WO2019176343A1 - 成膜方法 - Google Patents

成膜方法 Download PDF

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Publication number
WO2019176343A1
WO2019176343A1 PCT/JP2019/002927 JP2019002927W WO2019176343A1 WO 2019176343 A1 WO2019176343 A1 WO 2019176343A1 JP 2019002927 W JP2019002927 W JP 2019002927W WO 2019176343 A1 WO2019176343 A1 WO 2019176343A1
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WO
WIPO (PCT)
Prior art keywords
substrate
axis direction
target
film
targets
Prior art date
Application number
PCT/JP2019/002927
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English (en)
French (fr)
Japanese (ja)
Inventor
太平 水野
辰徳 磯部
Original Assignee
株式会社アルバック
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Publication date
Application filed by 株式会社アルバック filed Critical 株式会社アルバック
Priority to CN201980019108.6A priority Critical patent/CN111902562B/zh
Priority to JP2020505650A priority patent/JP7007457B2/ja
Priority to KR1020207029821A priority patent/KR102376098B1/ko
Publication of WO2019176343A1 publication Critical patent/WO2019176343A1/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
    • C23C14/0021—Reactive sputtering or evaporation
    • C23C14/0036—Reactive sputtering
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • 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
    • C23C14/08—Oxides
    • 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
    • C23C14/08—Oxides
    • C23C14/086—Oxides of zinc, germanium, cadmium, indium, tin, thallium or bismuth
    • 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

Definitions

  • the present invention relates to a film forming method, and more particularly, to a method for forming an indium oxide-based oxide film by reactive sputtering into which oxygen gas is introduced.
  • a manufacturing process of a flat panel display includes a process of forming a transparent conductive film, and an indium oxide-based oxide film such as an ITO film or an ITIO film may be used for such a transparent electrode film. is there.
  • a sputtering method is generally used (see, for example, Patent Document 1).
  • the directions perpendicular to each other in the substrate plane are X-axis directions.
  • a plurality of targets that are long in the Y-axis direction are arranged in parallel in the X-axis direction so that the length in the X-axis direction is longer than the substrate in the vacuum processing chamber. Yes (see, for example, Patent Document 2).
  • a gas pipe is arranged with the direction from each target toward the substrate facing upward and spaced from each target on the lower side of each target, and a reactive sputtering method is formed from a gas injection port formed in the gas pipe.
  • a reactive gas such as oxygen gas introduced during the film is introduced.
  • the reaction gas when the reaction gas is introduced through the gas pipe at the time of film formation, the reaction gas is once diffused in the space below each target, and then passes through each gap between adjacent targets. To be supplied. Thereby, it is suppressed that the reaction gas is supplied to the substrate in a biased manner, and a problem such as unevenness of reactivity within the substrate surface is prevented.
  • this conventional sputtering apparatus when this conventional sputtering apparatus is used to form an indium oxide-based oxide film by reactive sputtering on a larger substrate in recent years, the reaction gas may be supplied to the substrate in an uneven manner.
  • the film quality for example, the sheet resistance value (Rs)
  • JP-A-2015-994 Japanese Patent No. 4707669
  • the present invention provides a film forming method capable of suppressing nonuniform film quality in the X-axis direction of the substrate when forming an indium oxide-based oxide film on the substrate surface. It is the subject to provide.
  • a film forming method of the present invention for forming an indium oxide-based oxide film on a substrate surface has a direction orthogonal to each other in the substrate plane as an X-axis direction and a Y-axis direction, and a vacuum processing chamber.
  • a substrate and a target having a longer length in the X-axis direction than each other are concentrically opposed to each other, a rare gas and an oxygen gas are respectively introduced into a vacuum processing chamber in a vacuum atmosphere, and power is supplied to each target.
  • an indium oxide-based oxide film is formed on the substrate surface, and the direction from the target side to the substrate is the top, immediately below the substrate end region in the X-axis direction. And a step of introducing oxygen gas toward the substrate from at least one of the first position and the second position immediately below the extended region extending from the substrate end to the target end in the X-axis direction.
  • the film quality for example, sheet resistance value (Rs)
  • the substrate end region in the X-axis direction of the substrate, the substrate end faces inward within a range of 10% or less of the length in the X-axis direction of the substrate. The part that extends.
  • the oxygen gas is further introduced from both the first position and the second position toward the substrate. According to this, it was confirmed that the film quality (for example, the sheet resistance value (Rs)) in the X-axis direction of the substrate can be made even more uniform.
  • the film quality for example, the sheet resistance value (Rs)
  • the target is composed of a plurality of targets arranged in parallel in the X-axis direction, and the target juxtaposed region is a region in which these targets are juxtaposed.
  • the predetermined position may be lower than the target juxtaposition region, and oxygen gas may be introduced toward the target through a gap between two adjacent targets. it can.
  • omits one part and shows the sputtering device which can implement the film-forming method of embodiment of this invention.
  • a rectangular glass substrate (for example, a long side of 3400 mm) is a substrate Sw, an indium oxide-based oxide film is an ITO film, and an ITO film is formed on one surface of the substrate Sw by a reactive sputtering method.
  • the embodiment of the film forming method of the present invention will be described taking the case of forming a film as an example.
  • SM is a magnetron type sputtering apparatus capable of performing the film forming method of the present invention.
  • the direction from each target toward the substrate Sw is set upward with reference to the posture shown in FIG. 1, and the targets parallel to one surface (lower surface) of the substrate Sw as a film formation surface are arranged in parallel.
  • the direction is described as the X-axis direction, and the longitudinal direction of the target perpendicular to the X-axis direction is described as the Y-axis direction.
  • the sputtering apparatus SM is, for example, an in-line type, and has a vacuum chamber 1 that can be maintained at a predetermined degree of vacuum via a vacuum exhaust means (not shown) such as a rotary pump or a turbo molecular pump. It has come to define.
  • a substrate transfer means 2 is provided in the upper part of the vacuum chamber 1.
  • the substrate transport means 2 has a known structure, for example, has a carrier 21 that holds the substrate Sw in a state where the lower surface as a film formation surface is opened, and intermittently drives a drive means (not shown) to have a long side.
  • the substrate Sw can be sequentially transferred to a predetermined position in the vacuum processing chamber 11 in a posture that matches the X-axis direction.
  • a predetermined number of targets Tg having the same configuration are arranged in parallel at equal intervals in the X-axis direction on the lower side of the vacuum chamber 1 so as to face the substrate Sw in the vacuum processing chamber 11.
  • four targets Tg 1 , Tg 2 , Tg 3 , Tg 4 on the left side in the X-axis direction, and four targets Tg 5 , Tg 6 , Tg 7 , Tg 8 on the right side in the X-axis direction are shown. Only those shown in the figure are omitted, and those located between the targets Tg 4 and Tg 5 in the central region in the X-axis direction are omitted.
  • Each of the targets Tg 1 to Tg 8 is made of ITO having a predetermined composition ratio, and has a rectangular outline in plan view that is long in the Y-axis direction (see FIG. 2).
  • Each of the targets Tg 1 to Tg 8 has its unused sputtering surface Ts positioned on the same plane parallel to the substrate Sw, and a target juxtaposition region Ta is formed by arranging the targets Tg 1 to Tg 8 in parallel.
  • the length of the target juxtaposed region Ta in the X-axis direction is set to be longer than that of the substrate Sw.
  • the length of the target juxtaposed region Ta in the X-axis direction is determined by considering the uniformity of the thickness distribution of the ITO film in the X-axis direction when an ITO film is formed on the lower surface of the substrate Sw, for example. It is appropriately set to be 1.1 to 1.3 times the width in the direction.
  • the widths of the targets Tg 1 to Tg 8 in the X-axis direction are appropriately designed in consideration of the handleability of the targets Tg 1 to Tg 8 , but the targets Tg 1 to Tg 8 themselves are known. Since this is used, further explanation is omitted.
  • Each target Tg 1 to Tg 8 is joined to a backing plate Bp that cools each target Tg 1 to Tg 8 through a bonding material such as indium or tin during the sputtering, and is floated in the vacuum processing chamber 11. It is installed via an insulating material (not shown). Further, the first earth shield 31 and the first earth seal 31 and the substrate transport means 2 are positioned so as to surround the targets Tg 1 to Tg 8 so as to be sputtered particles on the inner wall of the vacuum chamber 1 and the carrier 21. A second earth shield 32 is disposed to prevent adhesion of etc.
  • magnet units 4 are respectively provided below the targets Tg 1 to Tg 8 (on the side opposite to the sputtering surface Ts). Since a known unit can be used as the magnet unit 4 itself, detailed description is omitted here.
  • Each magnet unit 4 forms a balanced closed-loop tunnel-like magnetic flux above each target Tg 1 to Tg 8 (on the sputtering surface Ts side), and is ionized in front of each target Tg 1 to Tg 8 . By capturing the electrons and secondary electrons generated by sputtering, the plasma density can be increased by increasing the electron density in front of each of the targets Tg 1 to Tg 8 .
  • Each magnet unit 4 is connected to a drive shaft 51 of a drive means 5 composed of a motor, an air cylinder, etc., and reciprocates integrally at a constant speed in parallel between two positions along the X-axis direction. You may do it.
  • Each The target Tg 1 ⁇ Tg 8, output cable Pk from the DC power supply Ps is respectively connected, a predetermined power having a negative potential to the target Tg 1 ⁇ Tg 8 is adapted to be respectively turned on. It should be noted that a plurality of the targets Tg 1 to Tg 8 are paired, and a predetermined voltage is alternately applied at a predetermined frequency (1 to 400 KHz) to a target paired by an AC power source. Also good.
  • the vacuum chamber 1 is provided with first gas introduction means 6 for introducing a rare gas such as Ar.
  • the gas introduction means 6 has a gas pipe 61 attached to the side wall of the vacuum chamber 1, and the gas pipe 61 communicates with a gas source outside the figure via a mass flow controller 62, and a rare gas is introduced into the vacuum processing chamber 11. Can be introduced at a predetermined flow rate.
  • a second gas introduction means 7 is provided at a predetermined position in the vacuum chamber 1 located below each of the targets Tg 1 to Tg 8 .
  • the second gas introduction means 7 has a plurality of gas pipes 71 that are long in the Y-axis direction and are arranged in parallel in the X-axis direction at equal intervals.
  • Each gas pipe 71 is made of stainless steel having a diameter of ⁇ 5 to 10 mm, for example, has a length in the Y-axis direction equivalent to each target Tg 1 to Tg 8, and has a gap Tp between each target Tg 1 to Tg 8. It arrange
  • One end of each gas pipe 71 is connected to a collective pipe 72, and the collective pipe 72 communicates with an oxygen gas source (not shown) via a mass flow controller 73.
  • injection ports 74 are opened at predetermined intervals on the target Tg 1 to Tg 8 side of each gas pipe 71.
  • oxygen gas is supplied toward the substrate Sw through the gaps Tp between the targets Tg 1 to Tg 8 .
  • the opening diameter of the injection port 74 is set as appropriate according to the thickness of the gas pipe 71, and is set, for example, in the range of ⁇ 0.2 mm to 1 mm (in this embodiment, set to 0.4 mm). .
  • the substrate Sw is transferred by the substrate transfer means 2 and set at a position concentric with the target juxtaposed region Ta in the vacuum chamber 1.
  • a rare gas having a predetermined flow rate is introduced through the first gas introducing means 6 and an oxygen gas having a predetermined flow rate is introduced through the second gas introducing means 7.
  • a predetermined power having a negative potential is applied to each of the targets Tg 1 to Tg 8 via the DC power source Ps to form a plasma atmosphere in the space between the target juxtaposed region Ta and the substrate Sw, and the plasma atmosphere
  • Each target Tg 1 to Tg 8 is sputtered with ions of rare gas therein, and a reaction product of sputtered particles and oxygen gas scattered from each target Tg 1 to Tg 8 is attached to and deposited on the lower surface of the substrate Sw to form an ITO film Is deposited.
  • the ITO film is formed by the sputtering apparatus SM, depending on the size of the substrate Sw (for example, the long side is 3400 mm), oxygen gas is supplied through all the gaps Tp between the targets Tg 1 to Tg 8.
  • the film quality for example, the sheet resistance value (Rs)
  • the portion extending from the substrate end to the inward direction within a range of 10% or less of the length of the substrate Sw in the X-axis direction is defined as the substrate end region Se and the substrate end to the target end (that is, the target Tg).
  • a portion extending toward the X-axis direction outer ends of 1 and Tg 8 is defined as an extension region Ea, and a predetermined position (this is a first position) immediately below the substrate end region Se and a predetermined position (this is a second position immediately below the extension region Ea).
  • the oxygen gas is introduced from at least one of the positions) toward the substrate Sw.
  • the first gas pipe 71a and the second gas pipe 71b exist at the first position
  • the third gas pipe 71c exists at the second position
  • the first and second gas pipes 71a and 71b oxygen gas is introduced toward the substrate Sw through the gap Tp between the targets only from the third gas pipe 71c (that is, four targets Tg 1 , Tg 2 , Tg 3 on the left side in the X-axis direction).
  • Tg 4 and the gaps Tp between the four targets Tg 5 , Tg 6 , Tg 7 , and Tg 8 on the right side in the X-axis direction oxygen gas is supplied to the substrate Sw only. ).
  • the film quality for example, sheet resistance value (Rs)
  • the film quality in the X-axis direction of the substrate Sw is substantially equal. it can.
  • it exceeds the range of 10% or less of the length in the X-axis direction of the substrate Sw from the substrate end it can be used as a product regardless of whether oxygen gas is introduced from the second position toward the substrate.
  • the film quality uniformity in the X-axis direction of the substrate cannot be obtained.
  • oxygen gas is introduced from the target juxtaposed region Ta toward the substrate Sw from the outside in the X-axis direction, the uniformity of the film quality cannot be obtained.
  • the targets Tg 1 to Tg 8 are made of ITO having a predetermined composition ratio and have an outline of 200 mm ⁇ 3400 mm ⁇ thickness 10 mm, and 17 targets Tg 1 to Tg 8 are installed in the vacuum chamber 1 at intervals of 250 mm. I did it. Further, (16) gas pipes 71 are respectively installed below the total gap Tp between the targets Tg 1 to Tg 8 so that oxygen gas can be selectively introduced. Further, the substrate Sw is a glass substrate having a long side of 3400 mm.
  • the power supplied from the DC power sources Ps to the targets Tg 1 to Tg 8 is set to 16 kW, and the pressure in the vacuum processing chamber 11 is 0.
  • the mass flow controller 62 was controlled to introduce Ar as a sputtering gas so that the pressure was maintained at 4 Pa, and oxygen gas was introduced at a predetermined flow rate.
  • FIG. 3 is a graph showing the standard value of the sheet resistance (Rs) with respect to the substrate position in the X-axis direction. Note that the standard value of the sheet resistance (Rs) is obtained by an average value. According to this, it was confirmed that the in-plane distribution of the sheet resistance value of the ITO film in the X-axis direction can be improved in the invention experiment 1 as compared with the comparative experiment.
  • the in-plane uniformity of the sheet resistance value was measured by appropriately changing the oxygen gas introduction position. According to this, when the variation in the in-plane distribution of the comparative experiment is 1, oxygen gas is supplied only from the third gas pipes 71c and 71c at the second position and the second gas pipes 71b and 71b at the first position. In the one to be introduced (Invention Experiment 1), the in-plane distribution was 0.2. Further, in the case where oxygen gas was introduced only from the first to third gas pipes 71a, 71a, 71b, 71b, 71c, 71c (Invention Experiment 2), the in-plane distribution was 0.3.
  • the in-plane distribution was 0.3.
  • the in-plane distribution is 0.4, and only the first position directly below the substrate end region Sa and It was found that the in-plane distribution was well improved when oxygen gas was introduced only from the second position directly under the extended region Ea.
  • SM Sputtering apparatus (in which the film forming method of the present invention can be carried out), 11 ... Vacuum processing chamber, 7 ... Second gas introduction means, 71 ... Gas pipe (for oxygen gas), Sw ... Glass substrate (substrate) , Sa: substrate end region, Se: substrate end, Tg 1 to Tg 8 ... ITO target, Tp: gap between targets.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physical Vapour Deposition (AREA)
  • Manufacturing Of Electric Cables (AREA)
PCT/JP2019/002927 2018-03-16 2019-01-29 成膜方法 WO2019176343A1 (ja)

Priority Applications (3)

Application Number Priority Date Filing Date Title
CN201980019108.6A CN111902562B (zh) 2018-03-16 2019-01-29 成膜方法
JP2020505650A JP7007457B2 (ja) 2018-03-16 2019-01-29 成膜方法
KR1020207029821A KR102376098B1 (ko) 2018-03-16 2019-01-29 성막 방법

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2018049058 2018-03-16
JP2018-049058 2018-03-16

Publications (1)

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WO2019176343A1 true WO2019176343A1 (ja) 2019-09-19

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JP (1) JP7007457B2 (zh)
KR (1) KR102376098B1 (zh)
CN (1) CN111902562B (zh)
TW (1) TWI736839B (zh)
WO (1) WO2019176343A1 (zh)

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JP2009041082A (ja) * 2007-08-10 2009-02-26 Ulvac Japan Ltd 薄膜形成方法
JP2009057608A (ja) * 2007-08-31 2009-03-19 Ulvac Japan Ltd スパッタリング装置
JP2009127108A (ja) * 2007-11-27 2009-06-11 Toppan Printing Co Ltd スパッタ装置
JP4707693B2 (ja) * 2007-05-01 2011-06-22 株式会社アルバック スパッタリング装置及びスパッタリング方法
JP2016183402A (ja) * 2015-03-26 2016-10-20 株式会社Ｓｃｒｅｅｎホールディングス スパッタリング装置およびスパッタリング方法

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KR20100030676A (ko) * 2007-08-20 2010-03-18 가부시키가이샤 알박 스퍼터링 방법
WO2011052355A1 (ja) * 2009-10-28 2011-05-05 キヤノンアネルバ株式会社 反応性スパッタ成膜装置、およびそれを用いた膜の製造方法
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JPH11269641A (ja) * 1998-03-23 1999-10-05 Nec Kagoshima Ltd 枚様式スパッタ装置
JP4707693B2 (ja) * 2007-05-01 2011-06-22 株式会社アルバック スパッタリング装置及びスパッタリング方法
JP2009041082A (ja) * 2007-08-10 2009-02-26 Ulvac Japan Ltd 薄膜形成方法
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JP2009127108A (ja) * 2007-11-27 2009-06-11 Toppan Printing Co Ltd スパッタ装置
JP2016183402A (ja) * 2015-03-26 2016-10-20 株式会社Ｓｃｒｅｅｎホールディングス スパッタリング装置およびスパッタリング方法

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JP7007457B2 (ja) 2022-01-24
KR102376098B1 (ko) 2022-03-18
TWI736839B (zh) 2021-08-21
CN111902562A (zh) 2020-11-06
KR20200132964A (ko) 2020-11-25
TW201945563A (zh) 2019-12-01
CN111902562B (zh) 2022-08-12
JPWO2019176343A1 (ja) 2021-02-04

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