US20110268983A1 - Film-forming treatment jig, plasma cvd apparatus, metal plate and osmium film forming method - Google Patents

Film-forming treatment jig, plasma cvd apparatus, metal plate and osmium film forming method Download PDF

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US20110268983A1
US20110268983A1 US12/808,894 US80889408A US2011268983A1 US 20110268983 A1 US20110268983 A1 US 20110268983A1 US 80889408 A US80889408 A US 80889408A US 2011268983 A1 US2011268983 A1 US 2011268983A1
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electrode
film
plate
chamber
hole
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Takeshi Shirato
Yuuji Honda
Hiroshi Sato
Masamichi Osawa
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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
    • C23C16/04—Coating on selected surface areas, e.g. using masks
    • C23C16/045—Coating cavities or hollow spaces, e.g. interior of tubes; Infiltration of porous substrates
    • 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
    • C23C16/505—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 radio frequency discharges
    • 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
    • C23C16/06—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
    • 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
    • C23C16/45587—Mechanical means for changing the gas flow
    • C23C16/45591—Fixed means, e.g. wings, baffles
    • 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
    • C23C16/458—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 supporting substrates in the reaction chamber
    • C23C16/4582—Rigid and flat substrates, e.g. plates or discs
    • C23C16/4587—Rigid and flat substrates, e.g. plates or discs the substrate being supported substantially vertically
    • 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
    • C23C16/505—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 radio frequency discharges
    • C23C16/509—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 radio frequency discharges using internal electrodes
    • 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
    • H01J37/32009—Arrangements for generation of plasma specially adapted for examination or treatment of objects, e.g. plasma sources
    • H01J37/32082—Radio frequency generated discharge
    • 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
    • H01J37/32009—Arrangements for generation of plasma specially adapted for examination or treatment of objects, e.g. plasma sources
    • H01J37/32082—Radio frequency generated discharge
    • H01J37/32091—Radio frequency generated discharge the radio frequency energy being capacitively coupled to the plasma
    • 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
    • H01J37/32623—Mechanical discharge control means
    • 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
    • H01J37/32623—Mechanical discharge control means
    • H01J37/32633—Baffles
    • 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
    • H01J37/32697—Electrostatic control
    • 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
    • H01J37/32899—Multiple chambers, e.g. cluster tools
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/12—All metal or with adjacent metals
    • Y10T428/12361—All metal or with adjacent metals having aperture or cut

Definitions

  • the present invention relates to a film-forming treatment jig for forming a thin film on a plate having a through hole of a micro diameter by a single plasma film-forming treatment, a plasma CVD (Chemical Vapor Deposition) apparatus using the film-forming treatment jig, a metal plate, and an osmium film forming method.
  • a film-forming treatment jig for forming a thin film on a plate having a through hole of a micro diameter by a single plasma film-forming treatment
  • a plasma CVD (Chemical Vapor Deposition) apparatus using the film-forming treatment jig, a metal plate, and an osmium film forming method.
  • FIG. 8 is a cross-sectional view showing a conventional plasma CVD apparatus in outline.
  • FIG. 9 is a front view showing an aperture plate.
  • the aperture plate 107 is a component for narrowing an electron beam in an electron microscope.
  • the plasma CVD apparatus shown in FIG. 8 is an apparatus for forming a metal film on the surface of the aperture plate 107 .
  • the conventional plasma CVD apparatus has a chamber 101 , and, in the chamber 101 , a gas shower electrode 102 as an upper electrode of a parallel flat plate type and a lower electrode 103 are arranged.
  • the gas shower electrode 102 is connected to a raw material gas supply source 104 .
  • the gas shower electrode 102 and the chamber 101 are connected to the ground potential.
  • a substrate 106 is placed, and on the substrate 106 , the aperture plate 107 is attached.
  • a radio frequency power source (RF power source) 109 is connected via a matching box 108 .
  • the aperture plate 107 shown in FIG. 9 is a plate-like member having a thickness of 10 to 500 ⁇ m, and has a first through hole (a through hole for the attachment) 107 a with a diameter of around 2 mm. Moreover, for the aperture plate 107 , a plurality of second through holes (not shown) with a diameter of around 2 to 100 ⁇ m is arranged, wherein the second through hole is a hole for narrowing the electron beam in an electron microscope.
  • the portions for which the formation of the metal film is necessary in the aperture plate 107 are a portion located near the second through hole on the front and back surfaces of the aperture plate, and the inside surface of the second through hole.
  • a method of forming the metal film on the aperture plate 107 using the above conventional plasma CVD apparatus is as follows.
  • the aperture plate 107 is attached, and the substrate 106 is placed on the lower electrode 103 in the chamber 101 . Subsequently, a raw material gas is supplied to the gas shower electrode 102 from the raw material gas supply source 104 , and the raw material gas is ejected from the gas shower electrode 102 in a shower shape toward the lower electrode 103 . Then, by outputting a radio frequency wave from the RF power source 109 to the lower electrode 103 via the matching box 108 , a metal film is formed on the surface of the aperture plate 107 and the inside surface of the second through hole by a plasma CVD method.
  • the substrate 106 is taken out of the chamber 101 , the aperture plate 107 is peeled off from the substrate 106 and attached on the substrate 106 so that the other surface (the back surface) of the aperture plate 107 is exposed, and the substrate 106 is placed on the lower electrode 103 in the chamber 101 .
  • the metal film is formed on the back surface of the aperture plate 107 and the inside surface of the second through hole.
  • an osmium film being the metal film on the front and back surfaces of the aperture plate and the inside surface of the second through hole.
  • the osmium film has high resistance properties against an electron beam, and, therefore, it is expected to exert high performance as compared with other metal films.
  • the present invention was achieved in view of the above circumstances, and an object thereof is to provide a film-forming treatment jig for forming a thin film on a plate having a through hole of a micro diameter by a single plasma film-forming treatment, and a plasma CVD apparatus using the film-forming treatment jig.
  • Another object of the present invention is to provide a metal plate having an osmium film formed on the inside surface of a through hole of a micro diameter with good uniformity.
  • Another object of the present invention is to provide a film-forming method of an osmium film for forming an osmium film on the surface of a metal member.
  • the film-forming treatment jig according to the present invention is a film-forming treatment jig including: a holding member for holding a plate, by clamping the plate having a through hole, in a state of exposing the through hole and the front and back surfaces of the plate; and an electrode member having the holding member attached thereon, wherein the electrode member is electrically connected to an electrode to which plasma electric power of a plasma CVD apparatus is applied.
  • the film-forming treatment jig since it has a holding member for holding a plate, by clamping the plate having a through hole, in a state of exposing the through hole and the front and back surfaces of the plate, the formation of a thin film on the plate becomes possible by a single plasma film-forming treatment.
  • the electrode member having the holding member attached thereon is one electrically connected to an electrode to which plasma electric power of a plasma CVD apparatus is applied, it is possible to make the electrode member function as a part of the electrode.
  • the electrode member preferably has a flange used to be placed on a transfer arm.
  • the plasma CVD apparatus according to the present invention is a plasma CVD apparatus including:
  • a second electrode disposed in the chamber, and disposed so as to face the first electrode
  • a power source electrically connected to at least one of the first electrode and the second electrode, for applying plasma electric power
  • a raw material gas introduction mechanism for introducing a raw material gas into the chamber
  • a film-forming treatment jig including: a holding member for holding a plate, by clamping the plate having a through hole, in a state of exposing the through hole and the front and back surfaces of the plate; and an electrode member having the holding member attached thereon, wherein
  • the electrode member functions as a part of the second electrode when a thin film is formed on the front and back surfaces of the plate held by the holding member and the inside surface of the through hole by a plasma CVD method, by electrically connecting the electrode member onto the second electrode and placing the plate held by the holding member between the first electrode and the second electrode.
  • the electrode member has a flange
  • the apparatus comprises a transfer mechanism for transferring the film-forming treatment jig into the chamber by placing the flange on a transfer arm.
  • the plasma CVD apparatus further includes a plasma wall arranged around the plate arranged in the chamber and placed between the first electrode and the second electrode, and that the plasma wall is connected to a float potential. This makes it possible to concentrate the flow of the raw material gas introduced into the chamber around the plate by the plasma wall, and also to confine the plasma around the plate by the plasma wall to raise the plasma density.
  • the raw material gas introduction mechanism it is preferable to introduce the raw material gas by the raw material gas introduction mechanism in a direction approximately parallel to the surface of the plate placed between the first electrode and the second electrode.
  • the plasma CVD apparatus according to the present invention is a plasma CVD apparatus including:
  • a lower electrode disposed in the chamber, and disposed so as to face the upper electrode, on the lower side;
  • a power source electrically connected to at least one of the upper electrode and the lower electrode to apply plasma electric power
  • a raw material gas introduction mechanism for introducing a raw material gas into the chamber, and for causing the raw material gas to flow from the upper electrode side toward the lower electrode side;
  • a film-forming treatment jig including: a holding member for holding a plate, by clamping the plate having a through hole, in a state of exposing the through hole and the front and back surfaces of the plate; an electrode member having the holding member attached thereon; and a flange provided to the electrode member;
  • the electrode member functions as a part of the second electrode when a thin film is formed on the front and back surfaces of the plate held by the holding member and the inside surface of the through hole by a plasma CVD method, by electrically connecting the electrode member onto the lower electrode, and placing the plate held by the holding member between the upper electrode and the lower electrode and placing the plate so that the surface thereof becomes approximately parallel to the direction vertical to the upper surface of the lower electrode.
  • the plate is an aperture plate, that the through hole has a diameter of 100 ⁇ m or less, and that the thin film is an osmium film.
  • the plasma electric power is preferably radio frequency power.
  • the metal plate according to the present invention is a metal plate including a plate having a through hole with a diameter of 100 ⁇ m or less, and an osmium film formed by a single film-forming treatment by a plasma CVD apparatus, on the inside surface of the through hole and on the front and back surfaces located near the through hole of the plate, wherein
  • the plasma CVD apparatus comprises:
  • a lower electrode disposed in the chamber, and disposed so as to face the upper electrode, on the lower side;
  • a power source electrically connected to at least one of the upper electrode and the lower electrode to apply plasma electric power
  • a holding member electrically connected to the lower electrode, for holding the plate in a state of exposing the through hole and the front and back surfaces of the plate by clamping the plate to place the plate between the upper electrode and the lower electrode;
  • a plasma wall arranged in the chamber, placed around the plate, and connected to a float potential
  • a raw material gas introduction mechanism for introducing a raw material gas into the chamber, for causing the raw material gas to flow from the upper electrode side toward the lower electrode side, and for causing the raw material gas to flow in a direction along the front and back surfaces of the plate.
  • the osmium film can be formed on the inside surface of the through hole of a micro diameter with better uniformity as compared with conventional techniques, and, since the osmium film is formed by a single film-forming treatment, the interface as is the case for a film formed by multiple treatments does not generate in the osmium film.
  • the thickness of the osmium film is preferably from 10 nm to 50 nm, inclusive.
  • the plasma electric power is preferably radio frequency power.
  • the metal plate may also be an aperture plate.
  • H 2 gas at a flow rate of 5 to 15 cc/min may be introduced, and the metal member may be heated to a temperature of 200 to 300° C. to form the film.
  • the metal member may also be a metal plate.
  • the inert gas may also be He or Ar.
  • the film-forming method of an osmium film by using RF discharge by radio frequency output power, and defining each range of the radio frequency output power density, and OsO 4 gas and pressure, the remaining of oxygen contained in the raw material gas in the osmium film formed on the metal member can be suppressed.
  • the osmium film has such properties as resistant to electron beams.
  • a film-forming treatment jig for forming a thin film for a plate having a through hole of a micro diameter by a single plasma film-forming treatment, and a plasma CVD apparatus using the film-forming treatment jig.
  • an aperture plate in which an osmium film is formed on the inside surface of the through hole of a micro diameter with good uniformity.
  • FIG. 1 is a plan view showing the whole constitution of a plasma CVD apparatus according to an Example according to the present invention.
  • FIG. 2 is a cross-sectional view along the 2 a - 2 a line shown in FIG. 1 .
  • FIG. 3 is a cross-sectional view schematically showing the film-forming chamber, the plasma power source and the raw material gas supply mechanism shown in FIG. 2 .
  • FIG. 4(A) is a side view showing a film-forming treatment jig holding an aperture plate
  • FIG. 4(B) is a top view of the film-forming treatment jig shown in FIG. 4(A) .
  • FIG. 5(A) is a drawing showing the situation when the film-forming treatment jig is transferred, and a plan view showing the state in which the film-forming treatment jig is placed on the transfer arm
  • FIG. 5(B) is a side view showing the film-forming treatment jig and the transfer arm shown in FIG. 5(A) .
  • FIG. 6 is a plan view showing a modified example of the film-forming treatment jig holding the aperture plate.
  • FIG. 7 is a cross-sectional view obtained by cutting the vicinity of the through hole of a micro diameter of the aperture plate for which an osmium film is formed by an experiment.
  • FIG. 8 is a cross-sectional view showing a conventional plasma CVD apparatus in outline.
  • FIG. 9 is a plan view showing an aperture plate.
  • FIG. 1 is a plan view showing the whole constitution of a plasma CVD apparatus by an Example according to the present invention.
  • FIG. 2 is a cross-sectional view along the 2 a - 2 a line shown in FIG. 1 .
  • FIG. 3 is a cross-sectional view schematically showing the film-forming chamber, the plasma power source and the raw material gas supply mechanism shown in FIG. 2 .
  • the plasma CVD apparatus has a cleaning chamber 1 and a film-forming chamber 2 .
  • the cleaning chamber 1 is connected to a transfer chamber 5 via a first gate 6
  • the transfer chamber 5 is connected to a first transfer mechanism 3 .
  • the first transfer mechanism 3 is one that transfers the film-forming treatment jig 8 in the transfer chamber 5 toward the lower side of the cleaning chamber 1 through the opened first gate 6 .
  • the film-forming chamber 2 is connected to the transfer chamber 5 via a second gate 7
  • the transfer chamber 5 is connected to a second transfer mechanism 4 .
  • the second transfer mechanism 4 is one for transferring the film-forming treatment jig 8 in the transfer chamber 5 toward the lower side of the film-forming chamber 2 through the opened second gate 7 .
  • the transfer chamber 5 , the film-forming chamber 2 and the periphery thereof will be described in detail with reference to FIGS. 2 and 3 .
  • the transfer chamber 5 has a freely openable and closable cover 9 .
  • a placement table 10 for placing the film-forming treatment jig 8 and a vertical movement mechanism 11 for vertically moving the film-forming treatment jig 8 placed on the placement table 10 are arranged.
  • the vertical movement mechanism 11 has a placement portion 11 a for placing the film-forming treatment jig 8 , and a movement mechanism 11 b for vertically moving the placement portion 11 a.
  • an evacuation mechanism such as a vacuum pump is connected, and is constituted to evacuate the inside of the transfer chamber 5 by the evacuation mechanism.
  • the insertion of the film-forming treatment jig 8 holding the aperture plate 107 into the transfer chamber 5 is performed by opening the cover 9 in a state where the second gate 7 is closed, placing the film-forming treatment jig 8 holding the aperture plate 107 on the placement table 10 , and, after that, closing the cover 9 .
  • the film-forming chamber 2 has an outer chamber 12 , and the outer chamber 12 is connected to the transfer chamber 5 via the freely openable and closable second gate 7 . Moreover, to the outer chamber 12 , such an evacuation mechanism as a vacuum pump is connected, and it is constituted so that the inside of the outer chamber 12 can be evacuated by the evacuation mechanism.
  • an inner chamber 13 is disposed inside the outer chamber 12 .
  • a gas shower electrode 14 as an upper electrode is arranged at the upper portion of the inner chamber 13 .
  • a first gas supply mechanism for supplying hydrogen gas and a second gas supply mechanism for supplying OsO 4 gas are connected to the gas shower electrode 14 .
  • the first gas supply mechanism has a hydrogen gas supply source 29 , and, to the hydrogen gas supply source 29 , one end of a pipe 18 is connected.
  • a pipe 18 To the other end of the pipe 18 , one end of a bulb 24 is connected, and, to the other end of the bulb 24 , one end of a pipe 17 is connected.
  • MFC mass flow controller
  • MFC mass flow controller
  • To the other end of the pipe 16 To the other end of the pipe 16 , one end of a bulb 23 is connected, and, to the other end of the bulb 23 , one end of a pipe 15 is connected.
  • the gas shower electrode 14 To the other end of the pipe 15 , the gas shower electrode 14 is connected.
  • the second gas supply mechanism has an OsO 4 gas supply source 30 , and, to the OsO 4 gas supply source 30 , one end of a pipe 22 is connected.
  • a pipe 22 To the other end of the pipe 22 , one end of a bulb 26 is connected, and, to the other end of the bulb 26 , one end of a pipe 21 is connected.
  • MFC mass flow controller
  • MFC mass flow controller
  • the OsO 4 gas supply source 30 has a heater 31 , and it is constituted so that the heater 31 heats and sublimates solid OsO 4 to generate OsO 4 gas. It is also constituted so that each of pipes 19 to 21 , bulbs 25 and 26 , and the mass flow controller 28 is heated by a heater (not shown) to around 80° C. This makes it possible to introduce the OsO 4 gas generated by the OsO 4 gas supply source 30 into the gas shower electrode 14 without the solidification.
  • the gas shower electrode 14 , the inner chamber 13 and the outer chamber 12 are connected to the ground potential.
  • a lower electrode 32 On the lower side of the inner chamber 13 , a lower electrode 32 is arranged, and, to the lower electrode 32 , a radio frequency power source (RF power source) 34 is connected via a matching box 33 .
  • the radio frequency power source may use a frequency in the range of 100 kHz to 27 MHz.
  • the apparatus has a vertical movement mechanism 35 for vertically moving the lower electrode 32 between the lower portion of the outer chamber 12 and the lower portion of the inner chamber 13 .
  • a transfer arm 4 a of the second transfer mechanism 4 holds the film-forming treatment jig 8 in the transfer chamber 5
  • the transfer arm 4 a moves the film-forming treatment jig 8 through the opened second gate 7 to the lower side of the outer chamber 12
  • the film-forming treatment jig 8 is placed on the lower electrode 32 to be attached or engaged or electrically connected thereto.
  • the transfer arm 4 a is returned into the transfer chamber 5 , and the second gate 7 is closed.
  • the vertical movement mechanism 35 raises the lower electrode 32 having the film-forming treatment jig 8 attached thereon to move the lower electrode 32 from the lower side of the outer chamber 12 to the lower portion of the inner chamber 13 , and, thereby, the film-forming treatment jig 8 electrically connected to the lower electrode 32 is disposed in the inner chamber 13 .
  • the aperture plate 107 is arranged between the gas shower electrode 14 and the lower electrode 32 , and is placed approximately parallel to the direction (shown by an arrow 36 ) in which the raw material gas is ejected in a shower shape from the gas shower electrode 14 .
  • the position is a film-forming position 38 when the aperture plate 107 is film-formed.
  • the film-forming treatment jig 8 is formed, for example, from SUS, and functions also as a part of the lower electrode. Consequently, when radio frequency power is applied to the lower electrode 32 from the RF power source 34 through the matching box 33 , the radio frequency power is applied to the aperture plate 107 through the film-forming treatment jig 8 . Meanwhile, the specific structure of the film-forming treatment jig 8 , the holding method for holding the aperture plate 107 and the like will be described later.
  • a plasma wall 37 made of ceramics or quartz or glass is arranged around the aperture plate 107 in the inner chamber 13 .
  • the plasma wall 37 has a role of rectifying the flow of the raw material gas introduced from the gas shower electrode 14 so as to concentrate around the aperture plate 107 , and a role of confining the plasma around the aperture plate 107 to raise the plasma density. Only when the plasma wall 37 can fulfill the role, the shape and the material thereof are changeable, and, in the Example, the shape as shown in FIG. 3 is adopted.
  • the plasma wall 37 has a cylindrical rectification member 37 a and a ring-shaped rectification member 37 b for controlling the flow of the raw material gas, and a cylindrical rectification member 37 c arranged outside the cylindrical rectification member 37 a to suppress the discharge between the inner chamber wall and the outer chamber wall.
  • Each upper portion of the cylindrical rectification members 37 a and 37 c is connected by the ring-shaped rectification member 37 b.
  • the plasma wall 37 is connected to a float potential 60 .
  • the ring-shaped rectification member 37 b and the cylindrical rectification member 37 a it is possible to concentrate the raw material gas from the gas shower electrode 14 around the aperture plate 107 , and, as the result, to improve the use efficiency of the raw material gas.
  • the cylindrical rectification member 37 c it is possible to suppress the diffusion of the plasma and to raise the plasma density, and to stabilize the discharge around the aperture plate 107 .
  • FIG. 4(A) is a front view showing the film-forming treatment jig holding the aperture plate
  • FIG. 4(B) is a plan view showing the film-forming treatment jig shown in
  • FIG. 5(A) is a drawing showing the situation when the film-forming treatment jig is transferred and a plan view showing the state where the film-forming treatment jig is placed on the transfer arm
  • FIG. 5(B) is a front view showing the film-forming treatment jig and the transfer arm shown in FIG. 5(A) .
  • the holding member 39 has a cylindrical shape.
  • the holding member 39 holds four aperture plates 107 in a state of clamping the flange.
  • the holding state is a state wherein the second through hole (the through hole of a micro diameter described in FIG. 9 ), and the front and back surfaces of the aperture plate 107 are exposed.
  • the holding member 39 is attached to a flange member 49 .
  • the flange member 49 has, as shown in FIG. 4(A) , a columnar member 49 a and a flange 49 b of a convex shape provided around the upper portion of the columnar member 49 a.
  • the flange 49 b is one to be placed on the transfer arm 4 a as shown in FIGS. 5(A) and 5(B) .
  • the state is set so that the film-forming treatment jig 8 may be transferred by the transfer arm 4 a.
  • the flange member 49 becomes an electrode member and functions as a part of the lower electrode.
  • FIGS. 4(A) and 4(B) four aperture plates 107 are held by the holding member 39 of the film-forming treatment jig 8 , and, as shown in FIGS. 2 and FIGS. 5(A) and 5(B) , the movement mechanism 11 b is raised to place the film-forming treatment jig 8 placed on the placement table 10 on the placement portion 11 a. Then, the movement mechanism 11 b is further raised to move the transfer arm 4 a to the lower side of the film-forming treatment jig 8 placed on the placement portion 11 a.
  • the flange 49 b of the film-forming treatment jig 8 is placed on the transfer arm 4 a.
  • the film-forming treatment jig 8 is placed on the transfer arm 4 a, to set such a state that the film-forming treatment jig 8 may be transferred by the transfer arm 4 a.
  • the film-forming treatment jig 8 is transferred from the transfer chamber 5 to the cleaning chamber 1 by the first transfer mechanism 3 , and the aperture plate 107 is subjected to a cleaning treatment.
  • the film-forming treatment jig 8 is transferred from the cleaning chamber 1 to the transfer chamber 5 by the first transfer mechanism 3 .
  • the state is set so that the film-forming treatment jig 8 may be transferred by the transfer arm 4 a, the film-forming treatment jig 8 is transferred by the second transfer mechanism 4 from the transfer chamber 5 to the film-forming chamber 2 , and the film-forming treatment jig 8 is positioned at the film-forming position 38 .
  • the first gas supply mechanism and the second gas supply mechanism supply hydrogen gas and OsO 4 gas to the gas shower electrode 14 , and the hydrogen gas and the OsO 4 gas are supplied from the gas shower electrode 14 toward the aperture plate 107 .
  • the reason why the raw material gas is flown from top to bottom (in the gravity direction) as the arrow 36 is that the OsO 4 gas has a large molecular weight.
  • the gas may be supplied to the front and back surfaces of the aperture plate with good uniformity, it is not necessarily flown from top to bottom, and the direction of flowing the raw material gas may appropriately be changed.
  • an osmium film having a thickness of 10 nm or more is formed on the front and back surfaces of the aperture plate 107 and the inside surface of the second through hole (the through hole of a micro diameter described in FIG. 9 ) by a single film-forming treatment with good uniformity by a plasma CVD method.
  • the chemical reaction on this occasion is as follows, wherein, as shown in formulae (1) and (2) below, the gas is ionized in the plasma and the film-forming reaction in the formula (3) below occurs on the aperture plate.
  • the reason why the osmium film is to be formed for the aperture plate 107 is that osmium film has higher resistance properties against an electron beam as compared with other metal films to actualize long life, and enables the focusing properties of an electron beam to rise.
  • the film-forming treatment jig 8 since the film-forming treatment jig 8 has the aforementioned structure, as shown in FIG. 2 , it is possible to transfer the film-forming treatment jig 8 by the transfer arm 4 a, and to attach or fit the transferred film-forming treatment jig 8 on or in the lower electrode 32 . Then, since the film-forming treatment jig 8 attached to the lower electrode 32 functions also as a lower electrode, as shown in FIG. 3 , by supplying radio frequency power to the lower electrode 32 , the radio frequency power can be applied to the aperture plate 107 through the film-forming treatment jig 8 .
  • the holding member 39 of the film-forming treatment jig 8 can hold the aperture plate 107 in a state of exposing the front and back surfaces thereof. Consequently, by performing a single film-forming treatment with the plasma CVD apparatus, it is possible to form an osmium film, for a plate having a through hole of a micro diameter such as the aperture plate 107 (one explained as the second through hole in FIG. 9 ), on the inside surface of the through hole and the portion located near the through hole on the front and back surfaces of the plate. Accordingly, the treatment time of the film-forming treatment for the plate can be reduced, and, as the result, the cost of the film-forming treatment can be lowered.
  • the plasma wall 37 connected to the float potential 60 is arranged around the aperture plate 107 , it is possible to concentrate the raw material gas from the gas shower electrode 14 around the aperture plate 107 , and to suppress the diffusion of the plasma and to concentrate the plasma for the aperture plate 107 to raise the plasma density. Consequently, even when a raw material gas for the film-forming that has a large molecular weight and is heavy such as OsO 4 gas is used, the osmium film can be formed on the inside surface of the through hole of a micro diameter with good uniformity.
  • the present invention is not limited to the above Example, but may be practiced in variously changed modes within the scope not deviating from the gist of the present invention.
  • the holding member 39 of the film-forming treatment jig may be so constituted as holding six aperture plates 107 .
  • the lower electrode 32 is connected to the radio frequency power source 34 , and the upper electrode 14 is connected to the ground potential, but the upper electrode 14 may be connected to the radio frequency power source and the lower electrode 32 may be connected to the ground potential, or the upper electrode 14 may be connected to a first radio frequency power source and the lower electrode 32 may be connected to a second radio frequency power source.
  • the radio frequency power source may be changed to another plasma power source. Examples of other plasma power sources include a power source for micro wave, a power source for DC discharge, and each of the pulse-modulated radio frequency power source, power source for micro wave and power source for DC discharge.
  • electrodes are arranged vertically such as the upper electrode 14 and the lower electrode 32 , but the arrangement is not limited to this, and electrodes may be arranged from side to side.
  • Radio frequency output power density 0.25 to 2.0 W/cm 2
  • Frequency of Radio frequency wave 13.56 MHz
  • OsO 4 gas flow rate 0.1 to 3 cc/min
  • H 2 gas flow rate 5 to 15 cc/min
  • Ar gas flow rate 5 to 15 cc/min
  • Film-forming time 10 to 50 seconds Heating temperature: 200 to 300° C.
  • Os film thickness 10 to 50 nm
  • FIG. 7 schematically shows the aperture plate 107 for which an osmium film 110 is formed by the experiment, and is a cross-sectional view of the aperture plate cut in the vicinity of the through hole (second through hole) 107 b of micro diameter (specifically 2 to 100 ⁇ m).
  • the osmium film 110 was formed by a single film-forming treatment, an interface is not formed unlike the case of thin films formed by such conventional technique as the double film-forming treatment, and that the osmium film 110 can be formed on the inside surface of the through hole 107 b of a micro diameter with good uniformity.
  • the peeling of the osmium film 110 is suppressed, and the osmium film 110 , that gives very good focusing properties of electron beams and has high resistance properties for electron beams to give long life, was formed for the through hole 107 b of a micro diameter.

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  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Plasma & Fusion (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Vapour Deposition (AREA)
  • Electrodes Of Semiconductors (AREA)
US12/808,894 2007-12-21 2008-12-22 Film-forming treatment jig, plasma cvd apparatus, metal plate and osmium film forming method Abandoned US20110268983A1 (en)

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JP2007-329867 2007-12-21
JP2007329867A JP5209954B2 (ja) 2007-12-21 2007-12-21 成膜処理用治具及びプラズマｃｖｄ装置
PCT/JP2008/073288 WO2009081897A1 (ja) 2007-12-21 2008-12-22 成膜処理用治具、プラズマｃｖｄ装置、金属プレート及びオスミウム膜の成膜方法

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US5354412A (en) * 1991-09-13 1994-10-11 Nippondenso Co., Ltd. Method of making a compound semiconductor device
EP0730266A2 (de) * 1995-02-06 1996-09-04 Hitachi, Ltd. Vorrichtung zur Plasmabehandlung eines Plattensubstrates und Verfahren zur Herstellung einer magnetischen Platte
US5653812A (en) * 1995-09-26 1997-08-05 Monsanto Company Method and apparatus for deposition of diamond-like carbon coatings on drills
US5900062A (en) * 1995-12-28 1999-05-04 Applied Materials, Inc. Lift pin for dechucking substrates
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US7045465B2 (en) * 1998-04-13 2006-05-16 Nec Electronics Corporation Particle-removing method for a semiconductor device manufacturing apparatus

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JPH069223A (ja) * 1992-06-25 1994-01-18 Kojundo Chem Lab Co Ltd 貴金属薄膜製造法
JPH0628992A (ja) * 1992-07-10 1994-02-04 Nec Corp 透過電子顕微鏡用アパーチャおよびその製造法
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JP3664472B2 (ja) * 2000-08-11 2005-06-29 株式会社 大和テクノシステムズ コーティング処理方法および絞りプレート
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Publication number Priority date Publication date Assignee Title
US4485759A (en) * 1983-01-19 1984-12-04 Multi-Arc Vacuum Systems Inc. Planetary substrate support apparatus for vapor vacuum deposition coating
US4485759B1 (de) * 1983-01-19 1987-02-10
US5354412A (en) * 1991-09-13 1994-10-11 Nippondenso Co., Ltd. Method of making a compound semiconductor device
EP0730266A2 (de) * 1995-02-06 1996-09-04 Hitachi, Ltd. Vorrichtung zur Plasmabehandlung eines Plattensubstrates und Verfahren zur Herstellung einer magnetischen Platte
US5653812A (en) * 1995-09-26 1997-08-05 Monsanto Company Method and apparatus for deposition of diamond-like carbon coatings on drills
US5900062A (en) * 1995-12-28 1999-05-04 Applied Materials, Inc. Lift pin for dechucking substrates
US7045465B2 (en) * 1998-04-13 2006-05-16 Nec Electronics Corporation Particle-removing method for a semiconductor device manufacturing apparatus
US6178919B1 (en) * 1998-12-28 2001-01-30 Lam Research Corporation Perforated plasma confinement ring in plasma reactors
US6506009B1 (en) * 2000-03-16 2003-01-14 Applied Materials, Inc. Apparatus for storing and moving a cassette
US20030148040A1 (en) * 2002-02-07 2003-08-07 Hiroshi Satoh Coating method and aperture plate

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US20140335281A1 (en) 2014-11-13
JP5209954B2 (ja) 2013-06-12
DE112008003378B4 (de) 2022-12-22
JP2009149949A (ja) 2009-07-09
DE112008003378T5 (de) 2011-01-13
WO2009081897A1 (ja) 2009-07-02
US9714468B2 (en) 2017-07-25

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