CN112626484A - Diamond coating system, coating method, terminal and readable storage medium - Google Patents

Diamond coating system, coating method, terminal and readable storage medium Download PDF

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Publication number
CN112626484A
CN112626484A CN202011376251.1A CN202011376251A CN112626484A CN 112626484 A CN112626484 A CN 112626484A CN 202011376251 A CN202011376251 A CN 202011376251A CN 112626484 A CN112626484 A CN 112626484A
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China
Prior art keywords
coating
plating
diamond
film
vacuum
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CN202011376251.1A
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Chinese (zh)
Inventor
孙浩斌
颜练武
张华�
李昌业
司守佶
王焕涛
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Penglai Superhard Compound Material Co ltd
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Penglai Superhard Compound Material Co ltd
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Priority to CN202011376251.1A priority Critical patent/CN112626484A/en
Publication of CN112626484A publication Critical patent/CN112626484A/en
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/56—Apparatus specially adapted for continuous coating; Arrangements for maintaining the vacuum, e.g. vacuum locks
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/02—Pretreatment of the material to be coated
    • C23C14/021—Cleaning or etching treatments
    • C23C14/022—Cleaning or etching treatments by means of bombardment with energetic particles or radiation
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/0635—Carbides
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24—Vacuum evaporation
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/54—Controlling or regulating the coating process
    • C23C14/542—Controlling the film thickness or evaporation rate
    • C23C14/545—Controlling the film thickness or evaporation rate using measurement on deposited material
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
    • C23C28/32—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer
    • C23C28/322—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer only coatings of metal elements only
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
    • C23C28/34—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates
    • C23C28/341—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates with at least one carbide layer
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/48—After-treatment of electroplated surfaces
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/54—Electroplating of non-metallic surfaces

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Electrochemistry (AREA)
  • Physical Vapour Deposition (AREA)

Abstract

The invention discloses a diamond coating system, a coating method, a terminal and a readable storage medium, and relates to the technical field of evaporation equipment, wherein connecting columns are fixed on two sides of the middle part of a bracket of the diamond coating system, and a bottom plate is arranged between the two connecting columns; a connecting disc is arranged at the top of the support, a telescopic rod is fixed on the connecting disc, and a cover body is fixed at the lower end of the telescopic rod; the cover body is hermetically connected with the bottom plate; a protection pad is arranged on the boss, an energy converter is fixed on the protection pad, an amplitude transformer is arranged on the upper side of the energy converter, a bus bar is arranged on the upper side of the amplitude transformer, a graphite heating electrode is arranged on the bus bar, and a micro-deposition crucible is arranged in the graphite heating electrode; an insulating thermal insulation plate is arranged between the graphite heating electrode and the bus board. According to the invention, the opening and closing of the cover body are controlled by the telescopic rod, so that the safety of a user can be ensured, the working efficiency can be improved, and the diamond coating time can be saved; and the control device is arranged on the second upright post and is far away from the microdeposition crucible, so that the safety of a user is further ensured.

Description

Diamond coating system, coating method, terminal and readable storage medium
Technical Field
The invention relates to the technical field of evaporation equipment, in particular to a diamond coating system, a coating method, a terminal and a readable storage medium.
Background
The diamond coating is a coating process for coating a diamond film with the thickness of several micrometers to dozens of micrometers on the surface of diamond or synthetic monocrystalline silicon or cubic zirconia and the like. Most of the devices for plating metal on the surface of diamond at present are vacuum micro-evaporation plating equipment. The equipment mainly comprises a vacuum pump, a diffusion pump communicated with the vacuum pump through a pipeline, and a plating chamber communicated with the diffusion pump through a pipeline with a valve.
Vacuum micro-evaporation plating belongs to one of physical vapor deposition technology, and is a plating method that by raising the temperature in a vacuum in a closed environment, plating element powder is sublimated and reaches the saturated vapor pressure of the plating element, and the plating element gas is condensed on diamond particles after the concentration of the plating element gas is supersaturated in the environment. The plating method has the advantages of simple plating equipment, lower cost compared with magnetron sputtering plating and rotary chemical plating, simple plating steps, more uniform diamond particle plating layer, less pores and denser tissue growth, and can achieve the purpose of controlling the thickness and the chemical composition of the plating layer to a certain extent by changing the plating temperature and the plating time in the vacuum micro-evaporation plating process although the scientific technology at the present stage cannot accurately control the plating layer obtained by growth.
In the vacuum coating technology, the prior document "application of vacuum coating technology in functional powder and industrialization prospect", compass can realize powder surface coating, powder surface modification and powder preparation by using the vacuum coating technology. The relation between the powder particle size and the design and process parameters of vacuum coating equipment during powder coating by a vacuum coating method is calculated and analyzed, and the uniform surface coating of powder with any particle size can be realized by an inclined rolling or middle screen method. The preparation method comprises the steps of preparing the nano-micro sheet carbon powder by using a plasma assisted vapor deposition technology, analyzing the composition, the structure and the specific surface area of the nano-micro sheet carbon powder by using an optical microscope, an atomic force microscope, a Raman spectrum, a specific surface tester and the like, loading a catalytic active substance by an impregnation method and testing the hydrogenation catalytic performance of the catalytic active substance. With the development of modern powder processing technologies such as 3D printing, powder metallurgy, injection molding and the like and the improvement of precision requirements, and the key role of high-performance functional powder in the aspects of printing ink, luminescence, display, LED, catalysis, tools and dies, thermology, energy and the like, the high-performance functional powder obtained by the vacuum coating technology is more and more a hot point of attention in all the related high-technology fields of materials such as consumer electronics, aerospace, military scientific research and the like.
However, the existing literature has poor safety and low working efficiency.
In order to solve the problem that the working efficiency is lower, the second prior document discloses development of multifunctional hot wire chemical vapor deposition diamond coating preparation equipment, and Liulusheng combines the principle of preparing a diamond film by an HFCVD method to develop the multifunctional hot wire chemical vapor deposition diamond coating preparation equipment according to the current situation of the domestic hot wire chemical vapor deposition diamond preparation equipment.
However, the second prior art document causes uneven plating due to uneven heat transfer in each part and different gas flow rates between the surface and the inside of the mixed powder.
In order to solve the problem of uneven plating, the third prior document provides a diamond film preparation and transmittance research institute, the university of western-land-postal-telecommunications college. The method is used for preparing the diamond film by a magnetron sputtering method, and the influence of three parameters of working pressure, sputtering current and coating time on the transmissivity of the diamond film is researched. The optimal technological parameters are obtained, namely the working air pressure is 1.3Pa, the sputtering current is 0.4A, and the coating time is 2 min. The plated diamond film can be used as a protective film and an antireflection film of an infrared element.
However, the carbide layer formed in the third prior art document is not uniform and the plated surface is not dense enough.
Prior art four (CN206580883U) provides a diamond-like coating preparation apparatus, comprising: vacuum cavity, heat tracing device, diffuser, flow controller. However, the prior art four-layer plating process causes non-uniform plating due to non-uniform heat transfer at each part and different gas flow rates between the surface and the inside of the mixed powder.
Furthermore, the invention discloses glass coated with an AF fingerprint-proof film on the surface of a diamond-like carbon coating film and a production process thereof. The process comprises the following steps: preparing a glass substrate, wherein a diamond-like carbon coating film is arranged on the surface of the glass substrate, an auxiliary transition layer containing Si atomic bonds is plated on the surface of the diamond-like carbon coating film, and then an AF fingerprint preventing film layer is sprayed on the surface of the auxiliary transition layer. The prior art penta-coated surfaces are not sufficiently dense.
In a word, the existing diamond coating system needs manual operation, so that the safety is poor, and the working efficiency is low; and the problems of uneven plating, uneven carbide layer generated, insufficiently compact plated surface and the like can be caused due to uneven heat transfer of each part and different gas circulation rates between the surface and the inside of the mixed powder in the plating process, so that the bonding performance of the plated layer and the diamond surface is influenced.
Disclosure of Invention
In order to overcome the problems in the related art, the disclosed embodiments of the present invention provide a diamond coating system, a coating method, a terminal and a readable storage medium. The technical scheme is as follows:
the diamond coating system provided by the invention is provided with:
a support;
connecting columns are fixed on two sides of the middle part of the bracket, and a bottom plate is arranged between the two connecting columns; the top of the support is provided with a connecting disc, a telescopic rod is fixed on the connecting disc through a bolt, and a cover body is fixed at the lower end of the telescopic rod through a bolt; the cover body is hermetically connected with the bottom plate;
the bracket is provided with a first upright post and a second upright post, and a cross beam is arranged between the two upright posts; a display screen is embedded in the front side of the second upright column, and a control button is embedded in the lower side of the display screen; and a main control device is arranged in the second upright post through a bolt.
According to the invention, the opening and closing of the cover body are controlled by the telescopic rod, so that the safety of a user can be ensured, the working efficiency can be improved, and the diamond coating time can be saved; and the control device is arranged on the second upright post and is far away from the microdeposition crucible, so that the safety of a user is further ensured.
Further, the bottom plate is provided with a fixing plate which is rectangular, a boss is integrally arranged on the upper side of the fixing plate, and a sealing gasket is arranged on the outer side of the boss; two sides of the fixing plate are fixedly connected with the two connecting columns; the outer wall of the boss is hermetically connected with the inner wall of the cover body.
The invention can ensure the vacuum state in the cover body through the lug boss and the sealing gasket, and ensure the diamond coating effect.
Further, a protection pad is arranged on the boss, an energy converter is fixed on the protection pad, an amplitude transformer is arranged on the upper side of the energy converter, a bus bar is arranged on the upper side of the amplitude transformer, a graphite heating electrode is arranged on the bus bar, and a micro-deposition crucible is arranged in the graphite heating electrode; and an insulating thermal insulation plate is arranged between the graphite heating electrode and the bus bar.
The invention not only keeps the basic function of vacuum micro-evaporation plating, but also can realize the control of mixed powder in the evaporation plating process; the novel graphite electrode that adopts of this use carries out direct heating to the microdeposition crucible, reduces electricity, heat energy loss, makes the inside temperature of plating in-process crucible even.
Furthermore, the micro-deposition crucible is in interference fit with the graphite heating electrode; the graphite heating device is characterized in that a limiting plate is arranged on the inner side of the graphite heating device, and a limiting groove matched with the limiting plate is formed in the outer wall of the microdeposition crucible.
According to the invention, the micro-deposition crucible and the graphite heating electrode can be relatively fixed through the matching of the limiting plate and the limiting groove, and the micro-deposition crucible is placed in the graphite heating electrode to shake, so that the film coating effect is influenced.
Further, a vacuum pump is arranged on the upper side of the cover body, and an air inlet electromagnetic valve is arranged on one side of the vacuum pump; the vacuum pump, the air inlet electromagnetic valve and the main control device are electrically connected.
Further, a liquid cold source is arranged in the second upright column and communicated with the bus board through a guide pipe.
Another object of the present invention is to provide a diamond coating method using the diamond coating system, the diamond coating method comprising the steps of:
step one, placing diamond particles to be coated in a vacuum chamber, and vacuumizing to 2 multiplied by 10-3Pa～6×10-2Heating to 90-120 ℃ when the pressure is Pa, and enabling the upper layer of the vacuum chamber to form water vapor;
step two, starting the high-voltage transformer, ionizing air into plasma under the condition of glow discharge when the output voltage of the high-voltage transformer is 2500-4500V and the current is 3-7A, bombarding, cleaning and activating the workpiece for 3-6 min by the plasma, and turning off a bombarding power supply to realize cleaning and activating of the diamond particles to be coated;
adding reaction raw materials into the deposition crucible, and controlling the telescopic rod to fall down through a control button until the telescopic rod is in close contact with the bottom plate; the vacuum pump is controlled by the control button to enable the interior of the cover body to be in a vacuum state;
electrifying the graphite heating electrode through a control button to uniformly heat the deposition crucible, assisting the deposition crucible to vibrate by the transducer and the amplitude transformer, sublimating the plating element powder formed by the strong carbide and reaching the saturated vapor pressure of the diamond particles to be plated;
step five, when the concentration of plating element gas formed by strong carbide in a deposition crucible is supersaturated, depositing a first plating layer formed by the elements formed by the strong carbide on the surfaces of the diamond particles after cleaning and activating treatment, wherein the plating time is 30-55 s, and the thickness of the first plating layer is 150-250 nm;
step six, electrifying the graphite heating electrode through a control button to uniformly heat the deposition crucible, assisting the deposition crucible to vibrate by the transducer and the amplitude transformer, sublimating the plating element powder formed by the carbide with high oxidation resistance and reaching the saturated vapor pressure of the diamond particles to be plated;
step seven, after the gas concentration of a plating element formed by the carbide with high oxidation resistance in the deposition crucible is supersaturated, depositing a second plating layer formed by the carbide forming element with high oxidation resistance on the first plating layer in the step five by using a vacuum micro-evaporation and powder metallurgy covering method, wherein the plating time is 20-35 s, and the thickness of the second plating layer is 150-350 nm;
step eight, plating a third plating layer made of Ni or Cu on the second plating layer in the step seven by an electroplating method, wherein the plating time is 15-35 s, and the thickness of the third plating layer is 50-550 mu m;
putting the diamond particles to be coated with the film in a vacuum chamber for film quality aging treatment, vacuumizing, and performing aging treatment on the film through repeated rapid cooling and heating for a plurality of times to stably coat the film;
step ten, after the aging treatment is finished, reducing the temperature of the deposition crucible through a liquid cooling source, connecting an air inlet electromagnetic valve with an air tank after the cooling process is finished, and introducing air into the vacuum environment to ensure that the internal air pressure is the same as the external air pressure; different gases can be stored in the gas tank to meet the needs of the plating environment;
step eleven, after the film coating is finished, measuring a transmission spectrum or a reflection spectrum of the diamond film coating, coating the film with the rate to be measured on a standard substrate, and setting the film coating time as t;
step twelve, measuring the transmission spectrum or the reflection spectrum of the coated standard substrate;
and thirteen, comparing the transmission spectrum or the reflection spectrum measured in the eleventh step and the reflection spectrum measured in the twelfth step, determining the peak positions before and after the film to be measured is plated by adopting a multimodal decomposition fitting technology, calculating the film plating thickness d according to the variation of the peak positions, and calculating the film plating rate v according to the film plating time t and the film plating thickness d.
Further, the diamond coating method comprises three-stage vacuum pumping, wherein the first coating is pumped to 1000-1200 Pa by a slide valve type vacuum pump, the second coating is pumped to 2-4 Pa by a Roots pump, and the third coating is pumped to 6 multiplied by 10 by a diffusion pump-2Pa～5×10-3Pa。
Further, in the step one, the vacuum chamber is a vertical double-door vacuum chamber.
Further, in the third step, the vacuum degree of the vacuum state in the cover body is 4 × 10-2～6×10-2Pa。
Further, in the fourth step, the strong carbide forming element is Ti or Cr.
Further, in the fourth step, the saturated vapor pressure is 2-6V, and the current is 5000-2500A.
Further, in the sixth step, the carbide forming element with higher oxidation resistance is W, Mo or Si.
Further, in the ninth step, the membrane is subjected to rapid heating and cooling treatment by introducing gas from the outside, wherein the introduced gas is nitrogen or oxygen.
Further, the temperature is rapidly increased to 100-150 ℃, and the temperature is rapidly decreased to 60 ℃.
Further, in the eleventh step, the method for plating the film to be measured in speed rate includes magnetron sputtering and vacuum evaporation coating methods.
Further, in the eleventh step, the substrate of the standard substrate is any one of optical glass, a quartz plate, a diamond plate, a silicon wafer or a germanium plate.
Further, in step thirteen, the method for determining the peak positions before and after plating the film to be measured by using the multimodal decomposition fitting technology includes:
(1) preliminarily determining the total number of main peaks and secondary peaks forming the spectrum on the original data spectrum;
(2) generating an initial structure of each peak through data analysis processing software or self-programming;
(3) determining a fitting target error value, and constructing a total fitting spectrum by continuously adjusting the proportion of each decomposition wavelet;
(4) comparing the difference between the fitting spectrum and the original spectrum, stopping fitting when the difference is smaller than a given fitting target error value, wherein the fitting spectrum formed by the obtained specific decomposition wavelet ratio is the target fitting spectrum, and the peak position of the spectrum is the finally determined accurate peak position;
(5) and (4) if the given fitting target error value can not be achieved after long-term fitting, returning to the step (1), modifying and adjusting the initial structure or the number of the decomposition wavelets, repeating the steps (2) to (4) until the target fitting error value is achieved, and determining the accurate peak position of the interference peak.
Another object of the present invention is to provide a computer-readable storage medium storing instructions which, when executed on a computer, cause the computer to perform the diamond coating method.
Another object of the present invention is to provide an information processing terminal comprising a memory and a processor, the memory storing a computer program that, when executed by the processor, causes the processor to execute the control program of the diamond coating method.
Another object of the present invention is to provide a computer-readable storage medium storing instructions which, when executed on a computer, cause the computer to perform the control functions of the diamond coating method.
The technical scheme provided by the embodiment of the invention has the following beneficial effects:
firstly, the cover body is controlled to open and close through the telescopic rod, so that the safety of a user can be ensured, the working efficiency can be improved, and the diamond coating time can be saved; and the control device is arranged on the second upright post and is far away from the microdeposition crucible, so that the safety of a user is further ensured.
Secondly, the invention can ensure the vacuum state in the cover body through the lug boss and the sealing gasket, and ensure the diamond coating effect.
Thirdly, the invention not only keeps the basic function of vacuum micro-evaporation plating, but also can realize the control of mixed powder in the evaporation plating process; the novel graphite electrode that adopts of this use carries out direct heating to the microdeposition crucible, reduces electricity, heat energy loss, makes the inside temperature of plating in-process crucible even.
Fourthly, the micro-deposition crucible and the graphite heating electrode can be ensured to be relatively fixed through the matching of the limiting plate and the limiting groove, and the micro-deposition crucible is placed in the graphite heating electrode to shake, so that the film coating effect is influenced.
Fifthly, the mixed powder is intermittently vibrated by the ultrasonic vibration auxiliary device, the relative position change among the particles is increased, each particle can be plated with a certain amount of metal elements with the same probability, and compared with the vacuum micro-evaporation plating equipment of a tube furnace, the effect is more uniform, and the purpose of improving the quality of the plated surface is achieved; according to the invention, the micro-deposition crucible is directly heated by the graphite electrode, so that the electric energy loss is reduced, the temperature control precision is increased, the uniform heating inside the crucible is ensured, the carbide types in the plating process are greatly reduced, and the surface quality of the plated layer can be greatly improved.
Sixth, the diamond coating method provided by the invention can directly and accurately measure the optical thickness coating rate of the film, is easy to realize on-line detection and real-time monitoring, breaks through the limitation of the traditional optical monitoring method, and can conveniently and accurately measure the ultra-low coating rate. The calibration precision of the coating rate is greatly improved, so that the method can be used for researching the stability of the coating rate and the change condition of the coating rate along with time, and has very important guiding significance for the precise monitoring of the coating process and the optimal design of a film system.
It is to be understood that both the foregoing general description and the following detailed description are exemplary and explanatory only and are not restrictive of the disclosure.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments consistent with the present disclosure and together with the description, serve to explain the principles of the disclosure.
FIG. 1 is a schematic diagram of a diamond coating system according to an embodiment of the present invention;
FIG. 2 is a schematic diagram of a backplane structure provided by an embodiment of the present invention;
FIG. 3 is a schematic view of an internal structure of a cover according to an embodiment of the present invention;
FIG. 4 is a schematic view of a microdeposition crucible according to an embodiment of the present invention;
reference numerals:
1. a first upright post; 2. a second upright post; 3. a cross beam; 4. connecting columns; 5. a base plate; 6. a cover plate; 7. a vacuum pump; 8. an air inlet solenoid valve; 9. a connecting disc; 10. a telescopic rod; 11. a display screen; 12. a control button; 13. a transducer; 14. an amplitude transformer; 15. an insulating thermal shield; 16. a bus bar; 17. a graphite heating electrode; 18. a microdeposition crucible; 19. a fixing plate; 20. a boss; 21. a gasket; 22. a limiting groove; 23. and a limiting plate.
Fig. 5 is a flow chart of a diamond coating method provided by the embodiment of the invention.
FIG. 6 is a flowchart of a method for determining peak positions before and after plating a film to be tested by using a multi-peak decomposition fitting technique according to an embodiment of the present invention.
FIG. 7 is a surface topography image of a plurality of sets of coated samples under different process parameters, provided by an embodiment of the present invention.
(a) Larger particle aggregates appear on the surface of the film; (b) dense island-like structures appear; (c) gaps between the islands become smaller; (d) the surface topography of (a) has both larger clusters of aggregates in (a) and islands of dense structure in (b). (d) The deposition rate of the film is fast and it is likely that some of the particles have not reached the surface to migrate and become coated with particles deposited later. (e) Large areas are not deposited in the middle and the periphery, and the areas and the shapes are different; (f) the islands are approximately the same size.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in detail below. In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein, but rather should be construed as broadly as the present invention is capable of modification in various respects, all without departing from the spirit and scope of the present invention.
It will be understood that when an element is referred to as being "secured to" another element, it can be directly on the other element or intervening elements may also be present. When an element is referred to as being "connected" to another element, it can be directly connected to the other element or intervening elements may also be present. As used herein, the terms "vertical," "horizontal," "left," "right," and the like are for purposes of illustration only and are not intended to represent the only embodiments.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
The invention is further described with reference to specific examples.
Example 1
As shown in fig. 1 to 4, a diamond coating system according to an embodiment of the present invention includes: the device comprises a first upright post 1, a second upright post 2, a cross beam 3, a connecting post 4, a bottom plate 5, a cover plate 6, a vacuum pump 7, an air inlet electromagnetic valve 8, a connecting disc 9, an expansion link 10, a display screen 11, a control button 12, an energy converter 13, an amplitude transformer 14, an insulating heat-insulating plate 15, a bus bar 16, a graphite heating electrode 17, a micro-deposition crucible 18, a fixing plate 19, a boss 20, a sealing gasket 21, a limiting groove 22 and a limiting plate 23.
Connecting columns 4 are fixed on two sides of the middle part of the bracket of the embodiment, and a bottom plate 5 is arranged between the two connecting columns 4; a connecting disc 9 is arranged at the top of the support, a telescopic rod 10 is fixed on the connecting disc 9 through a bolt, and a cover body 6 is fixed at the lower end of the telescopic rod 10 through a bolt; the cover body 6 is hermetically connected with the bottom plate 5; a vacuum pump 7 is arranged on the upper side of the cover body 6, and an air inlet electromagnetic valve 8 is arranged on one side of the vacuum pump 7; the vacuum pump 7 and the air inlet electromagnetic valve 8 are electrically connected with the main control device.
The bracket is provided with a first upright post 1 and a second upright post 2, and a cross beam 3 is arranged between the two upright posts; a display screen 11 is embedded in the front side of the second upright post 2, and a control button 12 is embedded in the lower side of the display screen 11; be provided with master control unit through the bolt in the second stand 2, be provided with the liquid cold source in the second stand 2, the liquid cold source passes through pipe and 16 intercommunications of cylinder manifold. The telescopic rod 10 is used for controlling the opening and closing of the cover body 6, so that the safety of a user can be ensured, the working efficiency can be improved, and the diamond coating time can be saved; and the control device of the invention is arranged on the second upright post 2 and is far away from the microdeposition crucible 18, thereby further ensuring the safety of users.
In this embodiment, the bottom plate 5 is provided with a fixing plate 19, the fixing plate 19 is rectangular, a boss 20 is integrally arranged on the upper side of the fixing plate 19, and a sealing gasket 21 is arranged on the outer side of the boss 20; two sides of the fixed plate 19 are fixedly connected with the two connecting columns 4; the outer wall of the boss 20 is hermetically connected with the inner wall of the cover body 6. The vacuum state in the cover body 6 can be ensured through the lug boss 20 and the sealing gasket 21, and the diamond coating effect is ensured.
In the embodiment, a protection pad is arranged on the boss 20, the transducer 13 is fixed on the protection pad, the amplitude transformer 14 is arranged on the upper side of the transducer 13, the bus bar 16 is arranged on the upper side of the amplitude transformer 14, the graphite heating electrode 17 is arranged on the bus bar 16, and the micro-deposition crucible 18 is arranged in the graphite heating electrode 17; an insulating thermal insulation plate 15 is arranged between the graphite heating electrode 17 and the bus bar 16. The invention not only keeps the basic function of vacuum micro-evaporation plating, but also can realize the control of mixed powder in the evaporation plating process; this use is novel to adopt graphite electrode to carry out direct heating to microdeposition crucible 18, reduces electricity, heat energy loss, makes the inside temperature of plating in-process crucible 18 even.
In this embodiment, the microdeposition crucible 18 and the graphite heating electrode 17 are in interference fit; a limiting plate 23 is arranged on the inner side of the graphite heating electrode, and a limiting groove 22 matched with the limiting plate 23 is arranged on the outer wall of the microdeposition crucible 18. The micro-deposition crucible 18 and the graphite heating electrode 17 can be ensured to be relatively fixed through the matching of the limiting plate 23 and the limiting groove 22, and the micro-deposition crucible 18 is placed to shake in the graphite heating electrode 17, so that the film coating effect is influenced.
The working principle of the invention is as follows: adding reaction raw materials into a deposition crucible 18, and controlling a telescopic rod 10 to fall down through a control button 12 until the reaction raw materials are in close contact with a bottom plate 5; the vacuum pump 7 is controlled by the control button 12 to make the inner part of the cover body 6 in a vacuum state; the graphite heating electrode 17 is electrified through the control button 12, so that the deposition crucible 18 is uniformly heated, the transducer 13 and the amplitude transformer 14 assist the deposition crucible 18 to vibrate, the plating element powder is sublimated and reaches the saturated vapor pressure of the plating element, and the plating element gas in the deposition crucible 18 is condensed on diamond particles after the concentration is supersaturated; after the reaction is finished, the temperature of the deposition crucible 18 is reduced by a liquid cooling source, after the cooling process is finished, the gas inlet electromagnetic valve 8 is connected with a gas tank, and gas is introduced into the vacuum environment to ensure that the internal gas pressure is the same as the external gas pressure; different gases may be stored in the gas tank to correspond to the needs of the plating environment.
Example 2
As shown in fig. 5, the diamond coating method provided by the embodiment of the invention includes the following steps:
s101, placing diamond particles to be coated in a vacuum chamber, and vacuumizing to 2 multiplied by 10-3Pa～6×10-2Heating to 90-120 ℃ when the pressure is Pa, and enabling the upper layer of the vacuum chamber to form water vapor;
s102, starting a high-voltage transformer, ionizing air into plasma under the condition of glow discharge when the output voltage of the high-voltage transformer is 2500-4500V and the current is 3-7A, bombarding, cleaning and activating a workpiece for 3-6 min by the plasma, and turning off a bombarding power supply to clean and activate diamond particles to be coated;
s103, adding reaction raw materials into the deposition crucible, and controlling the telescopic rod to fall down through a control button until the telescopic rod is in close contact with the bottom plate; the vacuum pump is controlled by the control button to enable the interior of the cover body to be in a vacuum state;
s104, electrifying the graphite heating electrode through a control button to uniformly heat the deposition crucible, assisting the deposition crucible to vibrate by the transducer and the amplitude transformer, sublimating the plating element powder formed by the strong carbide and reaching the saturated vapor pressure of the diamond particles to be plated;
s105, when the concentration of a plating element gas formed by strong carbide in a deposition crucible is supersaturated, depositing a first plating layer formed by the elements formed by the strong carbide on the surfaces of the diamond particles subjected to cleaning and activating treatment, wherein the plating time is 30-55S, and the thickness of the first plating layer is 150-250 nm;
s106, electrifying the graphite heating electrode through a control button, uniformly heating the deposition crucible, assisting the deposition crucible to vibrate by the transducer and the amplitude transformer, sublimating the plating element powder formed by the carbide with high oxidation resistance and reaching the saturated vapor pressure of the diamond particles to be plated;
s107, after the gas concentration of a plating element formed by the carbide with high oxidation resistance in the deposition crucible is supersaturated, depositing a second plating layer formed by the carbide forming element with high oxidation resistance on the first plating layer by using a vacuum micro-evaporation and powder metallurgy covering method in S105, wherein the plating time is 20-35S, and the thickness of the second plating layer is 150-350 nm;
s108, plating a third plating layer made of Ni or Cu on the second plating layer in the S107 by using an electroplating method, wherein the plating time is 15-35S, and the thickness of the third plating layer is 50-550 mu m;
s109, placing the diamond particles to be coated after coating in a vacuum chamber for film quality aging treatment, vacuumizing, and performing aging treatment on the coating through repeated rapid cooling and heating for a plurality of times to stably coat the coating;
s110, after the aging treatment is finished, reducing the temperature of the deposition crucible through a liquid cooling source, connecting an air inlet electromagnetic valve with an air tank after the cooling process is finished, and introducing air into the vacuum environment to enable the internal air pressure to be the same as the external air pressure; different gases can be stored in the gas tank to meet the needs of the plating environment;
s111, measuring a transmission spectrum or a reflection spectrum of the diamond coating after the coating is finished, coating the film with the rate to be measured on a standard substrate, and setting the coating time as t;
s112, measuring a transmission spectrum or a reflection spectrum of the coated standard substrate;
and S113, comparing the transmission spectrum or the reflection spectrum measured in S111 and S112, determining the peak positions before and after the film to be measured is plated by adopting a multimodal decomposition fitting technology, calculating the plating film thickness d according to the variation of the peak positions, and calculating the plating film rate v according to the plating film time t and the plating film thickness d.
The diamond coating method provided by the embodiment of the invention is three-stage vacuum pumping, the first coating is pumped to 1000-1200 Pa by using a slide valve type vacuum pump, the second coating is pumped to 2-4 Pa by using a Roots pump, and the third coating is pumped to 6 multiplied by 10 by using a diffusion pump-2Pa～5×10-3Pa。
In step S101 provided in the embodiment of the present invention, the vacuum chamber is a vertical double-door vacuum chamber.
In step S103 provided in the embodiment of the present invention, the vacuum degree of the interior of the cover body in the vacuum state is 4 × 10-2～6×10-2Pa。
In step S104 provided in the embodiment of the present invention, the strong carbide forming element is Ti or Cr.
In step S104 provided by the embodiment of the present invention, the saturated vapor pressure is 2-6V, and the current is 5000-2500A.
In step S106 provided in the embodiment of the present invention, the carbide forming element with high oxidation resistance is W, Mo or Si.
In step S109 provided in the embodiment of the present invention, the film is subjected to rapid temperature increase and temperature decrease by introducing gas from the outside, where the introduced gas is nitrogen or oxygen.
The temperature is rapidly increased to 100-150 ℃ and is rapidly reduced to 60 ℃ according to the embodiment of the invention.
In step S111 provided in the embodiment of the present invention, the method for plating the film to be measured includes magnetron sputtering and vacuum evaporation coating methods.
In step S111 provided in the embodiment of the present invention, the substrate of the standard substrate is any one of optical glass, a quartz plate, a sapphire plate, a silicon wafer, and a germanium plate.
As shown in fig. 6, in step S113 provided in the embodiment of the present invention, the method for determining peak positions before and after plating a film to be measured by using a multi-peak decomposition fitting technique includes:
s201, preliminarily determining the total number of main peaks and secondary peaks forming a spectrum on an original data spectrum;
s202, generating an initial structure of each peak through data analysis processing software or self-programming;
s203, determining a fitting target error value, and constructing a total fitting spectrum by continuously adjusting the proportion of each decomposition wavelet;
s204, comparing the difference between the fitting spectrum and the original spectrum, stopping fitting when the difference is smaller than a given fitting target error value, wherein the fitting spectrum formed by the obtained specific decomposition wavelet ratio is the target fitting spectrum, and the peak position of the spectrum is the finally determined accurate peak position;
s205, if the given fitting target error value can not be achieved after long-term fitting, returning to S201 again, modifying and adjusting the initial structure or number of the decomposition wavelets, repeating S202-S204 until the target fitting error value is achieved, and determining the accurate peak position of the interference peak.
The present invention is further described below in conjunction with the experimental results.
The diamond coating method provided by the invention can directly and accurately measure the optical thickness coating rate of the film, is easy to realize on-line detection and real-time monitoring, breaks through the limitation of the traditional optical monitoring method, and can very conveniently and accurately measure the ultralow coating rate. The calibration precision of the coating rate is greatly improved, so that the method can be used for researching the stability of the coating rate and the change condition of the coating rate along with time, and has very important guiding significance for the precise monitoring of the coating process and the optimal design of a film system.
Meanwhile, the performance of the product obtained by the coating method provided by the invention is shown in figure 7. And (3) surface appearance images of a plurality of groups of coating samples under different process parameters.
(a) As can be seen, larger particle aggregates appear on the surface of the film, and particles with smaller sizes are randomly scattered beside the film, so that the size difference is larger. (b) The dense island-shaped structure is generated, the size of the island is close, and the island fusion phenomenon is also accompanied. (c) And (c) the island is denser than the island (b), gaps among the islands are reduced, and the shape of the island is changed into a slender type gully shape to aggregate and grow. (d) The surface topography of (a) has both larger clusters of aggregates in (a) and islands of dense structure in (b). (d) The process parameters show that the deposition rate of the thin film is very fast at this time, and a part of particles may not have to migrate to the surface and are covered by the particles deposited later, so that the phenomenon of larger clusters appears in the areas 1, 2, 3 and the like in the step (d). (e) The medium black region represents clusters and island-like structures of aluminum, and the remaining portion represents a region not covered with aluminum particles. The non-deposited areas are distributed unevenly, large areas are not deposited in the middle and the periphery, and the areas and the shapes are different. (f) The island in (a) is more densely grown than (b) and more flat than (c), and the size of the island is approximately the same. (f) The process parameters of (a) indicate that the particles deposited on the surface have a higher energy but a lower number of particles per unit time, resulting in sufficient time for the particles to migrate to the surface and grow and agglomerate in place, resulting in an increased uniformity of the film and a tendency for the surface of the film to densify. The film thickness at this time was 4.1 μm, which is a thin film obtained in the whole experiment, indicating that a relatively flat surface morphology was obtained in the case of high energy and low deposition rate.
Other embodiments of the disclosure will be apparent to those skilled in the art from consideration of the specification and practice of the disclosure disclosed herein. This application is intended to cover any variations, uses, or adaptations of the disclosure following, in general, the principles of the disclosure and including such departures from the present disclosure as come within known or customary practice within the art to which the disclosure pertains. It is intended that the specification and examples be considered as exemplary only, with a true scope and spirit of the disclosure being indicated by the following claims.
It will be understood that the present disclosure is not limited to the precise arrangements described above and shown in the drawings and that various modifications and changes may be made without departing from the scope thereof. The scope of the present disclosure should be limited only by the attached claims.

Claims (10)

1. A diamond coating method, characterized in that the diamond coating method comprises:
placing diamond particles to be coated in a vacuum chamber, and vacuumizing to 2 x 10-3Pa～6×10-2Heating to 90-120 ℃ when the pressure is Pa, and enabling the upper layer of the vacuum chamber to form water vapor;
starting a high-voltage transformer, ionizing air into plasma under the condition of glow discharge when the output voltage of the high-voltage transformer is 2500-4500V and the current is 3-7A, bombarding, cleaning and activating the workpiece for 3-6 min by the plasma, and turning off a bombarding power supply to clean and activate the diamond particles to be coated;
adding reaction raw materials into a deposition crucible, and controlling a telescopic rod to fall down through a control button until the telescopic rod is in close contact with a bottom plate; the vacuum pump is controlled by the control button to enable the interior of the cover body to be in a vacuum state;
the graphite heating electrode is electrified through a control button, so that the deposition crucible is uniformly heated, the transducer and the amplitude transformer assist the deposition crucible to vibrate, and plating element powder formed by strong carbide is sublimated and reaches the saturated vapor pressure of the diamond particles to be plated;
when the concentration of a plating element gas formed by strong carbide in a deposition crucible is supersaturated, depositing a first plating layer formed by the strong carbide forming element on the surfaces of diamond particles subjected to cleaning and activation treatment, wherein the plating time is 30-55 s, and the thickness of the first plating layer is 150-250 nm;
the graphite heating electrode is electrified through the control button, so that the deposition crucible is uniformly heated, the transducer and the amplitude transformer assist the deposition crucible to vibrate, and the plating element powder formed by carbide with high oxidation resistance is sublimated and reaches the saturated vapor pressure of the diamond particles to be plated;
when the gas concentration of a plating element formed by carbide with high oxidation resistance in a deposition crucible is supersaturated, depositing a second plating layer formed by the carbide forming element with high oxidation resistance on the first plating layer by using a vacuum micro-evaporation and powder metallurgy covering method, wherein the plating time is 20-35 s, and the thickness of the second plating layer is 150-350 nm;
plating a third plating layer made of Ni or Cu on the second plating layer by an electroplating method, wherein the plating time is 15-35 s, and the thickness of the third plating layer is 50-550 mu m;
placing the diamond particles to be coated with the film in a vacuum chamber for film quality aging treatment, vacuumizing, and performing aging treatment on the film through repeated rapid cooling and heating for a plurality of times to stably coat the film;
after the aging treatment is finished, the temperature of the deposition crucible is reduced through a liquid cooling source, after the cooling process is finished, an air inlet electromagnetic valve is connected with an air tank, and air is introduced into the vacuum environment to enable the internal air pressure to be the same as the external air pressure; storing different gases in the gas tank to meet the needs of the plating environment;
after the film coating is finished, measuring a transmission spectrum or a reflection spectrum of the diamond film coating, coating the film with the rate to be measured on a standard substrate, and setting the film coating time as t;
measuring the transmission spectrum or the reflection spectrum of the coated standard substrate;
comparing the measured transmission spectrum or reflection spectrum, determining the peak position before and after coating the film to be measured by adopting a multimodal decomposition fitting technology, calculating the coating thickness d according to the variation of the peak position, and calculating the coating speed v according to the coating time t and the coating thickness d.
2. The diamond coating method according to claim 1, wherein the diamond coating method is a three-stage vacuum pumping, the first coating layer is pumped to 1000 to 1200Pa by a slide valve type vacuum pump, the second coating layer is pumped to 2 to 4Pa by a roots pump, and the third coating layer is pumped to 6 x 10 Pa by a diffusion pump-2Pa～5×10-3Pa；
The vacuum chamber is a vertical double-door vacuum chamber.
3. The diamond coating method according to claim 1, wherein the degree of vacuum in the inside of the cap body is 4 x 10 in vacuum state-2～6×10-2Pa；
The strong carbide forming element is Ti or Cr;
the saturated vapor pressure is 2-6V, and the current is 5000-2500A.
4. The diamond coating method according to claim 1, wherein the carbide forming element having high oxidation resistance is W, Mo or Si;
the membrane is subjected to rapid heating and cooling treatment by introducing gas from the outside, wherein the introduced gas is nitrogen or oxygen;
quickly heating to 100-150 deg.C, and quickly cooling to 60 deg.C.
5. The diamond coating method according to claim 1, wherein the method of coating a film to be measured in rate comprises magnetron sputtering and vacuum evaporation coating methods;
the substrate of the standard substrate is any one of optical glass, a quartz plate, a gem plate, a silicon wafer or a germanium plate;
the method for determining the peak positions before and after the film to be measured is plated by adopting the multimodal decomposition fitting technology comprises the following steps:
(1) preliminarily determining the total number of main peaks and secondary peaks forming the spectrum on the original data spectrum;
(2) generating an initial structure of each peak through data analysis processing software or self-programming;
(2) determining a fitting target error value, and constructing a total fitting spectrum by continuously adjusting the proportion of each decomposition wavelet;
(4) comparing the difference between the fitting spectrum and the original spectrum, stopping fitting when the difference is smaller than a given fitting target error value, wherein the fitting spectrum formed by the obtained specific decomposition wavelet ratio is the target fitting spectrum, and the peak position of the spectrum is the finally determined accurate peak position;
(5) and (4) if the given fitting target error value can not be achieved after long-term fitting, returning to the step (1), modifying and adjusting the initial structure or the number of the decomposition wavelets, repeating the steps (2) to (4) until the target fitting error value is achieved, and determining the accurate peak position of the interference peak.
6. A diamond coating system for realizing the diamond coating method according to any one of claims 1 to 5, wherein the diamond coating system is provided with:
a support;
connecting columns are fixed on two sides of the middle part of the bracket, and a bottom plate is arranged between the two connecting columns; the top of the support is provided with a connecting disc, a telescopic rod is fixed on the connecting disc through a bolt, and a cover body is fixed at the lower end of the telescopic rod through a bolt; the cover body is hermetically connected with the bottom plate;
the bracket is provided with a first upright post and a second upright post, and a cross beam is arranged between the two upright posts; a display screen is embedded in the front side of the second upright column, and a control button is embedded in the lower side of the display screen; and a main control device is arranged in the second upright post through a bolt.
7. The diamond coating system according to claim 6, wherein the base plate is provided with a fixing plate, the fixing plate is rectangular, a boss is integrally arranged on the upper side of the fixing plate, and a sealing gasket is arranged on the outer side of the boss; two sides of the fixing plate are fixedly connected with the two connecting columns; the outer wall of the boss is hermetically connected with the inner wall of the cover body;
a protection pad is arranged on the boss, an energy converter is fixed on the protection pad, an amplitude transformer is arranged on the upper side of the energy converter, a bus bar is arranged on the upper side of the amplitude transformer, a graphite heating electrode is arranged on the bus bar, and a micro-deposition crucible is arranged in the graphite heating electrode; an insulating heat-insulating plate is arranged between the graphite heating electrode and the bus bar;
the micro-deposition crucible is in interference fit with the graphite heating electrode; the graphite heating device is characterized in that a limiting plate is arranged on the inner side of the graphite heating device, and a limiting groove matched with the limiting plate is formed in the outer wall of the microdeposition crucible.
8. The diamond coating system according to claim 6, wherein a vacuum pump is provided on the upper side of the cover body, and an air inlet solenoid valve is provided on one side of the vacuum pump; the vacuum pump and the air inlet electromagnetic valve are electrically connected with the main control device;
and a liquid cold source is arranged in the second upright column and is communicated with the bus board through a guide pipe.
9. An information processing terminal comprising a memory and a processor, wherein the memory stores a computer program, and the computer program, when executed by the processor, causes the processor to execute a control program of the diamond coating method according to any one of claims 1 to 5.
10. A computer-readable storage medium storing instructions which, when executed on a computer, cause the computer to perform the control functions of the diamond coating method according to any one of claims 1 to 5.
CN202011376251.1A 2020-11-30 2020-11-30 Diamond coating system, coating method, terminal and readable storage medium Pending CN112626484A (en)

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Publication number Priority date Publication date Assignee Title
CN113893989A (en) * 2021-09-26 2022-01-07 浙江航威专用设备有限公司 Novel vacuum humidification coating film making machine

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CN103105190A (en) * 2011-11-14 2013-05-15 常州光电技术研究所 Accurate calibration method of film coating rate and application thereof
CN104233295A (en) * 2014-09-29 2014-12-24 泉州众志金刚石工具有限公司 Diamond coating method
CN109338325A (en) * 2018-11-19 2019-02-15 苏州沃盾纳米科技有限公司 A kind of control method and system of filming equipment, filming equipment and storage medium
CN110438444A (en) * 2019-08-27 2019-11-12 西安交通大学 A kind of plating tungsten diamond particles, tangsten plating process, its application and obtained diamond/copper composite material as copper-based reinforced phase
CN111575654A (en) * 2020-05-21 2020-08-25 南京航空航天大学 Ultrasonic vibration assisted vacuum micro-evaporation plating equipment

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Publication number Priority date Publication date Assignee Title
CN103105190A (en) * 2011-11-14 2013-05-15 常州光电技术研究所 Accurate calibration method of film coating rate and application thereof
CN104233295A (en) * 2014-09-29 2014-12-24 泉州众志金刚石工具有限公司 Diamond coating method
CN109338325A (en) * 2018-11-19 2019-02-15 苏州沃盾纳米科技有限公司 A kind of control method and system of filming equipment, filming equipment and storage medium
CN110438444A (en) * 2019-08-27 2019-11-12 西安交通大学 A kind of plating tungsten diamond particles, tangsten plating process, its application and obtained diamond/copper composite material as copper-based reinforced phase
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CN113893989A (en) * 2021-09-26 2022-01-07 浙江航威专用设备有限公司 Novel vacuum humidification coating film making machine

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Application publication date: 20210409