WO2017179680A1 - Procédé de fabrication de film hfn et film hfn - Google Patents

Procédé de fabrication de film hfn et film hfn Download PDF

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Publication number
WO2017179680A1
WO2017179680A1 PCT/JP2017/015210 JP2017015210W WO2017179680A1 WO 2017179680 A1 WO2017179680 A1 WO 2017179680A1 JP 2017015210 W JP2017015210 W JP 2017015210W WO 2017179680 A1 WO2017179680 A1 WO 2017179680A1
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Prior art keywords
film
raw material
gas
hfn
hfn film
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PCT/JP2017/015210
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English (en)
Japanese (ja)
Inventor
都田　昌之
善和 佐々木
梅田　優
楠原　昌樹
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株式会社ワコム研究所
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Priority to CN201780037112.6A priority Critical patent/CN109564873A/zh
Publication of WO2017179680A1 publication Critical patent/WO2017179680A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
    • C23C16/34—Nitrides
    • 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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
    • H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
    • H01L21/31—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to form insulating layers thereon, e.g. for masking or by using photolithographic techniques; After treatment of these layers; Selection of materials for these layers

Definitions

  • the present invention relates to a method for producing an HfN film and an HfN film.
  • CVD method has features such as a higher film formation speed and easier production of multilayer thin films than the PVD method, sol-gel method, and other film formation methods.
  • the MOCVD method is a CVD method using a compound containing an organic substance as a raw material, and has advantages such as high safety and no inclusion of halide in the film.
  • the raw material used for the MOCVD method is generally a solid powder or liquid, and these raw materials are put in a container, generally heated in a reduced pressure to vaporize the raw material, and sent into a film forming chamber by a carrier gas. Yes.
  • FIG. 12 is a schematic explanatory view of a thin film forming apparatus used in such MOCVD method.
  • 31 is a vaporizer
  • 32 is a combustion chamber
  • 33 is a reaction vessel
  • 34 is piping
  • 35 is a substantially conical shower nozzle.
  • the vaporizer 1 for example, vaporizes the raw material whose flow rate is controlled by transporting a mixed raw material in which a plurality of types (Ba, Sr, Ti) of liquid raw materials pressurized with He gas are mixed at a desired ratio. To do.
  • the vaporization conditions were a set temperature of 250 ° C. and a vaporization pressure of 2 kPa.
  • the source gas vaporized in the vaporizer 1 is mixed with the carrier gas Ar and introduced into the combustion chamber 32 via a pipe heated to 250 to 260 ° C.
  • the combustion chamber 32 has a structure in which oxygen and raw material gas are mixed and heated while passing through a narrow tube set at a desired temperature.
  • the raw material gas exiting the combustion chamber 32 is introduced into the reaction vessel 33 through the piping 34 and the shower nozzle 5 heated to 260 to 270 ° C. In the combustion chamber 32, it sets to the temperature which at least one part of the organic solvent in source gas burns.
  • the shower nozzle 35 can mix oxygen with the raw material gas as needed.
  • a deposition target substrate P on which a dielectric film is disposed facing the shower nozzle 35 with a predetermined interval is placed on a susceptor 36 made of aluminum nitride and heated by a heater 37.
  • a thermocouple is attached to the susceptor 36, and feedback control using a thermocouple instruction value and temperature control using electric power supplied to the heater 37 are possible.
  • the source gas vaporized in the vaporizer 31 is mixed in the combustion chamber 32 and introduced into the reaction vessel 33 through the shower nozzle 35, and a dielectric film is formed on the deposition target substrate P.
  • a film forming method was adopted in which ammonia (NH 3) or the like was added as a source gas from a vaporization tube upstream of the reaction chamber (reactor).
  • ammonia (NH 3) which is a raw material gas
  • a thin film forming raw material do not react well in a reaction vessel serving as a reaction chamber, which makes it impossible to form a film.
  • a raw material gas and a thin film forming raw material react in a reaction vessel serving as a reaction chamber so that a HfN film can be formed, and a stable raw material supply to a reaction section is possible, and long-term use is possible. It is an object of the present invention to provide a method for producing an HfN film and an HfN film.
  • a source gas vaporized by a vaporizer is supplied via a pipe, and the source gas is supplied to a deposition target substrate disposed opposite to the nozzle surface.
  • the shower nozzle is provided with an outer wall that expands around the inlet of the pipe, a peripheral wall that rises from the expanded end of the outer wall, and a nozzle surface that covers the end of the peripheral wall.
  • a film forming apparatus wherein a gas supply port is provided so as to supply a reaction gas directly to a reaction chamber, a wafer is mounted on the susceptor, and the temperature of the susceptor ranges from 250 ° C. to 270 ° C.
  • the raw material gas TEMAH has a flow rate of 0.2 CCM, a reaction chamber pressure of 4 Torr, and a reactive gas NH 3 flow rate of 9.0 CCM or more and 15.0 CCM or less. This is a method for manufacturing an HfN film.
  • the temperature of the susceptor is less than 250 ° C., thermal decomposition is not performed during film formation, which causes a problem that the film quality deteriorates. If the temperature of the susceptor exceeds 270 ° C., the film formation rate decreases. A malfunction occurs. Also, if the reactive gas NH 3 flow rate is less than 9.0 CCM, the oxygen concentration in the HfN film increases, and the oxygen concentration increases due to the elapsed days of the oxygen concentration in the HfN film. When the flow rate of the reaction gas NH 3 exceeds 15.0 CCM, there is a problem that the oxygen concentration increases depending on the elapsed days of the oxygen concentration in the HfN film.
  • the HfN film according to claim 2 of the present invention is characterized in that N / Hf is in the range of 0.734 or more and 0.757 or less and the oxygen concentration is 2,5 atomic% or less. It is.
  • the HfN film according to claim 3 of the present invention is characterized in that in the HfN film, the oxygen concentration in the film is 10 atomic days later and the fluctuation range is 0.01 atomic% or less. It is a HfN film.
  • the method for producing an HfN film according to claim 1 of the present invention it is possible to provide a method for producing an HfN film in which the oxygen concentration in the HfN film is reduced and the increase due to the elapsed days of the oxygen concentration is suppressed.
  • the HfN film according to the second and third aspects of the present invention it is possible to provide an HfN film in which the oxygen concentration in the HfN film is reduced and the increase in the oxygen concentration due to the elapsed days is suppressed.
  • the raw material gas and the thin film forming raw material react in a reaction vessel serving as a reaction chamber so that an HfN film can be formed, and a stable raw material supply to the reaction section is possible.
  • a method for producing an HfN film and an HfN film that can be used for a long period of time can be provided.
  • a virtual film formation rate a diagram of the relationship between the NH 3 flow rate.
  • FIG relationship in the manufacture of HfN film embodiment the XRF analysis strength, the NH 3 flow rate.
  • a virtual film formation rate a diagram of the relationship between the NH 3 flow rate.
  • 1 Dispersing unit body 2 gas passage, 3 Carrier gas, 4 Gas inlet, 5 Raw material solution, 6 Raw material supply hole, 7 Gas outlet, 8 Dispersion part, 9a, 9b, 9c, 9d screws, 10 rods, 11 Vaporizer, 12 heaters, 13 reaction vessel, 14 piping, 15 shower nozzle, 15a outer wall, 15b Nozzle surface, 15c perimeter wall, 16 reactive gas supply port, 17 Heater, 18 Means for cooling (cooling water), 20 vaporizer tubes, 21 Heating means (heater), 22 Vaporization part, 23 connections, 24 joints, 25 oxygen introduction means (oxygen supply port), 29 Raw material supply inlet, 31 vaporizer, 32 combustion chamber, 33 reaction vessel, 34 piping, 35 Almost conical shower nozzle, 36 Susceptor, 37 heater, 41 shower head, 42 shower nozzle, 43 shower plate, 61 substrate, 62 thin film, 63 Thin film.
  • a source gas vaporized by a vaporizer is supplied via a pipe, and the source gas is injected onto a deposition target substrate disposed opposite to the nozzle surface.
  • the shower nozzle is composed of an outer wall that expands around the inlet of the pipe, a peripheral wall that rises from the expanded end of the outer wall, and a nozzle surface that covers the end of the peripheral wall.
  • the susceptor temperature is in the range of 250 ° C. or higher and 270 ° C. or lower, and the flow rate of the reaction gas NH 3 is 9.0 CCM or higher and 15.0C.
  • This is a method for producing an HfN film characterized by being in a range of CM or less.
  • the HfN film according to the embodiment of the present invention is an HfN film characterized in that N / Hf is in the range of 0.734 or more and 0.757 or less and the oxygen concentration is 2,5 atomic% or less. is there.
  • the HfN film is characterized in that the oxygen concentration in the film is 10 atomic days later and the fluctuation range is 0.01 atomic% or less.
  • FIG. 8 shows a thin film deposition apparatus used in the MOCVD method of this embodiment.
  • 11 is a vaporizer
  • 12 is a heater
  • 13 is a reaction vessel
  • 14 is piping
  • 15 is a substantially conical shower nozzle
  • 16 is a reaction gas supplied directly to the reaction vessel (reaction chamber).
  • a gas supply port 17 is a heater.
  • the shower nozzle 15 can mix oxygen with the raw material gas inside the shower nozzle 15 as needed.
  • the deposition target substrate P for depositing a dielectric film disposed in the reaction vessel 13 is opposed to the shower nozzle 15 with a predetermined interval.
  • the peripheral wall 15c is integrally provided in the shower nozzle 15 between the outer wall 15a expanded from the center, and the nozzle surface 15b.
  • This peripheral wall 15c is for securing the distance between the outer wall 15a and the nozzle surface 15b, and can reduce the difference in flow velocity of the raw material gas between the vicinity of the center and the end of the nozzle surface 15b.
  • the height h of the peripheral wall 15c is set to be not less than half the maximum height of the shower nozzle 15, that is, the height H from the inlet 14a of the pipe 14 to the center of the nozzle surface 15b (h> H / 2). Is preferred.
  • the carrier gas vaporized by the vaporizer 11 is introduced into the reaction vessel 13 through the shower nozzle 15, the difference in flow rate of the raw material gas between the center and the end of the nozzle surface 15b is alleviated, and the nozzle surface 15b.
  • the pressure difference when introduced into the reaction vessel 13 can be relaxed (indicated by the length of the arrow in the figure), and a substantially uniform dielectric film can be formed on the deposition target substrate P.
  • the shower nozzle 15 integrally connecting with the piping 14 was disclosed, as shown in FIG.3 (B), the shower nozzle 15 is located above the front-end
  • TEMAH Hafnium nitride
  • ECH epichlorohydrin
  • the carrier gas is Ar, N 2 or the like.
  • the reaction gas is, for example, O 3, H 2 + N 2, O 2, H 2 S, CO, N 2 or the like.
  • the reaction gas is supplied after being diluted with a carrier gas Ar or N2.
  • the reactive gas (ammonia gas or the like) and the raw material solution are adjusted at a rate that satisfies the stoichiometric ratio of the membrane.
  • the raw material solution is appropriately changed.
  • FIG. 11 shows a shower head used in the thin film deposition apparatus according to this example.
  • a shower head 41 provided in the reaction vessel 13 (reaction chamber) is composed of a shower nozzle 42 and a shower plate 43.
  • a gas supply port 16 for supplying the reaction gas directly to the reaction vessel 13 (reaction chamber) is provided in the shower head 41.
  • a flow path for source gas and a flow path for ammonia gas or the like are formed separately. This configuration is means for preventing the source gas from being mixed with the ammonia gas, which is a reaction gas, and the upstream of the shower plate before reaching the substrate.
  • the shower head 41 has means for cooling the source gas and reaction gas supply passages.
  • (Vaporizer) 8 and 9 show a vaporizer according to this example.
  • a gas passage 2 formed inside the dispersion portion main body 1 constituting the dispersion portion a gas introduction port 4 for introducing the carrier gas 3 pressurized to the gas passage 2, and a gas Means (raw material supply hole) 6 for supplying the raw material solution 5 to the carrier gas passing through the passage 2, a gas outlet 7 for sending the carrier gas containing the dispersed raw material solution 5 to the vaporization section 22, and a gas passage 2, a dispersion part 8 having means (cooling water) 18 for cooling the carrier gas flowing in the inside, and one end connected to the reaction tube of the MOCVD apparatus and the other end connected to the gas outlet 7 of the dispersion part 8.
  • the vaporization tube 20 and a heating means (heater) 21 for heating the vaporization tube 20 are heated, and the carrier gas sent from the dispersion unit 8 in which the raw material solution is dispersed is heated and vaporized. And a vaporizing section 22 for the purpose.
  • FIG. 1 is a diagram showing the relationship between the virtual film formation rate and the NH 3 flow rate in the manufacture of the HfN film of the example.
  • FIG. 2 is a graph showing the relationship between the amount of oxygen in the HfN film and the number of days elapsed in the manufacture of the HfN film of the example.
  • the HfN film formed by thermal decomposition (conditions where the NH 3 flow rate is 0 at 400 ° C. and 300 ° C.) has a high oxygen value of 0.06 to 0.21, and the number of days elapsed The amount tended to increase and the film quality was found to be poor.
  • the oxygen amount is as high as 0.05 to 0.14 and the film quality is still poor.
  • the HfN film having a NH 3 flow rate of 5 CCM has an oxygen amount of 0.04 or less, and the oxygen amount does not change even in the number of days elapsed in the atmosphere.
  • FIG. 3 is a graph showing the relationship between the XRF analysis intensity and the NH 3 flow rate in the manufacture of the HfN film of the example.
  • the susceptor temperature is 300 ° C.
  • the numerical value of the XRF analysis intensity (O / Hf, N / Hf, C / Hf) is changed, and the film quality is poor.
  • the NH 3 flow rate is 5 CC or less, the XRF analysis intensity (O / Hf, N / Hf, C / Hf) values are stable and the film quality is good.
  • FIG. 4 is a diagram showing the relationship between the virtual film formation rate and the NH 3 flow rate under the condition of a susceptor temperature of 260 ° C. in the manufacture of the HfN film of the example. It was found that the NH 3 flow rate reached 9CCM and the virtual film formation rate reached 0.33 at the maximum. The deposition rate is stable when the NH 3 flow rate is between 9 CCM and 15 CCM.
  • FIG. 5 is a graph showing the relationship between the XRF analysis intensity O / Hf, N / Hf, C / Hf and the NH 3 flow rate at the susceptor temperature of 260 ° C. in the manufacture of the HfN film of the example. From the characteristic diagrams of O / Hf, N / Hf, and C / Hf, when the NH 3 flow rate is 5 CCM, the XRF analysis intensity O / Hf is not stable, whereas the NH 3 flow rate is 9 CCM and tends to be stable. It is in.
  • FIG. 6 is a graph showing the relationship between the amount of oxygen (atomic%) in the HfN film and the number of days elapsed at the susceptor temperature of 260 ° C. in the manufacture of the HfN film of the example. It was found that the amount of oxygen (atomic%) in the HfN film was stabilized with respect to the number of elapsed days when the NH 3 flow rate was 9 CCM to 15 CCM. When the NH 3 flow rate is less than 9 CCM or exceeds 15 CCM, the amount of oxygen (atomic%) in the HfN film tends to increase with respect to the number of days elapsed, which is not preferable.
  • FIG. 7 is a diagram showing the relationship between the virtual film formation rate and the susceptor temperature in the manufacture of the HfN film of the example. As the susceptor temperature increases from 260 ° C. to 400 ° C. and the susceptor temperature increases, the film formation rate decreases. Further, when the NH 3 flow rate is compared between 9 CCM and 20 CCM, it has been found that the film formation rate decreases as the NH 3 flow rate increases.
  • Table 1 shows the results of XPS analysis (atomic%) and N / Hf for Inventions 1, 2, 3, 4, 5, and 6.
  • Table 2 shows the XPS analysis (atomic%) and N / Hf measurement results of the comparative products 1, 2, 3, 4, 5, 6, 7, and 8.
  • the source gas and the thin film forming raw material react in a reaction vessel serving as a reaction chamber so that the HfN film can be formed, and stable to the reaction part. It is possible to provide a method for producing an HfN film and a HfN film that can be used for a long time and can be used for a long period of time, and contribute to the development of the semiconductor industry.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Physics & Mathematics (AREA)
  • Inorganic Chemistry (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Manufacturing & Machinery (AREA)
  • Computer Hardware Design (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Power Engineering (AREA)
  • Chemical Vapour Deposition (AREA)
  • Formation Of Insulating Films (AREA)

Abstract

L'invention concerne un procédé de fabrication de film HfN qui permet une alimentation stable en matière première à une unité de réaction et qui peut être utilisé pendant une longue période, et un film HfN. Le procédé de fabrication de film HfN utilise un dispositif de formation de film muni d'une buse de douche à laquelle un gaz de matière première, vaporisé par un vaporisateur, est fourni par l'intermédiaire d'une tuyauterie, et qui pulvérise le gaz de matière première sur un substrat pour la formation de film disposé d'une manière opposée à une surface de buse. La buse de douche comprend une paroi externe qui s'étend avec une ouverture d'introduction pour la tuyauterie au centre, une paroi périphérique s'élevant à partir de l'extrémité étendue de la paroi externe, et la surface de buse, qui recouvre l'extrémité de la paroi périphérique. Le procédé de fabrication de film HfN consiste à fournir une ouverture d'alimentation en gaz de façon à fournir un gaz de réaction directement dans une chambre de réaction, et à monter une tranche sur un suscepteur, lorsque le gaz de matière première TEMAH a un débit de 0,2 CCM et qu'une pression de chambre de réaction est de 4 torr, le suscepteur ayant une température dans une plage non inférieure à 250 °C et non supérieure à 270°C, et le gaz de réaction NH3 ayant un débit dans une plage non inférieure à 9,0 CCM et non supérieure à 15,0 CCM.
PCT/JP2017/015210 2016-04-14 2017-04-14 Procédé de fabrication de film hfn et film hfn WO2017179680A1 (fr)

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CN201780037112.6A CN109564873A (zh) 2016-04-14 2017-04-14 HfN膜的制造方法及HfN膜

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JP2016-081254 2016-04-14
JP2016081254A JP6758574B2 (ja) 2016-04-14 2016-04-14 ＨｆＮ膜の製造方法およびＨｆＮ膜

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CN111589616B (zh) * 2020-06-03 2021-08-10 江苏中大包装材料有限公司 一种半导体表面绝缘薄膜加工装置

Citations (3)

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JP2003282557A (ja) * 2002-03-27 2003-10-03 Ulvac Japan Ltd 成膜方法
US20070166913A1 (en) * 2006-01-19 2007-07-19 Samsung Electronics Co., Ltd. Semiconductor device and method of forming the same
WO2016159355A1 (fr) * 2015-04-01 2016-10-06 株式会社ワコム研究所 Procédé de formation de film et appareil de formation de film pour la formation d'un film de nitrure à l'aide d'un appareil mocvd, et douchette

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Publication number Priority date Publication date Assignee Title
US20050153571A1 (en) * 2003-11-17 2005-07-14 Yoshihide Senzaki Nitridation of high-k dielectric films
CN103668108A (zh) * 2013-12-10 2014-03-26 中国科学院微电子研究所 一种氧化物介质的原子层沉积方法

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Publication number Priority date Publication date Assignee Title
JP2003282557A (ja) * 2002-03-27 2003-10-03 Ulvac Japan Ltd 成膜方法
US20070166913A1 (en) * 2006-01-19 2007-07-19 Samsung Electronics Co., Ltd. Semiconductor device and method of forming the same
WO2016159355A1 (fr) * 2015-04-01 2016-10-06 株式会社ワコム研究所 Procédé de formation de film et appareil de formation de film pour la formation d'un film de nitrure à l'aide d'un appareil mocvd, et douchette

Non-Patent Citations (1)

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Title
SMITH, F. T. J.: "Structure and Electrical Properties of Sputtered Films of Hafnium and Hafnium Compounds", JOURNAL OF APPLIED PHYSICS, vol. 41, no. 10, 1970, pages 4227 - 4231, XP001310238 *

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CN109564873A (zh) 2019-04-02
JP2017191882A (ja) 2017-10-19
TW201807241A (zh) 2018-03-01
JP6758574B2 (ja) 2020-09-23

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