WO2021109377A1 - Coating equipment for preparing dlc and use thereof - Google Patents

Coating equipment for preparing dlc and use thereof Download PDF

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Publication number
WO2021109377A1
WO2021109377A1 PCT/CN2020/082801 CN2020082801W WO2021109377A1 WO 2021109377 A1 WO2021109377 A1 WO 2021109377A1 CN 2020082801 W CN2020082801 W CN 2020082801W WO 2021109377 A1 WO2021109377 A1 WO 2021109377A1
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Prior art keywords
chamber
power supply
gas
coating
pipeline
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PCT/CN2020/082801
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French (fr)
Chinese (zh)
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宗坚
张琳
代莹静
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江苏菲沃泰纳米科技有限公司
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Publication of WO2021109377A1 publication Critical patent/WO2021109377A1/en

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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
    • C23C16/00Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/26Deposition of carbon only
    • 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
    • C23C16/00Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/4401Means for minimising impurities, e.g. dust, moisture or residual gas, in the reaction chamber
    • C23C16/4408Means for minimising impurities, e.g. dust, moisture or residual gas, in the reaction chamber by purging residual gases from the reaction chamber or gas lines
    • 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
    • C23C16/00Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/455Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
    • 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
    • C23C16/00Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/458Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for supporting substrates in the reaction chamber
    • C23C16/4582Rigid and flat substrates, e.g. plates or discs
    • C23C16/4583Rigid and flat substrates, e.g. plates or discs the substrate being supported substantially horizontally
    • 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
    • C23C16/00Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/50Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating using electric discharges
    • C23C16/505Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating using electric discharges using radio frequency discharges
    • C23C16/509Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating using electric discharges using radio frequency discharges using internal electrodes
    • C23C16/5096Flat-bed apparatus
    • 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
    • C23C16/00Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/50Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating using electric discharges
    • C23C16/515Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating using electric discharges using pulsed discharges
    • 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
    • C23C16/00Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/54Apparatus specially adapted for continuous coating

Definitions

  • the invention relates to the field of coating, and further relates to a coating equipment for preparing DLC and its application.
  • DLC films Diamond Like Carbon, DLC are integrated to form a recent rise in the form of sp2 and sp 3 bonds metastable material, a short-range order, long range disorder film or film layer. It combines the excellent properties of diamond and graphite.
  • DLC diamond Like Carbon
  • mechanical properties DLC has high hardness and wear resistance, and the hardness related to the components can vary from 20 GPa to 80 GPa; in terms of optical properties, DLC has good light transmittance and anti-reflection function; in addition, DLC also has good properties The thermal conductivity and biocompatibility.
  • coating a layer of DLC film on the surface of glass, ceramics, etc. can further improve the wear resistance and hardness of glass, ceramics, etc.
  • depositing DLC on the plastic surface can also improve the wear resistance and hardness of the plastic surface.
  • the current methods for preparing DLC films can be divided into chemical vapor deposition (CVD) methods and physical vapor deposition (PVD) methods.
  • Chemical vapor deposition is a deposition process that uses the principle of chemical reaction to separate solid phase substances from gas phase substances and deposit them on the working surface to form a coating film. From the perspective of deposition conditions, in order to achieve a chemical reaction between the gas and the substrate interface, there must be a certain amount of activation energy during the deposition reaction. According to the different activation methods, it can be divided into hot filament chemical vapor deposition, laser chemical vapor deposition and plasma enhanced chemical vapor deposition.
  • Physical vapor deposition technology refers to a vapor deposition process performed under vacuum conditions when at least one deposition element is atomized (atomized).
  • the interface can be improved, the deposition rate is high, etc.
  • the specific methods of physical vapor deposition of DLC films mainly include: ion beam deposition, sputtering deposition, vacuum cathodic arc deposition and pulsed laser deposition.
  • Plasma-enhanced chemical vapor deposition (PECVD) method has many characteristics such as low deposition temperature, good winding properties, and uniform and dense films prepared, it has become one of the most commonly used methods for preparing DLC films.
  • Plasma-enhanced chemical vapor deposition is also called glow discharge method.
  • Common plasma-enhanced chemical vapor deposition techniques include: direct current glow discharge method, radio frequency glow discharge method, electron cyclotron resonance (ECR) chemical vapor deposition, etc., in recent years
  • RF-DC radio frequency-direct current glow discharge
  • MW-RF microwave-radio frequency
  • ECR-RF electron cyclotron resonance-radio frequency
  • the preparation process of diamond-like carbon films can be divided into the following four stages: (1) The generation process of the original matrix group, that is, the gas source molecule decomposes into neutral atoms and groups through inelastic collision with high-energy electrons. ; (2) Secondary reaction process, that is, the chemical reaction process between neutral atoms and groups or between neutral atoms and gas molecules; (3) Transmission process, that is, neutral atoms or groups to the surface of the substrate The diffusion process; (4) The surface reaction process, that is, the neutral group reacts with the surface to form a film.
  • the patent number is CN205803582U discloses a device for depositing diamond-like carbon films, which includes a vacuum chamber, a workbench and a vacuum system.
  • the vacuum system is first used to pump the vacuum chamber to working vacuum, the heating system is turned on, and the columnar arc source cleaning device is turned on Clean the workbench. After cleaning, open the rectangular planar arc chromium target to lay the bottom layer, and then open the rectangular planar arc graphite target to deposit the diamond-like carbon film.
  • the graphite target is used as the target material, the ionization rate is low, the deposition efficiency is slow, and there are problems of poor coating quality and high economic cost.
  • the patent number CN101082118A discloses a method for coating a diamond-like carbon film on a high-speed steel metal surface.
  • the method includes a, fixing a metal workpiece on a workpiece turntable in a vacuum chamber of an arc ion plating equipment and vacuuming; b. venting argon Enter the vacuum chamber and keep the vacuum stable, then turn on the ion source to activate the surface of the metal workpiece; c. Turn off the argon gas, load a negative bias between the metal workpiece and the vacuum chamber, and turn on the titanium arc source to deposit the surface of the metal workpiece Titanium transition layer; d.
  • An advantage of the present invention is to provide a coating device for preparing DLC and its application, wherein the coating device is used to coat a DLC film or film on the surface of a substrate to realize large-area coating, thereby realizing mass preparation of DLC film .
  • Another advantage of the present invention is to provide a coating device for preparing DLC and its application, wherein the coating device can etch and activate the surface of the substrate, which is beneficial for preparing the DLC film on the surface of the substrate.
  • Another advantage of the present invention is to provide a coating equipment for preparing DLC and its application, wherein the coating equipment can complete the coating at room temperature or low temperature, and the required time is short, which is beneficial to cost saving.
  • Another advantage of the present invention is to provide a coating equipment for preparing DLC and its application, wherein the coating equipment can be used to coat some substrates that are not resistant to high temperatures, so that the substrate is not easily damaged during the coating process.
  • Another advantage of the present invention is to provide a coating device for preparing DLC and its application, wherein the coating device can detect the reaction temperature in real time to further ensure the safety of the substrate.
  • Another advantage of the present invention is to provide a coating device for preparing DLC and its application, wherein the coating device combines radio frequency and/or pulse voltage to prepare the DLC film.
  • Another advantage of the present invention is to provide a coating device for preparing DLC and its application, wherein the coating device has better process controllability in the process of preparing DLC film, which is beneficial to the rapid preparation of target DLC film.
  • Another advantage of the present invention is to provide a coating equipment for preparing DLC and its application, wherein the coating equipment has a simple structure, is conducive to cleaning, and has a long service life.
  • the present invention further provides a coating equipment for preparing a DLC film on the surface of a substrate, wherein the coating equipment includes:
  • a cavity wherein the cavity has a cavity
  • a set of conveying pipelines A set of conveying pipelines
  • At least one air extraction device At least one air extraction device
  • At least one suction line At least one suction line
  • a power supply device and
  • At least one electrode holder wherein the electrode holder is arranged in the chamber for supporting the substrate, and the delivery pipeline is connected to the chamber and is used to pass gaseous materials into the chamber, wherein
  • the air extraction device is connected to the chamber through the air extraction pipeline and performs a negative pressure operation on the chamber and controls the air pressure in the chamber, wherein the power supply device is electrically connected to the electrode holder to
  • the coating equipment is provided for preparing the DLC film on the surface of the substrate by means of chemical vapor deposition.
  • the cavity has at least one suction port, at least one gas inlet, and at least one feed port communicating with the cavity
  • the delivery pipeline includes at least one gas source pipe, and at least A reaction raw material pipeline
  • the gas extraction port is connected to the gas extraction pipeline
  • the gas source pipeline is connected to the gas inlet for injecting gas into the chamber
  • the reaction raw material A pipe is connected to the feed port for filling the chamber with reaction raw materials.
  • it further comprises a hydrogen pipeline, wherein the hydrogen pipeline and the reaction raw material pipeline are connected to the same feed port, or the hydrogen pipeline and the reaction raw material pipeline are respectively connected to two The feed port.
  • the delivery pipeline further includes a doping raw material pipeline, wherein the doping raw material pipeline is connected to the feed port for filling the chamber with doping element reaction raw materials.
  • the suction port is located in the middle of the chamber, and the gas inlet and the feed port are both located on the side wall of the chamber.
  • the pumping device includes at least one first vacuum pump and at least one second vacuum pump, wherein the second vacuum pump serves as a backing pump of the first vacuum pump and passes through the pumping pipeline in cooperation.
  • a negative pressure operation is performed on the chamber and the air pressure in the chamber is maintained within a preset range.
  • the air in the chamber reduces the air pressure in the chamber to below 0.01 Pa.
  • the air pressure in the chamber is maintained between 0.01 and 100 Pa.
  • the first vacuum pump is implemented as a molecular pump
  • the second vacuum pump is implemented as including a roots pump and a dry pump.
  • the coating equipment further includes an exhaust gas treatment device, wherein the exhaust gas treatment device is connected to the gas extraction pipeline for processing and discharging the gas extracted by the gas extraction device.
  • the power supply device includes a radio frequency power supply and a pulse power supply to provide the radio frequency voltage and the pulse power supply respectively.
  • the power supply device includes a pulse power source, wherein the pulse power source has a positive terminal and a negative terminal, wherein the negative terminal is electrically connected to the electrode holder and provides a negative voltage, wherein the The cavity is grounded, and the electrode holder is insulated from the cavity.
  • the power supply device includes a pulse power supply, wherein the pulse power supply has a positive terminal and a negative terminal, wherein the electrode holder includes a multilayer metal plate, and the positive terminal of the pulse power supply The negative terminal and the negative terminal are respectively electrically connected to the metal plates of the electrode support, and the two adjacent metal plates of the electrode support are mutually positive and negative.
  • the power of the radio frequency voltage of the radio frequency power supply is 10-800W.
  • the pulse power supply provides a pulse bias voltage of -100V to -5000V, a pulse frequency of 20-300KHz, and a duty cycle of 10%-80%.
  • the pulsed power supply is implemented as a unidirectional pulsed power supply, a symmetrical bidirectional pulsed power supply, or an asymmetrical pulsed power supply.
  • the coating equipment further includes a housing, wherein the cavity, the delivery pipeline, the air extraction device, the air extraction pipeline, and the power supply device are all installed in the housing .
  • the present invention also provides a method for coating a DLC thin film, which uses a coating device to prepare the DLC thin film on the surface of a substrate based on hydrocarbon gas as a reaction raw material, including the steps:
  • the step (c) further includes the step of: (c.1) passing gas into the chamber through a gas source pipe, and providing a voltage to act on the gas in the chamber to Performing an etching treatment on the surface of the substrate; and (c.2) passing a reaction raw material gas into the chamber through at least one reaction raw material pipe, and providing a voltage to act on the gas in the chamber so that the substrate The DLC film is prepared on the surface of the material.
  • the gas flow rate of the gas passing into the chamber is 10 sccm to 1000 sccm.
  • the electrode holder is connected to a pulse power source to provide a pulse voltage to act on the gas in the chamber.
  • a negative terminal of the pulse power supply is electrically connected to the electrode holder, the cavity is grounded, and the electrode holder is insulated from the cavity.
  • a positive terminal and a negative terminal of the pulse power supply are respectively electrically connected to the multilayer metal plate of the electrode holder, and two adjacent metal plates of the electrode holder are mutually positive. negative electrode.
  • the electrode holder is connected to a pulse power supply and a radio frequency power supply to provide pulse voltage and radio frequency voltage to act on the gas in the chamber.
  • a second vacuum pump is used as a backing pump of a first vacuum pump to vacuum the chamber in a cooperative manner, wherein the second vacuum pump is implemented to include a dry pump and a roots pump , Wherein the first vacuum pump is implemented as a molecular pump.
  • Fig. 1 is a perspective schematic view of a coating equipment according to a preferred embodiment of the present invention.
  • Fig. 2 is a three-dimensional schematic diagram of the coating equipment according to the above-mentioned preferred embodiment of the present invention from another perspective.
  • Fig. 3 is a perspective schematic view of a second vacuum pump of the air pumping device of the coating equipment according to the above-mentioned preferred embodiment of the present invention.
  • Fig. 4 is a perspective schematic view of the first vacuum pump of the air pumping device of the coating equipment according to the above-mentioned preferred embodiment of the present invention.
  • Fig. 5 is a perspective schematic view of the box body of the coating equipment according to the above-mentioned preferred embodiment of the present invention.
  • Fig. 6 is a structural block diagram of the coating equipment according to the above-mentioned preferred embodiment of the present invention.
  • Fig. 7 is a structural block diagram of the conveying pipeline of the coating equipment according to the above-mentioned preferred embodiment of the present invention.
  • Fig. 8 is a structural block diagram of the air conveying pipeline of the coating equipment according to the above-mentioned preferred embodiment of the present invention.
  • Fig. 9 is a structural block diagram of the power supply device of the coating equipment according to the above-mentioned preferred embodiment of the present invention.
  • Fig. 10 is a perspective schematic view of the support of the coating equipment according to the above-mentioned preferred embodiment of the present invention.
  • the term “a” should be understood as “at least one” or “one or more”, that is, in one embodiment, the number of an element may be one, and in another embodiment, the number of the element The number can be multiple, and the term “one” cannot be understood as a restriction on the number.
  • Figures 1 to 10 show a coating device 100 according to a preferred embodiment of the present invention, wherein the coating device 100 is used for coating at least one layer of DLC film or layer on the surface of at least one substrate 600, wherein The coating equipment 100 can realize large-area coating, so as to realize the simultaneous coating of the DLC film on the surface of the substrate 600 in large quantities.
  • the coating device 100 adopts a plasma chemical vapor deposition method to prepare the DLC film or film layer on the surface of the substrate 600. That is, the DLC film is deposited on the surface of the substrate 600, thereby improving the mechanical, optical, or chemical properties of the surface of the substrate 600, wherein the substrate 600 has a predetermined shape and structure.
  • Products that need to be coated such as PCB circuit boards, mobile phones, electronic equipment, electronic product covers, electronic product display screens, mobile phone glass screens, computer screens, mobile phone back covers, electronic device shells, keyboard films or other types of products that need to be coated, etc.
  • the coating equipment 100 prepares the DLC film on the display screen of an electronic product, which can effectively solve the problems of the display screen of the electronic product that the display screen is not resistant to fall, wear resistance, and the surface strengthening cost is high.
  • the coating equipment 100 includes a cavity 10, a set of conveying pipelines 20, at least one air extraction device 30, at least one air extraction pipeline 40, A power supply device 50 and at least one electrode holder 60, wherein the cavity 10 has a closable cavity 101, wherein the electrode holder 60 is disposed in the cavity 101 of the cavity 10, wherein the The electrode holder 60 is used to support the substrate 600, wherein the delivery pipe 20 is connected to the chamber 101 of the cavity 10, and the delivery pipe 20 is used to feed the cavity 101 Gas raw materials such as plasma source gases such as nitrogen, carbon tetrafluoride or inert gases such as helium and argon, reactive gases such as hydrogen, hydrocarbon gas, or doped N, Si, F, B, etc.
  • plasma source gases such as nitrogen, carbon tetrafluoride or inert gases such as helium and argon
  • reactive gases such as hydrogen, hydrocarbon gas, or doped N, Si, F, B, etc.
  • the air extraction device 30 communicates with the chamber 101 of the cavity 10 through the air extraction line 40 and continuously extracts the gas in the chamber 101 through the air extraction line 40 to control the cavity
  • the DLC film or film layer is prepared on the surface of 600.
  • the cavity 10 has at least one suction port 11, at least one gas inlet 12, and at least one feed port 13 communicating with the cavity 101, wherein the conveying pipe 20 It includes at least one gas source pipeline 21, at least one hydrogen pipeline 22, and at least one reaction raw material pipeline 23, wherein the gas extraction port 11 is connected to the gas extraction pipeline 40 for the gas extraction device 30 to pass through the gas extraction pipeline 40 Extract the gas in the chamber 101, wherein the gas inlet 12 is connected to the gas source pipe 21 for introducing nitrogen, carbon tetrafluoride or helium or argon into the chamber 101 Inert gas or plasma source gas, etc., wherein the feed port 13 is connected to the hydrogen pipeline 22 and the reaction raw material pipeline 23, wherein the hydrogen pipeline 22 is used to pass into the chamber 101 Hydrogen, wherein the reaction raw material pipeline 23 is used to pass the reaction raw materials such as hydrocarbon gas into the chamber 101, such as gaseous raw materials such as alkanes, alkenes, and alkynes with 1-6 carbon atoms.
  • the reaction raw material pipeline 23 is
  • reaction raw material pipeline 23 can be used to transport liquid reaction raw materials, and then the vaporized reaction raw materials are passed into the chamber 101 through the feed port 13.
  • the cavity door of the cavity 10 may be provided with a window for the user to observe the coating condition in the cavity 101.
  • the air inlet 12 and the feed inlet 13 are both provided on the side wall of the cavity 10, wherein the air inlet 12 and the air source pipe 21 are connected in a closed connection, wherein the feed inlet 13 are respectively closed and connected with the hydrogen pipeline 22 and the reaction raw material pipeline 23, such as flange connections such as screw threads, sockets, and buckles.
  • the feed ports 13 are implemented as two, one of the feed ports 13 is used to connect to the hydrogen pipeline 22 for the independent hydrogen gas flow into the chamber 101, and the other The feed port 13 is used to connect to the reaction raw material pipeline 23 for separately passing the reaction raw materials into the chamber 101.
  • the feed port 13 can also be implemented as one, wherein the hydrogen pipe 22 and the reaction raw material pipe 23 are connected to the same feed port 13 together, so as to pass through the same feed port 13 respectively.
  • the feed port 13 passes hydrogen or reaction raw materials into the chamber 101.
  • the delivery pipeline 20 further includes a doping raw material pipeline 24, wherein the doping raw material pipeline 24 is connected to the feed port 13 for filling the chamber 101 with N and Si. , F, B and other auxiliary gases doped with elements.
  • the reaction raw material for the doped Si element includes, but is not limited to, silicon-containing organic compounds, including one of organic linear siloxanes, cyclosiloxanes, alkoxysilanes, and unsaturated carbon-carbon double bond-containing siloxanes. kind or multiple combinations.
  • the reaction raw materials of the doped N element include, but are not limited to, N 2 and nitrogen-containing hydrocarbons.
  • the raw materials for the doped F element include but are not limited to fluorocarbon compounds, and are further selected from carbon tetrafluoride and tetrafluoroethylene.
  • the reaction raw material for the doped element B includes but is not limited to borane with a boiling point lower than 300° C. under normal pressure, and further, pentaborane, hexaborane, etc. are selected.
  • the gas source pipeline 21, the hydrogen pipeline 22, the reaction raw material pipeline 23, and the doping raw material pipeline 24 can each be provided with an on-off valve to respectively control the opening and closing of the pipelines to realize gas Circulation and closure, or that the on-off valve can control the flow rate of the gas filled into the chamber 101, is not limited here.
  • the doping raw material pipeline 24 may be connected to an additional independent feed port 13 to separately charge the auxiliary gas of the doping element into the chamber 101.
  • the doping material pipe 24 may share the same feed port 13 with the hydrogen pipe 22 or the reaction material pipe 23 to fill the chamber 101 with gas or the like respectively.
  • the content of doping elements in the DLC film is preferably less than 10% of the atomic number.
  • the DLC film prepared by the coating equipment 100 is doped
  • the content of miscellaneous elements is less than 40%, and the thickness of the DLC film is preferably 10-800 nm.
  • the doping content of Si, Cu, N, F, Al and other elements should not be too much. These doping elements will form a bond with the carbon element in the DLC, which will damage the original DLC.
  • the structure changes the growth mode during the deposition process.
  • the doping element reaction gas source can also increase the ionization rate of the carbon-containing gas source, which is beneficial to realize the coating.
  • the suction port 11 is provided in the middle of the chamber 101 of the cavity 10, wherein the gas inlet 12 and the feed port 13 are both provided in the cavity.
  • the position of the side wall of the chamber 101 of the body 10 so that gas is filled from the gas inlet 12 and the feed port 13 of the side wall of the chamber 101, and from the chamber 101
  • the suction port 11 in the middle of the position is drawn out to ensure that the filled gas diffuses to the surface of each substrate 600 as evenly as possible, so that the surface of each substrate 600 is evenly plated as much as possible
  • the above DLC film is provided in the middle of the chamber 101 of the cavity 10.
  • the suction port 11 may be provided in the middle of the bottom or top wall of the chamber 101, and the suction port 11 may also be connected to a suction port provided in the middle of the chamber 101.
  • the air column, wherein the air inlet 12 and the feed inlet 13 may be located on the same side wall of the chamber 101, or may be located on different side walls of the chamber 101, respectively.
  • the suction port 11 may be provided at a side wall position of the chamber 101, and the air intake port 12 and the feed port 13 may be provided at the middle position of the chamber 101 or at the same position as the side wall of the chamber 101.
  • the position of the side wall opposite to the suction port 11 is not limited here.
  • the relative positions of the suction port 11, the gas inlet 12, and the feed port 13 in the chamber 101 can be preset according to actual needs, so as to meet the needs of mass production as much as possible.
  • the substrate needs to be uniformly coated to ensure uniformity of specifications.
  • the pumping device 30 includes at least one first vacuum pump 31 and at least one second vacuum pump 32, wherein the first vacuum pump 31 and the second vacuum pump 32 respectively pass through
  • the air extraction line 40 is connected to the air extraction port 11, wherein the second vacuum pump 32 serves as the backing pump of the first vacuum pump 31 and cooperates to perform negative pressure on the chamber 101 through the air extraction line 40.
  • the pressure operation is to draw a vacuum and maintain the air pressure in the chamber 101 within a preset range.
  • the chamber 101 is pumped with gas to be close to a vacuum state.
  • the air pressure in the chamber 101 is reduced to below 0.01 Pa, or even below 0.001 Pa.
  • the air extraction device 30 is used to continuously extract the gas in the chamber 101 through the air extraction pipe 40 so as to maintain the concentration of the gas in the chamber 101 within a certain range, Preferably, the air pressure in the chamber 101 is maintained between 0.01 and 100 Pa.
  • the staff Before the coating of the coating equipment 100, the staff opens the chamber 101 of the cavity 10, wherein the substrate 600 is placed on the electrode holder 60, and the electrode holder 60 is located in the cavity. Then, the worker seals and closes the chamber 101 of the cavity 10, and then turns on the coating equipment 100 for coating.
  • this embodiment also provides a coating method of the coating equipment 100, which includes the steps:
  • S02. Enter the stage of performing surface etching treatment or surface cleaning and activation on the surface of the substrate 600.
  • gas raw materials are continuously filled into the chamber 101 through the gas source pipeline 21 for the substrate 600
  • the surface of the material is etched.
  • argon or helium is introduced into the chamber 101 through the gas source pipe 21, wherein the flow rate is approximately 10 sccm to 1000 sccm, preferably 80 or 100 sccm.
  • the air extraction device 30 is used to continuously extract a certain amount of gas in the chamber 101 and maintain the air pressure in the chamber 101 within 0.01-100 Pa, preferably 8 Pa or 10 Pa or 100 Pa.
  • the power supply device 50 provides a pulse voltage to act on the gas in the chamber 101 to clean and activate the surface of the substrate 600, so as to achieve etching treatment on the surface of the substrate 600.
  • the power supply device 50 provides a high voltage pulse bias voltage of -100V to -5000V, a duty ratio of 1% to 90%, and a power supply time of 1-60 minutes (the power supply time is the time for the substrate in step S02 600 surface cleaning and activation time), preferably, the power supply device 50 provides a voltage of -3000V, a duty cycle of 20% or 30%, a frequency of 10kHz or 40kHz, and a power supply time of 5, 10, 20, or 30min and so on.
  • the gas source pipe 21 is closed to stop filling the chamber 101 with gas.
  • the gas source pipe 21 has the on-off valve, wherein The on-off valve is used to control the switching of the gas source pipeline 21 to realize opening or closing of the gas source pipeline 21.
  • step S02 continue to pass gas into the chamber 101 through the gas source pipe 21 for preparation on the surface of the substrate 600 by means of plasma chemical vapor deposition.
  • the DLC film optionally, the flow rate of the gas to be ionized that is passed into the chamber 101 can be changed adaptively.
  • the flow rate of the gas to be ionized filled into the chamber 101 through the gas source pipe 21 can be preset at Within a reasonable range, to prevent the phenomenon that the flow rate of the gas to be ionized filled into the chamber 101 is too high or too low, which will affect the surface ionization effect of the substrate 600.
  • the pulse voltage provided by the power supply device 50 is preset within a reasonable range to prevent the voltage from being too low to achieve a good cleaning and activating effect on the surface of the substrate 600, or the voltage is too high to damage the The risk of the substrate 600.
  • the power supply time of the power supply device 50 can be preset within a reasonable range to prevent that the power supply time is too short to achieve a good cleaning and activation effect on the surface of the substrate 600, or the power supply time is too long to prolong the entire coating The cycle of the process causes unnecessary waste.
  • the flow rate of the gas to be ionized filled into the chamber 101 is 10-200 sccm
  • the gas flow rate of hydrogen is 0-100 sccm
  • the gas flow rate of the reaction raw materials such as hydrocarbon gas is 50-1000 sccm or doped.
  • the gas flow rate of the elemental reaction raw materials is 0-100 sccm.
  • the air extraction device 30 is used to continuously extract a certain amount of gas in the chamber 101 and maintain the air pressure in the chamber 101 within 0.01-100 Pa, preferably 8 Pa or 10 Pa or 100 Pa.
  • the DLC film is prepared on the surface of the substrate 600 by the power supply device 50 providing radio frequency voltage and/or high-voltage pulse bias assisted plasma chemical vapor deposition, wherein the power supply device 50 provides radio frequency voltage
  • the power is 10-800W, or the pulse bias voltage is -100V to -5000V, the duty cycle is 10%-80%, and the power supply time of the power supply device 50 is 5-300 minutes, that is, in step S03
  • the time for coating the substrate 600 is approximately 5-300 minutes.
  • the voltage or power of the power supply device 50 can be preset. Under the action of the voltage provided by the power supply device 50, all the gas in the chamber 101 is basically Both can be ionized into plasma, so that a plasma environment is formed in the chamber 101, so that the coating device 100 can prepare the thin film on the surface of the substrate 600 by means of chemical vapor deposition.
  • the power supply device 50 can provide radio frequency and/or high voltage pulse bias to act on the gas in the chamber 101, wherein the power supply device 50 provides a radio frequency electric field to the cavity 101.
  • the gas to be ionized in the chamber 101 and the reaction material gas and other gases are discharged so that the chamber 101 is in a plasma environment and the reaction gas material is in a high-energy state.
  • the power supply device 50 generates a strong electric field in the chamber 101 by providing a strong voltage in a high-voltage pulse bias, so that the active particles in a high-energy state are accelerated by the strong electric field to deposit on the surface of the substrate 600, And form an amorphous carbon network structure.
  • the power supply device 50 provides the empty voltage or the low voltage state in the high-voltage pulse bias to allow the amorphous carbon network structure deposited on the surface of the substrate 600 to relax freely, and the carbon under the action of thermodynamics The structure is transformed into a stable phase-curved graphene sheet structure, and is embedded in an amorphous carbon network, thereby forming the DLC film on the surface of the substrate 600.
  • the gas source pipe 21 can be closed to stop filling the chamber 101 with the gas to be ionized, or filling the chamber 101
  • the gas flow rate can be preset within a reasonable range.
  • the hydrogen pipe 22 can be closed to prevent or stop filling the chamber 101 with hydrogen, or the gas flow rate of the hydrogen filled into the chamber 101 through the hydrogen pipe 22 can be preset. Set within a reasonable range.
  • the reaction raw material pipeline 23 can be controlled to switch, wherein the gas flow rate of the reaction raw materials filled into the chamber 101 through the reaction raw material pipeline 23 can be preset within a reasonable range.
  • the doping material pipe 24 can be closed to prevent or stop filling the chamber 101 with the doping element reaction material, or to be filled into the chamber through the doping material pipe 24
  • the gas flow rate of the doping element reaction raw material in 101 can be preset within a reasonable range.
  • the gas to be ionized such as nitrogen or argon, the hydrogen, the reaction raw material gas, or the doping element reaction raw material gas, which is charged into the chamber 101, determines the ratio of the flow rate of the gas flow.
  • the atomic ratio in the DLC film is affected, thereby affecting the quality of the DLC film.
  • the temperature, ionization rate, or deposition rate and other related parameters during the coating process can be adjusted, or through preset
  • the power supply time of the power supply device 50 is set to prevent the DLC film from being thinner and the hardness performance poor due to the coating time being too short, or the DLC film being thicker due to the coating time being too long, which affects transparency, etc. The occurrence of the phenomenon.
  • step S03 it is possible not to fill the chamber 101 with hydrogen at different flow rates, or to fill the chamber 101 with a certain amount of hydrogen to prepare DLC with different hydrogen content. film.
  • the DLC film with higher hydrogen content has higher lubricity and transparency than the DLC film with lower hydrogen content, and in the step S03, a certain amount is filled into the chamber 101 A large amount of hydrogen is conducive to the formation of SP 3 bonds during the coating process, which can increase the hardness of the DLC film to a certain extent, but as the hydrogen content further increases, the hardness of the DLC film will gradually decrease, so according to For different coating requirements, in the step S03, the chamber 101 can be selectively filled with a preset amount of hydrogen gas through the hydrogen pipe 22.
  • a certain amount of designated doping element reaction raw materials can be selectively filled into the chamber 101 through the doping raw material pipeline 24.
  • the reaction material containing fluorine is filled into the chamber, so that the prepared DLC film has a higher hydrophobic effect and transparency, but when the fluorine atom content exceeds 20%, the hardness of the DLC film Will be significantly reduced (less than 4H on the Mohs hardness).
  • step S04 After the coating time of step S03 ends, the on-off valves of the gas source pipeline 21, the hydrogen pipeline 22, the reaction raw material pipeline 23, and the doping raw material pipeline 24 of the delivery pipeline 20 Both are turned off, at the same time the power supply device 50 is turned off, and the air extraction device 30 is turned off.
  • the delivery pipeline 20 further includes an air delivery pipeline 25, wherein the cavity 10 further has at least one air inlet 14 communicating with the chamber 101, wherein the air delivery pipeline 25 is connected to the air inlet 14 of the chamber 101, wherein the air delivery pipe 25 is used to fill the chamber 101 with air so that the chamber 101 is in a normal pressure state. That is, a certain amount of air is filled into the chamber 101 through the air delivery pipe 25 to return the chamber 101 to a normal pressure state, so that the staff can open the chamber 101 and take out the substrate 600, So far, the coating process is over. In the entire coating process, the coating equipment 100 has better process controllability in the process of preparing the DLC film, which is beneficial to the rapid preparation of the target DLC film.
  • the chamber 101 can always be at room temperature or low temperature, that is, the coating equipment 100 can complete the coating at room temperature or low temperature, and the time required is relatively short, which is conducive to saving cost.
  • the coating equipment 100 can be used to coat some substrates that are not resistant to high temperatures, so that the substrates are not easily damaged during the coating process.
  • the coating equipment 100 of the present invention can always keep the substrate 600 in a relatively low temperature state during the entire coating process. The temperature of the substrate 600 is excessively increased.
  • the coating equipment 100 further includes an exhaust gas treatment device 70, wherein the exhaust gas treatment device 70 is connected to the exhaust pipe 40, and the exhaust gas treatment device 70 is used to process the exhaust gas The exhaust gas is extracted and discharged.
  • the exhaust gas treatment device 70 includes, but is not limited to, recycling or non-polluting treatment of reaction raw materials such as nitrogen, inert gas, hydrogen, hydrocarbon gas, or auxiliary gas doped with elements, etc., and then It is discharged to the outside world to prevent pollution to the environment and can be recycled.
  • the first vacuum pump 31 is implemented as a molecular pump, wherein the second vacuum pump 32 includes a roots pump 321 and a dry pump 322, wherein the pumping of the chamber 101
  • the air port 11, the first vacuum pump 31, the roots pump 321, the dry pump 322, and the exhaust gas treatment device 70 are all connected by the air extraction pipeline 40.
  • the gas in the chamber 101 is sequentially pumped out by the dry pump 322, the Roots pump 321, and the molecular pump, that is, the second vacuum pump 32 acts as a fore-stage pump to the chamber 101 first.
  • Evacuate wherein the first vacuum pump 31 serves as a secondary pump to further evacuate the chamber 101, and the gas extracted from the chamber 101 is processed or recovered by the exhaust gas processing device 70 Discharge to the outside world.
  • the second vacuum pump 32 includes at least one mechanical pump and serves as a backing pump for pumping air to the chamber 101, wherein the molecular pump serves as a two-stage pump set to further the chamber.
  • the ground is evacuated so that the air pressure in the chamber 101 can be maintained as low as possible.
  • the model parameter of the pipeline between the chamber 101 and the roots pump 321 is DN100, and the interface is IOS100.
  • the model parameter of the pipe between the Roots pump 321 and the dry pump 322 is DN63, and the interface is not limited.
  • the model parameter of the pipeline of the exhaust gas treatment device 70 is NB32, and the interface is not limited.
  • the power supply device 50 includes a radio frequency power supply 51 and a pulse power supply 52, wherein the radio frequency power supply 51 is directly loaded on the electrode plate in the chamber 101 of the cavity 10 A radio frequency electric field is generated inside to act on the gas in the chamber 101, wherein the pulse power source 52 is used to provide a high-voltage pulse bias to act on the gas in the chamber 101.
  • the radio frequency power supply 51 discharges the gas in the chamber 101, such as nitrogen or inert gas, and the reaction raw material gas, by providing a radio frequency electric field, so that the chamber 101 is in plasma.
  • the body environment and the reaction gas raw materials are in a high-energy state.
  • the pulse power supply 52 generates a strong electric field in the chamber 101 by providing a strong voltage in a high-voltage pulse bias, so that the active particles (that is, positive ions) in a high-energy state are subjected to the strong electric field to directionally accelerate the deposition on the chamber 101.
  • an amorphous carbon network structure is formed, and the pulse power source 52 provides a null voltage or a low voltage state in the high-voltage pulse bias to make the deposited on the surface of the substrate 600
  • the amorphous carbon network structure relaxes freely, and under the action of thermodynamics, the carbon structure transforms into a stable phase-the curved graphene sheet structure, and is embedded in the amorphous carbon network, so as to be on the surface of the substrate 600
  • the DLC film is formed.
  • the radio frequency power supply 51 can also be used as a plasma supporting power supply, wherein the radio frequency power supply 51 is composed of a radio frequency power source, an impedance matcher and an impedance power meter, and the radio frequency power supply 51 is installed in the cavity 10 to provide The radio frequency electric field acts on the gas in the chamber 101.
  • the radio frequency power supply 51 preferably provides radio frequency power of 13.56 MHz.
  • the radio frequency power supply 51 forms the radio frequency electric field in the cavity 101 of the cavity 10 by directly loading the radio frequency voltage on an electrode plate of the cavity 10 to act The gas in the chamber 101 satisfies the coating demand.
  • the radio frequency power supply 51 can also be implemented as an inductive coupling effect of a coil, that is, as an ICP to generate an alternating magnetic field in the chamber 101, so as to ensure that the chamber 101 is The gas is fully and uniformly ionized, which can also meet the coating requirements of the coating equipment 100, which is not limited here.
  • the pulse power supply 52 is implemented as a unidirectional negative pulse power supply, wherein the pulse power supply 52 has a negative terminal 521 and a positive terminal 522, wherein the negative terminal 521 is electrically connected to the electrode holder 60 and Provide negative pressure, wherein the positive terminal 522 is electrically connected to the cavity 10 and grounded at a positive or zero potential, wherein the electrode holder 60 and the cavity 10 are both made of conductive materials such as metal materials, wherein The electrode holder 60 is insulated from the cavity 10.
  • the entire electrode holder 60 is a negative electrode and has a negative pressure
  • the entire cavity 10 is grounded as a positive electrode
  • the electrode holder 60 is insulated from the cavity 10 to
  • the entire chamber 101 is placed in a strong electric field. Since the substrate 600 is placed on the electrode holder 60, under the action of the strong electric field, the active particles in a high-energy state will accelerate the deposition on the The surface of the substrate 600 is thus coated.
  • the pulse power source 52 ionizes the gas in the chamber 101 through the glow discharge effect, and at the same time has a directional pulling and accelerating effect on the positive ions in the chamber 101, so that the positive ions have The bombardment effect accelerates the deposition on the surface of the substrate 600, thereby preparing the dense and high-hardness DLC film on the surface of the substrate 600.
  • the electrode holder 60 can provide as much space as possible for installing and arranging a large number of the substrate 600, and a coating process can cover the electrode. All the substrates 600 on the support 60 are coated, so as to realize large-area coating, thereby realizing mass production of DLC thin films.
  • the radio frequency power supply 51 and the pulse power supply 52 jointly provide a voltage to act on the gas in the chamber 101, wherein the low power radio frequency discharge provided by the radio frequency power supply 51 Maintain the plasma environment in the chamber 101 and suppress the arc discharge phenomenon during the high-voltage discharge process (because arc discharge is a form of discharge that is further enhanced by glow discharge, the instantaneous current can reach more than tens or even hundreds of amperes. High current passing through the surface of the substrate will damage the substrate. Therefore, in order to ensure the safety of the substrate 600, it is necessary to suppress the arc discharge phenomenon during the coating process).
  • the pulse power source 52 increases the energy of the positive ions when they reach the surface of the substrate 600 to prepare the dense and transparent DLC film.
  • the power supply device 50 in the preferred embodiment is composed of the radio frequency power supply 51 and the pulse power supply 52 to meet the coating requirements.
  • the power supply device 50 can also be implemented as only one of the radio frequency power supply 51 or the pulse power supply 52, which can also meet the coating requirements.
  • the power supply device 50 can also be implemented as a microwave power supply and other power supplies to meet the coating requirements, which is not limited here.
  • the RF voltage power and power supply time of the RF power supply 51 can be adjusted and preset according to the coating requirements for different substrates, wherein the RF voltage power of the RF power supply 51 is preferably 10-800W,
  • the pulse bias voltage, pulse frequency, duty cycle, and power supply time provided by the pulse power supply 52 can be adjusted and preset, wherein the pulse power supply 52 provides a pulse bias voltage of -100V to -5000V, and the pulse The frequency is 20-300KHz, and the duty cycle is 10%-80%, which is not limited here.
  • the negative voltage of the pulse power supply 52 Since the magnitude of the negative voltage bias provided by the pulse power supply 52 is directly related to the ionization rate of the gas in the chamber 101 and the migration ability of positive ions to the surface of the substrate 600, the negative voltage of the pulse power supply 52 The higher the voltage, the higher the energy of the positive ions, and the higher the hardness of the prepared DLC. However, it should be noted that the higher the energy, the higher the bombardment energy of the positive ions on the surface of the substrate 600. On a microscopic scale, bombardment pits will be generated on the surface of the substrate 600 and will accelerate at the same time. The temperature of the surface of the substrate 600 increases, so the negative voltage of the pulse power source 52 should not be too high to prevent the surface temperature of the substrate 600 from excessively increasing and damaging the substrate 600. In addition, the higher the pulse frequency of the pulse power source 52 is, the continuous accumulation of electric charges on the surface of the insulating part of the substrate 600 can be avoided, thereby achieving suppression of the large arc phenomenon and increasing the deposition
  • the coating equipment 100 includes a temperature detector 80, wherein the temperature detector 80 is used to detect the reaction temperature in the chamber 101 during the coating process and provide feedback, such as prompting work in the form of a screen display Personnel or voice alarms, etc., further ensure that the temperature of the substrate is not easily too high.
  • the temperature detector 80 has a thermocouple 81, wherein the thermocouple 81 is disposed on the electrode holder 60 at an equivalent position to the substrate 600, and the thermocouple 81 can detect the The reaction temperature in the chamber 101, based on the reaction temperature detected by the thermocouple 81, the temperature detector 80 determines whether the temperature threshold of the substrate 600 is exceeded, and if it exceeds, the temperature detector 80 80 feeds back an abnormal signal that the temperature is too high to remind the staff to handle or suspend the coating equipment 100 in time. If it does not exceed, the reaction temperature on the surface of the substrate 600 is normal, that is, the substrate 600 is safe.
  • the electrode holder 60 is preferably implemented as a multi-layer metal plate structure, wherein each layer can place a certain amount of the substrate 600, wherein the electrode holder 60 has at least one insulating member 61, wherein the insulating member 61 is disposed between the electrode holder 60 and the wall of the chamber 101 to insulate the electrode holder 60 from the cavity 10.
  • the insulating member 61 is implemented to be made of insulating materials such as polytetrafluoroethylene.
  • the cavity 10 is not connected to the pulse power source 52, and the electrode holder 60 is implemented as including multiple metal plates, and adjacent layers are mutually connected to each other. Insulation, wherein the positive terminal 522 and the negative terminal 521 of the pulse power source 52 are electrically connected to the metal plates of the electrode holder 60 alternately, so that the adjacent metal plates of the electrode holder 60 are mutually connected.
  • the pulse power source 52 can be implemented as a positive and negative bidirectional pulse power source, so that each metal plate of the electrode holder 60 alternately forms a positive electrode or a negative electrode, and adjacent metal plates are always positive and negative to each other. So that the substrate 600 can be placed on the metal plate of each layer, and the surface of the substrate 600 on all the metal plates can be plated with the DLC film, and The quality of the DLC film is even better.
  • the pulse power supply 52 can also be implemented as a symmetrical bidirectional pulse power supply, that is, the positive pressure and the negative pressure provided by the pulse power supply 52 have the same magnitude.
  • the pulse power source 52 is implemented as an asymmetric bidirectional pulse power source, wherein the magnitude of the negative voltage value provided by the pulse power source 52 is greater than the magnitude of the positive voltage value to provide the quality of the DLC film, which is not limited here .
  • the shape and structure of the electrode holder 60 are not limited. Within the volume of the chamber 101, the shape or number of the electrode holder 60 can be adjusted adaptively.
  • the material of the cavity 10 is stainless steel.
  • the cavity 10 has an openable and closable sealed door 15 for a worker to open or seal the cavity 101 to place or take out the substrate 600 and the cavity 101.
  • the electrode holder 60 is detachably supported in the chamber 101, so that the electrode holder 60 can be taken out of the chamber 101, so that workers can pre-install the substrate 600 outside. On the electrode holder 60, and then place the electrode holder 60 in the chamber 101. At the same time, after one coating process is completed, the staff can take out the electrode holder 60 to take out all the substrates.
  • the material 600 is used to minimize damage to the substrate 600, to ensure the safety of the substrate 600, and to facilitate cleaning of the chamber 101 and the electrode holder 60.
  • the electrode holder 60 can be reused, that is, during the second coating, the electrode holder 60 can be used to install another batch of the substrate 600 again, and then be placed in the chamber 101 Re-coating is realized inside, which is conducive to mass production.
  • the parameters of the coating equipment 100 during the coating process are as follows: Air intake: Ar/N 2 /H 2 /CH 4 : 50-500 sccm, C 2 H 2 /O 2 : 10-200 sccm; before coating (I.e. the step S02 stage) the vacuum degree of the chamber 101: less than 2 ⁇ 10 -3 Pa; during coating (i.e. the step S03 stage) the vacuum degree of the chamber 101: 0.1-20 Pa; coating voltage : -300 ⁇ -3500V, duty cycle: 5 ⁇ 100%, frequency: 20 ⁇ 360KHz; coating time: 0.1 ⁇ 5hrs, the thickness of the DLC film is less than 50 nanometers, this is only an example, not the present invention limit.
  • the coating equipment 100 further includes a housing 90, in which the cavity 10, the delivery pipeline 20, the air extraction device 30, the air extraction pipeline 40, the power supply device 50, and the Both the exhaust gas treatment device 70 and the temperature detection device 80 can be installed in the housing 90.
  • the housing 90 has a control panel, wherein the control panel is used by the staff to control the on/off or working status of the air extraction device 30 and the power supply device 50, and display the coating of the coating equipment 100 Process progress and related parameters, etc.
  • this embodiment also provides the DLC film, wherein the DLC film is prepared by the coating equipment 100 and formed on the surface of the substrate 600. It is understandable that the DLC film may be one or more layers of DLC film formed on the surface of the substrate 600 by the coating equipment 100 through one or more coatings.

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Abstract

Provided in the present invention are a coating equipment for preparing DLC and a use thereof. The coating equipment comprises a cavity, a set of conveying pipelines, at least one air extracting device, at least one air extracting pipeline, a power supply device, and at least one electrode support. The cavity is provided with a chamber; the electrode support is arranged in the chamber so as to support a base material; the conveying pipelines communicate with the chamber and are used for introducing gas raw materials into the chamber; the air extracting device communicates with the chamber by means of the air extracting pipeline and is used for carrying out a negative pressure operation on the chamber and controlling the air pressure inside the chamber; and the power supply device is electrically connected to the electrode support so as to allow the coating equipment to prepare a DLC film on the surface of the base material by means of a chemical vapor deposition manner.

Description

用于制备DLC的镀膜设备及其应用Coating equipment for preparing DLC and its application 技术领域Technical field
本发明涉及镀膜领域,进一步涉及一种用于制备DLC的镀膜设备及其应用。The invention relates to the field of coating, and further relates to a coating equipment for preparing DLC and its application.
背景技术Background technique
[根据细则91更正 09.04.2020] 
类金刚石薄膜(Diamond Like Carbon,DLC)是近来兴起的一种以sp3sp2键的形式结合生成的亚稳态材料,是一种短程有序、长程无序的薄膜或膜层。它兼具了金刚石和石墨的优良特性。在力学性能方面,DLC具有较高的硬度、耐磨,与组分相关的硬度可从20GPa变化至80GPa;在光学性能方面,DLC透光性好、有增透功能;此外,DLC还具有良好的导热性和生物相容性。例如,在玻璃、陶瓷等表面镀上一层DLC薄膜,可进一步提高玻璃、陶瓷等的耐磨性和硬度。例如,将DLC沉积到塑料表面,也可以起到提高塑料表面耐磨性能和提升硬度的作用。
[Corrected according to Rule 91 09.04.2020]
DLC films (Diamond Like Carbon, DLC) are integrated to form a recent rise in the form of sp2 and sp 3 bonds metastable material, a short-range order, long range disorder film or film layer. It combines the excellent properties of diamond and graphite. In terms of mechanical properties, DLC has high hardness and wear resistance, and the hardness related to the components can vary from 20 GPa to 80 GPa; in terms of optical properties, DLC has good light transmittance and anti-reflection function; in addition, DLC also has good properties The thermal conductivity and biocompatibility. For example, coating a layer of DLC film on the surface of glass, ceramics, etc., can further improve the wear resistance and hardness of glass, ceramics, etc. For example, depositing DLC on the plastic surface can also improve the wear resistance and hardness of the plastic surface.
目前制备DLC薄膜的方法可以分为化学气相沉积(CVD)方法和物理气相沉积(PVD)方法。化学气相沉积是利用化学反应的原理,从气相物质中析出固相物质沉积于工作表面形成镀层薄膜的沉积工艺。从沉积条件看,要实现气体和基材界面的化学反应,在沉积反应过程中必须有一定的激活能。按激活方式的不同,可分为热丝化学气相沉积、激光化学气相沉积和等离子体增强化学气相沉积等。物理气相沉积技术是指在真空条件下,至少有一种沉积元素被雾化(原子化)的情况下,进行的气相沉积工艺,其特点是能够在各种基材上沉积膜层、膜基的界面可以得到改进、沉积速率高等。物理气相沉积DLC薄膜具体方法主要有:离子束沉积、溅射沉积、真空阴极电弧沉积以及脉冲激光沉积等。The current methods for preparing DLC films can be divided into chemical vapor deposition (CVD) methods and physical vapor deposition (PVD) methods. Chemical vapor deposition is a deposition process that uses the principle of chemical reaction to separate solid phase substances from gas phase substances and deposit them on the working surface to form a coating film. From the perspective of deposition conditions, in order to achieve a chemical reaction between the gas and the substrate interface, there must be a certain amount of activation energy during the deposition reaction. According to the different activation methods, it can be divided into hot filament chemical vapor deposition, laser chemical vapor deposition and plasma enhanced chemical vapor deposition. Physical vapor deposition technology refers to a vapor deposition process performed under vacuum conditions when at least one deposition element is atomized (atomized). It is characterized by the ability to deposit film layers and film bases on various substrates. The interface can be improved, the deposition rate is high, etc. The specific methods of physical vapor deposition of DLC films mainly include: ion beam deposition, sputtering deposition, vacuum cathodic arc deposition and pulsed laser deposition.
由于等离子体增强化学气相沉积(PECVD)方法具有沉积温度低,绕镀性好,制备的薄膜均匀致密等诸多特点而成为最常用的制备DLC薄膜的方法之一。等离子体增强化学气相沉积法又称辉光放电法,常见的等离子体增强化学气相沉积技术有:直流辉光放电法、射频辉光放电法、电子回旋共振(ECR)化学气相沉积等,近年来又出现了高沉积速率和大面积沉积的双射频-直流辉光放电(RF-DC) 法、微波-射频(MW-RF)辉光放电法、电子回旋共振-射频(ECR-RF)法等。经大量研究,类金刚石薄膜在制备过程中可分为以下四个阶段:(1)原始基体团的产生过程,即气源分子通过与高能电子发生非弹性碰撞,分解成中性原子和基团;(2)二次反应过程,即中性原子和基团之间或中性原子与气源分子之间碰撞发生的化学反应过程;(3)传输过程,即中性原子或基团向基体表面的扩散过程;(4)表面反应过程,也就是中性基团与表面反应形成薄膜。Because the plasma-enhanced chemical vapor deposition (PECVD) method has many characteristics such as low deposition temperature, good winding properties, and uniform and dense films prepared, it has become one of the most commonly used methods for preparing DLC films. Plasma-enhanced chemical vapor deposition is also called glow discharge method. Common plasma-enhanced chemical vapor deposition techniques include: direct current glow discharge method, radio frequency glow discharge method, electron cyclotron resonance (ECR) chemical vapor deposition, etc., in recent years The dual radio frequency-direct current glow discharge (RF-DC) method, microwave-radio frequency (MW-RF) glow discharge method, electron cyclotron resonance-radio frequency (ECR-RF) method, etc., with high deposition rate and large area deposition have appeared. . After a lot of research, the preparation process of diamond-like carbon films can be divided into the following four stages: (1) The generation process of the original matrix group, that is, the gas source molecule decomposes into neutral atoms and groups through inelastic collision with high-energy electrons. ; (2) Secondary reaction process, that is, the chemical reaction process between neutral atoms and groups or between neutral atoms and gas molecules; (3) Transmission process, that is, neutral atoms or groups to the surface of the substrate The diffusion process; (4) The surface reaction process, that is, the neutral group reacts with the surface to form a film.
专利号为CN205803582U公开了一种沉积类金刚石薄膜装置,包括真空室、工作台和真空系统,在使用时,先采用真空系统将真空室抽至工作真空,开启加热系统,开启柱状弧源清洗装置对工作台进行清洗,清洗好后,打开矩形平面弧铬靶进行打底层,然后打开矩形平面弧石墨靶沉积类金刚石薄膜。在镀膜过程中需要提供加热环境,采用石墨靶作为靶材,离化率偏低,沉积效率慢,存在镀膜质量较差和经济成本偏高的问题。The patent number is CN205803582U discloses a device for depositing diamond-like carbon films, which includes a vacuum chamber, a workbench and a vacuum system. When in use, the vacuum system is first used to pump the vacuum chamber to working vacuum, the heating system is turned on, and the columnar arc source cleaning device is turned on Clean the workbench. After cleaning, open the rectangular planar arc chromium target to lay the bottom layer, and then open the rectangular planar arc graphite target to deposit the diamond-like carbon film. In the coating process, it is necessary to provide a heating environment. The graphite target is used as the target material, the ionization rate is low, the deposition efficiency is slow, and there are problems of poor coating quality and high economic cost.
专利号为CN101082118A公开了一种高速钢金属表面镀制类金刚石薄膜的方法,该方法包括a、将金属工件固定在电弧离子镀膜设备真空室内的工件转盘上并抽真空;b、将氩气通入真空室,并保持真空度的稳定,然后开启离子源将金属工件表面活化;c、关闭氩气,在金属工件与真空室之间加载负偏压,并开启钛电弧源使金属工件表面沉积钛过渡层;d、开启石墨电弧源,设定石墨点弧源的初始放电频率,并控制石墨电弧源每放电一定脉冲数适当提高放电频率使金属工件表面沉积碳化钛过渡层;e、关闭钛电弧源,控制石墨电弧源的放电脉冲数使金属工件表面沉积类金刚石薄膜。可以看出,该方法以石墨电弧源作为靶材,存在离化率较低、沉积效率低等缺点。The patent number CN101082118A discloses a method for coating a diamond-like carbon film on a high-speed steel metal surface. The method includes a, fixing a metal workpiece on a workpiece turntable in a vacuum chamber of an arc ion plating equipment and vacuuming; b. venting argon Enter the vacuum chamber and keep the vacuum stable, then turn on the ion source to activate the surface of the metal workpiece; c. Turn off the argon gas, load a negative bias between the metal workpiece and the vacuum chamber, and turn on the titanium arc source to deposit the surface of the metal workpiece Titanium transition layer; d. Turn on the graphite arc source, set the initial discharge frequency of the graphite point arc source, and control the graphite arc source to a certain number of pulses per discharge to appropriately increase the discharge frequency to deposit a titanium carbide transition layer on the surface of the metal workpiece; e. Turn off titanium Arc source, control the number of discharge pulses of the graphite arc source to deposit diamond-like carbon film on the surface of the metal workpiece. It can be seen that this method uses a graphite arc source as the target material, which has disadvantages such as low ionization rate and low deposition efficiency.
因此,如何提供一种结构简单,成本较低,适于大批量制备高质量的DLC薄膜的镀膜设备,是目前急需解决的问题。Therefore, how to provide a coating equipment with simple structure and low cost, suitable for mass preparation of high-quality DLC thin films, is a problem that needs to be solved urgently at present.
发明内容Summary of the invention
本发明的一个优势在于提供一用于制备DLC的镀膜设备及其应用,其中所述镀膜设备用于在基材表面镀上DLC薄膜或者膜层,实现大面积镀膜,从而实现大批量制备DLC薄膜。An advantage of the present invention is to provide a coating device for preparing DLC and its application, wherein the coating device is used to coat a DLC film or film on the surface of a substrate to realize large-area coating, thereby realizing mass preparation of DLC film .
本发明的另一个优势在于提供一用于制备DLC的镀膜设备及其应用,其中所述镀膜设备能够对基材表面进行刻蚀与活化,有利于在所述基材表面制备所述 DLC薄膜。Another advantage of the present invention is to provide a coating device for preparing DLC and its application, wherein the coating device can etch and activate the surface of the substrate, which is beneficial for preparing the DLC film on the surface of the substrate.
本发明的另一个优势在于提供一用于制备DLC的镀膜设备及其应用,其中所述镀膜设备能够在常温或者低温下完成镀膜,所需时间较短,有利于节省成本。Another advantage of the present invention is to provide a coating equipment for preparing DLC and its application, wherein the coating equipment can complete the coating at room temperature or low temperature, and the required time is short, which is beneficial to cost saving.
本发明的另一个优势在于提供一用于制备DLC的镀膜设备及其应用,其中所述镀膜设备能够用于对一些不耐高温的基材进行镀膜,实现在镀膜过程中不易损坏基材。Another advantage of the present invention is to provide a coating equipment for preparing DLC and its application, wherein the coating equipment can be used to coat some substrates that are not resistant to high temperatures, so that the substrate is not easily damaged during the coating process.
本发明的另一个优势在于提供一用于制备DLC的镀膜设备及其应用,其中所述镀膜设备能够实时检测反应温度,进一步确保所述基材的安全性。Another advantage of the present invention is to provide a coating device for preparing DLC and its application, wherein the coating device can detect the reaction temperature in real time to further ensure the safety of the substrate.
本发明的另一个优势在于提供一用于制备DLC的镀膜设备及其应用,其中所述镀膜设备结合射频和/或脉冲电压实现制备所述DLC薄膜。Another advantage of the present invention is to provide a coating device for preparing DLC and its application, wherein the coating device combines radio frequency and/or pulse voltage to prepare the DLC film.
本发明的另一个优势在于提供一用于制备DLC的镀膜设备及其应用,其中所述镀膜设备在制备DLC薄膜的过程中工艺可控性较好,有利于快速制备目标DLC薄膜。Another advantage of the present invention is to provide a coating device for preparing DLC and its application, wherein the coating device has better process controllability in the process of preparing DLC film, which is beneficial to the rapid preparation of target DLC film.
本发明的另一个优势在于提供一用于制备DLC的镀膜设备及其应用,其中所述镀膜设备结构简单,利于清洁,使用寿命较高。Another advantage of the present invention is to provide a coating equipment for preparing DLC and its application, wherein the coating equipment has a simple structure, is conducive to cleaning, and has a long service life.
依本发明的一个方面,本发明进一步提供一镀膜设备,用于在基材表面制备DLC薄膜,其中所述镀膜设备包括:According to one aspect of the present invention, the present invention further provides a coating equipment for preparing a DLC film on the surface of a substrate, wherein the coating equipment includes:
一腔体,其中所述腔体具有一腔室;A cavity, wherein the cavity has a cavity;
一组输送管路;A set of conveying pipelines;
至少一抽气装置;At least one air extraction device;
至少一抽气管路;At least one suction line;
一供电装置;以及A power supply device; and
至少一电极支架,其中所述电极支架被设置于所述腔室以供支撑该基材,其中所述输送管路被连通于所述腔室并用于向所述腔室内通入气体原料,其中所述抽气装置通过所述抽气管路连通于所述腔室并对所述腔室进行负压操作和控制所述腔室内的气压,其中所述供电装置电连接于所述电极支架,以供所述镀膜设备通过化学气相沉积的方式在该基材的表面制备该DLC薄膜。At least one electrode holder, wherein the electrode holder is arranged in the chamber for supporting the substrate, and the delivery pipeline is connected to the chamber and is used to pass gaseous materials into the chamber, wherein The air extraction device is connected to the chamber through the air extraction pipeline and performs a negative pressure operation on the chamber and controls the air pressure in the chamber, wherein the power supply device is electrically connected to the electrode holder to The coating equipment is provided for preparing the DLC film on the surface of the substrate by means of chemical vapor deposition.
在一些实施例中,所述腔体具有与所述腔室相通的至少一抽气口、至少一进气口以及至少一进料口,其中所述输送管路包括至少一气源管道、以及至少一反应原料管道,其中所述抽气口被连通于所述抽气管路,其中所述气源管道被连通 于所述进气口以用于向所述腔室内通入气体,其中所述反应原料管道被连通于所述进料口以用于向所述腔室内充入反应原料。In some embodiments, the cavity has at least one suction port, at least one gas inlet, and at least one feed port communicating with the cavity, wherein the delivery pipeline includes at least one gas source pipe, and at least A reaction raw material pipeline, wherein the gas extraction port is connected to the gas extraction pipeline, wherein the gas source pipeline is connected to the gas inlet for injecting gas into the chamber, wherein the reaction raw material A pipe is connected to the feed port for filling the chamber with reaction raw materials.
在一些实施例中,还包括一氢气管道,其中所述氢气管道和所述反应原料管道被连通于同一所述进料口,或者所述氢气管道和所述反应原料管道被分别连通于两个所述进料口。In some embodiments, it further comprises a hydrogen pipeline, wherein the hydrogen pipeline and the reaction raw material pipeline are connected to the same feed port, or the hydrogen pipeline and the reaction raw material pipeline are respectively connected to two The feed port.
[根据细则91更正 09.04.2020] 
在一些实施例中,所述输送管路进一步包括一掺杂原料管道,其中所述掺杂原料管道被连通于所述进料口以用于向所述腔室内充入掺杂元素反应原料。
[Corrected according to Rule 91 09.04.2020]
In some embodiments, the delivery pipeline further includes a doping raw material pipeline, wherein the doping raw material pipeline is connected to the feed port for filling the chamber with doping element reaction raw materials.
在一些实施例中,所述抽气口位于所述腔室的中部,其中所述进气口和所述进料口均位于所述腔室的侧壁。In some embodiments, the suction port is located in the middle of the chamber, and the gas inlet and the feed port are both located on the side wall of the chamber.
在一些实施例中,其中所述抽气装置包括至少一第一真空泵和至少一第二真空泵,其中所述第二真空泵作为所述第一真空泵的前级泵共同协作地通过所述抽气管路对所述腔室进行负压操作并维持所述腔室内的气压处于预设范围内。In some embodiments, the pumping device includes at least one first vacuum pump and at least one second vacuum pump, wherein the second vacuum pump serves as a backing pump of the first vacuum pump and passes through the pumping pipeline in cooperation. A negative pressure operation is performed on the chamber and the air pressure in the chamber is maintained within a preset range.
在一些实施例中,其中所述腔室内空气至使所述腔室内的气压降至0.01Pa以下。In some embodiments, the air in the chamber reduces the air pressure in the chamber to below 0.01 Pa.
在一些实施例中,其中维持所述腔室内的气压在0.01至100Pa之间。In some embodiments, the air pressure in the chamber is maintained between 0.01 and 100 Pa.
在一些实施例中,其中所述第一真空泵被实施为分子泵,其中所述第二真空泵被实施为包括罗茨泵和干泵。In some embodiments, wherein the first vacuum pump is implemented as a molecular pump, and wherein the second vacuum pump is implemented as including a roots pump and a dry pump.
在一些实施例中,所述镀膜设备进一步包括一尾气处理装置,其中所述尾气处理装置被连通于所述抽气管路,以用于处理经所述抽气装置抽出的气体并进行排放。In some embodiments, the coating equipment further includes an exhaust gas treatment device, wherein the exhaust gas treatment device is connected to the gas extraction pipeline for processing and discharging the gas extracted by the gas extraction device.
在一些实施例中,所述供电装置包括一射频电源和一脉冲电源,以分别提供射频电压和所述脉冲电源。In some embodiments, the power supply device includes a radio frequency power supply and a pulse power supply to provide the radio frequency voltage and the pulse power supply respectively.
在一些实施例中,所述供电装置包括一脉冲电源,其中所述脉冲电源具有一正极端和一负极端,其中所述负极端被电连接于所述电极支架并提供负压,其中所述腔体并接地,并且所述电极支架与所述腔体之间绝缘。In some embodiments, the power supply device includes a pulse power source, wherein the pulse power source has a positive terminal and a negative terminal, wherein the negative terminal is electrically connected to the electrode holder and provides a negative voltage, wherein the The cavity is grounded, and the electrode holder is insulated from the cavity.
在一些实施例中,所述供电装置包括一脉冲电源,其中所述脉冲电源具有一正极端和一负极端,其中所述电极支架包括多层金属板,其中所述脉冲电源的所述正极端和所述负极端分别电连接于所述电极支架的各层金属板,并使所述电极支架的相邻的两个金属板互为正负极。In some embodiments, the power supply device includes a pulse power supply, wherein the pulse power supply has a positive terminal and a negative terminal, wherein the electrode holder includes a multilayer metal plate, and the positive terminal of the pulse power supply The negative terminal and the negative terminal are respectively electrically connected to the metal plates of the electrode support, and the two adjacent metal plates of the electrode support are mutually positive and negative.
在一些实施例中,所述射频电源的射频电压的功率为10-800W。In some embodiments, the power of the radio frequency voltage of the radio frequency power supply is 10-800W.
在一些实施例中,所述脉冲电源提供脉冲偏压的电压为-100V至-5000V,脉冲频率为20-300KHz,占空比为10%-80%。In some embodiments, the pulse power supply provides a pulse bias voltage of -100V to -5000V, a pulse frequency of 20-300KHz, and a duty cycle of 10%-80%.
在一些实施例中,所述脉冲电源被实施为单向脉冲电源、对称式双向脉冲电源或者非对称式脉冲电源。In some embodiments, the pulsed power supply is implemented as a unidirectional pulsed power supply, a symmetrical bidirectional pulsed power supply, or an asymmetrical pulsed power supply.
在一些实施例中,所述镀膜设备进一步包括一壳体,其中所述腔体、所述输送管路、所述抽气装置、所述抽气管路以及供电装置均被安装于所述壳体。In some embodiments, the coating equipment further includes a housing, wherein the cavity, the delivery pipeline, the air extraction device, the air extraction pipeline, and the power supply device are all installed in the housing .
本发明还提供一DLC薄膜的镀膜方法,其通过一镀膜设备在基材表面基于碳氢气体为反应原料制备所述DLC薄膜,包括步骤:The present invention also provides a method for coating a DLC thin film, which uses a coating device to prepare the DLC thin film on the surface of a substrate based on hydrocarbon gas as a reaction raw material, including the steps:
(a)将该基材置于所述镀膜设置的一腔体的一腔室内的一电极支架;(a) The substrate is placed in an electrode holder in a cavity of a cavity provided with the coating;
(b)对所述腔室进行负压产生操作;以及(b) Perform a negative pressure generating operation on the chamber; and
(c)以化学气相沉积的方式在该基材的表面制备DLC薄膜。(c) Prepare a DLC film on the surface of the substrate by chemical vapor deposition.
在一些实施例中,所述步骤(c)进一步包括步骤:(c.1)通过一气源管道通入气体于所述腔室,并提供电压作用于所述腔室内的所述气体,以对该基材表面进行刻蚀处理;以及(c.2)通过至少一反应原料管道通入一反应原料气体于所述腔室,并提供电压作用于所述腔室内的气体,以在该基材的表面制备所述DLC薄膜。In some embodiments, the step (c) further includes the step of: (c.1) passing gas into the chamber through a gas source pipe, and providing a voltage to act on the gas in the chamber to Performing an etching treatment on the surface of the substrate; and (c.2) passing a reaction raw material gas into the chamber through at least one reaction raw material pipe, and providing a voltage to act on the gas in the chamber so that the substrate The DLC film is prepared on the surface of the material.
在一些实施例中,通入所述腔室内的所述气体的气体流量为10sccm~1000sccm。In some embodiments, the gas flow rate of the gas passing into the chamber is 10 sccm to 1000 sccm.
在一些实施例中,将所述电极支架连接于一脉冲电源,以提供脉冲电压作用于所述腔室内的气体。In some embodiments, the electrode holder is connected to a pulse power source to provide a pulse voltage to act on the gas in the chamber.
在一些实施例中,将所述脉冲电源的一负极端电连接于所述电极支架,所述腔体接地,并且所述电极支架与所述腔体之间绝缘。In some embodiments, a negative terminal of the pulse power supply is electrically connected to the electrode holder, the cavity is grounded, and the electrode holder is insulated from the cavity.
在一些实施例中,将所述脉冲电源的一正极端和一负极端分别电连接于所述电极支架的多层金属板,并使所述电极支架的相邻的两个金属板互为正负极。In some embodiments, a positive terminal and a negative terminal of the pulse power supply are respectively electrically connected to the multilayer metal plate of the electrode holder, and two adjacent metal plates of the electrode holder are mutually positive. negative electrode.
在一些实施例中,将所述电极支架连接于一脉冲电源和一射频电源,以提供脉冲电压和射频电压作用于所述腔室内的气体。In some embodiments, the electrode holder is connected to a pulse power supply and a radio frequency power supply to provide pulse voltage and radio frequency voltage to act on the gas in the chamber.
在一些实施例中,其中以一第二真空泵作为一第一真空泵的前级泵共同协作地方式对所述腔室进行抽真空,其中所述第二真空泵被实施为包括干泵和罗茨泵,其中所述第一真空泵被实施为分子泵。In some embodiments, a second vacuum pump is used as a backing pump of a first vacuum pump to vacuum the chamber in a cooperative manner, wherein the second vacuum pump is implemented to include a dry pump and a roots pump , Wherein the first vacuum pump is implemented as a molecular pump.
附图说明Description of the drawings
图1是根据本发明的一个优选实施例的一镀膜设备的立体示意图。Fig. 1 is a perspective schematic view of a coating equipment according to a preferred embodiment of the present invention.
图2是根据本发明的上述优选实施例的所述镀膜设备的另一视角的立体示意图。Fig. 2 is a three-dimensional schematic diagram of the coating equipment according to the above-mentioned preferred embodiment of the present invention from another perspective.
图3是根据本发明的上述优选实施例的所述镀膜设备的抽气装置的第二真空泵的立体示意图。Fig. 3 is a perspective schematic view of a second vacuum pump of the air pumping device of the coating equipment according to the above-mentioned preferred embodiment of the present invention.
图4是根据本发明的上述优选实施例的所述镀膜设备的抽气装置的第一真空泵的立体示意图。Fig. 4 is a perspective schematic view of the first vacuum pump of the air pumping device of the coating equipment according to the above-mentioned preferred embodiment of the present invention.
图5是根据本发明的上述优选实施例的所述镀膜设备的箱体的立体示意图。Fig. 5 is a perspective schematic view of the box body of the coating equipment according to the above-mentioned preferred embodiment of the present invention.
图6是根据本发明的上述优选实施例的所述镀膜设备的结构框图。Fig. 6 is a structural block diagram of the coating equipment according to the above-mentioned preferred embodiment of the present invention.
图7是根据本发明的上述优选实施例的所述镀膜设备的输送管路的结构框图。Fig. 7 is a structural block diagram of the conveying pipeline of the coating equipment according to the above-mentioned preferred embodiment of the present invention.
图8是根据本发明的上述优选实施例的所述镀膜设备的空气输送管路的结构框图。Fig. 8 is a structural block diagram of the air conveying pipeline of the coating equipment according to the above-mentioned preferred embodiment of the present invention.
图9是根据本发明的上述优选实施例的所述镀膜设备的供电装置的结构框图。Fig. 9 is a structural block diagram of the power supply device of the coating equipment according to the above-mentioned preferred embodiment of the present invention.
图10是根据本发明的上述优选实施例的所述镀膜设备的支架的立体示意图。Fig. 10 is a perspective schematic view of the support of the coating equipment according to the above-mentioned preferred embodiment of the present invention.
具体实施方式Detailed ways
以下描述用于揭露本发明以使本领域技术人员能够实现本发明。以下描述中的优选实施例只作为举例,本领域技术人员可以想到其他显而易见的变型。在以下描述中界定的本发明的基本原理可以应用于其他实施方案、变形方案、改进方案、等同方案以及没有背离本发明的精神和范围的其他技术方案。The following description is used to disclose the present invention so that those skilled in the art can implement the present invention. The preferred embodiments in the following description are only examples, and those skilled in the art can think of other obvious variations. The basic principles of the present invention defined in the following description can be applied to other embodiments, modifications, improvements, equivalents, and other technical solutions that do not deviate from the spirit and scope of the present invention.
本领域技术人员应理解的是,在本发明的揭露中,术语“纵向”、“横向”、“上”、“下”、“前”、“后”、“左”、“右”、“竖直”、“水平”、“顶”、“底”、“内”、“外”等指示的方位或位置关系是基于附图所示的方位或位置关系,其仅是为了便于描述本发明和简化描述,而不是指示或暗示所指的装置或元件必须具有特定的方位、以特定的方位构造和操作,因此上述术语不能理解为对本发明的限制。Those skilled in the art should understand that, in the disclosure of the present invention, the terms "longitudinal", "lateral", "upper", "lower", "front", "rear", "left", "right", " The orientation or positional relationship indicated by "vertical", "horizontal", "top", "bottom", "inner", "outer", etc. are based on the orientation or positional relationship shown in the drawings, which is only for the convenience of describing the present invention And to simplify the description, rather than indicating or implying that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore the above terms should not be construed as limiting the present invention.
可以理解的是,术语“一”应理解为“至少一”或“一个或多个”,即在一个实施例中,一个元件的数量可以为一个,而在另外的实施例中,该元件的数量可以为多个,术语“一”不能理解为对数量的限制。It can be understood that the term "a" should be understood as "at least one" or "one or more", that is, in one embodiment, the number of an element may be one, and in another embodiment, the number of the element The number can be multiple, and the term "one" cannot be understood as a restriction on the number.
在本说明书的描述中,参考术语“一个实施例”、“一些实施例”、“示例”、 “具体示例”、或“一些示例”等的描述意指结合该实施例或示例描述的具体特征、结构、材料或者特点包含于本发明的至少一个实施例或示例中。在本说明书中,对上述术语的示意性表述不必须针对的是相同的实施例或示例。而且,描述的具体特征、结构、材料或者特点可以在任一个或多个实施例或示例中以合适的方式结合。此外,在不相互矛盾的情况下,本领域的技术人员可以将本说明书中描述的不同实施例或示例以及不同实施例或示例的特征进行结合和组合。In the description of this specification, descriptions with reference to the terms "one embodiment", "some embodiments", "examples", "specific examples", or "some examples" etc. mean specific features described in conjunction with the embodiment or example , Structures, materials or features are included in at least one embodiment or example of the present invention. In this specification, the schematic representations of the above terms do not necessarily refer to the same embodiment or example. Moreover, the described specific features, structures, materials or characteristics can be combined in any one or more embodiments or examples in a suitable manner. In addition, those skilled in the art can combine and combine the different embodiments or examples and the features of the different embodiments or examples described in this specification without contradicting each other.
如图1至图10所示为本发明的一个优选实施例的一镀膜设备100,其中所述镀膜设备100用于在至少一基材600表面镀上至少一层DLC薄膜或者膜层,其中所述镀膜设备100能够实现大面积镀膜,从而实现同时在大批量的所述基材600的表面镀上所述DLC薄膜。Figures 1 to 10 show a coating device 100 according to a preferred embodiment of the present invention, wherein the coating device 100 is used for coating at least one layer of DLC film or layer on the surface of at least one substrate 600, wherein The coating equipment 100 can realize large-area coating, so as to realize the simultaneous coating of the DLC film on the surface of the substrate 600 in large quantities.
在本实施例中,所述镀膜设备100采用等离子体化学气相沉积的方法在所述基材600的表面制备所述DLC薄膜或者膜层。即所述DLC薄膜被沉积于所述基材600的表面,从而提升所述基材600的表面的力学方面、光学方面或者化学方面等性质,其中所述基材600如具备预设形状结构的需镀膜产品,如PCB电路板、手机、电子设备、电子产品盖板、电子产品显示屏幕、手机玻璃屏幕、电脑屏幕、手机后盖、电子设备外壳、键盘膜或者其他类型的需镀膜产品等,在此不受限制。例如,所述镀膜设备100在电子产品显示屏幕上制备所述DLC薄膜,能够有效地解决该电子产品显示屏幕不耐摔、不耐磨以及表面强化成本高的问题。In this embodiment, the coating device 100 adopts a plasma chemical vapor deposition method to prepare the DLC film or film layer on the surface of the substrate 600. That is, the DLC film is deposited on the surface of the substrate 600, thereby improving the mechanical, optical, or chemical properties of the surface of the substrate 600, wherein the substrate 600 has a predetermined shape and structure. Products that need to be coated, such as PCB circuit boards, mobile phones, electronic equipment, electronic product covers, electronic product display screens, mobile phone glass screens, computer screens, mobile phone back covers, electronic device shells, keyboard films or other types of products that need to be coated, etc. There is no restriction here. For example, the coating equipment 100 prepares the DLC film on the display screen of an electronic product, which can effectively solve the problems of the display screen of the electronic product that the display screen is not resistant to fall, wear resistance, and the surface strengthening cost is high.
如图1、图2、图5和图6所示,优选地,所述镀膜设备100包括一腔体10、一组输送管路20、至少一抽气装置30、至少一抽气管路40、一供电装置50以及至少一电极支架60,其中所述腔体10具有一可封闭的腔室101,其中所述电极支架60被设置于所述腔体10的所述腔室101,其中所述电极支架60用于支撑所述基材600,其中所述输送管路20被连通于所述腔体10的所述腔室101,其中所述输送管路20用于向所述腔室101内通入气体原料,所述气体原料如氮气、四氟化碳或者氦气、氩气等惰性气体的等离子体源气体、氢气、碳氢气体等的反应气体或者N、Si、F、B等掺杂元素的辅助气体。所述抽气装置30通过所述抽气管路40连通所述腔体10的所述腔室101并通过所述抽气管路40持续地抽出所述腔室101内的气体,以控制所述腔室101内的气压,其中所述供电装置50用于提供射频和/或脉冲电压作用于所述腔室101内的气体,以供所述镀膜设备100通过化学气相沉积的方式在所述基材600的表面制备所述DLC薄膜或者 膜层。As shown in Figure 1, Figure 2, Figure 5 and Figure 6, preferably, the coating equipment 100 includes a cavity 10, a set of conveying pipelines 20, at least one air extraction device 30, at least one air extraction pipeline 40, A power supply device 50 and at least one electrode holder 60, wherein the cavity 10 has a closable cavity 101, wherein the electrode holder 60 is disposed in the cavity 101 of the cavity 10, wherein the The electrode holder 60 is used to support the substrate 600, wherein the delivery pipe 20 is connected to the chamber 101 of the cavity 10, and the delivery pipe 20 is used to feed the cavity 101 Gas raw materials such as plasma source gases such as nitrogen, carbon tetrafluoride or inert gases such as helium and argon, reactive gases such as hydrogen, hydrocarbon gas, or doped N, Si, F, B, etc. Auxiliary gas for miscellaneous elements. The air extraction device 30 communicates with the chamber 101 of the cavity 10 through the air extraction line 40 and continuously extracts the gas in the chamber 101 through the air extraction line 40 to control the cavity The air pressure in the chamber 101, wherein the power supply device 50 is used to provide radio frequency and/or pulse voltage to act on the gas in the chamber 101 for the coating equipment 100 to deposit on the substrate by chemical vapor deposition. The DLC film or film layer is prepared on the surface of 600.
如图7所示,进一步地,所述腔体10具有与所述腔室101相通的至少一抽气口11、至少一进气口12以及至少一进料口13,其中所述输送管路20包括至少一气源管道21、至少一氢气管道22以及至少一反应原料管道23,其中所述抽气口11被接入所述抽气管路40以供所述抽气装置30通过所述抽气管路40抽出所述腔室101内的气体,其中所述进气口12被接入所述气源管道21以供向所述腔室101内通入氮气、四氟化碳或者氦气、氩气等惰性气体或者等离子体源气体等,其中所述进料口13被接入所述氢气管道22和所述反应原料管道23,其中所述氢气管道22用于向所述腔室101内通入氢气,其中所述反应原料管道23用于向所述腔室101内通入碳氢气体等反应原料,所述碳氢气体例如1-6碳原子数的烷烃、烯烃、炔烃等气态原料的其中一种或者多种组合,或者由更高碳原子数的液态的碳氢原料汽化而成的气态原料等的其中一种或者多种组合。也就是说,所述反应原料管道23可以用来输送液态的反应原料,然后将经汽化后的反应原料通过所述进料口13通入所述腔室101内。As shown in FIG. 7, further, the cavity 10 has at least one suction port 11, at least one gas inlet 12, and at least one feed port 13 communicating with the cavity 101, wherein the conveying pipe 20 It includes at least one gas source pipeline 21, at least one hydrogen pipeline 22, and at least one reaction raw material pipeline 23, wherein the gas extraction port 11 is connected to the gas extraction pipeline 40 for the gas extraction device 30 to pass through the gas extraction pipeline 40 Extract the gas in the chamber 101, wherein the gas inlet 12 is connected to the gas source pipe 21 for introducing nitrogen, carbon tetrafluoride or helium or argon into the chamber 101 Inert gas or plasma source gas, etc., wherein the feed port 13 is connected to the hydrogen pipeline 22 and the reaction raw material pipeline 23, wherein the hydrogen pipeline 22 is used to pass into the chamber 101 Hydrogen, wherein the reaction raw material pipeline 23 is used to pass the reaction raw materials such as hydrocarbon gas into the chamber 101, such as gaseous raw materials such as alkanes, alkenes, and alkynes with 1-6 carbon atoms. One or more combinations thereof, or one or more combinations of gaseous raw materials formed by vaporizing liquid hydrocarbon raw materials with higher carbon number. In other words, the reaction raw material pipeline 23 can be used to transport liquid reaction raw materials, and then the vaporized reaction raw materials are passed into the chamber 101 through the feed port 13.
进一步地,所述腔体10的腔门上可设有视窗,以供用户观察所述腔室101内的镀膜情况。所述进气口12与所述进料口13均设于所述腔体10的侧壁,其中所述进气口12与所述气源管道21之间封闭连接,其中所述进料口13分别与所述氢气管道22和所述反应原料管道23之间封闭连接,如为螺纹、套接、卡扣等法兰连接。Further, the cavity door of the cavity 10 may be provided with a window for the user to observe the coating condition in the cavity 101. The air inlet 12 and the feed inlet 13 are both provided on the side wall of the cavity 10, wherein the air inlet 12 and the air source pipe 21 are connected in a closed connection, wherein the feed inlet 13 are respectively closed and connected with the hydrogen pipeline 22 and the reaction raw material pipeline 23, such as flange connections such as screw threads, sockets, and buckles.
更进一步地,所述进料口13被实施为两个,其中一个所述进料口13用于接入所述氢气管道22以供向所述腔室101内单独通入氢气,另一所述进料口13用于接入所述反应原料管道23以供向所述腔室101内单独通入反应原料。可选地,所述进料口13也可以被实施为一个,其中所述氢气管道22和所述反应原料管道23被共同接入同一所述进料口13,以供分别经由同一所述进料口13向所述腔室101内通入氢气或者反应原料。Furthermore, the feed ports 13 are implemented as two, one of the feed ports 13 is used to connect to the hydrogen pipeline 22 for the independent hydrogen gas flow into the chamber 101, and the other The feed port 13 is used to connect to the reaction raw material pipeline 23 for separately passing the reaction raw materials into the chamber 101. Optionally, the feed port 13 can also be implemented as one, wherein the hydrogen pipe 22 and the reaction raw material pipe 23 are connected to the same feed port 13 together, so as to pass through the same feed port 13 respectively. The feed port 13 passes hydrogen or reaction raw materials into the chamber 101.
更优选地,所述输送管路20进一步包括一掺杂原料管道24,其中所述掺杂原料管道24被接入所述进料口13以供向所述腔室101内充入N、Si、F、B等掺杂元素的辅助气体。例如,掺杂的Si元素的反应原料包括但不限于含硅有机化合物,包括有机直链硅氧烷、环硅氧烷、烷氧基硅烷、含不饱和碳碳双键硅氧烷的其中一种或者多种组合。进一步地,选择六甲基二硅氧烷、四甲基二乙烯基 二硅氧烷、六甲基环三硅氧烷、八甲基环四硅氧烷。例如,掺杂的N元素的反应原料包括但不限于N 2、含氮碳氢化合物。例如,掺杂的F元素的反应原料包括但不限于氟碳化合物,进一步地,选自四氟化碳、四氟乙烯。例如,掺杂的B元素的反应原料包括但不限于常压下沸点低于300℃的硼烷,进一步地,选择戊硼烷、己硼烷等。 More preferably, the delivery pipeline 20 further includes a doping raw material pipeline 24, wherein the doping raw material pipeline 24 is connected to the feed port 13 for filling the chamber 101 with N and Si. , F, B and other auxiliary gases doped with elements. For example, the reaction raw material for the doped Si element includes, but is not limited to, silicon-containing organic compounds, including one of organic linear siloxanes, cyclosiloxanes, alkoxysilanes, and unsaturated carbon-carbon double bond-containing siloxanes. Kind or multiple combinations. Further, hexamethyldisiloxane, tetramethyldivinyldisiloxane, hexamethylcyclotrisiloxane, and octamethylcyclotetrasiloxane are selected. For example, the reaction raw materials of the doped N element include, but are not limited to, N 2 and nitrogen-containing hydrocarbons. For example, the raw materials for the doped F element include but are not limited to fluorocarbon compounds, and are further selected from carbon tetrafluoride and tetrafluoroethylene. For example, the reaction raw material for the doped element B includes but is not limited to borane with a boiling point lower than 300° C. under normal pressure, and further, pentaborane, hexaborane, etc. are selected.
可以理解的是,所述气源管道21、所述氢气管道22、所述反应原料管道23以及所述掺杂原料管道24均能够被分别设置一开关阀以分别控制管道的开关,实现气体的流通与关闭,或者所述开关阀能够控制被充入所述腔室101内的气体的流量大小,在此不受限制。It is understandable that the gas source pipeline 21, the hydrogen pipeline 22, the reaction raw material pipeline 23, and the doping raw material pipeline 24 can each be provided with an on-off valve to respectively control the opening and closing of the pipelines to realize gas Circulation and closure, or that the on-off valve can control the flow rate of the gas filled into the chamber 101, is not limited here.
可选地,所述掺杂原料管道24可以被接入额外独立的所述进料口13以单独向所述腔室101内充入所述掺杂元素的辅助气体。或者,所述掺杂原料管道24可以与所述氢气管道22或者所述反应原料管道23共用同一个所述进料口13以向所述腔室101分别充入气体等。Optionally, the doping raw material pipeline 24 may be connected to an additional independent feed port 13 to separately charge the auxiliary gas of the doping element into the chamber 101. Alternatively, the doping material pipe 24 may share the same feed port 13 with the hydrogen pipe 22 or the reaction material pipe 23 to fill the chamber 101 with gas or the like respectively.
值得一提的是,在制备所述DLC薄膜时,掺杂元素的含量在所述DLC薄膜中的原子数比例优选地小于10%,经所述镀膜设备100制备的所述DLC薄膜中,掺杂元素含量低于40%,所述DLC薄膜厚度优选为10-800nm。熟知本领域技术人员应当理解的是,Si、Cu、N、F、Al等元素的掺杂含量不宜太多,这些掺杂元素与DLC中的碳元素会产生成键作用,破坏原来DLC的微观结构,改变沉积过程中的生长模式,当掺杂元素的含量进一步提高时,可能出现相分离或者完全改变DLC中类金刚石结构,使所述DLC薄膜丧失了耐磨、高硬度的性能。此外,根据不同的镀膜工艺需求,所述掺杂元素反应气源也可以增加含碳气源的离化率,有利于实现镀膜。It is worth mentioning that when preparing the DLC film, the content of doping elements in the DLC film is preferably less than 10% of the atomic number. The DLC film prepared by the coating equipment 100 is doped The content of miscellaneous elements is less than 40%, and the thickness of the DLC film is preferably 10-800 nm. Those skilled in the art should understand that the doping content of Si, Cu, N, F, Al and other elements should not be too much. These doping elements will form a bond with the carbon element in the DLC, which will damage the original DLC. The structure changes the growth mode during the deposition process. When the content of doping elements is further increased, phase separation may occur or the diamond-like structure in the DLC may be completely changed, so that the DLC film loses the performance of wear resistance and high hardness. In addition, according to different coating process requirements, the doping element reaction gas source can also increase the ionization rate of the carbon-containing gas source, which is beneficial to realize the coating.
在本实施例中,所述抽气口11被设置于所述腔体10的所述腔室101的中部位置,其中所述进气口12和所述进料口13均被设置于所述腔体10的所述腔室101的侧壁位置,以使气体从所述腔室101的侧壁的所述进气口12和所述进料口13被充入,并从所述腔室101的中部位置的所述抽气口11被抽出,以确保被充入的气体尽量均匀地扩散至每个所述基材600的表面,从而尽可能地使每个基材600的表面被均匀地镀上所述DLC薄膜。In this embodiment, the suction port 11 is provided in the middle of the chamber 101 of the cavity 10, wherein the gas inlet 12 and the feed port 13 are both provided in the cavity. The position of the side wall of the chamber 101 of the body 10 so that gas is filled from the gas inlet 12 and the feed port 13 of the side wall of the chamber 101, and from the chamber 101 The suction port 11 in the middle of the position is drawn out to ensure that the filled gas diffuses to the surface of each substrate 600 as evenly as possible, so that the surface of each substrate 600 is evenly plated as much as possible The above DLC film.
可选地,所述抽气口11可以被设置于所述腔室101的底壁或者顶壁的中部,所述抽气口11也可以被连通于被设置于所述腔室101的中部的一抽气柱,其中 所述进气口12和所述进料口13可以位于所述腔室101的同一侧壁,也可以分别位于所述腔室101的不同侧壁。可选地,所述抽气口11可以被设置于所述腔室101的侧壁位置,所述进气口12和所述进料口13可以被设置于所述腔室101的中部位置或者与所述抽气口11相反的侧壁位置等,在此不受限制。Optionally, the suction port 11 may be provided in the middle of the bottom or top wall of the chamber 101, and the suction port 11 may also be connected to a suction port provided in the middle of the chamber 101. The air column, wherein the air inlet 12 and the feed inlet 13 may be located on the same side wall of the chamber 101, or may be located on different side walls of the chamber 101, respectively. Optionally, the suction port 11 may be provided at a side wall position of the chamber 101, and the air intake port 12 and the feed port 13 may be provided at the middle position of the chamber 101 or at the same position as the side wall of the chamber 101. The position of the side wall opposite to the suction port 11 is not limited here.
可以理解的是,所述抽气口11、所述进气口12以及所述进料口13在所述腔室101的相对位置能够被根据实际需求进行预设,以尽可能地满足大批量的所述基材被均匀镀膜的需求,以确保规格统一化。It is understandable that the relative positions of the suction port 11, the gas inlet 12, and the feed port 13 in the chamber 101 can be preset according to actual needs, so as to meet the needs of mass production as much as possible. The substrate needs to be uniformly coated to ensure uniformity of specifications.
如图3和图4所示,优选地,所述抽气装置30包括至少一第一真空泵31和至少一第二真空泵32,其中所述第一真空泵31和所述第二真空泵32分别通过所述抽气管路40被连通于所述抽气口11,其中所述第二真空泵32作为所述第一真空泵31的前级泵共同协作地通过所述抽气管路40对所述腔室101进行负压操作如抽真空并维持所述腔室101内的气压处于预设范围内。进一步地,所述腔室101被抽出气体以接近真空状态,优选地,所述腔室101内的气压被降至0.01Pa以下,甚至0.001Pa以下。在镀膜过程中,所述抽气装置30用于通过所述抽气管路40持续地将所述腔室101内的气体抽出以使维持所述腔室101内的气体的浓度在一定范围内,优选地,所述腔室101内的气压被维持在0.01至100Pa之间。As shown in Figures 3 and 4, preferably, the pumping device 30 includes at least one first vacuum pump 31 and at least one second vacuum pump 32, wherein the first vacuum pump 31 and the second vacuum pump 32 respectively pass through The air extraction line 40 is connected to the air extraction port 11, wherein the second vacuum pump 32 serves as the backing pump of the first vacuum pump 31 and cooperates to perform negative pressure on the chamber 101 through the air extraction line 40. The pressure operation is to draw a vacuum and maintain the air pressure in the chamber 101 within a preset range. Further, the chamber 101 is pumped with gas to be close to a vacuum state. Preferably, the air pressure in the chamber 101 is reduced to below 0.01 Pa, or even below 0.001 Pa. During the coating process, the air extraction device 30 is used to continuously extract the gas in the chamber 101 through the air extraction pipe 40 so as to maintain the concentration of the gas in the chamber 101 within a certain range, Preferably, the air pressure in the chamber 101 is maintained between 0.01 and 100 Pa.
在所述镀膜设备100镀膜前,工作人员将所述腔体10的所述腔室101打开,其中所述基材600被放置于所述电极支架60,其中所述电极支架60位于所述腔室101,然后,工作人员将所述腔体10的所述腔室101密封关闭,然后开启所述镀膜设备100进行镀膜。Before the coating of the coating equipment 100, the staff opens the chamber 101 of the cavity 10, wherein the substrate 600 is placed on the electrode holder 60, and the electrode holder 60 is located in the cavity. Then, the worker seals and closes the chamber 101 of the cavity 10, and then turns on the coating equipment 100 for coating.
进一步地,本实施例还提供了所述镀膜设备100的镀膜方法,包括步骤:Further, this embodiment also provides a coating method of the coating equipment 100, which includes the steps:
S01、对所述腔室101进行负压产生操作如抽真空,在镀膜时,通过所述抽气装置30将所述腔室101内的空气抽出以控制所述腔室101内的气压在预设范围内,以尽量降低所述腔室101内残留的空气影响镀膜质量,直到所述腔室101内气压达到预设气压范围。S01. Perform a negative pressure generation operation on the chamber 101, such as vacuuming. During film coating, the air in the chamber 101 is pumped out by the air pumping device 30 to control the air pressure in the chamber 101 in advance. It is set within the range to minimize the effect of the remaining air in the chamber 101 on the coating quality until the air pressure in the chamber 101 reaches the preset air pressure range.
S02、进入对所述基材600表面进行表面刻蚀处理或者表面清洗与活化阶段,具体地,将气体原料经由所述气源管道21被持续充入所述腔室101以供对所述基材进行表面刻蚀处理,优选地,通过所述气源管道21向所述腔室101内通入氩气或者氦气,其中通流量大致为10sccm~1000sccm,优选为80或100sccm。 同时,所述抽气装置30用于持续地一定量地抽出所述腔室101内的气体并维持所述腔室101内的气压保持在0.01-100Pa以内,优选为8Pa或10Pa或者100Pa。同时,所述供电装置50提供脉冲电压作用于所述腔室101内的气体,以清洗和活化所述基材600的表面,从而实现对所述基材600的表面进行刻蚀处理。优选地,所述供电装置50提供-100V至-5000V的高压脉冲偏压,占空比1%至90%,供电时间为1-60分钟以内(供电时间即为步骤S02中对所述基材600表面进行清洗与活化的时间),优选地,所述供电装置50提供电压为-3000V,占空比为20%或30%,频率为10kHz或者40kHz,供电时间为5、10、20、或者30min等。S02. Enter the stage of performing surface etching treatment or surface cleaning and activation on the surface of the substrate 600. Specifically, gas raw materials are continuously filled into the chamber 101 through the gas source pipeline 21 for the substrate 600 The surface of the material is etched. Preferably, argon or helium is introduced into the chamber 101 through the gas source pipe 21, wherein the flow rate is approximately 10 sccm to 1000 sccm, preferably 80 or 100 sccm. At the same time, the air extraction device 30 is used to continuously extract a certain amount of gas in the chamber 101 and maintain the air pressure in the chamber 101 within 0.01-100 Pa, preferably 8 Pa or 10 Pa or 100 Pa. At the same time, the power supply device 50 provides a pulse voltage to act on the gas in the chamber 101 to clean and activate the surface of the substrate 600, so as to achieve etching treatment on the surface of the substrate 600. Preferably, the power supply device 50 provides a high voltage pulse bias voltage of -100V to -5000V, a duty ratio of 1% to 90%, and a power supply time of 1-60 minutes (the power supply time is the time for the substrate in step S02 600 surface cleaning and activation time), preferably, the power supply device 50 provides a voltage of -3000V, a duty cycle of 20% or 30%, a frequency of 10kHz or 40kHz, and a power supply time of 5, 10, 20, or 30min and so on.
可选地,在所述步骤S02结束后,关闭所述气源管道21以停止向所述腔室101内充入气体,具体地,所述气源管道21具有所述开关阀,其中所述开关阀用于控制所述气源管道21的开关,以实现打开或者关闭所述气源管道21。Optionally, after the step S02 ends, the gas source pipe 21 is closed to stop filling the chamber 101 with gas. Specifically, the gas source pipe 21 has the on-off valve, wherein The on-off valve is used to control the switching of the gas source pipeline 21 to realize opening or closing of the gas source pipeline 21.
可选地,在所述步骤S02结束后,继续通过所述气源管道21向所述腔室101内通入气体,以供通过等离子体化学气相沉积的方式在所述基材600的表面制备所述DLC薄膜。可选地,被通入所述腔室101内的待离化的气体流量能够被适应性地改变。Optionally, after the step S02 is completed, continue to pass gas into the chamber 101 through the gas source pipe 21 for preparation on the surface of the substrate 600 by means of plasma chemical vapor deposition. The DLC film. Optionally, the flow rate of the gas to be ionized that is passed into the chamber 101 can be changed adaptively.
值得一提的是,在对所述基材600表面进行清洗与活化阶段的过程中,通过所述气源管道21充入所述腔室101内的待离化的气体流量能够被预设在合理范围内,以防止被充入所述腔室101内的待离化气体的流量过高或者过低均会影响所述基材600表面离化效果的现象。所述供电装置50提供的所述脉冲电压被预设在合理范围内,以防止电压过低达不到对所述基材600表面进行良好的清洗与活化效果,或者电压过高存在损坏所述基材600的风险。所述供电装置50的供电时间能够被预设在合理范围内,以防止供电时间过短达不到对所述基材600表面进行良好的清洗与活化效果,或者供电时间过长会延长整个镀膜工艺的周期,造成不必要的浪费。It is worth mentioning that in the process of cleaning and activating the surface of the substrate 600, the flow rate of the gas to be ionized filled into the chamber 101 through the gas source pipe 21 can be preset at Within a reasonable range, to prevent the phenomenon that the flow rate of the gas to be ionized filled into the chamber 101 is too high or too low, which will affect the surface ionization effect of the substrate 600. The pulse voltage provided by the power supply device 50 is preset within a reasonable range to prevent the voltage from being too low to achieve a good cleaning and activating effect on the surface of the substrate 600, or the voltage is too high to damage the The risk of the substrate 600. The power supply time of the power supply device 50 can be preset within a reasonable range to prevent that the power supply time is too short to achieve a good cleaning and activation effect on the surface of the substrate 600, or the power supply time is too long to prolong the entire coating The cycle of the process causes unnecessary waste.
S03、在所述基材600表面进行镀膜,具体地,通过所述气源管道21向所述腔室101内充入气体,通过所述氢气管道22向所述腔室101内充入氢气,和通过所述反应原料管道23向所述腔室101内充入碳氢气体或者经气化后碳氢气体等反应原料,或者进一步地通过所述掺杂原料管道24向所述腔室101内充入掺杂原料等气体。优选地,被充入所述腔室101内的待离化的气体的流量为 10-200sccm、氢气的气体流量为0-100sccm、碳氢气体等反应原料的气体流量为50-1000sccm或者掺杂元素反应原料的气体流量为0-100sccm。同时,所述抽气装置30用于持续地一定量地抽出所述腔室101内的气体并维持所述腔室101内的气压保持在0.01-100Pa以内,优选为8Pa或10Pa或者100Pa。同时,利用所述供电装置50提供射频电压和/或高压脉冲偏压辅助等离子体化学气相沉积的方式制备所述DLC薄膜于所述基材600的表面,其中所述供电装置50提供射频电压的功率为10-800W,或者提供脉冲偏压的电压为-100V至-5000V,占空比为10%-80%,所述供电装置50的供电时间为5-300分钟,即所述步骤S03中,对所述基材600进行镀膜的时间大致为5-300分钟。S03, coating the surface of the substrate 600, specifically, filling the chamber 101 with gas through the gas source pipe 21, and filling the chamber 101 with hydrogen through the hydrogen pipe 22; And filling the chamber 101 with reaction materials such as hydrocarbon gas or gasified hydrocarbon gas through the reaction raw material pipeline 23, or further into the chamber 101 through the doping raw material pipeline 24 Fill the gas with dopant raw materials. Preferably, the flow rate of the gas to be ionized filled into the chamber 101 is 10-200 sccm, the gas flow rate of hydrogen is 0-100 sccm, and the gas flow rate of the reaction raw materials such as hydrocarbon gas is 50-1000 sccm or doped. The gas flow rate of the elemental reaction raw materials is 0-100 sccm. At the same time, the air extraction device 30 is used to continuously extract a certain amount of gas in the chamber 101 and maintain the air pressure in the chamber 101 within 0.01-100 Pa, preferably 8 Pa or 10 Pa or 100 Pa. At the same time, the DLC film is prepared on the surface of the substrate 600 by the power supply device 50 providing radio frequency voltage and/or high-voltage pulse bias assisted plasma chemical vapor deposition, wherein the power supply device 50 provides radio frequency voltage The power is 10-800W, or the pulse bias voltage is -100V to -5000V, the duty cycle is 10%-80%, and the power supply time of the power supply device 50 is 5-300 minutes, that is, in step S03 The time for coating the substrate 600 is approximately 5-300 minutes.
需要理解的是,在所述步骤S03中,所述供电装置50的电压或者功率能够被预设,在所述供电装置50提供的电压作用下,所述腔室101内的所有的气体基本上均能够被离化为等离子体,使得所述腔室101内形成等离子体环境,以便于所述镀膜设备100以化学气相沉积的方式在所述基材600的表面制备所述薄膜。It should be understood that in the step S03, the voltage or power of the power supply device 50 can be preset. Under the action of the voltage provided by the power supply device 50, all the gas in the chamber 101 is basically Both can be ionized into plasma, so that a plasma environment is formed in the chamber 101, so that the coating device 100 can prepare the thin film on the surface of the substrate 600 by means of chemical vapor deposition.
在所述步骤S03中,具体地,所述供电装置50能够提供射频和/或高压脉冲偏压作用于所述腔室101内的气体,其中所述供电装置50通过提供射频电场对所述腔室101内的待离化的气体和所述反应原料气体等气体进行放电以使所述腔室101内处于等离子体环境和所述反应气体原料处于高能量状态。所述供电装置50通过提供高压脉冲偏压中的强电压在所述腔室101内产生强电场,以使处于高能量状态的活性粒子受到强电场作用加速沉积于所述基材600的表面,并形成非晶态碳网络结构。所述供电装置50通过提供高压脉冲偏压中的空电压或者低电压的状态,以使被沉积于所述基材600表面的非晶态碳网络结构进行自由驰豫,并在热力学作用下碳结构向稳定相--弯曲石墨烯片层结构转变,并埋置于非晶态碳网络中,从而在所述基材600表面形成所述DLC薄膜。In the step S03, specifically, the power supply device 50 can provide radio frequency and/or high voltage pulse bias to act on the gas in the chamber 101, wherein the power supply device 50 provides a radio frequency electric field to the cavity 101. The gas to be ionized in the chamber 101 and the reaction material gas and other gases are discharged so that the chamber 101 is in a plasma environment and the reaction gas material is in a high-energy state. The power supply device 50 generates a strong electric field in the chamber 101 by providing a strong voltage in a high-voltage pulse bias, so that the active particles in a high-energy state are accelerated by the strong electric field to deposit on the surface of the substrate 600, And form an amorphous carbon network structure. The power supply device 50 provides the empty voltage or the low voltage state in the high-voltage pulse bias to allow the amorphous carbon network structure deposited on the surface of the substrate 600 to relax freely, and the carbon under the action of thermodynamics The structure is transformed into a stable phase-curved graphene sheet structure, and is embedded in an amorphous carbon network, thereby forming the DLC film on the surface of the substrate 600.
值得一提的是,在所述步骤S03中,所述气源管道21能够被关闭,以停止向所述腔室101内充入待离化的气体,或者向所述腔室101内充入的气体流量能够被预设在合理范围内。所述氢气管道22能够被关闭,以不向或者中途停止向所述腔室101内充入氢气,或者通过所述氢气管道22向所述腔室101内充入的氢气的气体流量能够被预设在合理范围内。所述反应原料管道23能够被控制开关,其中通过所述反应原料管道23向所述腔室101内充入反应原料的气体流量能够被预设在合理范围内。所述掺杂原料管道24能够被关闭,以不向或者中途 停止向所述腔室101内充入所述掺杂元素反应原料,或者通过所述掺杂原料管道24被充入所述腔室101内的掺杂元素反应原料的气体流量能够被预设在合理范围内。It is worth mentioning that in the step S03, the gas source pipe 21 can be closed to stop filling the chamber 101 with the gas to be ionized, or filling the chamber 101 The gas flow rate can be preset within a reasonable range. The hydrogen pipe 22 can be closed to prevent or stop filling the chamber 101 with hydrogen, or the gas flow rate of the hydrogen filled into the chamber 101 through the hydrogen pipe 22 can be preset. Set within a reasonable range. The reaction raw material pipeline 23 can be controlled to switch, wherein the gas flow rate of the reaction raw materials filled into the chamber 101 through the reaction raw material pipeline 23 can be preset within a reasonable range. The doping material pipe 24 can be closed to prevent or stop filling the chamber 101 with the doping element reaction material, or to be filled into the chamber through the doping material pipe 24 The gas flow rate of the doping element reaction raw material in 101 can be preset within a reasonable range.
需要理解的是,被充入所述腔室101内的待离化的气体如氮气或氩气、所述氢气、所述反应原料气体或者所述掺杂元素反应原料气体的气流流量的比例决定了所述DLC薄膜中的原子比,从而影响所述DLC薄膜的质量。通过预设所述供电装置50提供的射频和/或脉冲偏压的功率大小或者电压大小等参数,能够实现调控在镀膜过程中的温度大小、离化率或者沉积速率等相关参数,或者通过预设所述供电装置50的供电时间,防止因镀膜时间过短而导致所述DLC薄膜较薄、硬度表现差等现象,或者因镀膜时间过长而导致所述DLC薄膜较厚而影响透明性等现象的发生。It should be understood that the gas to be ionized, such as nitrogen or argon, the hydrogen, the reaction raw material gas, or the doping element reaction raw material gas, which is charged into the chamber 101, determines the ratio of the flow rate of the gas flow. The atomic ratio in the DLC film is affected, thereby affecting the quality of the DLC film. By presetting parameters such as the power or voltage of the radio frequency and/or pulse bias provided by the power supply device 50, the temperature, ionization rate, or deposition rate and other related parameters during the coating process can be adjusted, or through preset The power supply time of the power supply device 50 is set to prevent the DLC film from being thinner and the hardness performance poor due to the coating time being too short, or the DLC film being thicker due to the coating time being too long, which affects transparency, etc. The occurrence of the phenomenon.
[根据细则91更正 09.04.2020] 
也就是说,在所述步骤S03中,能够不向所述腔室101内充入不同流量的氢气,或者向所述腔室101内充入一定量的氢气,以制备含不同氢含量的DLC薄膜。可以理解的是,氢含量较高的DLC薄膜相较于氢含量较低的DLC薄膜有着更高的润滑性和透明性,而在所述步骤S03中,向所述腔室101内充入一定量的氢气,有利于镀膜过程中SP3键的形成,在一定程度上可以提高了所述DLC薄膜的硬度,但随着氢含量的进一步提高,所述DLC薄膜的硬度会逐步下降,因此根据不同的镀膜需求,在所述步骤S03中,可以选择性地通过所述氢气管道22向所述腔室101内充入预设量的氢气气体。
[Corrected according to Rule 91 09.04.2020]
That is to say, in the step S03, it is possible not to fill the chamber 101 with hydrogen at different flow rates, or to fill the chamber 101 with a certain amount of hydrogen to prepare DLC with different hydrogen content. film. It is understandable that the DLC film with higher hydrogen content has higher lubricity and transparency than the DLC film with lower hydrogen content, and in the step S03, a certain amount is filled into the chamber 101 A large amount of hydrogen is conducive to the formation of SP 3 bonds during the coating process, which can increase the hardness of the DLC film to a certain extent, but as the hydrogen content further increases, the hardness of the DLC film will gradually decrease, so according to For different coating requirements, in the step S03, the chamber 101 can be selectively filled with a preset amount of hydrogen gas through the hydrogen pipe 22.
相应地,在所述步骤S03中,能够选择性地通过所述掺杂原料管道24向所述腔室101内充入一定量的指定的掺杂元素反应原料。例如,向所述腔室内充入含氟元素的反应原料,使得制备的所述DLC薄膜具有更高的膜层疏水效果和透明度,但当氟原子含量超过20%时,所述DLC薄膜的硬度会显著降低(低于莫氏硬度4H)。Correspondingly, in the step S03, a certain amount of designated doping element reaction raw materials can be selectively filled into the chamber 101 through the doping raw material pipeline 24. For example, the reaction material containing fluorine is filled into the chamber, so that the prepared DLC film has a higher hydrophobic effect and transparency, but when the fluorine atom content exceeds 20%, the hardness of the DLC film Will be significantly reduced (less than 4H on the Mohs hardness).
S04、当所述步骤S03的镀膜时间结束后,所述输送管路20的所述气源管道21、所述氢气管道22、所述反应原料管道23以及所述掺杂原料管道24的开关阀均被关闭,同时关闭所述供电装置50,关闭所述抽气装置30。S04. After the coating time of step S03 ends, the on-off valves of the gas source pipeline 21, the hydrogen pipeline 22, the reaction raw material pipeline 23, and the doping raw material pipeline 24 of the delivery pipeline 20 Both are turned off, at the same time the power supply device 50 is turned off, and the air extraction device 30 is turned off.
如图8所示,进一步地,所述输送管路20进一步包括一空气输送管道25,其中所述腔体10进一步具有连通所述腔室101的至少一空气进口14,其中所述空气输送管道25连通所述腔室101的所述空气进口14,其中所述空气输送管道 25用于向所述腔室101内充入空气以使所述腔室101处于常压状态。即通过所述空气输送管道25向所述腔室101内充入一定量的空气使所述腔室101回归常压状态,以便于工作人员打开所述腔室101并取出所述基材600,至此一次镀膜工艺结束。在整个镀膜工艺过程中,所述镀膜设备100在制备DLC薄膜的过程中工艺可控性较好,有利于快速制备目标DLC薄膜。As shown in FIG. 8, further, the delivery pipeline 20 further includes an air delivery pipeline 25, wherein the cavity 10 further has at least one air inlet 14 communicating with the chamber 101, wherein the air delivery pipeline 25 is connected to the air inlet 14 of the chamber 101, wherein the air delivery pipe 25 is used to fill the chamber 101 with air so that the chamber 101 is in a normal pressure state. That is, a certain amount of air is filled into the chamber 101 through the air delivery pipe 25 to return the chamber 101 to a normal pressure state, so that the staff can open the chamber 101 and take out the substrate 600, So far, the coating process is over. In the entire coating process, the coating equipment 100 has better process controllability in the process of preparing the DLC film, which is beneficial to the rapid preparation of the target DLC film.
可以看出的是,在整个镀膜过程中,所述腔室101内能够始终处于常温或者低温状态,即所述镀膜设备100能够在常温或者低温下完成镀膜,所需时间较短,有利于节省成本。也就是说,所述镀膜设备100能够用于对一些不耐高温的基材进行镀膜,实现在镀膜过程中不易损坏基材。相较于磁控溅射等物理气相沉积的方式实现镀膜的方法,本发明的所述镀膜设备100在整个镀膜过程中能够始终保持所述基材600处于温度相对较低的状态,而不会过度升高所述基材600的温度。It can be seen that during the entire coating process, the chamber 101 can always be at room temperature or low temperature, that is, the coating equipment 100 can complete the coating at room temperature or low temperature, and the time required is relatively short, which is conducive to saving cost. In other words, the coating equipment 100 can be used to coat some substrates that are not resistant to high temperatures, so that the substrates are not easily damaged during the coating process. Compared with the method of realizing film coating by physical vapor deposition such as magnetron sputtering, the coating equipment 100 of the present invention can always keep the substrate 600 in a relatively low temperature state during the entire coating process. The temperature of the substrate 600 is excessively increased.
优选地,所述镀膜设备100进一步包括一尾气处理装置70,其中所述尾气处理装置70被连通于所述抽气管路40,其中所述尾气处理装置70用于处理经所述抽气装置30抽出的气体并进行排放,其中所述尾气处理装置70包括但不限于对氮气、惰性气体、氢气、碳氢气体等反应原料或者掺杂元素的辅助气体等进行回收处理或者无污染处理等,然后排放至外界,以防止对环境造成污染,并且能够实现回收利用。Preferably, the coating equipment 100 further includes an exhaust gas treatment device 70, wherein the exhaust gas treatment device 70 is connected to the exhaust pipe 40, and the exhaust gas treatment device 70 is used to process the exhaust gas The exhaust gas is extracted and discharged. The exhaust gas treatment device 70 includes, but is not limited to, recycling or non-polluting treatment of reaction raw materials such as nitrogen, inert gas, hydrogen, hydrocarbon gas, or auxiliary gas doped with elements, etc., and then It is discharged to the outside world to prevent pollution to the environment and can be recycled.
如图3所示,进一步地,所述第一真空泵31被实施为一分子泵,其中所述第二真空泵32包括一罗茨泵321和一干泵322,其中所述腔室101的所述抽气口11、所述第一真空泵31、所述罗茨泵321、所述干泵322以及所述尾气处理装置70之间均由所述抽气管路40连通。具体地,所述腔室101内的气体依次经所述干泵322、所述罗茨泵321以及所述分子泵抽出,即所述第二真空泵32作为前级泵先对所述腔室101进行抽气,其中所述第一真空泵31作为二级泵对所述腔室101进行进一步地抽真空,并其中所述腔室101内被抽出的气体经所述尾气处理装置70处理或者回收后排放至外界。As shown in FIG. 3, further, the first vacuum pump 31 is implemented as a molecular pump, wherein the second vacuum pump 32 includes a roots pump 321 and a dry pump 322, wherein the pumping of the chamber 101 The air port 11, the first vacuum pump 31, the roots pump 321, the dry pump 322, and the exhaust gas treatment device 70 are all connected by the air extraction pipeline 40. Specifically, the gas in the chamber 101 is sequentially pumped out by the dry pump 322, the Roots pump 321, and the molecular pump, that is, the second vacuum pump 32 acts as a fore-stage pump to the chamber 101 first. Evacuate, wherein the first vacuum pump 31 serves as a secondary pump to further evacuate the chamber 101, and the gas extracted from the chamber 101 is processed or recovered by the exhaust gas processing device 70 Discharge to the outside world.
需要指出的是,所述第二真空泵32包括至少一个机械泵,并作为对所述腔室101抽气的前级泵,其中所述分子泵作为二级泵组地对所述腔室进行进一步地抽真空,以使所述腔室101内的气压能够尽量地维持在较低的范围内。It should be pointed out that the second vacuum pump 32 includes at least one mechanical pump and serves as a backing pump for pumping air to the chamber 101, wherein the molecular pump serves as a two-stage pump set to further the chamber. The ground is evacuated so that the air pressure in the chamber 101 can be maintained as low as possible.
在本实施例中,所述腔室101与所述罗茨泵321之间的管道的型号参数为DN100,接口IOS100。所述罗茨泵321与所述干泵322之间的管道的型号参数 为DN63,接口不限。所述尾气处理装置70的管道的型号参数为NB32,接口不限。熟知本领域的人员应当理解的是,所述腔室101与所述罗茨泵321之间的管道、所述罗茨泵321与所述干泵322之间的管道以及所述尾气处理装置70的管道的型号规格能够根据实际镀膜需求被预设,在此不做限制。In this embodiment, the model parameter of the pipeline between the chamber 101 and the roots pump 321 is DN100, and the interface is IOS100. The model parameter of the pipe between the Roots pump 321 and the dry pump 322 is DN63, and the interface is not limited. The model parameter of the pipeline of the exhaust gas treatment device 70 is NB32, and the interface is not limited. Those skilled in the art should understand that the pipeline between the chamber 101 and the roots pump 321, the pipeline between the roots pump 321 and the dry pump 322, and the exhaust gas treatment device 70 The type and specifications of the pipeline can be preset according to the actual coating requirements, and there is no restriction here.
如图9所示,进一步地,所述供电装置50包括一射频电源51和一脉冲电源52,其中所述射频电源51通过直接加载在电极板上在所述腔体10的所述腔室101内产生射频电场,以作用于所述腔室101内的气体,其中所述脉冲电源52用于提供高压脉冲偏压作用于所述腔室101内的气体。具体地,在镀膜时,所述射频电源51通过提供射频电场对所述腔室101内的气体如氮气或者惰性气体和所述反应原料气体等气体进行放电以使所述腔室101内处于等离子体环境和所述反应气体原料处于高能量状态。所述脉冲电源52通过提供高压脉冲偏压中的强电压在所述腔室101内产生强电场,以使处于高能量状态的活性粒子(即正离子)受到强电场作用定向地加速沉积于所述基材600的表面,并形成非晶态碳网络结构,和所述脉冲电源52通过提供高压脉冲偏压中的空电压或者低电压的状态,以使被沉积于所述基材600表面的非晶态碳网络结构进行自由驰豫,并在热力学作用下碳结构向稳定相--弯曲石墨烯片层结构转变,并埋置于非晶态碳网络中,从而在所述基材600表面形成所述DLC薄膜。As shown in FIG. 9, further, the power supply device 50 includes a radio frequency power supply 51 and a pulse power supply 52, wherein the radio frequency power supply 51 is directly loaded on the electrode plate in the chamber 101 of the cavity 10 A radio frequency electric field is generated inside to act on the gas in the chamber 101, wherein the pulse power source 52 is used to provide a high-voltage pulse bias to act on the gas in the chamber 101. Specifically, during film coating, the radio frequency power supply 51 discharges the gas in the chamber 101, such as nitrogen or inert gas, and the reaction raw material gas, by providing a radio frequency electric field, so that the chamber 101 is in plasma. The body environment and the reaction gas raw materials are in a high-energy state. The pulse power supply 52 generates a strong electric field in the chamber 101 by providing a strong voltage in a high-voltage pulse bias, so that the active particles (that is, positive ions) in a high-energy state are subjected to the strong electric field to directionally accelerate the deposition on the chamber 101. On the surface of the substrate 600, an amorphous carbon network structure is formed, and the pulse power source 52 provides a null voltage or a low voltage state in the high-voltage pulse bias to make the deposited on the surface of the substrate 600 The amorphous carbon network structure relaxes freely, and under the action of thermodynamics, the carbon structure transforms into a stable phase-the curved graphene sheet structure, and is embedded in the amorphous carbon network, so as to be on the surface of the substrate 600 The DLC film is formed.
所述射频电源51也可以作为等离子体配套电源,其中所述射频电源51由射频功率源、阻抗匹配器以及阻抗功率计组成,其中所述射频电源51被安装于所述腔体10,以提供射频电场作用于所述腔室101内的气体。所述射频电源51优选地提供射频功率为13.56MHz。The radio frequency power supply 51 can also be used as a plasma supporting power supply, wherein the radio frequency power supply 51 is composed of a radio frequency power source, an impedance matcher and an impedance power meter, and the radio frequency power supply 51 is installed in the cavity 10 to provide The radio frequency electric field acts on the gas in the chamber 101. The radio frequency power supply 51 preferably provides radio frequency power of 13.56 MHz.
进一步地,所述射频电源51通过直接加载在被设置于所述腔体10的一电极板上的射频电压,在所述腔体10的所述腔室101内形成所述射频电场,以作用于所述腔室101内的气体,从而满足镀膜需求。可选地,所述射频电源51还可以被实施为通过线圈的电感耦合作用,即作为ICP在所述腔室101内产生交变磁场,以通过快速变化的磁场确保了所述腔室101内的气体充分和均匀地电离,也能够满足所述镀膜设备100的镀膜需求,在此不受限制。Further, the radio frequency power supply 51 forms the radio frequency electric field in the cavity 101 of the cavity 10 by directly loading the radio frequency voltage on an electrode plate of the cavity 10 to act The gas in the chamber 101 satisfies the coating demand. Optionally, the radio frequency power supply 51 can also be implemented as an inductive coupling effect of a coil, that is, as an ICP to generate an alternating magnetic field in the chamber 101, so as to ensure that the chamber 101 is The gas is fully and uniformly ionized, which can also meet the coating requirements of the coating equipment 100, which is not limited here.
优选地,所述脉冲电源52被实施为单向负脉冲电源,其中所述脉冲电源52具有一负极端521和一正极端522,其中所述负极端521被电连接于所述电极支架60并提供负压,其中所述正极端522被电连接于所述腔体10并接地处于正极 或者零电位,其中所述电极支架60和所述腔体10均由导电材料如金属材料制成,其中所述电极支架60与所述腔体10之间绝缘。也就是说,在镀膜过程中,整个所述电极支架60均为负极且具有负压,整个所述腔体10接地为正极,且所述电极支架60与所述腔体10之间绝缘,以使整个所述腔室101处于强电场,由于所述基材600被放置于所述电极支架60,因此,在所述强电场的作用下,处于高能量状态的活性粒子会加速沉积于所述基材600的表面,从而实现镀膜。Preferably, the pulse power supply 52 is implemented as a unidirectional negative pulse power supply, wherein the pulse power supply 52 has a negative terminal 521 and a positive terminal 522, wherein the negative terminal 521 is electrically connected to the electrode holder 60 and Provide negative pressure, wherein the positive terminal 522 is electrically connected to the cavity 10 and grounded at a positive or zero potential, wherein the electrode holder 60 and the cavity 10 are both made of conductive materials such as metal materials, wherein The electrode holder 60 is insulated from the cavity 10. That is to say, during the coating process, the entire electrode holder 60 is a negative electrode and has a negative pressure, the entire cavity 10 is grounded as a positive electrode, and the electrode holder 60 is insulated from the cavity 10 to The entire chamber 101 is placed in a strong electric field. Since the substrate 600 is placed on the electrode holder 60, under the action of the strong electric field, the active particles in a high-energy state will accelerate the deposition on the The surface of the substrate 600 is thus coated.
需要说明的是,所述脉冲电源52通过辉光放电效应使所述腔室101内的气体电离,同时对所述腔室101内的正离子具有定向牵引加速的作用,使得所述正离子具有轰击效果地加速沉积于所述基材600的表面,从而在所述基材600表面制备致密的高硬度的所述DLC薄膜。It should be noted that the pulse power source 52 ionizes the gas in the chamber 101 through the glow discharge effect, and at the same time has a directional pulling and accelerating effect on the positive ions in the chamber 101, so that the positive ions have The bombardment effect accelerates the deposition on the surface of the substrate 600, thereby preparing the dense and high-hardness DLC film on the surface of the substrate 600.
可以看出的是,由于整个所述电极支架60均为负极端,所述电极支架60能够提供尽量大的空间可用于安装布置大量的所述基材600,且一次镀膜过程能够对所述电极支架60上的所有的所述基材600完成镀膜,从而实现大面积镀膜,从而实现大批量制备DLC薄膜。It can be seen that, since the entire electrode holder 60 is a negative terminal, the electrode holder 60 can provide as much space as possible for installing and arranging a large number of the substrate 600, and a coating process can cover the electrode. All the substrates 600 on the support 60 are coated, so as to realize large-area coating, thereby realizing mass production of DLC thin films.
值得一提的是,在所述步骤S03中,所述射频电源51和所述脉冲电源52共同提供电压作用于所述腔室101内的气体,其中所述射频电源51提供的低功率射频放电维持所述腔室101内的等离子体环境,并抑制高压放电过程中的弧光放电现象(由于弧光放电是在辉光放电进一步加强的放电形式,瞬间电流可以达到几十甚至几百安培以上,这些高电流通过基材表面将会损坏基材,因此为了确保所述基材600的安全性,因此在镀膜过程中需要抑制弧光放电现象)。同时,所述脉冲电源52增加了正离子到达所述基材600表面时的能量,以制备出致密透明的所述DLC薄膜。It is worth mentioning that in the step S03, the radio frequency power supply 51 and the pulse power supply 52 jointly provide a voltage to act on the gas in the chamber 101, wherein the low power radio frequency discharge provided by the radio frequency power supply 51 Maintain the plasma environment in the chamber 101 and suppress the arc discharge phenomenon during the high-voltage discharge process (because arc discharge is a form of discharge that is further enhanced by glow discharge, the instantaneous current can reach more than tens or even hundreds of amperes. High current passing through the surface of the substrate will damage the substrate. Therefore, in order to ensure the safety of the substrate 600, it is necessary to suppress the arc discharge phenomenon during the coating process). At the same time, the pulse power source 52 increases the energy of the positive ions when they reach the surface of the substrate 600 to prepare the dense and transparent DLC film.
需要指出的是,本优选实施例中的所述供电装置50由所述射频电源51和所述脉冲电源52共同组成,以满足镀膜需求。在可选的情况下,根据不同的镀膜需求,所述供电装置50也可以仅被实施为所述射频电源51或者所述脉冲电源52中的其中一种,也能够满足镀膜需求。熟知本领域的人员应当理解的是,所述供电装置50也可以被实施为微波电源等其他电源以满足镀膜需求,在此不受限制。It should be pointed out that the power supply device 50 in the preferred embodiment is composed of the radio frequency power supply 51 and the pulse power supply 52 to meet the coating requirements. In an optional case, according to different coating requirements, the power supply device 50 can also be implemented as only one of the radio frequency power supply 51 or the pulse power supply 52, which can also meet the coating requirements. Those skilled in the art should understand that the power supply device 50 can also be implemented as a microwave power supply and other power supplies to meet the coating requirements, which is not limited here.
值得一提的是,根据对不同基材的镀膜需求,所述射频电源51的射频电压功率和供电时间能够被调整预设,其中所述射频电源51的射频电压的功率优选 为10-800W,相应地,所述脉冲电源52提供的脉冲偏压、脉冲频率、占空比以及供电时间均能够被调整预设,其中所述脉冲电源52提供脉冲偏压的电压为-100V至-5000V,脉冲频率为20-300KHz,占空比为10%-80%,在此不受限制。It is worth mentioning that the RF voltage power and power supply time of the RF power supply 51 can be adjusted and preset according to the coating requirements for different substrates, wherein the RF voltage power of the RF power supply 51 is preferably 10-800W, Correspondingly, the pulse bias voltage, pulse frequency, duty cycle, and power supply time provided by the pulse power supply 52 can be adjusted and preset, wherein the pulse power supply 52 provides a pulse bias voltage of -100V to -5000V, and the pulse The frequency is 20-300KHz, and the duty cycle is 10%-80%, which is not limited here.
由于所述脉冲电源52提供的负压偏值的大小直接关系到所述腔室101内的气体的离化率和正离子到达所述基材600表面的迁移能力,因此所述脉冲电源52的负压电压越高,使得所述正离子的能量越高,从而使制备的所述DLC的硬度就越高。但是需要注意的是,能量越高的所述正离子对所述基材600表面的轰击能量就越高,在微观尺度上,在所述基材600的表面上会产生轰击坑,同时会加速所述基材600表面的温度升高,因此所述脉冲电源52的负压电压不宜过高,以防止所述基材600表面的温度过度升高而损坏所述基材600。另外,所述脉冲电源52的脉冲频率越高,可以避免所述基材600的绝缘部分的表面的电荷持续累积,从而实现抑制大电弧现象和增加所述DLC薄膜的沉积厚度极限。Since the magnitude of the negative voltage bias provided by the pulse power supply 52 is directly related to the ionization rate of the gas in the chamber 101 and the migration ability of positive ions to the surface of the substrate 600, the negative voltage of the pulse power supply 52 The higher the voltage, the higher the energy of the positive ions, and the higher the hardness of the prepared DLC. However, it should be noted that the higher the energy, the higher the bombardment energy of the positive ions on the surface of the substrate 600. On a microscopic scale, bombardment pits will be generated on the surface of the substrate 600 and will accelerate at the same time. The temperature of the surface of the substrate 600 increases, so the negative voltage of the pulse power source 52 should not be too high to prevent the surface temperature of the substrate 600 from excessively increasing and damaging the substrate 600. In addition, the higher the pulse frequency of the pulse power source 52 is, the continuous accumulation of electric charges on the surface of the insulating part of the substrate 600 can be avoided, thereby achieving suppression of the large arc phenomenon and increasing the deposition thickness limit of the DLC film.
进一步地,所述镀膜设备100包括一温度检测器80,其中所述温度检测器80用于检测在镀膜过程中所述腔室101内的反应温度并进行反馈,如以画面展示的方式提示工作人员或者语音警报等,进一步确保所述基材的温度不易过高。具体地,所述温度检测器80具有一热电偶81,其中所述热电偶81被与所述基材600等效位置地设置于所述电极支架60,其中所述热电偶81能够检测所述腔室101内的反应温度,从而根据所述热电偶81检测到的所述反应温度,所述温度检测器80判断是否超过所述基材600的温度阈值,若超过,则所述温度检测器80反馈温度过高的异常信号,以提醒工作人员及时处理或者暂停所述镀膜设备100等,若不超过,则所述基材600表面的反应温度正常,即所述基材600安全。Further, the coating equipment 100 includes a temperature detector 80, wherein the temperature detector 80 is used to detect the reaction temperature in the chamber 101 during the coating process and provide feedback, such as prompting work in the form of a screen display Personnel or voice alarms, etc., further ensure that the temperature of the substrate is not easily too high. Specifically, the temperature detector 80 has a thermocouple 81, wherein the thermocouple 81 is disposed on the electrode holder 60 at an equivalent position to the substrate 600, and the thermocouple 81 can detect the The reaction temperature in the chamber 101, based on the reaction temperature detected by the thermocouple 81, the temperature detector 80 determines whether the temperature threshold of the substrate 600 is exceeded, and if it exceeds, the temperature detector 80 80 feeds back an abnormal signal that the temperature is too high to remind the staff to handle or suspend the coating equipment 100 in time. If it does not exceed, the reaction temperature on the surface of the substrate 600 is normal, that is, the substrate 600 is safe.
如图10所示,优选地,所述电极支架60被实施为多层金属板的结构,其中每层均能够放置一定量的所述基材600,其中所述电极支架60具有至少一绝缘件61,其中所述绝缘件61被设置于所述电极支架60与所述腔室101的壁之间,以使所述电极支架60与所述腔体10之间绝缘。优选地,所述绝缘件61被实施为由聚四氟乙烯等绝缘材料制成。As shown in FIG. 10, the electrode holder 60 is preferably implemented as a multi-layer metal plate structure, wherein each layer can place a certain amount of the substrate 600, wherein the electrode holder 60 has at least one insulating member 61, wherein the insulating member 61 is disposed between the electrode holder 60 and the wall of the chamber 101 to insulate the electrode holder 60 from the cavity 10. Preferably, the insulating member 61 is implemented to be made of insulating materials such as polytetrafluoroethylene.
在本优选实施例的另一种实施方式中,所述腔体10并未连接于所述脉冲电源52,其中所述电极支架60被实施为包括多层金属板,且相邻层之间相互绝缘,其中所述脉冲电源52的所述正极端522和所述负极端521分别相间地电连接于 所述电极支架60的各层金属板,使得所述电极支架60的相邻的金属板互为正负极。进一步地,所述脉冲电源52能够被实施为正负双向脉冲电源,使得所述电极支架60的各金属板分别交替式地形成正极或者负极,且相邻的金属板始终互为正负极,以使每一层的所述金属板上均能够被放置所述基材600,且使得所有的所述金属板上的所述基材600的表面均能够被镀上所述DLC薄膜,且所述DLC薄膜的质量更加优秀。In another implementation of this preferred embodiment, the cavity 10 is not connected to the pulse power source 52, and the electrode holder 60 is implemented as including multiple metal plates, and adjacent layers are mutually connected to each other. Insulation, wherein the positive terminal 522 and the negative terminal 521 of the pulse power source 52 are electrically connected to the metal plates of the electrode holder 60 alternately, so that the adjacent metal plates of the electrode holder 60 are mutually connected. For the positive and negative poles. Further, the pulse power source 52 can be implemented as a positive and negative bidirectional pulse power source, so that each metal plate of the electrode holder 60 alternately forms a positive electrode or a negative electrode, and adjacent metal plates are always positive and negative to each other. So that the substrate 600 can be placed on the metal plate of each layer, and the surface of the substrate 600 on all the metal plates can be plated with the DLC film, and The quality of the DLC film is even better.
可选地,所述脉冲电源52也能够被实施为对称式双向脉冲电源,即所述脉冲电源52提供的正压与负压的值的大小相同。或者所述脉冲电源52被实施为非对称式双向脉冲电源,其中所述脉冲电源52提供的负压值的大小大于正压值的大小,以提供所述DLC薄膜的质量,在此不受限制。Optionally, the pulse power supply 52 can also be implemented as a symmetrical bidirectional pulse power supply, that is, the positive pressure and the negative pressure provided by the pulse power supply 52 have the same magnitude. Or the pulse power source 52 is implemented as an asymmetric bidirectional pulse power source, wherein the magnitude of the negative voltage value provided by the pulse power source 52 is greater than the magnitude of the positive voltage value to provide the quality of the DLC film, which is not limited here .
需要指出的是,所述电极支架60的形状结构不做限制,在所述腔室101的容积大小内,所述电极支架60的形状大小或者数量能够做适应性的调整。优选地,所述腔体10的材料选用不锈钢。进一步地,所述腔体10具有一可开合的密封门15,以供工作人员打开或者密封关闭所述腔室101,以放置或者取出所述基材600与所述腔室101。It should be pointed out that the shape and structure of the electrode holder 60 are not limited. Within the volume of the chamber 101, the shape or number of the electrode holder 60 can be adjusted adaptively. Preferably, the material of the cavity 10 is stainless steel. Further, the cavity 10 has an openable and closable sealed door 15 for a worker to open or seal the cavity 101 to place or take out the substrate 600 and the cavity 101.
进一步地,所述电极支架60被可拆卸地支撑于所述腔室101,以使所述电极支架60能够被取出于所述腔室101,以便于工作人员在外界预先安装所述基材600于所述电极支架60,然后将所述电极支架60放置于所述腔室101内,同时在一次镀膜工艺结束后,工作人员能够通过将所述电极支架60取出,以取出全部的所述基材600,以尽量降低对所述基材600的损伤,保证所述基材600的安全,同时便于清洁所述腔室101和所述电极支架60。此外,所述电极支架60能够被重复利用,即在第二次镀膜时,所述电极支架60能够被用于再次安装另一批量的所述基材600,然后被置于所述腔室101内实现再次镀膜,有利于大批量生产。Further, the electrode holder 60 is detachably supported in the chamber 101, so that the electrode holder 60 can be taken out of the chamber 101, so that workers can pre-install the substrate 600 outside. On the electrode holder 60, and then place the electrode holder 60 in the chamber 101. At the same time, after one coating process is completed, the staff can take out the electrode holder 60 to take out all the substrates. The material 600 is used to minimize damage to the substrate 600, to ensure the safety of the substrate 600, and to facilitate cleaning of the chamber 101 and the electrode holder 60. In addition, the electrode holder 60 can be reused, that is, during the second coating, the electrode holder 60 can be used to install another batch of the substrate 600 again, and then be placed in the chamber 101 Re-coating is realized inside, which is conducive to mass production.
举例地,所述镀膜设备100在镀膜过程中的各参数如下:进气量:Ar/N 2/H 2/CH 4:50-500sccm,C 2H 2/O 2:10-200sccm;镀膜前(即所述步骤S02阶段)所述腔室101的真空度:小于2×10 -3Pa;镀膜时(即所述步骤S03阶段)所述腔室101的真空度:0.1~20Pa;镀膜电压:-300~-3500V,占空比:5~100%,频率:20~360KHz;镀膜时间:0.1~5hrs,所述DLC薄膜的厚度小于50纳米,在此仅作举例,并不对本发明作为限制。 For example, the parameters of the coating equipment 100 during the coating process are as follows: Air intake: Ar/N 2 /H 2 /CH 4 : 50-500 sccm, C 2 H 2 /O 2 : 10-200 sccm; before coating (I.e. the step S02 stage) the vacuum degree of the chamber 101: less than 2×10 -3 Pa; during coating (i.e. the step S03 stage) the vacuum degree of the chamber 101: 0.1-20 Pa; coating voltage : -300~-3500V, duty cycle: 5~100%, frequency: 20~360KHz; coating time: 0.1~5hrs, the thickness of the DLC film is less than 50 nanometers, this is only an example, not the present invention limit.
进一步地,所述镀膜设备100还包括一壳体90,其中所述腔体10、所述输送管路20、所述抽气装置30、所述抽气管路40、所述供电装置50、所述尾气处理装置70以及所述温度检测装置80均能够被安装于所述壳体90。进一步地,所述壳体90具有一控制面板,其中所述控制面板用于工作人员控制所述抽气装置30和所述供电装置50的开关或者工作状态,以及显示所述镀膜设备100的镀膜工艺的进程和相关参数等。Further, the coating equipment 100 further includes a housing 90, in which the cavity 10, the delivery pipeline 20, the air extraction device 30, the air extraction pipeline 40, the power supply device 50, and the Both the exhaust gas treatment device 70 and the temperature detection device 80 can be installed in the housing 90. Further, the housing 90 has a control panel, wherein the control panel is used by the staff to control the on/off or working status of the air extraction device 30 and the power supply device 50, and display the coating of the coating equipment 100 Process progress and related parameters, etc.
进一步地,本实施例还提供了所述DLC薄膜,其中所述DLC薄膜由所述镀膜设备100制备,并形成于所述基材600的表面。可以理解的是,所述DLC薄膜可以由所述镀膜设备100经一次或者多次镀膜在所述基材600表面形成的一层或者多层DLC薄膜。Furthermore, this embodiment also provides the DLC film, wherein the DLC film is prepared by the coating equipment 100 and formed on the surface of the substrate 600. It is understandable that the DLC film may be one or more layers of DLC film formed on the surface of the substrate 600 by the coating equipment 100 through one or more coatings.
本领域的技术人员应理解,上述描述及附图中所示的本发明的实施例只作为举例而并不限制本发明。本发明的目的已经完整并有效地实现。本发明的功能及结构原理已在实施例中展示和说明,在没有背离所述原理下,本发明的实施方式可以有任何变形或修改。Those skilled in the art should understand that the above description and the embodiments of the present invention shown in the accompanying drawings are only examples and do not limit the present invention. The purpose of the present invention has been completely and effectively achieved. The functions and structural principles of the present invention have been shown and explained in the embodiments. Without departing from the principles, the implementation of the present invention may have any deformation or modification.

Claims (30)

  1. 一镀膜设备,用于在基材表面制备DLC薄膜,其特征在于,其中所述镀膜设备包括:A coating equipment for preparing a DLC film on the surface of a substrate, wherein the coating equipment includes:
    一腔体,其中所述腔体具有一腔室;A cavity, wherein the cavity has a cavity;
    一组输送管路;A set of conveying pipelines;
    至少一抽气装置;At least one air extraction device;
    至少一抽气管路;At least one suction line;
    一供电装置;以及A power supply device; and
    至少一电极支架,其中所述电极支架被设置于所述腔室以供支撑该基材,其中所述输送管路被连通于所述腔室并用于向所述腔室内通入气体原料,其中所述抽气装置通过所述抽气管路连通于所述腔室并对所述腔室进行负压操作和控制所述腔室内的气压,其中所述供电装置电连接于所述电极支架,以供所述镀膜设备通过化学气相沉积的方式在该基材的表面制备该DLC薄膜。At least one electrode holder, wherein the electrode holder is arranged in the chamber for supporting the substrate, and the delivery pipeline is connected to the chamber and is used to pass gaseous materials into the chamber, wherein The air extraction device is connected to the chamber through the air extraction pipeline and performs a negative pressure operation on the chamber and controls the air pressure in the chamber, wherein the power supply device is electrically connected to the electrode holder to The coating equipment is provided for preparing the DLC film on the surface of the substrate by means of chemical vapor deposition.
  2. 根据权利要求1所述镀膜设备,其中所述腔体具有与所述腔室相通的至少一抽气口.至少一进气口以及至少一进料口,其中所述输送管路包括至少一气源管道.以及至少一反应原料管道,其中所述抽气口被连通于所述抽气管路,其中所述气源管道被连通于所述进气口以用于向所述腔室内通入气体,其中所述反应原料管道被连通于所述进料口以用于向所述腔室内充入反应原料。The coating equipment according to claim 1, wherein the cavity has at least one suction port communicating with the chamber, at least one gas inlet and at least one feed port, wherein the delivery pipeline includes at least one gas source Pipe. And at least one reaction raw material pipeline, wherein the gas extraction port is connected to the gas extraction pipeline, wherein the gas source pipeline is connected to the gas inlet for injecting gas into the chamber, wherein The reaction raw material pipeline is connected to the feed port for charging the reaction raw material into the chamber.
  3. 根据权利要求2所述镀膜设备,其中还包括一氢气管道,其中所述氢气管道和所述反应原料管道被连通于同一所述进料口。4. The coating equipment according to claim 2, further comprising a hydrogen pipeline, wherein the hydrogen pipeline and the reaction raw material pipeline are connected to the same feed port.
  4. 根据权利要求2所述的镀膜设备,其中还包括一氢气管道,其中所述氢气管道和所述反应原料管道被分别连通于两个所述进料口。3. The coating equipment according to claim 2, further comprising a hydrogen pipeline, wherein the hydrogen pipeline and the reaction raw material pipeline are respectively connected to the two feed ports.
  5. [根据细则91更正 09.04.2020] 
    根据权利要求2所述镀膜设备,所述输送管路进一步包括一掺杂原料管道,其中所述掺杂原料管道被连通于所述进料口以用于向所述腔室内充入掺杂元素反应原料。
    [Corrected according to Rule 91 09.04.2020]
    The coating equipment according to claim 2, wherein the delivery pipeline further comprises a doping material pipeline, wherein the doping material pipeline is connected to the feed port for filling the chamber with doping elements Reaction raw materials.
  6. 根据权利要求2所述镀膜设备,其中所述抽气口位于所述腔室的中部,其中所述进气口和所述进料口均位于所述腔室的侧壁。4. The coating equipment according to claim 2, wherein the suction port is located in the middle of the chamber, and the gas inlet and the feed port are both located on the side wall of the chamber.
  7. 根据权利要求1所述镀膜设备,其中所述抽气装置包括至少一第一真空泵和至少一第二真空泵,其中所述第二真空泵作为所述第一真空泵的前级泵共同协作地通过所述抽气管路对所述腔室进行负压操作并维持所述腔室内的气压处于预设范围内。4. The coating equipment according to claim 1, wherein the pumping device includes at least one first vacuum pump and at least one second vacuum pump, wherein the second vacuum pump serves as a backing pump of the first vacuum pump and passes through the The air extraction pipeline performs a negative pressure operation on the chamber and maintains the air pressure in the chamber within a preset range.
  8. 根据权利要求7所述镀膜设备,其中所述腔室内的气压降至0.01Pa以下。8. The coating equipment according to claim 7, wherein the air pressure in the chamber is reduced to less than 0.01 Pa.
  9. 根据权利要求7所述镀膜设备,其中所述腔室内的气压被维持在0.01至100Pa之 间。The coating equipment according to claim 7, wherein the air pressure in the chamber is maintained between 0.01 and 100 Pa.
  10. 根据权利要求7所述镀膜设备,其中所述第一真空泵被实施为分子泵,其中所述第二真空泵被实施为包括罗茨泵和干泵。8. The coating apparatus according to claim 7, wherein the first vacuum pump is implemented as a molecular pump, and wherein the second vacuum pump is implemented as including a roots pump and a dry pump.
  11. 根据权利要求7所述镀膜设备,其中所述镀膜设备进一步包括一尾气处理装置,其中所述尾气处理装置被连通于所述抽气管路,以用于处理经所述抽气装置抽出的气体并进行排放。7. The coating equipment according to claim 7, wherein the coating equipment further comprises an exhaust gas processing device, wherein the exhaust gas processing device is connected to the gas extraction pipeline for processing the gas extracted by the gas extraction device and Discharge.
  12. [根据细则91更正 09.04.2020] 
    根据权利要求1所述镀膜设备,其中所述供电装置包括一射频电源和一脉冲电源,以分别提供射频电压和脉冲电压。
    [Corrected according to Rule 91 09.04.2020]
    The coating equipment according to claim 1, wherein the power supply device includes a radio frequency power supply and a pulse power supply to provide radio frequency voltage and pulse voltage respectively.
  13. [根据细则91更正 09.04.2020] 
    根据权利要求1所述镀膜设备,其中所述供电装置包括一脉冲电源,其中所述脉冲电源具有一正极端和一负极端,其中所述负极端被电连接于所述电极支架并提供负压,其中所述腔体接地,并且所述电极支架与所述腔体之间绝缘。
    [Corrected according to Rule 91 09.04.2020]
    The coating equipment according to claim 1, wherein the power supply device comprises a pulse power supply, wherein the pulse power supply has a positive terminal and a negative terminal, wherein the negative terminal is electrically connected to the electrode holder and provides a negative voltage , Wherein the cavity is grounded, and the electrode holder is insulated from the cavity.
  14. 根据权利要求1所述镀膜设备,其中所述供电装置包括一脉冲电源,其中所述脉冲电源具有一正极端和一负极端,其中所述电极支架包括多层金属板,其中所述脉冲电源的所述正极端和所述负极端分别电连接于所述电极支架的各层金属板,并使所述电极支架的相邻的两个金属板互为正负极。The coating equipment according to claim 1, wherein the power supply device includes a pulse power supply, wherein the pulse power supply has a positive terminal and a negative terminal, wherein the electrode holder includes a multilayer metal plate, wherein the pulse power supply The positive terminal and the negative terminal are respectively electrically connected to the metal plates of each layer of the electrode support, and two adjacent metal plates of the electrode support are mutually positive and negative.
  15. 根据权利要求12所述镀膜设备,其中所述射频电源的射频电压的功率为10-800W。The coating equipment according to claim 12, wherein the power of the radio frequency voltage of the radio frequency power supply is 10-800W.
  16. 根据权利要求12至14中任一所述镀膜设备,其中所述脉冲电源提供脉冲偏压的电压为-100V至-5000V,脉冲频率为20-300KHz,占空比为10%-80%。The coating equipment according to any one of claims 12 to 14, wherein the pulse power supply provides a pulse bias voltage of -100V to -5000V, a pulse frequency of 20-300KHz, and a duty ratio of 10%-80%.
  17. 根据权利要求12所述镀膜设备,其中所述脉冲电源选自单向脉冲电源.对称式双向脉冲电源或者非对称式脉冲电源中的一种。The coating equipment according to claim 12, wherein the pulse power supply is selected from one of a unidirectional pulse power supply, a symmetrical bidirectional pulse power supply, or an asymmetric pulse power supply.
  18. 根据权利要求1至15中任一所述镀膜设备,其中所述镀膜设备进一步包括一壳体,其中所述腔体、所述输送管路、所述抽气装置、所述抽气管路以及供电装置均被安装于所述壳体。The coating equipment according to any one of claims 1 to 15, wherein the coating equipment further comprises a housing, wherein the cavity, the conveying pipeline, the air extraction device, the air extraction pipeline, and the power supply The devices are all installed in the housing.
  19. 一DLC薄膜的镀膜方法,其特征在于,其通过一镀膜设备在基材表面基于碳氢气体为反应原料制备所述DLC薄膜,包括步骤:A method for coating a DLC thin film is characterized in that it uses a coating device to prepare the DLC thin film on the surface of a substrate based on hydrocarbon gas as a reaction raw material, including the steps:
    (a)将该基材置于所述镀膜设置的一腔体的一腔室内的一电极支架;(a) The substrate is placed in an electrode holder in a cavity of a cavity provided with the coating;
    (b)对所述腔室进行负压产生操作;以及(b) Perform a negative pressure generating operation on the chamber; and
    (c)以化学气相沉积的方式在该基材的表面制备DLC薄膜。(c) Prepare a DLC film on the surface of the substrate by chemical vapor deposition.
  20. 根据权利要求19所述镀膜方法,其中所述步骤(c)进一步包括步骤:(c.1)通 过一气源管道通入气体于所述腔室,并提供电压作用于所述腔室内的所述气体,以对该基材表面进行刻蚀处理;以及(c.2)通过至少一反应原料管道通入一反应原料气体于所述腔室,并提供电压作用于所述腔室内的气体,以在该基材的表面制备所述DLC薄膜。The coating method according to claim 19, wherein the step (c) further comprises the step of: (c.1) introducing gas into the chamber through a gas source pipe, and providing a voltage to act on all the chambers in the chamber. The gas is used to perform an etching treatment on the surface of the substrate; and (c.2) a reaction raw material gas is introduced into the chamber through at least one reaction raw material pipe, and a voltage is applied to the gas in the chamber, The DLC film is prepared on the surface of the substrate.
  21. 根据权利要求20所述镀膜方法,其中所述步骤(c)中,通入所述腔室内的所述气体的气体流量为10sccm~1000sccm。22. The coating method according to claim 20, wherein in the step (c), the gas flow rate of the gas passing into the chamber is 10 sccm to 1000 sccm.
  22. 根据权利要求20所述镀膜方法,其中所述步骤(c)中,将所述电极支架连接于一脉冲电源,以提供脉冲电压作用于所述腔室内的气体。22. The coating method according to claim 20, wherein in the step (c), the electrode holder is connected to a pulse power source to provide a pulse voltage to act on the gas in the chamber.
  23. 根据权利要求22所述镀膜方法,其中所述步骤(c)中,其中所述脉冲电源提供脉冲偏压的电压为-100V至-5000V,脉冲频率为20-300KHz,占空比为10%-80%。22. The coating method according to claim 22, wherein in the step (c), wherein the pulse power supply provides a pulse bias voltage of -100V to -5000V, a pulse frequency of 20-300KHz, and a duty ratio of 10%- 80%.
  24. 根据权利要求22所述镀膜方法,其中将所述脉冲电源的一负极端电连接于所述电极支架,所述腔体接地,并且所述电极支架与所述腔体之间绝缘。The coating method according to claim 22, wherein a negative terminal of the pulse power supply is electrically connected to the electrode holder, the cavity is grounded, and the electrode holder is insulated from the cavity.
  25. 根据权利要求22所述镀膜方法,其中将所述脉冲电源的一正极端和一负极端分别电连接于所述电极支架的多层金属板,并使所述电极支架的相邻的两个金属板互为正负极。22. The coating method according to claim 22, wherein a positive terminal and a negative terminal of the pulse power supply are respectively electrically connected to the multilayer metal plate of the electrode holder, and the two adjacent metals of the electrode holder are The plates are positive and negative to each other.
  26. 根据权利要求20所述镀膜方法,其中所述步骤(c)中,将所述电极支架连接于一脉冲电源和一射频电源,以提供射频电压和脉冲电压作用于所述腔室内的气体。22. The coating method according to claim 20, wherein in step (c), the electrode holder is connected to a pulse power supply and a radio frequency power supply to provide radio frequency voltage and pulse voltage to the gas in the chamber.
  27. 根据权利要求24所述镀膜方法,其中所述步骤(c)中,其中一射频电源的射频电压的功率为10-800W,所述脉冲电源提供脉冲偏压的电压为-100V至-5000V,脉冲频率为20-300KHz,占空比为10%-80%。The coating method according to claim 24, wherein in the step (c), the power of the RF voltage of one of the RF power sources is 10-800W, and the pulsed power source provides pulse bias voltages of -100V to -5000V, and pulse The frequency is 20-300KHz, and the duty cycle is 10%-80%.
  28. 根据权利要求20所述镀膜方法,其中以一第二真空泵作为一第一真空泵的前级泵共同协作地方式对所述腔室进行抽真空。22. The coating method of claim 20, wherein a second vacuum pump is used as a backing pump of the first vacuum pump to evacuate the chamber in a cooperative manner.
  29. 根据权利要求28所述镀膜方法,其中维持所述腔室内的气压在0.01至100Pa之间。The coating method according to claim 28, wherein the air pressure in the chamber is maintained between 0.01 and 100 Pa.
  30. 根据权利要求28所述镀膜方法,其中所述第二真空泵被实施为包括干泵和罗茨泵,其中所述第一真空泵被实施为分子泵。The coating method according to claim 28, wherein the second vacuum pump is implemented to include a dry pump and a Roots pump, and wherein the first vacuum pump is implemented as a molecular pump.
PCT/CN2020/082801 2019-12-04 2020-04-01 Coating equipment for preparing dlc and use thereof WO2021109377A1 (en)

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