WO2011010655A1 - Procédé de formation d'un film de revêtement composé d'α-tantale et film de revêtement - Google Patents

Procédé de formation d'un film de revêtement composé d'α-tantale et film de revêtement Download PDF

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WO2011010655A1
WO2011010655A1 PCT/JP2010/062221 JP2010062221W WO2011010655A1 WO 2011010655 A1 WO2011010655 A1 WO 2011010655A1 JP 2010062221 W JP2010062221 W JP 2010062221W WO 2011010655 A1 WO2011010655 A1 WO 2011010655A1
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tantalum
substrate
film
gas
process gas
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PCT/JP2010/062221
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English (en)
Japanese (ja)
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周司 小平
知之 吉浜
恒吉 鎌田
和正 堀田
純一 濱口
茂雄 中西
聡 豊田
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株式会社アルバック
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Priority to JP2011523670A priority Critical patent/JPWO2011010655A1/ja
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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
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/3457—Sputtering using other particles than noble gas ions
    • 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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer
    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic System or AIIIBV compounds with or without impurities, e.g. doping materials
    • H01L21/28—Manufacture of electrodes on semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/268
    • H01L21/283—Deposition of conductive or insulating materials for electrodes conducting electric current
    • H01L21/285—Deposition of conductive or insulating materials for electrodes conducting electric current from a gas or vapour, e.g. condensation
    • H01L21/28506—Deposition of conductive or insulating materials for electrodes conducting electric current from a gas or vapour, e.g. condensation of conductive layers
    • H01L21/28512—Deposition of conductive or insulating materials for electrodes conducting electric current from a gas or vapour, e.g. condensation of conductive layers on semiconductor bodies comprising elements of Group IV of the Periodic System
    • H01L21/2855—Deposition of conductive or insulating materials for electrodes conducting electric current from a gas or vapour, e.g. condensation of conductive layers on semiconductor bodies comprising elements of Group IV of the Periodic System by physical means, e.g. sputtering, evaporation

Definitions

  • the present invention relates to a method for forming a film made of ⁇ -tantalum and the film.
  • a barrier metal layer is provided between the base and the wiring, thereby preventing deterioration of the wiring caused by diffusion of the conductive material constituting the wiring toward the base.
  • the barrier metal layer is formed by forming a thin film made of a metal or a metal compound on a substrate by a PVD method such as sputtering or a vapor phase growth method.
  • a barrier metal layer made of tantalum nitride (TaN), tantalum (Ta), and a combination of them is formed on a base made of a low dielectric constant (low-k) material or silicon oxide (SiO 2 ).
  • a semiconductor element having a copper wiring is disclosed (Patent Document 1).
  • a thin film Ta used as a conventional barrier metal layer has a problem of high specific resistance. This is because the tantalum thin film contains tantalum ( ⁇ tantalum) whose crystal system is cubic and tantalum ( ⁇ tantalum) whose crystal system is tetragonal, and it is difficult to sufficiently reduce the specific resistance. .
  • An aspect according to the present invention provides a method of forming a film made of ⁇ -tantalum on a substrate, and a film made of ⁇ -tantalum formed by the film-forming method, which is made of the ⁇ -tantalum from the substrate. It is an object of the present invention to provide a film made of ⁇ -tantalum in which a conductor or a semiconductor is arranged on at least one of the front and rear sides of the film made of ⁇ -tantalum as viewed in the film direction.
  • the film forming method of ⁇ tantalum according to the aspect of the present invention is a method of forming a film of ⁇ tantalum on a substrate by using a sputtering method, and is a first method including an inert gas and a nitrogen gas.
  • a process gas is introduced into the vacuum chamber, and after the introduction of the first process gas, a first gas comprising at least one of an inert gas and a nitrogen gas is formed so as to have a nitrogen partial pressure at which a film made of ⁇ -tantalum is formed.
  • a film made of ⁇ -tantalum is formed on the substrate by introducing the process gas 2 into the vacuum chamber and controlling the plasma.
  • the film formation method of the ⁇ -tantalum after the first process gas is introduced, an underlayer made of tantalum nitride is formed on the substrate, and an underlayer made of tantalum nitride is formed on the substrate, A film made of ⁇ -tantalum is formed on the substrate.
  • the method for forming a film made of ⁇ -tantalum is characterized in that silicon is used as the base material.
  • the method for forming a film made of ⁇ -tantalum is characterized in that silicon oxide or quartz is used as the substrate material.
  • the film made of ⁇ tantalum in the aspect according to the present invention is a film made of ⁇ tantalum formed by the film forming method, and the film made of ⁇ tantalum in the direction from the substrate toward the film made of ⁇ tantalum.
  • a conductor or a semiconductor is disposed at at least one of the front position and the rear position.
  • the coating made of ⁇ tantalum according to the embodiment of the present invention is a barrier having a low specific resistance, in which a conductor or semiconductor is disposed on at least one of the coating made of ⁇ tantalum when the coating made of ⁇ tantalum is viewed from the substrate.
  • the conductor or semiconductor material can be prevented from diffusing into the substrate, and the adhesion of the conductor or semiconductor to the substrate can be enhanced.
  • FIG. 3A is an X-ray diffraction spectrum of a film made of ⁇ -tantalum shown in FIG. 3A. Sectional drawing of the film which consists of (beta) tantalum and (alpha) tantalum formed into a film on the base
  • FIG. 3A is an X-ray diffraction spectrum of a film made of ⁇ -tantalum shown in FIG. 3A. Sectional drawing of the film which consists of (beta) tantalum and (alpha) tantalum formed into a film on the base
  • FIG. 4A is an X-ray diffraction spectrum of a film made of ⁇ -tantalum and ⁇ -tantalum shown in FIG. 4A. Sectional drawing of the film which consists of (beta) tantalum formed into a film on the base
  • the film formation method of ⁇ tantalum is a method of forming a film of ⁇ tantalum on a substrate using a sputtering method, and is a first process gas including an inert gas and a nitrogen gas.
  • a second process gas consisting of an inert gas and / or nitrogen gas so as to achieve a nitrogen partial pressure at which a film made of ⁇ -tantalum is formed and step A introducing ⁇ Step B for forming a coating made of ⁇ -tantalum on the substrate.
  • sputtering method a general sputtering method capable of forming a metal thin film on a substrate can be applied, and examples thereof include sputtering methods such as magnetron sputtering and reactive sputtering.
  • a target in the sputtering method a target made of Ta (hereinafter referred to as Ta target) is used.
  • the pressure in the sputtering method can be a pressure used in a known sputtering method, for example, 1.0 ⁇ 10 ⁇ 6 Pa or more and 400 Pa or less.
  • the substrate temperature in the sputtering method may be a temperature used in a known sputtering method, and may be, for example, from ⁇ 50 ° C. to 600 ° C.
  • the substrate is not particularly limited as long as it is made of a material that can withstand the temperature at the time of film formation by sputtering.
  • a substrate made of silicon a substrate made of silicon oxide, a substrate made of quartz, a substrate made of metal, etc. Is mentioned.
  • the substrate may be one in which another thin film or the like is previously formed as a base layer on the substrate.
  • the inert gas is not particularly limited as long as it is an inert gas used for sputtering, and examples thereof include argon (Ar), krypton (Kr), helium (He), and the like. Of these, Ar, which is generally easily available and inexpensive, is more preferable.
  • the nitrogen gas (N 2 ) may be a nitrogen gas having a purity generally used in sputtering, and the higher the purity, the better.
  • ⁇ tantalum According to the film formation method of ⁇ tantalum according to the present embodiment, it is possible to form a film of ⁇ tantalum on the substrate, which has been difficult in the past.
  • a thin film made of tantalum was formed by sputtering using a Ta target in an inert gas atmosphere such as Ar. It was a thin film made of ⁇ -tantalum and ⁇ -tantalum.
  • a film made of ⁇ -tantalum can be formed on the substrate by performing the following step A and the following step B in order.
  • the film-forming method of the film which consists of alpha tantalum of this embodiment is demonstrated by the 1st aspect and the 2nd aspect.
  • a cathode electrode 4 is fixed to the ceiling of the vacuum chamber 10, and a Ta target 5 is disposed on the surface thereof.
  • a DC power supply 9 for applying a negative voltage is connected to the cathode electrode 4.
  • a magnetic circuit 8 made of a permanent magnet is provided at the back surface position of the cathode electrode 4 outside the vacuum chamber 10, and the magnetic flux formed by the magnetic circuit 8 penetrates the cathode electrode 4 and the Ta target 5, and the Ta target 5
  • a leakage magnetic field is formed on the surface. When sputtering is performed, electrons are trapped in the leakage magnetic field, and the plasma is densified.
  • a substrate electrode 6 is provided on the bottom surface of the vacuum chamber 10, and a substrate 7 is disposed on the surface of the substrate electrode 6 so as to face the Ta target 5 substantially in parallel.
  • the substrate electrode 6 is connected to a high frequency power source 13 for applying a high frequency bias power.
  • the base electrode 6 is provided with a heater 11 electrically insulated by an insulating portion 11a, and the temperature of the base 7 can be adjusted to ⁇ 50 ° C. to 600 ° C.
  • the vacuum chamber 10 is provided with a gas inlet 2 and a vacuum exhaust 3.
  • a gas cylinder of Ar and nitrogen gas constituting the process gas is connected to the gas inlet 2 so that the respective flow rates can be adjusted individually.
  • a vacuum pump is connected to the vacuum exhaust port 3 (a gas cylinder and a vacuum pump are not shown).
  • the step A in the present embodiment is a step of introducing a first process gas composed of an inert gas and a nitrogen gas into the vacuum chamber 10.
  • the flow rate of the first process gas introduced into the vacuum chamber 10 from the gas inlet 2 is the sum of the flow rate of the inert gas and the flow rate of the nitrogen gas.
  • the flow rate of the inert gas in the first process gas is not particularly limited and can be, for example, 1.0 sccm or more and 30 sccm or less.
  • the flow rate of the nitrogen gas in the first process gas is not particularly limited and can be, for example, 0.01 sccm or more and 30 sccm or less.
  • the sccm is a unit expressed in cm 3 / min (1 atm, 0 ° C.).
  • step A by introducing the first process gas in advance in step A, the gas flow rate and pressure in the vacuum chamber 10 can be stabilized, and a film made of ⁇ -tantalum is sputtered in step B described later.
  • the generation of plasma during formation can be stabilized.
  • the pressure in the vacuum chamber 10 into which the first process gas is introduced in the step A is preferably a pressure range suitable for the sputtering method of 1.0 ⁇ 10 ⁇ 6 Pa to 400 Pa, more preferably 0.001 Pa. It is 10 Pa or less, More preferably, it is 0.01 Pa or more and 1.0 Pa or less. When the pressure is in the above range, a film made of ⁇ -tantalum can be efficiently formed on the substrate in Step B described later.
  • the plasma is controlled by setting a second process gas made of an inert gas and / or a nitrogen gas so as to have a nitrogen partial pressure at which a film made of ⁇ -tantalum is formed. Is a step of forming a film of ⁇ -tantalum on the substrate.
  • the second process gas is put into the vacuum chamber 10 under the atmosphere of the first process gas introduced in the step A, and the partial pressure of nitrogen in the vacuum chamber 10 is changed to that of ⁇ tantalum. It shall be suitable for formation.
  • the flow rate of the second process gas introduced into the vacuum chamber 10 from the gas inlet 2 is the sum of the flow rate of the inert gas and the flow rate of the nitrogen gas.
  • the flow rate of the inert gas is preferably 5.0 sccm or more and 20 sccm or less, more preferably 5.0 sccm or more and 15 sccm or less, and further preferably 8.0 sccm or more and 12 sccm or less.
  • the flow rate of nitrogen gas is preferably 0.01 sccm or more and 5.0 sccm or less, more preferably 0.05 sccm or more and 2.5 sccm or less, and further preferably 0.1 sccm or more and 1.0 sccm or less.
  • the sccm is a unit expressed in cm 3 / min (1 atm, 0 ° C.).
  • the flow rate ratio between the inert gas of the second process gas and the nitrogen gas introduced into the vacuum chamber 10 (the flow rate of the inert gas: the flow rate of the nitrogen gas) is preferably 2000: 1 to 1: 1, : 1 to 2: 1 is more preferable, and 120: 1 to 8: 1 is more preferable.
  • the above range includes the flow ratio at both ends.
  • the inside of the vacuum chamber 10 can be set to a nitrogen partial pressure at which a film made of ⁇ -tantalum is formed.
  • the preferable ranges of the partial pressures of the inert gas and the nitrogen gas in the vacuum chamber 10 in which the second process gas is set are as follows.
  • the partial pressure of the inert gas in the vacuum chamber 10 in which the second process gas is set is preferably 0.03 Pa or more and 5.0 Pa or less, more preferably 0.03 Pa or more and 1.0 Pa or less, and more preferably 0.03 Pa or more. 0.5 Pa or less is more preferable.
  • the nitrogen partial pressure (nitrogen gas partial pressure) in the vacuum chamber 10 in which the second process gas is set is preferably 0.001 Pa or more and 0.02 Pa or less, more preferably 0.001 Pa or more and 0.01 Pa or less, and 0 More preferably 0.003 Pa or more and 0.007 Pa or less.
  • the DC power source 9 When the inside of the vacuum chamber 10 is stabilized at the nitrogen partial pressure at which the ⁇ tantalum film is formed, the DC power source 9 is started, a negative voltage is applied to the cathode electrode 4 to start discharging, and the surface of the Ta target 5 Sputtering can be performed by generating plasma. At this time, a high frequency bias may be applied to the base electrode 6 by a high frequency power source 13.
  • the power of the DC power supply 9 is preferably 5.0 kW or more and 30 kW or less, more preferably 10 kW or more and 25 kW or less, and most preferably 15 kW or more and 20 kW or less because the effect of the present embodiment is excellent.
  • the frequency is preferably 1.0 MHz to 13.56 MHz because the effect of the present embodiment is excellent.
  • a film made of ⁇ -tantalum can be formed on the substrate 7.
  • the thickness of the film made of ⁇ -tantalum to be formed can be set to a desired thickness by appropriately adjusting the sputtering time.
  • the film can be formed with a thickness of 1 nm to 200 ⁇ m.
  • the surface of the substrate 7 on which the ⁇ -tantalum film is formed is not particularly limited, and may be, for example, the surface of a substrate made of silicon or the surface of a substrate made of silicon oxide. Further, a surface on which a thin film made of TaN or the like is previously formed as a base layer may be used.
  • ⁇ Second aspect> A second mode of the film forming method of ⁇ -tantalum according to this embodiment will be described with reference to the sputtering apparatus 1 shown in FIG.
  • the configuration of the sputtering apparatus 1 is the same as the configuration of the sputtering apparatus 1 described in the first aspect.
  • the step A in the present embodiment is a step of introducing a first process gas composed of an inert gas and a nitrogen gas into the vacuum chamber 10.
  • the flow rate of the first process gas introduced into the vacuum chamber 10 from the gas inlet 2 is the sum of the flow rate of the inert gas and the flow rate of the nitrogen gas.
  • the flow rate of the inert gas in the first process gas is preferably 5.0 sccm or more and 20 sccm or less, more preferably 5.0 sccm or more and 15 sccm or less, and most preferably 8.0 sccm or more and 12 sccm or less.
  • the flow rate of nitrogen gas in the first process gas is preferably 15 sccm or more and 60 sccm or less, more preferably 20 sccm or more and 40 sccm or less, and most preferably 25 sccm or more and 35 sccm or less.
  • the sccm is a unit expressed in cm 3 / min (1 atm, 0 ° C.).
  • the flow rate ratio between the inert gas and nitrogen gas of the first process gas introduced into the vacuum chamber 10 is preferably 1: 2 to 1: 5. : 2 to 1: 4 is more preferable, and 1: 2.5 to 1: 3.5 is most preferable.
  • the above range includes the flow ratio at both ends.
  • the pressure in the vacuum chamber 10 into which the first process gas has been introduced in the step A can be 1.0 ⁇ 10 ⁇ 6 Pa or more and 400 Pa or less, and more preferably, 0.1. It is 01 Pa or more and 10 Pa or less, More preferably, it is 0.1 Pa or more and 1.0 Pa or less.
  • the nitrogen partial pressure of the vacuum chamber 10 into which the first process gas is introduced in the step A is preferably a nitrogen partial pressure when a thin film made of known TaN is formed by a sputtering method. 0.03 Pa to 5.0 Pa, preferably 0.03 Pa to 1.0 Pa, and more preferably 0.03 Pa to 0.5 Pa.
  • a base layer made of TaN can be formed on the substrate 7.
  • sputtering method sputtering can be performed by starting the DC power supply 9, applying a negative voltage to the cathode electrode 4 to start discharge, and generating plasma on the surface of the Ta target 5. At this time, a high frequency bias may be applied to the base electrode 6 by a high frequency power source 13.
  • the plasma is controlled by setting a second process gas made of an inert gas and / or a nitrogen gas so as to have a nitrogen partial pressure at which a film made of ⁇ -tantalum is formed.
  • a film made of ⁇ -tantalum is formed on the substrate 7.
  • the inert gas is put as the second process gas in the vacuum chamber 10 under the first process gas atmosphere introduced in the step A, and the nitrogen partial pressure in the vacuum chamber 10 is continuously lowered.
  • a film made of ⁇ -tantalum can be formed on the substrate 7 by sputtering as described above.
  • the method of continuously lowering the nitrogen partial pressure in the vacuum chamber 10 is performed by stopping the inflow of nitrogen gas and flowing in only the inert gas when setting the second process gas. be able to.
  • the same amount of gas as the inflowing gas is exhausted to keep the pressure of the vacuum chamber 10 constant. Therefore, by switching to the inflow of only the inert gas, the nitrogen gas remaining in the vacuum chamber 10 is changed. The concentration can be lowered continuously. Therefore, when the inflow of only the inert gas is continued, the nitrogen partial pressure in the vacuum chamber 10 finally becomes substantially zero.
  • the coating made of ⁇ -tantalum passes through the nitrogen partial pressure formed on the substrate 7. That is, when the nitrogen partial pressure in the vacuum chamber 10 is a nitrogen partial pressure at which a TaN film can be formed, sputtering is started to form a TaN underlayer on the substrate 7, and the nitrogen partial pressure is continuously maintained as described above. By continuing the sputtering while lowering, the film of ⁇ tantalum starts to be formed on the substrate 7 when the film of ⁇ tantalum reaches the nitrogen partial pressure formed on the substrate 7.
  • sputtering is continued while further reducing the nitrogen partial pressure, whereby a film made of ⁇ -tantalum is formed on the previously formed film made of ⁇ -tantalum.
  • the nitrogen partial pressure finally becomes substantially zero, but even in this case, the formation of the film made of ⁇ -tantalum is continued by continuing the sputtering.
  • the thickness of the film made of ⁇ -tantalum to be formed can be set to a desired thickness by appropriately adjusting the sputtering time.
  • the film can be formed with a thickness of 1 nm to 200 ⁇ m.
  • the pressure in the vacuum chamber 10 in which the second process gas is set in the step B is preferably a pressure range suitable for the sputtering method of 1.0 ⁇ 10 ⁇ 6 Pa to 400 Pa, more preferably 0.001 Pa. It is 10 Pa or less, More preferably, it is 0.01 Pa or more and 1.0 Pa or less.
  • the flow rate of the second process gas that flows into the vacuum chamber 10 from the gas inlet 2 is the sum of the flow rate of the inert gas and the flow rate of the nitrogen gas.
  • the flow rate of the inert gas is preferably 5.0 sccm or more and 20 sccm or less, more preferably 5.0 sccm or more and 15 sccm or less, and further preferably 8.0 sccm or more and 12 sccm or less.
  • the flow rate of nitrogen gas is preferably 0 sccm or more and 0.5 sccm or less, more preferably 0 sccm or more and 0.25 sccm or less, and most preferably 0 sccm.
  • the sccm is a unit expressed in cm 3 / min (1 atm, 0 ° C.).
  • the power of the DC power source 9 is preferably 5.0 kW or more and 30 kW or less, more preferably 10 kW or more and 25 kW or less, and most preferably 15 kW or more and 20 kW or less because the effect of the present embodiment is excellent.
  • the frequency is preferably 1.0 MHz or more and 13.56 MHz or less because the effect of the present embodiment is excellent.
  • a base layer made of TaN can be formed on the substrate 7, and a film made of ⁇ -tantalum can be further formed thereon.
  • the substrate 7 is covered with a shutter or the like until the nitrogen partial pressure in the vacuum chamber 10 becomes a nitrogen partial pressure at which a film made of ⁇ -tantalum is formed. It is only necessary to prevent the base layer made of
  • the surface of the substrate 7 on which the ⁇ -tantalum film is formed is not particularly limited, and may be, for example, the surface of a substrate made of silicon or the surface of a substrate made of silicon oxide. Further, a surface on which a thin film made of TaN or the like is previously formed as a base layer may be used.
  • the nitrogen partial pressure at which a film made of ⁇ -tantalum is formed is obtained. . That is, as shown in FIG. 2, it was found that the specific resistance of the Ta thin film formed when the nitrogen gas was flow rate F in FIG. 2 indicates the flow rate of nitrogen gas introduced into the vacuum chamber 10 (unit: sccm). The vertical axis of FIG. 2 indicates that the vacuum chamber 10 is sufficiently stabilized at the nitrogen gas flow rate indicated on the horizontal axis. The specific resistance (unit: ⁇ ⁇ cm) of the Ta thin film formed by sputtering is shown. The formed Ta thin film has a thickness of about 100 mm, and the underlying layer is TaN.
  • the Ta thin film formed at a nitrogen flow rate of 5 sccm or more in FIG. 2 is a thin film made of TaN.
  • the nitrogen flow rate is 5 sccm or less
  • the specific resistance of the formed Ta thin film is lower than that of the TaN thin film, and the specific resistance decreases most when the nitrogen flow rate F is in the range of 0.1 sccm to 1.0 sccm.
  • the Ta thin film formed in this nitrogen flow rate range was a thin film made of ⁇ -tantalum.
  • Example 1 and Comparative Examples 1 and 2 sputtering was performed using the sputtering apparatus 1 shown in FIG.
  • Example 1 A process gas is adjusted in the order of steps A, C, B, and D shown in Table 1 to control plasma, and a base layer 22 made of TaN is formed on the silicon wafer 21 by sputtering, and ⁇ is further formed thereon. A film 23 made of tantalum was formed (see FIG. 3A).
  • step A a first process gas having an Ar flow rate of 10.0 sccm and a nitrogen gas flow rate of 30.0 sccm was introduced into the vacuum chamber 10 from the gas inlet 2 and maintained for 15 seconds in order to stabilize the gas flow rate of the vacuum chamber 10. .
  • step C the power of the plasma generating DC power source 9 is set to 18.0 kW, the power of the substrate bias high frequency power source 13 (1.0 to 13.56 MHz) is set to 600 W, and the same process gas as in step A is used. Sputtering was then performed for 3.0 seconds to form a base layer 22 (thickness: about 20 nm) made of TaN on the silicon wafer 21.
  • step B the first process gas was switched to the second process gas while maintaining the power of the plasma generating DC power supply 9 and the power of the substrate bias high frequency power supply 13 at the same conditions as in step C.
  • the second process gas had an Ar flow rate of 10.0 sccm and a nitrogen gas flow rate of 0.0 sccm. Switching to the second process gas, sputtering was performed for 15.0 seconds, and a film 23 (thickness: about 100 nm) made of ⁇ -tantalum was formed on the underlayer made of TaN.
  • the plasma generating DC power supply 9 and the substrate bias high frequency power supply 13 were turned off, the process gas was stopped, and the process gas was exhausted for 15.0 seconds.
  • step S101 a process gas having an Ar flow rate of 10.0 sccm and a nitrogen gas flow rate of 30.0 sccm was introduced into the vacuum chamber 10 from the gas inlet 2 and maintained for 15 seconds in order to stabilize the gas flow rate of the vacuum chamber 10.
  • step S102 the power of the plasma generating DC power source 9 is set to 18.0 kW
  • the power of the substrate bias high-frequency power source 13 (1.0 to 13.56 MHz) is set to 600 W
  • the same process gas as in step S101 is used.
  • sputtering was performed for 3.0 seconds, and a thin film layer 25 (thickness: about 20 nm) made of TaN was formed on the silicon wafer 24.
  • step S103 the process gas was switched to a process gas having an Ar flow rate of 10.0 sccm and a nitrogen gas flow rate of 0.0 sccm and maintained for 20 seconds, and nitrogen gas was removed from the vacuum chamber 10 to make the vacuum chamber 10 an Ar atmosphere.
  • step S104 the power of the plasma generating DC power source 9 and the power of the substrate bias high frequency power source 13 are set to the same conditions as in step S102, and the process gas is kept under the same conditions as in step S103 for 15.0 seconds of sputtering.
  • a film 26 (thickness: about 100 nm) made of ⁇ tantalum and ⁇ tantalum was formed on the underlayer 25 made of TaN.
  • the plasma generating DC power supply 9 and the substrate bias high frequency power supply 13 were turned off, the process gas was stopped, and the process gas was exhausted for 15.0 seconds.
  • step S201 a process gas having an Ar flow rate of 10.0 sccm and a nitrogen gas flow rate of 0.0 sccm was introduced into the vacuum chamber 10 from the gas inlet 2 and maintained for 15 seconds in order to stabilize the gas flow rate of the vacuum chamber 10.
  • step S202 the power of the DC power source 9 for generating plasma is set to 18.0 kW
  • the power of the substrate bias high frequency power source 13 (1.0 to 13.56 MHz) is set to 600 W
  • Sputtering was performed for 3.0 seconds, and a film (thickness: about 20 nm) made of ⁇ -tantalum was formed on the silicon wafer 27.
  • step S203 sputtering was further performed for 10.0 seconds under the same conditions as in step S202, and a film 28 (thickness: about 100 nm) made of ⁇ -tantalum was further formed.
  • the plasma generating DC power supply 9 and the substrate bias high frequency power supply 13 were turned off, the process gas was stopped, and the process gas was exhausted for 15.0 seconds.

Abstract

La présente invention concerne un procédé permettant de former sur une base, à l'aide d'un procédé de pulvérisation, un film de revêtement composé d'α-tantale, procédé caractérisé en ce qu'un film de revêtement (23) composé d'α-tantale est formé sur une base (21) en régulant le plasma grâce à l'introduction, dans une chambre à vide, d'un premier gaz de traitement composé d'un gaz inerte et d'azote, puis à l'introduction, dans la chambre à vide, d'un second gaz de traitement composé d'un gaz inerte et/ou d'azote, après l'introduction du premier gaz de traitement, de sorte que la pression partielle de l'azote dans la chambre à vide se situe à un niveau auquel est formé un film de revêtement composé d'α-tantale.
PCT/JP2010/062221 2009-07-21 2010-07-21 Procédé de formation d'un film de revêtement composé d'α-tantale et film de revêtement WO2011010655A1 (fr)

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JP2011523670A JPWO2011010655A1 (ja) 2009-07-21 2010-07-21 αタンタルからなる被膜の成膜方法、及びその被膜

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111926289A (zh) * 2020-08-19 2020-11-13 重庆文理学院 一种钽涂层制备方法

Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS498425A (fr) * 1972-03-28 1974-01-25
JPH05171417A (ja) * 1991-12-26 1993-07-09 Sharp Corp タンタル金属薄膜の製造方法
JPH05507115A (ja) * 1990-10-26 1993-10-14 インターナシヨナル・ビジネス・マシーンズ・コーポレーシヨン 薄膜状のアルファＴａを形成するための方法および構造
JPH05289091A (ja) * 1992-04-07 1993-11-05 Sharp Corp 電極基板
JPH08325721A (ja) * 1995-05-31 1996-12-10 Nec Corp 低抵抗タンタル薄膜の製造方法及び低抵抗タンタル配線並びに電極
JP2001044788A (ja) * 1999-05-27 2001-02-16 Murata Mfg Co Ltd 弾性表面波装置及びその製造方法
JP2001335919A (ja) * 2000-03-21 2001-12-07 Murata Mfg Co Ltd αタンタル膜の製造方法、αタンタル膜及びそれを用いた素子
JP2002115044A (ja) * 2000-10-10 2002-04-19 Murata Mfg Co Ltd タンタル膜の製造方法、タンタル膜及びそれを用いた素子
JP2004536463A (ja) * 2001-07-19 2004-12-02 トリコン ホールディングス リミティド タンタル膜の堆積
JP2006517614A (ja) * 2003-02-05 2006-07-27 ヒューレット−パッカード デベロップメント カンパニー エル．ピー． 混相の圧縮性タンタル薄膜及びそれを形成するための方法

Patent Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS498425A (fr) * 1972-03-28 1974-01-25
JPH05507115A (ja) * 1990-10-26 1993-10-14 インターナシヨナル・ビジネス・マシーンズ・コーポレーシヨン 薄膜状のアルファＴａを形成するための方法および構造
JPH05171417A (ja) * 1991-12-26 1993-07-09 Sharp Corp タンタル金属薄膜の製造方法
JPH05289091A (ja) * 1992-04-07 1993-11-05 Sharp Corp 電極基板
JPH08325721A (ja) * 1995-05-31 1996-12-10 Nec Corp 低抵抗タンタル薄膜の製造方法及び低抵抗タンタル配線並びに電極
JP2001044788A (ja) * 1999-05-27 2001-02-16 Murata Mfg Co Ltd 弾性表面波装置及びその製造方法
JP2001335919A (ja) * 2000-03-21 2001-12-07 Murata Mfg Co Ltd αタンタル膜の製造方法、αタンタル膜及びそれを用いた素子
JP2002115044A (ja) * 2000-10-10 2002-04-19 Murata Mfg Co Ltd タンタル膜の製造方法、タンタル膜及びそれを用いた素子
JP2004536463A (ja) * 2001-07-19 2004-12-02 トリコン ホールディングス リミティド タンタル膜の堆積
JP2006517614A (ja) * 2003-02-05 2006-07-27 ヒューレット−パッカード デベロップメント カンパニー エル．ピー． 混相の圧縮性タンタル薄膜及びそれを形成するための方法

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111926289A (zh) * 2020-08-19 2020-11-13 重庆文理学院 一种钽涂层制备方法
CN111926289B (zh) * 2020-08-19 2022-10-21 重庆文理学院 一种钽涂层制备方法

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