CN113061857B - Method and equipment for depositing film by ion-assisted, inclined sputtering and reactive sputtering - Google Patents

Method and equipment for depositing film by ion-assisted, inclined sputtering and reactive sputtering Download PDF

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CN113061857B
CN113061857B CN202110268042.3A CN202110268042A CN113061857B CN 113061857 B CN113061857 B CN 113061857B CN 202110268042 A CN202110268042 A CN 202110268042A CN 113061857 B CN113061857 B CN 113061857B
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substrate
cavity
sputtering
gas
tilted
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CN113061857A (en
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唐云俊
王昱翔
周虹玲
周东修
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Zhejiang Aiweipu Technology Co ltd
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Zhejiang Aiweipu Technology Co ltd
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    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/0021Reactive sputtering or evaporation
    • C23C14/0036Reactive sputtering
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/0617AIII BV compounds, where A is Al, Ga, In or Tl and B is N, P, As, Sb or Bi
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/08Oxides
    • C23C14/081Oxides of aluminium, magnesium or beryllium
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/50Substrate holders
    • C23C14/505Substrate holders for rotation of the substrates
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/54Controlling or regulating the coating process
    • C23C14/541Heating or cooling of the substrates
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/56Apparatus specially adapted for continuous coating; Arrangements for maintaining the vacuum, e.g. vacuum locks
    • C23C14/568Transferring the substrates through a series of coating stations

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  • Engineering & Computer Science (AREA)
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  • Organic Chemistry (AREA)
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Abstract

The invention discloses a method for depositing a film by ion-assisted, inclined sputtering and reactive sputtering, which comprises the following steps of debugging operation parameters, compiling a hysteresis loop menu, firstly determining basic parameters, wherein the basic parameters comprise the power of an ion source power supply, the power of a radio frequency power supply connected with a target material, the power of a pulse power supply, the inclination angle of a substrate table, the pressure of process gas, the flow change of the process gas and the process time, then setting the parameters, operating according to the set parameters, finishing the appointed process time, and downloading a substrate.

Description

Method and equipment for depositing film by ion-assisted, inclined sputtering and reactive sputtering
Technical Field
The present invention belongs to the field of film physical vapor deposition systemAnd more particularly to ion-assisted, tilted sputtering, reactive sputtering of oxides, nitrides, e.g. of Al 2 O 3 、AlN x A method of making a thin film.
Background
Oxide, nitride films, e.g. Al 2 O 3 The film is an important functional film material.
Due to Al 2 O 3 The film has high dielectric constant, high heat conductivity and strong radiation damage resistance. The composite material has the advantages of strong alkali ion penetration resistance, transparency in a wide wavelength range and other excellent physical and chemical properties, so that the composite material can be widely applied to various fields such as microelectronic devices, electroluminescent devices, optical waveguide devices, corrosion-resistant coatings and the like.
Al 2 O 3 Thin films are widely used in the fabrication of microelectronic devices, one important application being for insulating layers.
Since many different 3D structures are usually present on the substrate surface during the fabrication of electronic devices, this requires deposition of Al 2 O 3 The film has the advantages of high deposition rate, uniformity of film thickness, high dielectric constant, and high coverage rate (conformal) for 3D structures on the substrate.
Al 2 O 3 The preparation method of the film has various methods, such as ion-assisted sputtering, radio frequency magnetron sputtering, pulse reaction magnetron sputtering, chemical vapor deposition, atomic layer deposition, sol-gel method and the like.
The film prepared by ion-assisted deposition has the characteristics of high film-substrate bonding strength, high film density and the like, and is widely applied to the preparation of structural film materials and functional film materials, particularly optical film preparation. But the deposition rate is very low, typically less than 0.1nm/sec.
Radio frequency magnetron sputtering Al 2 O 3 The film speed is very low, and high-power operation is needed in the film preparation process, so that the temperature of a system cavity is high, particles in the cavity are increased, the technological process is unstable, the temperature of a substrate is high, and the like; and cannot form a taller to 3D structures on the substrateWrapping rate (consistency).
The pulse reaction magnetron sputtering has high film deposition rate, can keep the uniformity of the film in a large area range, and can effectively solve the problem of preparing Al 2 O 3 The discharge effect in thin films has become a hot point of research. However, the conventional impulse reactive magnetron sputtering cannot form a high coverage rate (conformal) of the 3D structure on the substrate.
Reactive sputtering, which generally has a "hysteresis loop" effect, i.e., the current or voltage of the target changes with the flow of the reactive gas, resulting in sudden change; and the voltage/current change of the gradually increasing section of the gas flow is not overlapped with the voltage/current change of the gradually decreasing section of the gas flow, so as to form a hysteresis loop, as shown in fig. 1. This is due to the different escape voltages of the sputtered material at different reactant gas flow rates at the surface of the metal target. Under the condition of the reaction gas flow less than the point A, metal materials are mainly sputtered, the target material voltage is higher, the sputtering rate is also high, and the sputtering mode is called as a metal mode; under the condition of the reaction gas flow rate larger than the point B, oxide materials are mainly sputtered, the target material voltage is lower, the sputtering rate is also low, and the sputtering mode is called as a poisoning mode; between points A-B, metal and oxide mixed materials are sputtered, and the material is called as a transition mode; the B-C point area can form a stable oxide film, has a high sputtering rate and is an ideal stable process area.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a reactive sputtering method and equipment adopting ion assistance, inclined sputtering, a mixing power supply and substrate cooling, and overcomes the defects of low deposition rate of the existing alumina film, low coating rate of a 3D structure on a substrate and higher substrate temperature.
In order to achieve the purpose, the invention provides the following technical scheme: a method for depositing film by ion-assisted, inclined sputtering and reactive sputtering comprises the following steps,
s1: debugging the operation parameters, firstly compiling a hysteresis loop menu, uploading a substrate, operating the hysteresis loop menu, drawing and recording a hysteresis loop, determining the numerical value of each parameter during stable reactive sputtering, recording the numerical value as a specified value, and downloading the substrate after debugging is finished;
s2: setting parameters, namely uploading the substrate to a substrate table of the process cavity;
s2.1: rotating the substrate table to a specified inclination angle phi, and then enabling the substrate table to rotate around the center of the substrate at the rotating speed omega;
s2.2: opening a process gas flowmeter, introducing a specified gas flow into a vacuum chamber of the process cavity, and controlling the pressure p in the vacuum chamber of the process cavity to a specified value;
s2.3: setting a coil current I _ t of the top magnet and a coil current I _ b of the bottom magnet to a specified value to generate a magnetic field to guide plasma;
s2.4: setting the power Pw of an ion source power supply to a specified value so as to generate plasma in a vacuum chamber of the process cavity;
s2.5: setting the radio frequency power supply power Pwr and the pulse power supply power Pwp which are connected with the target to a specified value and frequency f, and setting the inversion time t to the specified value;
s3: and operating according to the set parameters, finishing the appointed process time, and downloading the substrate.
Further, in step S1, when the hysteresis loop menu is compiled, basic parameters including power of the ion source and rf power of the target, power of the pulse power, an inclination angle of the substrate table, a pressure of the process gas, a flow change of the process gas, and a process time are determined, and then the hysteresis loop menu is operated.
Further, in step S1, when the hysteresis loop menu is operated, the system records the target current and voltage variation values along with the reactant gas, and simultaneously draws a hysteresis loop, where the point of sudden increase of the target current in the hysteresis loop is a poisoning point, and the corresponding reactant gas Flow is labeled as Flow _ pp.
Further, in step S1, a reactive gas Flow value Flow _ stable at the time of stable reactive sputtering is determined (Flow _ pp-Y) < Flow _ stable < Flow _ pp-X,
wherein X =1-2sccm; y = X + a; a =2-3sccm.
Further, in step S1, after determining the flow rate of the reactive gas during the stable reactive sputtering, if the basic parameter is to be changed, the hysteresis loop menu is recompiled and then the operation is performed again.
Further in step S2.1, the substrate table is tilted at an angle of phi =30-80 degrees and the substrate table is rotated at a rotation speed omega =0-60RPM.
Further in step S2.2, the process gas has a flow rate of 0-200sccm and the pressure in the vacuum chamber of the process chamber is p =1-20mTorr.
Further in step S2.3, the coil current I _ t =0-200A of the top magnet; coil current I _ b =0-200A of the bottom magnet.
Further in step S2.4, the ion source power supply Pw =0-10kW.
Further in step S2.5, the rf power Pwr =0-10kW is connected to the target; the power Pwp =0-10kW of the pulse power supply; the frequency of the pulse power supply is f =1-400kHz; the reversal time t =0-20 μ sec.
The utility model provides an equipment of supplementary, slope sputtering of ion, reactive sputtering deposit film, includes the technology cavity, is provided with plasma source, target holder and substrate platform in the technology cavity, be provided with the gas around the front of substrate platform and spray the unit, still include substrate conveying vacuum cavity and substrate and upload the cavity, the technology cavity is connected with substrate conveying vacuum cavity, and is provided with first vacuum valve between the two, substrate is uploaded the cavity and is connected with substrate conveying vacuum cavity and is provided with the second vacuum valve between the two, substrate is uploaded the cavity and still is provided with the door that supplies the substrate to put into, be provided with the manipulator in the substrate conveying vacuum cavity.
The gas spraying unit further comprises a plurality of spray holes, the plurality of spray holes are uniformly distributed on the inner side of the gas spraying ring along the circumference, and a gas passage communicated with the spray holes is formed in the gas spraying ring.
Furthermore, a sealing unit is arranged on the front surface of the substrate platform, the sealing unit is arranged along the outline shape of the substrate platform, the substrate is arranged on the sealing unit, a cavity is formed between the substrate and the substrate platform, and a gas channel communicated to the cavity is formed in the substrate platform.
Furthermore, a cooling channel is arranged in the substrate table, and a cooling medium is introduced into the cooling channel.
The plasma source is provided with a plasma source, a substrate table, a target support and a substrate table, wherein the plasma source is arranged in a plasma chamber, the target support is positioned below the plasma source, the front surface of the target support is obliquely arranged at an angle with the central axis of the plasma source, and the front surface of the substrate table faces to the front surface of the target support and is far away from the central axis of the plasma source.
Further, a top magnet and/or a bottom magnet is disposed within the chamber, the top magnet being located at the plasma source and the bottom magnet being located at the substrate table.
Further, the top magnet is arranged at an angle of 0-90 degrees with respect to the central axis of the plasma source, and the bottom magnet is arranged at an angle of 0-90 degrees with respect to the central axis of the substrate table.
Compared with the prior art, the invention has the beneficial effects that: overcoming the existing oxide and nitride films, such as Al 2 O 3 The method has the defects of low film deposition rate, low coating rate on the 3D structure on the substrate and high substrate temperature, and can realize Al 2 O 3 Film deposition rate>1nm/sec; coating rate of 3D structure>50 percent; substrate temperature<50℃。
Drawings
FIG. 1 is a schematic diagram of a hysteresis loop in the prior art;
FIG. 2 is a schematic view of the structure of the process chamber of the present invention;
FIG. 3 is a schematic perspective view of a gas spray unit in the reactive sputtering apparatus;
FIG. 4 is a cross-sectional view of a gas spray unit in the reactive sputtering apparatus;
FIG. 5 is a schematic view of a substrate table having a baffle plate;
FIG. 6 is a cross-sectional view of a substrate table;
FIG. 7 is an overall view of an apparatus for ion-assisted, tilted sputtering, reactive sputtering deposition of thin films in accordance with the present invention;
FIG. 8 is a schematic diagram of a hysteresis loop of the present invention;
FIG. 9 is a photograph of an FIB under process conditions according to one embodiment.
Reference numerals: 10. a process chamber; 101. a first vacuum valve; 11. a substrate transfer vacuum chamber; 111. a manipulator; 112. a second vacuum valve; 12. a substrate uploading cavity; 2. a plasma source; 3. a target holder; 4. a substrate stage; 42. a baffle plate; 43. a shaft; 45. an air injection ring; 51. a top magnet; 52. a bottom magnet; 6. a substrate; 71. spraying a hole; 73. an air passage; 81. a seal ring; 82. a gas channel; 83. a cavity; 84. a vacuum pump; 85. a capacitance manometer; 86. a controller; 87. a valve; 88. a mass flow controller; 89. a cooling channel.
Detailed Description
In the description of the present invention, it should be noted that, for the terms of orientation, such as "central", "lateral (X)", "longitudinal (Y)", "vertical (Z)", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise", etc., indicate that the orientation and positional relationship are based on the orientation or positional relationship shown in the drawings, and are only for the convenience of describing the present invention and simplifying the description, but do not indicate or imply that the referred device or element must have a specific orientation, be constructed and operated in a specific orientation, and should not be construed as limiting the specific scope of the present invention.
Furthermore, if the terms "first" and "second" are used for descriptive purposes only, they are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features. Thus, a definition of "a first" or "a second" feature may explicitly or implicitly include one or more of the features, and in the description of the invention, "a number" or "a number" means two or more unless explicitly specified otherwise.
Ion-assisted, tilted sputtering, reactive sputtering of oxide, nitride films, e.g. Al 2 O 3 、AlN x Apparatus for thin film deposition, comprising a substrate6 upload chamber 12 (LL), as shown in fig. 7. The substrate 6 loading chamber 12 is provided with a door, and when opened, a cassette of substrates 6 carrying the substrates 6 can be placed therein. A second vacuum valve 87112 is arranged between the substrate 6 loading chamber 12 and the substrate 6 transferring vacuum chamber 83 and the body 11. LL is pumped to vacuum by vacuum pump 84.
Ion-assisted, tilted sputtering, reactive sputtering of oxide, nitride films, e.g. Al 2 O 3 The apparatus for thin film deposition also includes a vacuum chamber 83 (TM) for transporting the substrate 6, as shown in FIG. 7. The substrate 6 transfer vacuum chamber 83 is provided with a robot 111 in the body 11. A second vacuum valve 87112 is arranged between the conveying vacuum cavity 83 and the process cavity 10, and a first vacuum valve 87101 is arranged between the conveying vacuum cavity 83 11 of the substrate 6 and the upper loading cavity 12 of the substrate 6. The robot 111 in the substrate 6 transfer vacuum chamber 83 body 11 can grasp a given substrate 6 from the substrate 6 upper load chamber 12 into the substrate 6 transfer vacuum chamber 83 body 11 while the second vacuum valve 87112 between the substrate 6 transfer vacuum chamber 83 body 11 and the substrate 6 upper load chamber 12 is opened, and thereafter the second vacuum valve 87112 is closed. The robot 111 then transfers the substrate 6 to the substrate stage 4 of the process chamber 10 while the first vacuum valve 87101 between the transfer vacuum chamber 83 and the process chamber 10 is opened, thereby completing the process of loading the substrate 6.
Ion-assisted, tilted sputtering, reactive sputtering of oxide, nitride films, e.g. Al 2 O 3 、AlN x The thin film deposition apparatus includes a process chamber 10, as shown in FIG. 2. A plasma source 2, a target support 3 and a substrate table 4 are arranged in the process cavity 10, and a gas spraying unit is arranged around the front face of the substrate table 4.
The preferred gas spraying unit of this embodiment includes the gas injection ring 45, and the substrate table 4 is used for placing the substrate 6 in the middle of corresponding gas injection ring 45, the gas spraying unit also includes a plurality of spray orifices 71, and a plurality of spray orifices 71 are evenly distributed along the circumference at the inboard of gas injection ring 45, be provided with the air flue 73 with spray orifice 71 intercommunication on the gas injection ring 45.
One end of the air channel 73 is a gas inlet which is connected with a gas source.
In this embodiment, in order to make the gas flow ejected from all the nozzle holes 71 uniform, it is preferable that the path distances of the gas passages 73 from the inlets of the gas passages 73 to all the nozzle holes 71 are the same, and a multi-stage channel form may be adopted, each channel is divided into two branches as a next-stage channel, the path distances of the two branches of the same stage are the same, and the last-stage channel forms the nozzle holes 71.
In the preferred embodiment, an openable baffle 42 is disposed in front of the substrate table 4, the baffle 42 in the preferred embodiment is rotatably connected to the plate on the substrate table 4 via a shaft 43, and preferably driven by a motor, the baffle 42 can rotate around the shaft 43, so that it covers or uncovers the substrate 6 on the substrate table 4, although the baffle 42 can also cover or uncover the substrate 6 in a translational manner.
In the preferred embodiment, a sealing unit is disposed on the front surface of the substrate stage 4, the sealing unit is disposed along the contour of the substrate stage 4, the substrate 6 is disposed on the sealing unit, the sealing unit can be, for example, a sealing ring 81, a cavity 83 is formed between the substrate 6 and the substrate stage 4, a gas passage 82 communicated with the cavity 83 is opened on the substrate stage 4, the substrate 6 can be attached to the sealing unit by connecting the gas passage 82 to a vacuum pump 84, and the substrate stage 4 can be manufactured simply.
A capacitance manometer 85 for measuring a flow rate of gas drawn from the cavity 83 may be provided between the gas passage 82 and the vacuum pump 84, and a controller 86 for cooperating with the capacitance manometer 85 may be further included, the controller 86 controlling the flow rate of the drawn gas to thereby control the pressure of the gas in the cavity 83.
Preferably, a branch between the gas channel 82 and the capacitance manometer 85 is provided, which is provided with a valve 87 and a mass flow controller 88, and the gas in the cavity 83 can be introduced into the cavity 83 by opening the valve 87, and the constant pressure of the gas in the cavity 83 is controlled by the valve 87, the mass flow controller 88, the capacitance manometer 85, the controller 86 and the vacuum pump 84 together during the deposition process.
During deposition, the gas within the cavity 83 may act as a thermal conductor between the substrate 6 and the substrate table 4, such that the substrate 6 and the substrate table 4 are thermally conductive.
In the preferred embodiment, a cooling channel 89 is formed in the substrate stage 4, a cooling medium is introduced into the cooling channel 89, and water or a water-alcohol mixture, for example, is introduced into the cooling channel 89 as a cooling medium to flow through the substrate stage 4, so as to accelerate heat dissipation.
The preferred target holder 3 of this embodiment is located below the plasma source 2, and the front surface of the target holder 3 is disposed at an angle inclined to the central axis 43 of the plasma source 2, and the front surface of the substrate stage 4 faces the front surface of the target holder 3 and is away from the central axis 43 of the plasma source 2.
Wherein the preferred substrate table 4 may employ a rotation mechanism to enable in-situ rotation of the substrate 6 about the axis 43.
Of course, the substrate stage 4 as a whole can be rotated relative to the target holder 3 to adjust the angle between it and the target holder 3.
The central axis 43 of the plasma source 2 is the plasma path in this embodiment, and the substrate table 4 keeps the substrate away from the plasma path, but directs the substrate towards the sputtering surface of the target on the target holder 3 to maximize deposition of sputtered material on the substrate.
The target holder 3 in this embodiment preferably can rotate the target material by using a rotating mechanism, but the inclination angle of the target holder 3 is preferably adjustable, but these are not essential.
In the preferred embodiment, a top magnet 51 and/or a bottom magnet 52 are disposed in the chamber, wherein the top magnet 51 is located at the plasma source 2 and the bottom magnet 52 is located at the substrate stage 4.
The preferred embodiment of the top magnet 51 is disposed at an angle of 0-90 deg. to the axis 43 of the plasma source 2.
The preferred embodiment of the bottom magnet 52 is disposed at an angle of 0-90 deg. to the centerline of the substrate table 4.
The two magnets may be electromagnetic coils or ring magnets. The top and bottom magnets 51, 52 may generate magnetic fields with asymmetric strengths, thereby forming magnetic field lines that may be manipulated to control the concentration of ions emitted by the plasma source 2 and reaching the target.
Separation deviceSub-assisted, oblique sputtering, reactive sputtering of oxide, nitride films, e.g. Al 2 O 3 、AlN x The film deposition method comprises the following steps:
s1: debugging the operation parameters, firstly compiling a hysteresis loop menu, uploading the substrate 6, operating the hysteresis loop menu, drawing and recording a hysteresis loop, determining the numerical value of each parameter during stable reactive sputtering, recording the numerical value as a specified value, and downloading the substrate 6 after debugging is finished;
s2: setting parameters, namely uploading a substrate 6 onto a substrate table 4 of a process cavity 10;
s2.1: rotating the substrate table 4 to a specified inclination angle phi, and then enabling the substrate table 4 to rotate around the center of the substrate 6 at the rotating speed omega;
s2.2: opening a process gas flowmeter, introducing a specified gas flow into a vacuum cavity 83 chamber of the process chamber 10, and controlling the pressure p in the vacuum cavity 83 chamber of the process chamber 10 to a specified value;
s2.3: setting the coil current I _ t of the top magnet 51 and the coil current I _ b of the bottom magnet 52 to specified values to generate a magnetic field to guide plasma;
s2.4: setting the ion source power Pw to a specified value to generate a plasma in the vacuum chamber 83 of the process chamber 10;
s2.5: setting the radio frequency power supply power Pwr and the pulse power supply power Pwp connected with the target to a specified value and frequency f, and setting the reversal time t to the specified value;
s3: and operating according to the set parameters to finish the appointed process time, and downloading the substrate 6.
In this embodiment, preferably, in step S1, when the hysteresis loop menu is compiled, first, the basic parameters, the power of the ion source power and the rf power connected to the target, the power of the pulse power, the tilt angle of the substrate stage 4, the process gases (Ar, O), and the power of the rf power are determined 2 、N 2 ) The pressure of (a); flow of process gases, e.g. Ar, O 2 、N 2 A change in gas flow rate; and (5) the process time is shortened, and then the hysteresis loop menu is operated. The process gas in this embodiment includes Ar, O 2 、N 2
This examplePreferably, in step S1, the target current and voltage are recorded by the system along with the reaction gas (O) while running the hysteresis loop menu 2 、N 2 ) The flow change value is drawn, a hysteresis loop is drawn at the same time, and the point of sudden increase of the target current in the hysteresis loop is the poisoning point corresponding to the reaction gas (O) 2 、N 2 ) The Flow is labeled Flow _ pp. The reaction gas in this embodiment is a gas involved in the reaction of the process gas, and includes O 2 、N 2。
In step S1, the reactive gas such as O during stable reactive sputtering is determined 2 ,N 2 Flow value of gas Flow _ stable:
(Flow_pp-Y)<Flow_stable<Flow_pp-X,
wherein X =1-2sccm; y = X + a; a =2-3sccm.
As shown in FIG. 8 and Table 1, under the condition that Flow _ pp was measured to be 36sccm, O was taken in accordance with the above formula 2 The flow rates are 33.8, 34.2, 34.4, 34.6 and 34.8sccm, and the stable film thickness and refractive index can be obtained by respectively operating the film deposition process, which indicates that the stable film deposition process is formed in the interval, i.e., indicates that the process S1 is completed.
Table 1:
Figure BDA0002972806900000091
Figure BDA0002972806900000101
this embodiment is preferred in step S1 when the reactive gas, such as O, is determined to be stable during reactive sputtering 2 、N 2 After the flow value is obtained, if the basic parameters need to be changed, the hysteresis loop menu is recompiled and then the operation is carried out again.
As shown in table 2, which are several cases of the specific implementation of the process run S2 process.
Table 2:
B C D E F G H I G L M
Deg w w w mTorr sccm sccm sec nm nm/sec
75 3500 3200 1000 3 90 29.4 1000 1042.8 0.63 1.043
65 3500 3200 1000 3 90 29.4 1040 1034.9 0.58 0.995
55 3500 3200 1000 3 90 29.0 1155 1053.9 0.57 0.912
45 3500 3200 1000 3 90 28.8 1320 1032.7 0.50 0.785
35 3500 3200 1000 3 90 28.6 1575 1045.7 0.25 0.664
25 3500 3200 1000 3 90 28.0 2200 1060.0 0.75 0.482
in Table 2, B is the tilt angle of the substrate table 4; c is the power of the ion source power supply; d is the radio frequency power supply power connected with the target material; e is the power of the pulse power supply; f is process gas Ar and O 2 Pressure of(ii) a G is Ar flow; h is O 2 Flow rate; i is deposition time; g is the thickness of the coating film; l is the mean square error σ% of the film thickness; m is the deposition rate.
The basic parameter of the process, namely the inclination angle of the substrate table 4, is changed from 25 degrees to 75 degrees, the inclination angle of each substrate table 4 needs to execute a process debugging process S1, and the corresponding stable process O is obtained 2 Flow rate, e.g. when the substrate table 4 is tilted at an angle of 25 degrees, O stabilizing the process 2 The flow rate was 28.0sccm. H value (O) in Table 2 2 Flow) are respectively O of the stabilization process measured through the S1 process and corresponding to the B value (the inclination angle of the substrate table 4) 2 And (4) flow rate.
In step S2.1, the substrate stage 4 is inclined at an angle of phi =30 to 80 degrees, and the rotation speed of the substrate stage 4 is ω =0 to 60RPM; in step S2.2, process gases, e.g. Ar, O 2 、N 2 The flow rate of (1) is 0-200sccm, and the air pressure P =1-20mTorr in the PM cavity; in step S2.3, the coil current I _ t =0-200A of the top magnet 51; coil current I _ b =0-200A of bottom magnet 52; in step S2.4, the ion source power Pw =0-10kW; in step S2.5, the rf power Pwr =0-10kW; the power Pwp =0-10kW of the pulse power supply; the frequency of the pulse power supply is f =1-400kHz; the reversal time t =0-20 μ sec.
In a certain implementation and operation process case, the inclination angle phi of the substrate table 4 is =75 degrees, and the rotation speed omega of the substrate table 4 is =30RPM; in step S2.2, the flow rate of Ar is 90sccm; o is 2 The flow rate of (2) is 29.4sccm; the air pressure P =3mTorr in the process chamber 10; in step S2.3, the coil current I _ t =100A of the top magnet 51; coil current I _ b =190A of bottom magnet 52; in step S2.4, the ion source power supply power Pw =3.5kW; in step S2.5, the rf power Pwr =3.2kW for the target; the power Pwp of the pulse power source is =1kW; frequency f =40kHz; inversion time t =10 μ sec. The process was run to obtain a film thickness uniformity of 0.63% thickness mean square error and a deposition rate of 1.043nm/sec.
In another implementation and operation process case, the inclination angle phi of the substrate table 4 is =45 degrees, and the rotation speed omega of the substrate table 4 is =30RPM;in step S2.2, the flow rate of Ar is 90sccm; o is 2 The flow rate of (2) is 29.4sccm; the air pressure P =3mTorr in the process chamber 10; in step S2.3, the coil current I _ t =100A of the top magnet 51; coil current I _ b =190A of bottom magnet 52; in step S2.4, the ion source power Pw =3.5kW; in step S2.5, the rf power Pwr =3.2kW for the target; the power Pwp =1kW of the pulse power supply; frequency f =40kHz; inversion time t =10 μ sec. The process was run to obtain a film thickness uniformity of 0.50% thickness mean square deviation and a deposition rate of 0.785nm/sec.
As can be seen from table 2, the uniformity of the thickness of the obtained film can meet the requirement of high-precision film deposition (the mean square deviation of the thickness is required to be less than 1.0%); meanwhile, the deposition rate is proportional to the inclination angle of the substrate stage 4, i.e., the higher the inclination angle of the substrate stage 4, the larger the deposition rate.
In another implementation and operation process case, the inclination angle phi of the substrate table 4 is =45 degrees, and the rotation speed omega of the substrate table 4 is =30RPM; in step S2.2, the flow rate of Ar is 90sccm; o is 2 The flow rate of (2) is 29.4sccm; the air pressure P =3mTorr in the process chamber 10; in step S2.3, the coil current I _ t =100A of the top magnet 51; coil current I _ b =190A of bottom magnet 52; in step S2.4, the ion source power Pw =3.5kW; in step S2.5, the rf power Pwr =3.2kW for the target; the power Pwp =1kW of the pulse power supply; frequency f =40kHz; inversion time t =10 μ sec. The thickness uniformity of the film obtained by the operation of the process is that the thickness mean square deviation is 0.50 percent, and the deposition rate is 0.785nm/sec; FIG. 9 also shows a photograph of a FIB (Focused Ion Beam) under the process conditions, and it can be seen that the process achieves a coverage (coherence) of the 3D structure of t 0 T =50%, wherein t 0 Is the thickness of the film deposited on the surface of the 3D structure, and t is the thickness of the film deposited on the side surface of the 3D structure.
In a certain implementation and operation process case, the inclination angle phi of the substrate table 4 is =75 degrees, and the rotation speed omega of the substrate table 4 is =30RPM; in step S2.2, the flow rate of Ar is 90sccm; o is 2 The flow rate of (2) is 29.4sccm; the air pressure P =3mTorr in the process chamber 10; in step S2.3, the wires of the top magnet 51Coil current I _ t =100A; coil current I _ b =190A of bottom magnet 52; in step S2.4, the ion source power supply power Pw =3.5kW; in step S2.5, the rf power Pwr =3.2kW for the target; the power Pwp =1kW of the pulse power supply; frequency f =40kHz; inversion time t =10 μ sec. The thickness of the film obtained by the operation of the process was about 500nm, the thickness uniformity was such that the mean square deviation of the thickness was 0.63%, the deposition rate was 1.043nm/sec, and the surface temperature of the substrate 6 was measured by using a temperature spot plate at the same time<48 ℃ as shown in Table 3.
In another certain implementation and operation process case, the inclination angle phi of the substrate table 4 is =75 degrees, and the rotation speed omega of the substrate table 4 is =30RPM; in step S2.2, ar and O 2 The flow rate of (2) is 90sccm; o is 2 The flow rate of (2) is 29.4sccm; the air pressure in the PM cavity is P =3mTorr; in step S2.3, the coil current I _ t =100A of the top magnet 51; coil current I _ b =190A of bottom magnet 52; in step S2.4, the ion source power supply power Pw =3.5kW; in step S2.5, the rf power Pwr =3.2kW for the target; the power Pwp =1kW of the pulse power supply; frequency f =40kHz; the inversion time t =10 μ sec. The thickness of the film obtained by the operation of the process is about 2um, the thickness uniformity is that the mean square deviation of the thickness is 0.63 percent, the deposition rate is 1.043nm/sec, and simultaneously, the surface temperature of the substrate 6 is measured by using a temperature spot plate<48 ℃ as shown in Table 3.
Table 3:
Figure BDA0002972806900000121
it should be noted that different substrate stage 4 tilt angle processes can be used in different applications to suit specific film deposition process requirements. In general, the smaller the tilt angle of the substrate table 4, the larger the wrap rate of the 3D structure, but the smaller the deposition rate.
The above description is only a preferred embodiment of the present invention, and the protection scope of the present invention is not limited to the above embodiments, and all technical solutions belonging to the idea of the present invention belong to the protection scope of the present invention. It should be noted that modifications and embellishments within the scope of the invention may occur to those skilled in the art without departing from the principle of the invention, and are considered to be within the scope of the invention.

Claims (15)

1. A method for depositing a film by ion-assisted, inclined sputtering and reactive sputtering is characterized by comprising the following steps,
s1: debugging the operation parameters, firstly compiling a hysteresis loop menu, uploading a substrate, operating the hysteresis loop menu, drawing and recording a hysteresis loop, determining the numerical value of each parameter during stable reactive sputtering, recording the numerical value as a specified value, and downloading the substrate after debugging is finished;
when the hysteresis loop menu is operated, the system records the target current and voltage change values along with the reaction gas, simultaneously draws a hysteresis loop, and marks the point of sudden increase of the target current in the hysteresis loop as a poisoning point and the corresponding reaction gas Flow as Flow _ pp;
determining a reaction gas Flow value Flow _ stable during stable reactive sputtering:
(Flow_pp-Y)<Flow_stable<Flow_pp-X,
wherein X =1-2sccm; y = X + a; a =2-3sccm;
s2: setting parameters, namely uploading the substrate to a substrate table of the process cavity;
s2.1: rotating the substrate table to a specified inclination angle phi, and then enabling the substrate table to rotate around the center of the substrate at a rotation speed omega;
s2.2: opening a process gas flowmeter, introducing a specified gas flow into a vacuum chamber of the process cavity, and controlling the pressure p in the vacuum chamber of the process cavity to a specified value;
s2.3: setting a coil current I _ t of the top magnet and a coil current I _ b of the bottom magnet to a specified value to generate a magnetic field to guide plasma;
s2.4: setting the power Pw of an ion source power supply to a specified value so as to generate plasma in a vacuum chamber of the process cavity;
s2.5: setting the radio frequency power supply power Pwr and the pulse power supply power Pwp which are connected with the target to a specified value and frequency f, and setting the inversion time t to the specified value;
s3: and operating according to the set parameters, finishing the appointed process time, and downloading the substrate.
2. The method of ion assisted, tilted sputtering, reactive sputtering deposition of thin films as claimed in claim 1, wherein: in step S1, when compiling the hysteresis loop menu, first, basic parameters are determined, where the basic parameters include power of the ion source power supply, power of the rf power supply connected to the target, power of the pulse power supply, tilt angle of the substrate stage, pressure of the process gas, flow change of the process gas, and process time, and then, the hysteresis loop menu is operated.
3. The method of ion assisted, tilted sputtering, reactive sputtering deposition of thin films as claimed in claim 2, wherein: in step S1, after determining the reactive gas flow value during stable reactive sputtering, if the basic parameter is to be changed, the hysteresis loop menu is recompiled and then the operation is performed again.
4. The method of ion assisted, tilted sputtering, reactive sputtering deposition of thin films as claimed in claim 3, wherein: in step S2.1, the substrate table is tilted at an angle of phi =30-80 degrees, and the substrate table is rotated at a rotation speed omega =0-60RPM.
5. The method of ion assisted, tilted sputtering, reactive sputtering deposition of thin films as claimed in claim 4, wherein: in step S2.2, the process gas has a flow rate of 0-200sccm and the pressure in the vacuum chamber of the process chamber is p =1-20mTorr.
6. The method of ion assisted, tilted sputtering, reactive sputtering deposition of thin films as claimed in claim 5, wherein: in step S2.3, the coil current I _ t =0-200A of the top magnet; the coil current I _ b =0-200A of the bottom magnet.
7. The method of claim 6, wherein the step of depositing the film comprises: in step S2.4, the ion source power supply Pw =0-10kW.
8. The method of ion assisted, tilted sputtering, reactive sputtering deposition of thin films as claimed in claim 7, wherein: in step S2.5, the rf power Pwr =0-10kW; the power Pwp =0-10kW of the pulse power supply; the frequency of the pulse power supply is f =1-400kHz; the reversal time t =0-20 μ sec.
9. The utility model provides an equipment of supplementary, slope sputtering of ion, reactive sputtering deposition film, includes the technology cavity, is provided with plasma source, target holder and substrate platform in the technology cavity, the front of substrate platform is provided with gas around and sprays unit, its characterized in that: the vacuum substrate processing device is characterized by further comprising a substrate conveying vacuum cavity and a substrate uploading cavity, the process cavity is connected with the substrate conveying vacuum cavity, a first vacuum valve is arranged between the process cavity and the substrate conveying vacuum cavity, the substrate uploading cavity is connected with the substrate conveying vacuum cavity, a second vacuum valve is arranged between the substrate uploading cavity and the substrate conveying vacuum cavity, the substrate uploading cavity is further provided with a door for placing a substrate, and a manipulator is arranged in the substrate conveying vacuum cavity.
10. The apparatus for ion assisted, tilted sputter, reactive sputter deposition of thin films as claimed in claim 9, wherein: the gas spraying unit comprises a gas spraying ring, a substrate table corresponds to the middle of the gas spraying ring and is used for placing a substrate, the gas spraying unit further comprises a plurality of spray holes, the plurality of spray holes are evenly distributed on the inner side of the gas spraying ring along the circumference, and a gas passage communicated with the spray holes is formed in the gas spraying ring.
11. The apparatus for ion assisted, tilted sputter, reactive sputter deposition of thin films as claimed in claim 10, wherein: the surface in front of the substrate platform is provided with a sealing unit, the sealing unit is arranged along the outline shape of the substrate platform, the substrate is arranged on the sealing unit, a cavity is formed between the substrate and the substrate platform, and a gas channel communicated to the cavity is formed in the substrate platform.
12. The apparatus for ion assisted, tilted sputter, reactive sputter deposition of thin films as claimed in claim 11, wherein: and a cooling channel is arranged in the substrate platform, and a refrigerant is introduced into the cooling channel.
13. The apparatus for ion assisted, tilted sputter, reactive sputter deposition of thin films as claimed in claim 12, wherein: the target support is positioned below the plasma source, the front surface of the target support and the central axis of the plasma source are obliquely arranged at an angle, and the front surface of the substrate table faces the front surface of the target support and is far away from the central axis of the plasma source.
14. The apparatus for ion assisted, tilted sputtering, reactive sputtering deposition of thin films according to claim 13, wherein: a top magnet and/or a bottom magnet are arranged in the process cavity, the top magnet is located at the plasma source, and the bottom magnet is located at the substrate table.
15. The apparatus for ion assisted, tilted sputter, reactive sputter deposition of thin films as claimed in claim 14, wherein: the top magnet is arranged at an angle of 0-90 degrees with the central axis of the plasma source, and the bottom magnet is arranged at an angle of 0-90 degrees with the central line of the substrate table.
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