CN113667955A - Plastic surface metallization reactive sputtering plasma control system and method - Google Patents

Plastic surface metallization reactive sputtering plasma control system and method Download PDF

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Publication number
CN113667955A
CN113667955A CN202111033753.9A CN202111033753A CN113667955A CN 113667955 A CN113667955 A CN 113667955A CN 202111033753 A CN202111033753 A CN 202111033753A CN 113667955 A CN113667955 A CN 113667955A
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plasma
reactive sputtering
gas
controller
information
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毕君
高原
田先亮
郭大伊
黄安琪
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Guangdong Industry Technical College
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Guangdong Industry Technical College
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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
    • C23C14/22Coating 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
    • C23C14/542Controlling the film thickness or evaporation rate
    • 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
    • C23C14/0042Controlling partial pressure or flow rate of reactive or inert gases with feedback of measurements
    • 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
    • C23C14/34Sputtering
    • C23C14/3464Sputtering using more than one target
    • 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
    • C23C14/34Sputtering
    • C23C14/35Sputtering by application of a magnetic field, e.g. magnetron sputtering
    • C23C14/352Sputtering by application of a magnetic field, e.g. magnetron sputtering using more than one target
    • 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
    • C23C14/542Controlling the film thickness or evaporation rate
    • C23C14/544Controlling the film thickness or evaporation rate using measurement in the gas phase
    • 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
    • C23C14/548Controlling the composition

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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)
  • Physics & Mathematics (AREA)
  • Fluid Mechanics (AREA)
  • Physical Vapour Deposition (AREA)

Abstract

The invention discloses a system and a method for controlling a metallized reactive sputtering plasma on a plastic surface, and relates to a metallized vacuum reactive sputtering coating technology on the plastic surface. The method is provided aiming at the problem of single closed-loop feedback in the prior art, and comprises the steps of obtaining target current and voltage information, plasma spectrum information and gas partial pressure information in real time and inputting the target current and voltage information, the plasma spectrum information and the gas partial pressure information into a controller in the step of forming a thin film on the surface of a substrate through reactive sputtering of a target material, and the controller adjusts the flow rate of mixed gas and/or adjusts the target current and voltage so as to stabilize the sputtering deposition rate and the components of the sputtered thin film. The method has the advantages that spectrum feedback is taken as a main part, gas feedback and current and voltage feedback are considered, faster, more accurate and more stable control is achieved, and the uniformity of the coating film can be improved.

Description

Plastic surface metallization reactive sputtering plasma control system and method
Technical Field
The invention relates to a plastic surface metallization vacuum reactive sputtering coating technology, in particular to a plastic surface metallization reactive sputtering plasma control system and a plastic surface metallization reactive sputtering plasma control method.
Background
As is well known, vacuum coating technology is widely used in many industries, and is called as a key core technology in industries such as flat panel display, solar photovoltaic, new electronic information, energy-saving glass, and the like. The challenge of the vacuum coating process technology in the future market lies in the large-scale production of high-quality precision optical films, electrical films and the like. At present, with the progress of magnetron sputtering technology and the technological breakthrough of sputtering technology monitoring, the method is gradually applied to the preparation of high-quality optical films.
The reactive sputtering method is a technique for forming a compound thin film, and the conventional method, reactive sputtering, in which the flow rate of a reactive gas is initially set so that sputtering is in an appropriate oxidation mode, belongs to open-loop control. When the technological parameters are changed, the gas flow and the target current voltage cannot be automatically adjusted, so that the reaction is insufficient, the sputtering rate is changed, and the coating is uneven. Particularly, for some metal targets such as titanium, nickel, niobium and the like, the reaction sputtering hysteresis curve is narrow, the working process is not easy to be stably controlled, and the defects of low sputtering rate, unsatisfactory quality of a deposited film layer, unstable control repeatability of metal compound components, arc striking, target poisoning and the like exist.
The improvement measures generally adopt a closed-loop control system, a gas sensor is used for detecting the back pressure of reaction gas in the reactive sputtering, and a mass flow meter is used for adjusting the flow rate of the reaction gas to realize the control of the components of the compound. For smaller substrates, this closed loop control of a single supervisory channel can be effective. When a substrate with a large area and a high requirement for uniformity of a film layer are required at that time, it is difficult to realize high-speed, precise and stable control by using only a single input control of a gas sensor, which brings a difficulty in producing a compound thin film with high performance and high quality.
Disclosure of Invention
The invention aims to provide a system and a method for controlling a plastic surface metallization reactive sputtering plasma, so as to solve the control problem caused by a large substrate area.
The invention relates to a method for controlling metallized reactive sputtering plasma on the surface of plastic, which comprises the following steps:
vacuumizing the vacuum coating chamber;
introducing mixed gas into the vacuum coating chamber;
a step of forming a plasma reactive sputtering region by glow discharge;
forming a film on the surface of the substrate by reactive sputtering of a target material;
in the step of forming a film on the surface of a substrate by reactive sputtering of a target material, target current and voltage information, plasma spectrum information and gas partial pressure information are acquired in real time and input into a controller, and the controller adjusts the flow rate of mixed gas and/or adjusts the target current and voltage, so that the sputtering deposition rate is stable and the components of the sputtered film are stable.
The specific steps for acquiring the plasma spectrum information are as follows: and obtaining the intensity of a specific spectrum in the plasma reactive sputtering emission spectrum, carrying out difference operation through filtering, amplification and preset working point signals, and feeding back an operation result to the controller.
The specific steps for acquiring the gas partial pressure information are as follows: and detecting the partial pressure value of the mixed gas, converting the ratio of the partial pressure value to the total pressure value of the vacuum coating chamber into a potential signal, and feeding the potential signal back to the controller after amplifying the potential signal.
The specific steps for acquiring the target current and voltage information are as follows: amplifying the error between the output value and the given value by using a high-gain operational amplifier, and if the output value deviates from the given value, feeding the output error of the amplifier back to the controller; the output value is a voltage value of the power supply.
According to the output error and the potential signal, the controller adjusts the pulse width of the power supply to stabilize the output voltage value at a given voltage value.
Twin targets are used as target-type structures for reactive sputtering.
The collection position of the plasma spectrum information at least comprises two ends of the plasma reaction sputtering area.
The collection position of the plasma spectrum information also comprises the middle position of the plasma reactive sputtering area.
The mixed gas is a mixture of a working gas and a reaction gas.
A plasma control system for metallized reactive sputtering of plastic surface comprises a vacuum coating chamber, a power supply, a controller and a piezoelectric valve, wherein the power supply, the controller and the piezoelectric valve are arranged outside the vacuum coating chamber; the piezoelectric valve is used for mixing gas flow;
a gas inlet, an optical fiber probe and a gas sensor are arranged in the vacuum coating chamber;
the controller carries out film coating by using the plastic surface metallization reaction sputtering plasma control method.
The invention relates to a system and a method for controlling metallized reactive sputtering plasma on the surface of plastic, which at least comprise the following advantages:
1. and (3) acquiring target current and voltage information, plasma spectrum information and gas partial pressure information respectively by adopting multi-channel sensing feedback, and performing comprehensive control through an algorithm. The spectrum feedback is taken as the main point, and the gas feedback and the current and voltage feedback are considered, so that the control is quicker, more accurate and more stable.
2. Because the installation position of the optical probe directly determines the spectrum characteristic signal acquisition effect, the invention carries out measurement at the two ends and the middle position of the plasma reactive sputtering area, can monitor the reaction condition of the whole sputtering area in real time, has more accurate feedback spectrum information and can improve the uniformity of coating.
3. The plasma reaction spectrum and the monitoring of the gas partial pressure are combined, so that the precise control of the metal compound components can be realized.
4. The rapid feedback real-time control of the sputtering process is realized through potential signals of the ratio of the partial pressure of the gas to the total pressure of the vacuum chamber, the feedback of the target current and the voltage and the like, and the stability of the sputtering deposition rate is realized.
Drawings
FIG. 1 is a schematic structural diagram of a plasma control system for the metallization reaction sputtering of a plastic surface according to the present invention.
FIG. 2 is a schematic diagram of a plasma control system for the metallization reaction sputtering of a plastic surface according to the present invention.
Reference numerals: the device comprises a vacuum coating chamber 1, a substrate 2, a gas inlet 3, a fiber probe 4, a gas sensor 5, a baffle plate 6, a target 7, a power supply 8, a controller 9, a reaction gas flow piezoelectric valve 10 and a working gas flow piezoelectric valve 11.
Detailed Description
The invention relates to a plastic surface metallization reactive sputtering plasma control system, which is shown in figure 1 and comprises a vacuum coating chamber 1, wherein a substrate 2 is arranged in the vacuum coating chamber 1, and a target 7 is arranged on the other side opposite to the substrate 2. A gas inlet 3 is provided between the substrate 2 and the target 7, and a fiber probe 4 and a gas sensor 5 are provided on the side of the gas inlet 3 near the target 7.
A reaction gas flow piezoelectric valve 10, a working gas flow piezoelectric valve 11, a power supply 8 and a controller 9 are arranged outside the vacuum coating chamber 1.
And the voltage output end of the power supply 8 extends into the vacuum coating chamber 1 and is connected with the target 7.
The output ends of the reaction gas flow piezoelectric valve 10 and the working gas flow piezoelectric valve 11 are collinear and then extend into the vacuum coating chamber 1 to be communicated with the gas inlet 3.
The controller 9 is respectively and electrically connected with a control end of the power supply 8, a feedback end of the optical fiber probe 4, a feedback end of the gas sensor 5, a control end of the reaction gas flow piezoelectric valve 10 and a control end of the working gas flow piezoelectric valve 11.
The target 7 is a twin target.
The vacuum coating chamber 1 is provided with shielding plates 6 at two ends of a target 7 respectively.
The gas inlet 3 and the gas sensor 5 are respectively and symmetrically arranged at two ends of the target 7.
The controller 9 is also electrically connected with the feedback end of the power supply 8.
The fiber probe 4 is provided in plural, for example, also at both ends and at a middle position of a plasma reactive sputtering zone between the target 7 and the substrate 2.
The control method of the metallized reactive sputtering plasma on the surface of the plastic can be realized by using the control system, and the working principle of the control system is shown in figure 2.
Firstly, extracting partial vacuum in a vacuum coating chamber to reach a certain vacuum degree; and setting the process parameter information of the controller in advance according to the specific process requirement.
Then, a preset mixed gas is introduced into the vacuum coating chamber. The mixed gas is obtained by mixing working gas and reaction gas.
And presetting target current voltage, so that the working gas and the reaction gas glow discharge form a plasma reactive sputtering area, and the target material is sputtered on the surface of the substrate to form a film.
The change of the reactive sputtering state is judged through the multi-channel sensing feedback circuit, the flow of the working gas and the flow of the reactive gas are adjusted in real time according to the change of the reactive sputtering state, and the stability of the sputtering current and the sputtering voltage is kept.
And finally, the whole reactive sputtering process is controlled by the controller in real time through multi-path closed loop feedback:
the optical fiber probes 4 acquire emission spectrum information in the plasma, and the wavelength of specific light is acquired through the band-pass filter, so that the reaction degree of the materials and the gas is monitored and fed back to the controller 9. The controller 9 adjusts the target current voltage and the working gas and reaction gas partial pressures by an algorithm.
The gas sensor 5 obtains the partial pressure of the gas in the vacuum and feeds the gas back to the controller 9 directly. The controller 9 controls the introduced reaction gas by adjusting the reaction gas flow piezoelectric valve 10 through an algorithm, and controls the flow of the working gas by the working gas flow piezoelectric valve 11.
For the twin target structure, the power supply 8 has two output terminals for electrical connection respectively for providing a working voltage to the target. Two output terminals and a control terminal of the power supply 8 are respectively connected to the controller 9, and if the voltage value of the fed back output terminal deviates from the voltage set value, the controller 9 corrects the pulse width of the power supply 8, thereby stabilizing the output voltage value at the voltage set value.
The whole reactive sputtering plasma control system takes plasma spectrum feedback as a main part, gives consideration to multi-channel sensing feedback of gas feedback and target current and voltage feedback, and controls the power supply 8 and the two piezoelectric valves through the controller 9 to better control the whole reactive sputtering process.
It will be apparent to those skilled in the art that various other changes and modifications may be made in the above-described embodiments and concepts and all such changes and modifications are intended to be within the scope of the appended claims.

Claims (10)

1. A plastic surface metallization reactive sputtering plasma control method comprises the following steps:
vacuumizing the vacuum coating chamber;
introducing mixed gas into the vacuum coating chamber;
a step of forming a plasma reactive sputtering region by glow discharge;
forming a film on the surface of the substrate by reactive sputtering of a target material;
it is characterized in that the preparation method is characterized in that,
in the step of forming a film on the surface of a substrate by reactive sputtering of a target material, target current and voltage information, plasma spectrum information and gas partial pressure information are acquired in real time and input into a controller, and the controller adjusts the flow rate of mixed gas and/or adjusts the target current and voltage, so that the sputtering deposition rate is stable and the components of the sputtered film are stable.
2. The method for controlling the sputtering plasma for the metallization reaction on the surface of the plastic as claimed in claim 1, wherein the specific steps for obtaining the spectral information of the plasma are as follows: and obtaining the intensity of a specific spectrum in the plasma reactive sputtering emission spectrum, carrying out difference operation through filtering, amplification and preset working point signals, and feeding back an operation result to the controller.
3. The method for controlling the sputtering plasma of the metallization reaction on the surface of the plastic as claimed in claim 2, wherein the specific steps of obtaining the information of the partial pressure of the gas are as follows: and detecting the partial pressure value of the mixed gas, converting the ratio of the partial pressure value to the total pressure value of the vacuum coating chamber into a potential signal, and feeding the potential signal back to the controller after amplifying the potential signal.
4. The method for controlling the sputtering plasma of the metallization reaction on the surface of the plastic as claimed in claim 3, wherein the specific steps of obtaining the target current and voltage information are as follows: amplifying the error between the output value and the given value by using a high-gain operational amplifier, and if the output value deviates from the given value, feeding the output error of the amplifier back to the controller; the output value is a voltage value of the power supply.
5. The method as claimed in claim 4, wherein the controller adjusts the pulse width of the power supply to stabilize the output voltage at a predetermined value according to the output error and the potential signal.
6. A plastic surface metallization reactive sputtering plasma control method as claimed in claim 1 wherein a twin target is used as the reactive sputtering target type structure.
7. The method as claimed in claim 1, wherein the collection position of the plasma spectrum information at least comprises two ends of the plasma reactive sputtering region.
8. The method as claimed in claim 7, wherein the position for collecting the spectral information of the plasma further includes a middle position of the reactive sputtering region of the plasma.
9. The method as claimed in claim 1, wherein the mixed gas is a mixture of working gas and reactive gas.
10. A plasma control system for the metallized reactive sputtering of a plastic surface is characterized by comprising a vacuum coating chamber, a power supply, a controller and a piezoelectric valve, wherein the power supply, the controller and the piezoelectric valve are arranged outside the vacuum coating chamber; the piezoelectric valve is used for mixing gas flow;
a gas inlet, an optical fiber probe and a gas sensor are arranged in the vacuum coating chamber;
the controller is used for coating by using a plastic surface metallization reactive sputtering plasma control method as claimed in any one of claims 1 to 9.
CN202111033753.9A 2021-09-03 2021-09-03 Plastic surface metallization reactive sputtering plasma control system and method Pending CN113667955A (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103866248A (en) * 2014-04-02 2014-06-18 广州市光机电技术研究院 Reactive sputtering plasma control system and method
CN107630201A (en) * 2017-10-30 2018-01-26 广州市光机电技术研究院 A kind of reactive sputter-deposition rate stabilization control system and method

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103866248A (en) * 2014-04-02 2014-06-18 广州市光机电技术研究院 Reactive sputtering plasma control system and method
CN107630201A (en) * 2017-10-30 2018-01-26 广州市光机电技术研究院 A kind of reactive sputter-deposition rate stabilization control system and method

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