CN112760608A - Method for preventing interlayer air bleeding in carbon fiber composite material surface film deposition process - Google Patents

Method for preventing interlayer air bleeding in carbon fiber composite material surface film deposition process Download PDF

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Publication number
CN112760608A
CN112760608A CN202011464917.9A CN202011464917A CN112760608A CN 112760608 A CN112760608 A CN 112760608A CN 202011464917 A CN202011464917 A CN 202011464917A CN 112760608 A CN112760608 A CN 112760608A
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China
Prior art keywords
antenna
film
coating
air pressure
carbon fiber
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Pending
Application number
CN202011464917.9A
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Chinese (zh)
Inventor
赵栋才
周晖
吴春华
武生虎
何延春
杨拉毛草
李学磊
马占吉
肖更竭
王虎
杨淼
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Lanzhou Institute of Physics of Chinese Academy of Space Technology
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Lanzhou Institute of Physics of Chinese Academy of Space Technology
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Priority to CN202011464917.9A priority Critical patent/CN112760608A/en
Publication of CN112760608A publication Critical patent/CN112760608A/en
Pending legal-status Critical Current

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Classifications

    • 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
    • C23C14/34—Sputtering
    • C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
    • 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
    • C23C14/14—Metallic material, boron or silicon
    • C23C14/18—Metallic material, boron or silicon on other inorganic substrates
    • C23C14/185—Metallic material, boron or silicon on other inorganic substrates by cathodic sputtering
    • 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

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

Abstract

The invention discloses a method for preventing interlayer deflation in the process of depositing a carbon fiber composite surface film, wherein an intermittent control strategy is adopted in the film coating process, the intermittent inspection basis is air pressure detection, compared with the initial working air pressure, the proportion of the increase of the air pressure in a vacuum chamber in the film coating process is set as a film coating pause criterion, the film coating is paused until the temperature is reduced, and then the film coating is restarted until the whole film coating process is completed; the invention can effectively prevent the composite material from exhausting and polluting the medium film layer caused by temperature rise in the film coating process, and maintain the performance of the film layer.

Description

Method for preventing interlayer air bleeding in carbon fiber composite material surface film deposition process
Technical Field
The invention belongs to the technical field of satellite antenna microwave transmission, thermal control and protection, and particularly relates to a method for preventing interlayer deflation in a carbon fiber composite material surface film deposition process.
Background
As an important load of a satellite, an antenna is being developed in a direction of light weight and high accuracy.
The lightweight requires that the antenna must be made of composite materials; the high precision requires the high processing precision of the antenna, and the temperature difference of the on-orbit working temperature of the antenna is small. However, the composite material has poor conductivity and anisotropy, and the antenna needs to be metallized; in the in-orbit working process of the antenna, the antenna is subjected to high and low temperature alternation and space environment irradiation, and proper protective measures need to be carried out on the antenna.
At present, the conductivity of the antenna is improved by plating a metal film Al or Ag on the surface of a composite material, and the surface of the antenna is coated with a solar screen to realize temperature control and environmental protection. The two functions are realized through a composite film structure, so that the processing steps of the antenna can be reduced, and the reliability is improved. The invention aims to provide a plating method of a temperature control and environmental protection film layer, and a dielectric film layer and a protection film layer can be plated on the surface of a material-conforming antenna by the method.
Disclosure of Invention
In view of this, the invention provides a method for preventing interlayer outgassing in a deposition process of a carbon fiber composite surface film, which can avoid heating of an antenna and a vacuum chamber by various particles (ions) in a magnetron sputtering process, prevent volatilization of resin materials in the composite material, cause pollution to a film layer, and reduce performance of the film layer.
The technical scheme for realizing the invention is as follows:
a method for preventing interlayer air bleeding in the deposition process of a carbon fiber composite material surface film adopts an intermittent control strategy in the film coating process, the intermittent inspection basis is air pressure detection, the air pressure rise in a vacuum chamber in the film coating process is set as a film coating pause criterion in proportion to the initial working air pressure, the film coating is paused until the temperature is reduced, and then the film coating is restarted until the whole film coating process is completed.
Further, the invention specifically comprises the following steps:
the method comprises the following steps that firstly, the surface of an antenna is cleaned according to the structure of an antenna composite material so as to meet the requirement of preparing a dielectric film layer or a protective film layer;
secondly, loading the antenna into a vacuum chamber;
step three, after the antenna is loaded, vacuumizing to a background vacuum, heating to a process temperature, and keeping for 4 hours;
step four, introducing Ar gas and reaction gas O2When the magnetic control source baffle is closed or the antenna is moved to a position far away from the sputtering source, the magnetic control power supply is started to adjust the working parameters of the dielectric film layer;
step five, reading the air pressure value in the vacuum chamber, then opening the magnetic control source baffle, or moving the antenna to a film coating area, and starting the coating of the dielectric film layer;
step six, when the air pressure is increased by 1-3% relative to the air pressure read in the step five, suspending the film coating process and waiting for the antenna to be cooled; the specific boosting numerical value is determined according to the accuracy of a vacuum gauge, but the smaller the boosting relative value is, the better the boosting relative value is, otherwise, the absorption rate of the dielectric film is greatly influenced;
step seven, after cooling, continuously repeating the steps four to six until the whole film coating process is finished;
and step eight, after the film coating process is finished and the temperature is reduced to the temperature capable of opening the vacuum chamber, introducing air into the vacuum chamber, and taking out the antenna to finish the coating of the dielectric film layer.
Further, in step one, the surface is cleaned by ultrasonic methods or scrubbed with cotton cloth dipped in acetone/ethanol several times until the color of the cotton cloth no longer changes.
Further, in the fourth step, Ar gas is introduced by a direct flow control method.
Further, in step four, O2The gas is introduced in a mode of linkage with the spectrum or in a mode of linkage with the power discharge voltage.
Has the advantages that:
by adopting the technology of the invention, the composite material outgas and pollution of the medium film layer caused by temperature rise in the film coating process can be effectively prevented, and the performance of the film layer is maintained.
Detailed Description
The present invention will be described in detail with reference to examples.
The invention provides a method for preventing interlayer outgassing in the deposition process of a carbon fiber composite material surface film. During the coating process, the temperature of the vacuum chamber and the substrate can be increased due to the action of ions (particles), electrons and the like, various organic matters in the composite material can be volatilized when the temperature is increased, the film layer is blackened, the emissivity of the medium film layer is improved, the absorptivity is also improved, and the expected thermal control performance index cannot be reached. The intermittent coating mode is adopted, the air pressure rise is taken as a criterion, and the coating time is controlled, so that the heating of various particles (ions) to the antenna and the vacuum chamber in the magnetron sputtering process is avoided, the resin materials in the composite material are prevented from volatilizing, the pollution to the film layer is prevented, and the performance of the film layer is reduced.
Example 1: magnetron sputtering coating of SiO2。
Description of the apparatus: in the larger twin magnetron sputtering equipment, the cathode is columnar, and the target material is a silicon target.
(1) Cleaning the surface of the antenna: scrubbing the surface for many times by using cotton cloth dipped with acetone/ethanol until the color of the cotton cloth is not changed any more so as to meet the requirement of SiO2And (5) preparing a film.
(2) Loading into a vacuum chamber: the antenna samples were loaded into the vacuum chamber as designed before coating.
(3) Background vacuum maintenance: after the antenna sample is loaded, the vacuum is pumped to 10-4Pa, keeping for 4 h.
(4) Pre-sputtering: and introducing 390sccm of Ar gas, and turning on the magnetic control power supply under the condition that the antenna is moved to a position far away from the sputtering source.
(5) Reaction gas O2A gas. O is2The milk passing amount is adjusted according to the output voltage of the power supply, and the voltage is set to 375V.
(6) Coating a film layer: the pressure of the vacuum chamber is 0.33Pa when the magnetron cathode works stably. And moving the antenna sample to a coating area, and starting the coating of the dielectric film layer.
(7) And (3) film coating suspension: when the air pressure is increased to 0.34Pa, the coating process is suspended.
(8) Cooling and maintaining: and setting the coating pause time to be 10min, and waiting for the antenna sample to be cooled.
(9) Continuously plating a film layer: and (5) after cooling, continuously repeating the steps (4) to (8) until the whole film coating process is finished.
(10) And (3) finishing coating: and after the film coating process is finished and the vacuum chamber is cooled for 30min, introducing air into the vacuum chamber, taking out the antenna sample, and finishing the coating of the dielectric film layer.
Example 2: and (4) carrying out magnetron sputtering plating on Ge.
Description of the apparatus: magnetron sputtering equipment for mounting strip sputtering cathode, and germanium target is selected as target material
(1) Cleaning the surface of the antenna: and (3) scrubbing the surface for multiple times by adopting cotton cloth dipped with acetone/ethanol until the color of the cotton cloth is not changed any more so as to meet the preparation requirement of the Ge film.
(2) Loading into a vacuum chamber: the antenna samples were loaded into the vacuum chamber as designed before coating.
(3) Background vacuum maintenance: after the antenna sample is loaded, the vacuum is pumped to 10-4Pa, keeping for 4 h.
(4) Pre-sputtering: and introducing 100sccm of Ar gas, starting the magnetic control power supply under the condition that the antenna is moved to a position far away from the sputtering source, and setting the output power of the power supply to be 2500W. .
(5) Coating a film layer: the pressure of the vacuum chamber is 0.4Pa when the magnetron cathode works stably. And moving the antenna sample to the film coating area, and starting the Ge film layer coating.
(6) And (3) film coating suspension: when the air pressure is increased to 0.41Pa, the coating process is suspended.
(7) Cooling and maintaining: and setting the coating pause time to be 10min, and waiting for the antenna sample to be cooled.
(8) Continuously plating a film layer: and (5) after cooling, continuously repeating the steps (4) to (7) until the whole film coating process is finished.
(9) And (3) finishing coating: and after the film coating process is finished and the vacuum chamber is cooled for 30min, introducing air into the vacuum chamber, taking out the antenna sample, and finishing the coating of the dielectric film layer.
In summary, the above description is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (5)

1. The method for preventing interlayer air bleeding in the deposition process of the carbon fiber composite material surface film is characterized in that an intermittent control strategy is adopted in the coating process, the intermittent inspection is based on air pressure detection, compared with the initial working air pressure, the proportion of the increase of the air pressure in a vacuum chamber in the coating process is set as a coating suspension criterion, the coating is suspended until the temperature is reduced, and then the coating is restarted until the whole coating process is completed.
2. The method for preventing interlayer outgassing in the carbon fiber composite surface film deposition process according to claim 1, comprising the following steps:
the method comprises the following steps that firstly, the surface of an antenna is cleaned according to the structure of an antenna composite material so as to meet the requirement of preparing a dielectric film layer or a protective film layer;
secondly, loading the antenna into a vacuum chamber;
step three, after the antenna is loaded, vacuumizing to a background vacuum, heating to a process temperature, and keeping for 4 hours;
step fourAr gas and reaction gas O are introduced2When the magnetic control source baffle is closed or the antenna is moved to a position far away from the sputtering source, the magnetic control power supply is started to adjust the working parameters of the dielectric film layer;
step five, reading the air pressure value in the vacuum chamber, then opening the magnetic control source baffle, or moving the antenna to a film coating area, and starting the coating of the dielectric film layer;
step six, when the air pressure is increased by 1-3% relative to the air pressure read in the step five, suspending the film coating process and waiting for the antenna to be cooled;
step seven, after cooling, continuously repeating the steps four to six until the whole film coating process is finished;
and step eight, after the film coating process is finished and the temperature is reduced to the temperature capable of opening the vacuum chamber, introducing air into the vacuum chamber, and taking out the antenna to finish the coating of the dielectric film layer.
3. The method for preventing interlayer outgassing during deposition of a film on a carbon fiber composite surface of claim 2, wherein in step one, the surface is cleaned by ultrasonic methods or scrubbed with cotton cloth dipped in acetone/ethanol for multiple times until the color of the cotton cloth no longer changes.
4. The method for preventing interlayer outgassing during the deposition of a thin film on the surface of a carbon fiber composite material according to claim 2, wherein in the fourth step, Ar gas is introduced by a direct flow control method.
5. The method for preventing interlayer outgassing during the deposition of a thin film on a carbon fiber composite surface of claim 2, wherein in step four, O is2The gas is introduced in a mode of linkage with the spectrum or in a mode of linkage with the power discharge voltage.
CN202011464917.9A 2020-12-14 2020-12-14 Method for preventing interlayer air bleeding in carbon fiber composite material surface film deposition process Pending CN112760608A (en)

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Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0529227A (en) * 1991-07-17 1993-02-05 Canon Inc Deposited film formation method
JP2000282224A (en) * 1999-03-29 2000-10-10 Sumitomo Heavy Ind Ltd Device and method for film formation
JP2001026885A (en) * 1999-07-16 2001-01-30 Meiku:Kk Thin film forming device
CN1636077A (en) * 2002-02-21 2005-07-06 科鲁斯技术有限公司 Method and device for coating a substrate
CN2832828Y (en) * 2005-10-27 2006-11-01 北京实力源科技开发有限责任公司 Vacuum coating system
CN101100739A (en) * 2007-08-02 2008-01-09 哈尔滨工业大学 Method for preparing thin film by using magnetron sputtering
CN102094183A (en) * 2010-12-22 2011-06-15 中国工程物理研究院激光聚变研究中心 Cold-wall batch reactor
CN104498880A (en) * 2014-12-16 2015-04-08 中国科学院长春光学精密机械与物理研究所 Method for preparing large-area high-quality thick aluminum film by adopting discontinuous coevaporation for multiple times
CN107043914A (en) * 2017-04-21 2017-08-15 武汉理工大学 A kind of batch (-type) magnetically controlled DC sputtering preparation method of amorphous cobalt based magnetic thin film
CN111118472A (en) * 2020-01-07 2020-05-08 山东理工大学 Preparation method of silicon carbide film continuous carbon fiber plate

Patent Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0529227A (en) * 1991-07-17 1993-02-05 Canon Inc Deposited film formation method
JP2000282224A (en) * 1999-03-29 2000-10-10 Sumitomo Heavy Ind Ltd Device and method for film formation
JP2001026885A (en) * 1999-07-16 2001-01-30 Meiku:Kk Thin film forming device
CN1636077A (en) * 2002-02-21 2005-07-06 科鲁斯技术有限公司 Method and device for coating a substrate
CN2832828Y (en) * 2005-10-27 2006-11-01 北京实力源科技开发有限责任公司 Vacuum coating system
CN101100739A (en) * 2007-08-02 2008-01-09 哈尔滨工业大学 Method for preparing thin film by using magnetron sputtering
CN102094183A (en) * 2010-12-22 2011-06-15 中国工程物理研究院激光聚变研究中心 Cold-wall batch reactor
CN104498880A (en) * 2014-12-16 2015-04-08 中国科学院长春光学精密机械与物理研究所 Method for preparing large-area high-quality thick aluminum film by adopting discontinuous coevaporation for multiple times
CN107043914A (en) * 2017-04-21 2017-08-15 武汉理工大学 A kind of batch (-type) magnetically controlled DC sputtering preparation method of amorphous cobalt based magnetic thin film
CN111118472A (en) * 2020-01-07 2020-05-08 山东理工大学 Preparation method of silicon carbide film continuous carbon fiber plate

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Y OKUHARA ET AL.: "Near-infrared reflection from Al-doped ZnO films prepared by multi-target reactive sputtering", 《MATERIALS SCIENCE AND ENGINEERING》 *
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