufactured without exposing the organic EL device A to plasma.
  • the source gas supply port 63 is formed downward from the source gas supply structure 60, and the second plasma excitation gas supply port 82 is upward from the plasma excitation gas supply structure 80.
  • the source gas supply port 63 and the second plasma excitation gas supply port 82 are in the horizontal direction or in an oblique direction other than the vertically downward direction, and more preferably in the direction of 45 degrees obliquely from the horizontal direction. It may be formed toward.
  • the source gas supply structure 60 is formed with a plurality of source gas supply pipes 61 extending in parallel with each other.
  • the source gas supply pipes 61 are arranged at equal intervals in the source gas supply structure 60.
  • source gas supply ports 63 for supplying the source gas in the horizontal direction are formed as shown in FIG.
  • the source gas supply ports 63 are arranged at equal intervals in the source gas supply pipe 61 as shown in FIG.
  • Adjacent source gas supply ports 63 are formed in directions opposite to each other in the horizontal direction.
  • the plasma excitation gas supply structure 80 may also have the same configuration as the source gas supply structure 60.
  • the source gas supply structure 61 and the source gas supply pipe 61 of the source gas supply structure 60 and the second plasma excitation gas supply pipe 81 of the plasma excitation gas supply structure 80 are substantially lattice-shaped. 60 and a gas supply structure 80 for plasma excitation are arranged.
  • the source gas supplied from the source gas supply port 63 is mainly deposited on the source gas supply port 63 as silicon nitride, the deposited silicon nitride is removed by dry cleaning during maintenance.
  • the source gas supply port 63 is formed downward, it is difficult for plasma to enter the source gas supply port 63, so that the silicon nitride deposited in the source gas supply port 63 reaches the inside. It may not be completely removed.
  • plasma generated during dry cleaning enters the inside of the source gas supply port 63.
  • silicon nitride can be completely removed up to the inside of the source gas supply port 63. Therefore, after maintenance, the source gas can be appropriately supplied from the source gas supply port 63, and the silicon nitride film 23 can be formed more appropriately.
  • the source gas supply structure 61 so that the source gas supply pipe 61 of the source gas supply structure 60 and the second plasma excitation gas supply pipe 81 of the plasma excitation gas supply structure 80 are substantially lattice-shaped. 60 and a gas supply structure 80 for plasma excitation are arranged. Therefore, it is easier to manufacture the source gas supply structure 60 and the plasma excitation gas supply structure 80 than to make each source gas supply structure 60 and the plasma excitation gas supply structure 80 itself into a substantially lattice shape. Can do. Further, it is possible to easily pass the plasma generated in the plasma generation region R1.
  • the source gas supply port 63 may be formed so that its inner diameter increases in a tapered shape from the inside to the outside as shown in FIG. In such a case, plasma is more likely to enter the source gas supply port 63 during dry cleaning. Therefore, silicon nitride deposited on the source gas supply port 63 can be more reliably removed.
  • the second plasma excitation gas supply port 82 may be formed so that its inner diameter increases in a tapered shape from the inside to the outside.
  • the silane gas is used as the silane gas.
  • the silane gas is not limited to the silane gas.
  • disilane (Si 2 H 6 ) gas it has been found that, for example, when disilane (Si 2 H 6 ) gas is used, the step coverage of the silicon nitride film 23 is further improved as compared with the case where silane gas is used.
  • the plasma is generated by the microwave from the radial line slot antenna 42.
  • the generation of the plasma is not limited to the present embodiment.
  • the plasma for example, CCP (capacitively coupled plasma), ICP (inductively coupled plasma), ECRP (electron cyclotron resonance plasma), HWP (helicon wave excited plasma) or the like may be used.
  • CCP capacively coupled plasma
  • ICP inductively coupled plasma
  • ECRP electrotron cyclotron resonance plasma
  • HWP helicon wave excited plasma
  • the silicon nitride film 23 is formed in a low temperature environment where the temperature of the glass substrate G is 100 ° C. or lower, it is preferable to use high-density plasma.
  • this invention manufactures another organic electronic device. It can also be applied to For example, also when manufacturing an organic transistor, an organic solar cell, organic FET (Field Effect Transistor) etc. as an organic electronic device, the film-forming method of the silicon nitride film of this invention is applicable. Furthermore, the present invention can be widely applied to the case where a silicon nitride film is formed on a substrate in a low temperature environment where the temperature of the substrate is 100 ° C. or lower, besides the manufacture of such an organic electronic device.

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JP6613196B2 (ja) * 2016-03-31 2019-11-27 株式会社Ｊｏｌｅｄ 有機ｅｌ表示パネル
JP6742165B2 (ja) * 2016-06-14 2020-08-19 東京エレクトロン株式会社 窒化珪素膜の処理方法および窒化珪素膜の形成方法
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