CN112111715A - Method and system for improving sheet resistance stability of high-resistance film - Google Patents

Method and system for improving sheet resistance stability of high-resistance film Download PDF

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Publication number
CN112111715A
CN112111715A CN202011001933.4A CN202011001933A CN112111715A CN 112111715 A CN112111715 A CN 112111715A CN 202011001933 A CN202011001933 A CN 202011001933A CN 112111715 A CN112111715 A CN 112111715A
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chamber
coating
resistance film
improving
sheet resistance
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Inventor
陈明飞
王金科
朱启煌
刘永成
龙泷
谭宏
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Enam Optoelectronic Material Co ltd
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Enam Optoelectronic Material 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
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34Sputtering
    • 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
    • C23C14/08Oxides
    • C23C14/083Oxides of refractory metals or yttrium
    • 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
    • C23C14/086Oxides of zinc, germanium, cadmium, indium, tin, thallium or bismuth
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01BCABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B5/00Non-insulated conductors or conductive bodies characterised by their form
    • H01B5/14Non-insulated conductors or conductive bodies characterised by their form comprising conductive layers or films on insulating-supports

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  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
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  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physical Vapour Deposition (AREA)

Abstract

The invention discloses a method and a system for improving the sheet resistance stability of a high-resistance film, which comprises the following steps: sputtering a target material on the substrate cleaned by the plasma through a vacuum sputtering method to obtain the high-resistance film; the temperature of the substrate is 90-150 ℃; the distance between the target and the substrate is 90-120 mm. The preparation method improves the preparation process of the high-resistance film, and improves the sheet resistance stability of the film layer; the process gas in the scheme of the invention is blown to the target surface, so that oxygen in the sputtering atmosphere is fully contacted with the sputtered target material atomic group, the high-resistance film is fully oxidized, and the sheet resistance stability of the high-resistance film is further improved.

Description

Method and system for improving sheet resistance stability of high-resistance film
Technical Field
The invention relates to the technical field of display devices, in particular to a method and a system for improving the sheet resistance stability of a high-resistance film.
Background
With the development of the internet, electronic devices have occupied more and more places in people's daily life. Touch screens are important components of electronic devices such as mobile phones, tablet computers, electronic books and the like, and can be generally divided into an external embedded (On-Cell) and an embedded (In-Cell) according to the composition structure, wherein the external embedded (On-Cell) refers to a method for embedding a touch panel between a color filter substrate and a polarizer of a display screen, namely, a touch sensor is arranged On a liquid crystal panel, and due to the fact that a touch layer is additionally arranged, the touch sensor is thick, and the color is prone to be uneven during touch control. In-Cell (In-Cell) is a method of embedding touch panel functions into liquid crystal pixels, that is, embedding touch sensor functions into a display screen, so that the thickness of the entire module can be reduced and the manufacturing cost of the touch screen can be greatly reduced.
In order to prevent the external electric field from adversely affecting the embedded touch screen, a special film material (i.e., a high resistance film) is usually required to be plated on the In-Cell surface to form a thin film with high impedance and good conductivity to achieve the functions of preventing touch signal interference and static electricity, so the performance of the high resistance film is directly related to the touch effect of the embedded touch screen. The high-resistance film is thin and large in sheet resistance, performance requirements such as static resistance and the like of increasingly light and thin electronic display screens can be well met, however, the high-resistance film in the prior art is placed in a normal-temperature environment test process due to the fact that electrons and oxygen vacancies are needed to conduct electricity, oxygen in the high-resistance film overflows into the environment or oxygen in the environment permeates into the high-resistance film, and the oxygen vacancies in the high-resistance film change, so that the sheet resistance of the high-resistance film changes.
Therefore, it is of great significance to improve the manufacturing process of the high-resistance film to improve the sheet resistance stability.
Disclosure of Invention
The present invention is directed to solving at least one of the problems of the prior art. Therefore, the invention provides a method for improving the sheet resistance stability of a high-resistance film, which can effectively improve the sheet resistance stability of the film.
The invention also provides a system for improving the stability of the sheet resistance of the high-resistance film.
A method according to an embodiment of the invention comprises the steps of:
sputtering a target material on the substrate cleaned by the plasma through a vacuum sputtering method to obtain the high-resistance film; the method is characterized in that: the temperature of the substrate is 90-150 ℃; the distance between the target and the substrate is 90-120 mm.
According to some embodiments of the invention, the target is an indium oxide doped zirconia ceramic target; preferably, the ratio of the amounts of indium and zirconium is 1 (0.3 to 0.5).
According to some embodiments of the invention, the process gas used in the vacuum sputtering method is Ar and O2A mixture of (a); the partial pressure of Ar is 0.1-0.25 Pa, and O is2The partial pressure of (A) is between 0.01 and 0.025 Pa.
According to some embodiments of the invention, the process gas is blown against the target surface. The process gas in the scheme of the invention is blown to the target surface, so that oxygen in the sputtering atmosphere is fully contacted with the sputtered target material atomic group, the high-resistance film is fully oxidized, and the sheet resistance stability of the high-resistance film is further improved.
According to some embodiments of the invention, the substrate temperature is 100 to 150 ℃.
According to some embodiments of the invention, the target surface magnetic field strength is 200-600 gauss; preferably, the magnetic field intensity of the target surface is 400-600 gauss.
According to some embodiments of the present invention, the distance between the target and the substrate is 90 to 120 mm; preferably, the distance between the target and the substrate is 100-120 mm.
And adjusting the temperature of the substrate, the magnetic field intensity of the target surface, the target base distance, the sputtering air pressure and the sputtering power, and synergistically improving the energy of the target material atomic groups when the target material atomic groups are deposited on the surface of the substrate.
According to some embodiments of the invention, the process gas is distributed in a multi-stage manner. Through multistage formula gas distribution, improve the homogeneity of gas distribution, further improve the stability of rising resistance film.
According to some embodiments of the invention, the method further comprises plasma cleaning the substrate prior to sputter coating the substrate. By online vacuum plasma cleaning, the surface condition is improved, the film adhesion is improved, and the film growth is improved. The plasma cleaning can be realized by arranging a plasma cleaning plate or a plasma generator and the like. The intensity of plasma cleaning can be confirmed using white glass, and the cleaning intensity is increased without affecting the transmittance of the white glass.
According to some embodiments of the invention, the method further comprises the operation of removing moisture before coating; preferably, the background vacuum of the device during sputtering is < 5 x 10-04Pa. Background vacuum of the device is lower than 5 x 10-4Pa, ensuring that the vacuum system is airtight, releasing water vapor from the substrate and the substrate frame, and performing water vapor removal operation before film coating so as to improve the stability of the device.
The method according to the embodiment of the invention has at least the following beneficial effects: according to the invention, the preparation process of the high-resistance film is improved, the sheet resistance stability of the film layer is improved, and the high-resistance film prepared by the process of the scheme of the invention can be stored for a long time.
The system comprises a loading chamber, a coating chamber and a unloading chamber which are connected with each other in sequence, wherein the coating chamber is connected with the loading chamber or the unloading chamber through a buffer chamber respectively;
the device comprises a coating chamber, a sputtering chamber, a target material and a gas distribution mechanism, wherein the coating chamber comprises a coating section, the sputtering chamber is arranged in the coating section, the target material and the gas distribution mechanism are arranged in the sputtering chamber and used for coating, the gas distribution mechanism comprises a base, a gas distribution pipeline, a ground plate and a gas guide plate, the ground plate and the gas guide plate are fixedly arranged on the base, a gas guide groove is arranged between the gas guide plate and the ground plate, a gas guide hole is arranged in the ground plate, and the gas distribution pipeline is communicated with the gas guide groove through the gas guide hole; the air guide grooves are distributed on two sides of the target material and are higher than the upper surface of the target material. The gas guide plate is positioned above the target material, and a groove structure is arranged on one surface of the gas guide plate facing the target material, so that gas is blown to the target surface along the groove of the gas guide plate.
According to some embodiments of the invention, the gas distribution mechanism is a plurality of groups; preferably, there are two per group. The multi-group distribution mechanism promotes the uniformity of air distribution, and further synergistically promotes the stability of the high-resistance film sheet resistance.
According to some embodiments of the invention, the number of coating sections is at least one; transition sections are arranged at the front and the rear of each coating section. And a transition section is arranged to reduce the atmosphere interference between coating sections.
According to some embodiments of the invention, a water vapor removing device is arranged in the buffer chamber and/or the over-plating section at the front end of the first film-plating section; the moisture removing device is selected from at least one of a cold trap or a condensate pump. And removing water vapor released by the cavity, the substrate frame, the substrate and the like, and eliminating the influence of the water vapor on the sputtering process.
According to some embodiments of the invention, a heating device is arranged in the buffer chamber and/or the coating chamber; preferably, the heating means comprises a multi-segment or multi-segment control heating panel. The multi-section heating is adopted, and the temperature uniformity of the substrate is improved.
According to some embodiments of the invention, the system comprises a pre-coating cleaning line, the pre-coating cleaning line being a water cleaning line. And cleaning by a water washing mechanism to remove the dirt on the surface of the substrate.
According to some embodiments of the invention, the washing line is provided with a drying mechanism at an end thereof, the drying mechanism comprising an air knife blowing mechanism and/or an infrared heater. Clean compressed air is introduced by an air knife to blow dry the water on the surface of the substrate or remove the water vapor on the surface of the substrate by infrared heating.
According to some embodiments of the invention, a plasma cleaning mechanism is arranged in a buffer chamber or a coating chamber at the front end of the coating chamber; preferably, the plasma cleaning mechanism is a plasma cleaning plate or a plasma generator; if the plasma cleaning plate is used, the plasma cleaning mechanism is positioned in the buffer chamber; if the plasma generator is used, the plasma cleaning mechanism is positioned in the film coating chamber. The substrate is cleaned by vacuum plasma on line through a coating line, so that the surface condition is improved, the adhesive force of the film layer is improved, and the growth of the film layer is improved.
The device according to the embodiment of the invention has at least the following advantages: the device of the scheme of the invention is used for preparing the high-resistance film, so that the high-resistance film with better sheet resistance stability can be obtained; install new air guide plate additional on former ground plate to set up the air guide groove in air guide plate bottom, the trench position is higher than the target surface, makes gaseous air guide groove along the air guide plate blow to the target surface, improves target position gas distribution mode ingeniously, makes process gas blow to the target surface, makes the oxygen in the sputtering atmosphere fully contact with the target material radical of sputtering, and then makes high resistant film sheet resistance stability better.
Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention.
Drawings
FIG. 1 is a top view of an air distribution mechanism in an embodiment of the present invention;
FIG. 2 is a sectional view taken along line A-A of FIG. 1;
FIG. 3 is an enlarged view of a portion I of FIG. 2;
fig. 4 is an overall view of a prior art gas distribution mechanism.
Description of reference numerals:
1. a target material; 2. a gas distribution mechanism; 21. a gas distribution pipeline; 22. a ground plate; 23. a gas guide plate; 231. and a gas guide groove.
Detailed Description
In order to explain technical contents, achieved objects, and effects of the present invention in detail, the following description is made with reference to the accompanying drawings in combination with the embodiments. The test methods used in the examples are all conventional methods unless otherwise specified; the materials, reagents and the like used are commercially available reagents and materials unless otherwise specified. The structure which is not particularly described in the coating system of the scheme of the invention adopts the structure of a conventional coating system. The term "target surface" refers to "upper surface of the target material", and the term "base distance" refers to "distance between the target material and the substrate".
The embodiment of the invention is as follows: a method for improving the sheet resistance stability of a high-resistance film comprises the following steps: sputtering a target material on a substrate by a vacuum sputtering method to obtain the high-resistance film; wherein, the process gas adopted by the vacuum sputtering method is high-purity Ar (99.999%) and high-purity O2(99.999%) mixture, partial pressure of Ar 0.15Pa, O2The partial pressure of the catalyst is 0.015-0.018 Pa; the process gas is blown to the target surface, and other process parameters are as follows:
target material: indium oxide doped zirconia ceramic target material, wherein the mass ratio of indium to zirconium is 1: 0.35.
substrate temperature: 130 ℃.
A sputtering power supply: a direct current pulse power supply.
Magnetic field intensity of sputtering cathode target surface: 400 gauss.
The distance between the target and the substrate is 100 mm.
A washing line is arranged for cleaning before film coating, a hairbrush is adopted for cleaning in the washing line, and the hairbrush is dried and baked by an air knife.
Plasma cleaning: 2kW, 90 s.
Background vacuum of a sputtering chamber: not more than 1.33 x 10-3Pa。
Sputtering power: 1.5W/cm2
And (3) coating area running speed: 1.1 m/min.
Substrate: alkali-free glass (glass substrates are commonly used for LCD cells).
The process is realized by a film coating system which sequentially comprises a film loading chamber, a first buffer chamber, a film coating chamber, a second buffer chamber and a film unloading chamber which are connected with each other; the coating chamber sequentially comprises a first transition section, a coating section and a second transition section, a sputtering chamber is arranged in the coating section, a target material 1 for coating and a gas distribution mechanism 2 are arranged in the sputtering chamber, as shown in fig. 1-3, the gas distribution mechanism 2 comprises a base, a gas distribution pipeline 21, a grounding plate 22 and a gas guide plate 23, the grounding plate 22 and the gas guide plate 23 are fixedly arranged on the base, a gas guide groove 231 is arranged between the gas guide plate 23 and the grounding plate 22, a gas guide hole is arranged in the grounding plate 22, and the gas distribution pipeline 21 is communicated with the gas guide groove 231 through the gas guide hole; the air guide grooves 231 are distributed on both sides of the target 1 and are higher than the upper surface of the target 1. A new air guide plate 23 is additionally arranged on the original grounding plate 22, the air guide plate 23 is of a 7-shaped structure, a groove is formed in the bottom of the air guide plate, the position of the groove is higher than that of the target surface, and air is blown to the target surface along the groove of the air guide plate 23.
At least one coating section is provided; transition sections are arranged at the front and the rear of each coating section.
The first buffer chamber and the first over-plating section are respectively provided with a cold trap, and the first buffer chamber is also internally provided with a vacuum plasma cleaning mechanism.
The sheet resistance values and changes of the high resistance films prepared under different oxygen partial pressures are shown in the following table 1:
TABLE 1
Figure BDA0002694638500000061
The table shows that the high-resistance film prepared by the scheme of the invention has high sheet resistance and good stability even after being placed for 28 days (at normal temperature, the humidity is 50-70%).
The comparative example of the invention is: the preparation process of the high-resistance film is different from the embodiment in that plasma cleaning is not adopted, the partial pressure of Ar is 0.4Pa, and O is adopted2The partial pressure is between 0.025Pa and 0.030Pa, a conventional gas distribution mode (shown in figure 4) is adopted, gas guide grooves are respectively arranged at two sides of the target material, gas holes are arranged in the grooves, gas enters an internal gas path of the target position from an external gas path, is sprayed out from the gas holes of the gas guide grooves, passes through the gas holes of the grounding plate and enters a target position area. The sheet resistance values and changes thereof of the high resistance films prepared under different oxygen partial pressures are shown in the following table 2:
TABLE 2
Figure BDA0002694638500000062
In addition, the sheet resistance changes of the substrate at the temperature of 60 ℃, the target base distance of 80mm and the target surface magnetic field intensity of 800 gauss are respectively considered, and the results show that the substrate, the target surface magnetic field intensity, the target base distance, the sputtering air pressure and the sputtering power have certain synergistic effect on improving the stability of the high-resistance film, and the change has certain change, but the change amplitude influence is about 10 times.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all equivalent changes made by using the contents of the present specification and the drawings, or applied directly or indirectly to the related technical fields, are included in the scope of the present invention.

Claims (10)

1. A method for improving the sheet resistance stability of a high-resistance film is characterized by comprising the following steps: the method comprises the following steps: sputtering a target material on the substrate cleaned by the plasma through a vacuum sputtering method to obtain the high-resistance film; the temperature of the substrate is 90-150 ℃; the distance between the target and the substrate is 90-120 mm.
2. The method for improving sheet resistance stability of a high resistance film according to claim 1, wherein: the method also comprises the operation of removing water vapor before coating.
3. The method for improving sheet resistance stability of a high resistance film according to claim 1, wherein: the process gas adopted by the vacuum sputtering method is Ar and O2A mixture of (a); the partial pressure of Ar is 0.05-0.25 Pa, and O is2The partial pressure of (A) is between 0.01 and 0.025 Pa.
4. The method for improving sheet resistance stability of high resistance film according to claim 3, wherein: the process gas is blown against the target surface.
5. The method for improving sheet resistance stability of a high resistance film according to claim 1, wherein: the magnetic field intensity of the target surface is 200-600 gauss; preferably, the magnetic field intensity of the target surface is 400-600 gauss.
6. The method for improving sheet resistance stability of a high resistance film according to claim 1, wherein: the method also comprises the operation of removing water vapor before film coating; preferably, the background vacuum of the device during sputtering is < 5 x 10-04Pa。
7. A system for improving the stability of high-resistance film sheet resistance sequentially comprises a sheet loading chamber, a film coating chamber and a sheet unloading chamber which are connected with each other, wherein the film coating chamber is connected with the sheet loading chamber or the sheet unloading chamber through a buffer chamber respectively; the method is characterized in that:
the device comprises a coating chamber, a sputtering chamber, a target material and a gas distribution mechanism, wherein the coating chamber comprises a coating section, the sputtering chamber is arranged in the coating section, the target material and the gas distribution mechanism are arranged in the sputtering chamber and used for coating, the gas distribution mechanism comprises a base, a gas distribution pipeline, a ground plate and a gas guide plate, the ground plate and the gas guide plate are fixedly arranged on the base, a gas guide groove is arranged between the gas guide plate and the ground plate, a gas guide hole is arranged in the ground plate, and the gas distribution pipeline is communicated with the gas guide groove through the gas guide hole; the air guide grooves are distributed on two sides of the target material and are higher than the upper surface of the target material.
8. The system for improving the sheet resistance stability of a high resistance film according to claim 7, wherein: the air distribution mechanisms are in a plurality of groups; preferably, there are two per group.
9. The system for improving the sheet resistance stability of a high resistance film according to claim 7, wherein: at least one coating section is arranged, and transition sections are arranged at the front and the rear of each coating section; preferably, a water vapor removing device is arranged in the buffer chamber and/or the over-plating section which is positioned at the front end of the first film plating section; the moisture removing device is selected from at least one of a cold trap or a condensate pump.
10. The system for improving the sheet resistance stability of a high resistance film according to claim 7, wherein: a plasma cleaning mechanism is arranged in a buffer chamber or a coating chamber at the front end of the coating chamber; preferably, the plasma cleaning mechanism is a plasma cleaning plate or a plasma generator.
CN202011001933.4A 2020-09-22 2020-09-22 Method and system for improving sheet resistance stability of high-resistance film Pending CN112111715A (en)

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