CN110331385A - A kind of low temperature chemical vapor deposition device for thin tube inner wall plated film - Google Patents

A kind of low temperature chemical vapor deposition device for thin tube inner wall plated film Download PDF

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Publication number
CN110331385A
CN110331385A CN201910586736.4A CN201910586736A CN110331385A CN 110331385 A CN110331385 A CN 110331385A CN 201910586736 A CN201910586736 A CN 201910586736A CN 110331385 A CN110331385 A CN 110331385A
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CN
China
Prior art keywords
tubule
container
vacuum
vacuum chamber
discharge tube
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Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
CN201910586736.4A
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Chinese (zh)
Inventor
张庆瑜
马春雨
苗春雨
石德权
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Dalian University of Technology
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Dalian University of Technology
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Priority to CN201910586736.4A priority Critical patent/CN110331385A/en
Publication of CN110331385A publication Critical patent/CN110331385A/en
Withdrawn legal-status Critical Current

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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
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical 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
    • C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
    • C23C16/34—Nitrides
    • C23C16/345—Silicon nitride
    • 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
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical 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
    • C23C16/458—Chemical 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
    • C23C16/4581—Chemical 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 characterised by material of construction or surface finish of the means for supporting the substrate
    • 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
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical 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
    • C23C16/50—Chemical 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
    • 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
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical 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
    • C23C16/52—Controlling or regulating the coating process

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Plasma & Fusion (AREA)
  • Chemical Vapour Deposition (AREA)

Abstract

The invention belongs to field of film preparation, it is related to a kind of low temperature chemical vapor deposition device for thin tube inner wall plated film, including plasma discharge electrode, vacuum insulation sealing device, discharge tube, two air inlet pipe, tubule container, tubule receptacle fixture, vacuum displacement control device and vacuum chamber.Plasma discharge electrode is fixed on vacuum insulation sealing device, is placed in discharge tube, and discharge tube is connected with air inlet pipe；Gas needed for plasma discharge is passed through by air inlet pipe, the tubule container of inner wall plated film is needed to be fixed in tubule receptacle fixture, the relative motion between discharge tube and tubule container is realized by vacuum displacement control device, and the inner wall coating process of tubule container is completed in vacuum chamber.The present invention realizes the low temperature chemical vapor deposition of tubule container inner wall by tubulose plasma discharge；It by the relative motion between discharge tube and container, solves the uniformity of inside pipe wall plated film, realizes the low-temperature epitaxy of film, minimum temperature can be to room temperature.

Description

A kind of low temperature chemical vapor deposition device for thin tube inner wall plated film
Technical field
The invention belongs to technical field of film preparation, are related to a kind of low temperature chemical vapor deposition for thin tube inner wall plated film Device.
Background technique
Container inner wall plated film has extensive demand.For example, the container of various high molecular polymer materials is in medicine, food Equal fields have a wide range of applications, but these are poor to the barrier property of polymeric material confrontation gas, so that its internal solution is easy Rotten, the shelf-life is short.In addition, the problem that the container of various glass materials is undesirable there is also hydrophobicity.Therefore, it is necessary at these Container inner wall deposits layer protecting film on surface.But due to tubule bore is small and draw ratio is big etc., current various films Technology of preparing is all difficult to realize the uniform coated of thin tube inner wall.The present invention utilizes capillary discharge method, has invented a kind of for thin The low temperature chemical vapor deposition technology of inside pipe wall plated film can pass through low temperature chemical vapor deposition inside the tubule of a variety of substrates Prepare various compound films.
Summary of the invention
In view of the problems of the existing technology, it is heavy to provide a kind of low temperature chemical vapor for thin tube inner wall plated film by the present invention Product device.
The technical solution adopted by the present invention are as follows:
A kind of low temperature chemical vapor deposition device for thin tube inner wall plated film, the low temperature chemical vapor deposition device include 3, two plasma discharge electrode 1, vacuum insulation sealing device 2, discharge tube air inlet pipe, tubule container 6, tubule container are fixed Device 7, vacuum displacement control device 8 and vacuum chamber 9.
The plasma discharge electrode 1 is fixed on vacuum insulation sealing device 2, and plasma discharge electrode 1 is deep Enter in discharge tube 3.The plasma discharge electrode 1 is made by metal material, including stainless steel, tungsten, molybdenum, titanium, tantalum Deng diameter is between 0.1~5mm, and length is between 10~500mm.
The vacuum insulation sealing device 2 is fixed on 9 lower surface of vacuum chamber, is connect by vacuum flange with vacuum chamber 9. Vacuum insulation sealing device 2 is made of metal to ceramic sealing part and insulating materials, and metal to ceramic sealing part is put for plasma Electrode 1 is connected with vacuum flange, plays sealing and power conduction, and insulating materials is used for plasma discharge electrode 1 and vacuum Insulation between room 9, including polytetrafluoroethylene (PTFE), oxide ceramics, quartz glass.
The discharge tube 3 is vertical in vacuum chamber 9, and 3 bottom end of discharge tube is connect with plasma discharge electrode 1, is put 3 top of fulgurite is corresponding with 6 mouthfuls of tubule container；3 top of discharge tube is connected to air inlet pipe B5, and lower part is connected to air inlet pipe A4, air inlet Pipe A4, B5 pass through 9 side wall of vacuum chamber and communicate with the outside world, and for being passed through gas needed for plasma discharge, i.e. air inlet pipe A4, B5 is used In the distribution of film deposition process.The discharge tube 3 is made by insulating materials, and insulating materials includes quartz, glass and ceramics Pipe etc., internal diameter is between 1~100mm, and length is between 10~1000mm.
The tubule container 6 for needing inner wall plated film is fixed in tubule receptacle fixture 7, the fixed dress of tubule container 7 are set to connect with vacuum displacement control device 8.Wherein, the inner wall coating process of tubule container 6 is completed in vacuum chamber 9.
The tubule receptacle fixture 7 for plating film container needed for fixed, according to specific container geometry and Size production, needs vessel port and the outlet of discharge tube 3 is staggered relatively.
The vacuum displacement control device 8 is set to and is fixed on 9 upper surface of vacuum chamber.Vacuum displacement control device 8 includes Driving shaft is transmitted axis, interior magnet rotor, outer magnet rotor and isolating seal set, by isolating seal therein set and vacuum chamber 9 Surface connection.The driving shaft and outer magnet rotor are set to outside vacuum chamber 9, are connected to the motor, described to be transmitted axis, interior magnet rotor Inside vacuum chamber 9, it is connect wherein being transmitted axis with tubule container 6.Motor drives outer magnet rotor to rotate by driving shaft, leads to The magneticaction for crossing permanent magnet generation is transmitted motion to and is transmitted on the interior magnet rotor that axis is connected, and realizes power transmitting Purpose, and then realize that tubule container 6 rotates, i.e., it is realized between discharge tube 3 and tubule container 6 by vacuum displacement control device 8 Relative motion.
Use process of the invention are as follows: vacuum chamber 9 is evacuated to 0.1Pa~5Pa, is passed through respectively by air inlet pipe A4, B5 Gas needed for plasma discharge, 1~50sccm of flow needed for regulating gas adjust electric discharge air pressure 1Pa~50Pa, make plasma Body discharge electrode 1 generates plasma discharge by connecting plasma discharge power supply at a given pressure, is discharged by control The preparation of thin tube inner wall film needed for parameter, gaseous species and ratio are realized, by between control discharge tube 3 and tubule container 6 Distance and speed of related movement, realize 6 inner wall membrane of tubule container low temperature chemical vapor deposition preparation.
Beneficial effects of the present invention: the present invention realizes the low temperature of tubule container inner wall by tubulose plasma discharge Vapor deposition is learned, by the relative motion between discharge tube and container, the uniformity of inside pipe wall plated film is solved, realizes film Low-temperature epitaxy, minimum temperature can be to room temperature.
Detailed description of the invention
Fig. 1 is the schematic diagram of thin tube inner wall low temperature chemical vapor deposition technology of the invention.
In figure: 1 plasma discharge electrode；2 vacuum insulation sealing devices；3 discharge tubes；4 air inlet pipe A；5 air inlet pipe B；6 Tubule container；7 tubule receptacle fixtures；8 vacuum displacement control devices；9 vacuum chambers.
Specific embodiment
Below in conjunction with attached drawing and technical solution, a specific embodiment of the invention is further illustrated.
As shown in Figure 1, plasma discharge electrode 1 is generated at a given pressure by connecting plasma discharge power supply Plasma discharge, the preparation of film needed for being realized by control discharge parameter, gaseous species and ratio, by controlling discharge tube 3 The distance between tubule container 6 and speed of related movement realize the low temperature chemical vapor deposition system of 6 inner wall membrane of tubule container It is standby.
Embodiment 1:
The structure and composition of this embodiment is as shown in Figure 1.Vacuum chamber 9 is evacuated to 3Pa.Plasma discharge electrode 1 For stainless steel, diameter 2mm, long 50mm.Vacuum insulation sealing device 2 is the metal flange of ceramic seal, diameter 150mm.Electric discharge Pipe 3 is internal diameter 4mm double-layer quartz glass tube, long 250mm.The PVC hose that air inlet pipe A4 and B5 are internal diameter 6mm passes through vacuum valve point Not about SiH4And N2Gas cylinder connection.Tubule container 6 is 10ml control injection medicament vial, internal diameter~10mm.SiH4And N2Stream Amount is 12sccm, adjusts electric discharge air pressure 20Pa.Plasma discharge is driven using the AC power source of 25kHz, discharge power 100W, deposition rate 100nm/min, prepared film clarity are greater than 90%.
Embodiment described above only expresses embodiments of the present invention, and but it cannot be understood as to the invention patent Range limitation, it is noted that for those skilled in the art, without departing from the inventive concept of the premise, also Several modifications and improvements can be made, these are all belonged to the scope of protection of the present invention.

Claims (5)

1. a kind of low temperature chemical vapor deposition device for thin tube inner wall plated film, which is characterized in that the cryochemistry gas Phase precipitation equipment includes plasma discharge electrode (1), vacuum insulation sealing device (2), discharge tube (3), two air inlet pipe, carefully Tubular container (6), tubule receptacle fixture (7), vacuum displacement control device (8) and vacuum chamber (9)；
The plasma discharge electrode (1) is fixed on vacuum insulation sealing device (2), plasma discharge electrode (1) Go deep into discharge tube (3)；The plasma discharge electrode (1) is made by metal material；
The vacuum insulation sealing device (2) is fixed on vacuum chamber (9) lower surface, is connected by vacuum flange and vacuum chamber (9) It connects；Vacuum insulation sealing device (2) is made of metal to ceramic sealing part and insulating materials, and metal to ceramic sealing part is used for plasma Body discharge electrode (1) is connected with vacuum flange, plays sealing and power conduction, and insulating materials is used for plasma discharge electrode (1) insulation between vacuum chamber (9)；
The discharge tube (3) is vertical in vacuum chamber (9), and discharge tube (3) bottom end and plasma discharge electrode (1) are even It connects, discharge tube (3) top is corresponding with tubule container (6) mouth；Discharge tube (3) top is connected to air inlet pipe B5, lower part and air inlet pipe A4 connection, air inlet pipe A4, B5 pass through vacuum chamber (9) side wall and communicate with the outside world, and air inlet pipe A4, B5 is matched for film deposition process Gas；The discharge tube (3) is made by insulating materials；
The tubule container (6) for needing inner wall plated film is fixed on tubule receptacle fixture (7), wherein tubular container 6 Vessel port and the outlet of discharge tube (3) are staggered relatively；Wherein, the inner wall coating process of tubule container (6) is complete in vacuum chamber (9) At；
The tubule receptacle fixture (7) is connect with vacuum displacement control device (8), and vacuum displacement control device (8) is set In being fixed on vacuum chamber (9) upper surface；It drives tubule container (6) mobile by vacuum displacement control device (8), and then realizes and put Relative motion between fulgurite (3) and tubule container (6).
2. a kind of low temperature chemical vapor deposition device for thin tube inner wall plated film according to claim 1, feature exist In the plasma discharge electrode (1) includes stainless steel, tungsten, molybdenum, titanium, tantalum, and diameter is long between 0.1~5mm Degree is between 10~500mm.
3. a kind of low temperature chemical vapor deposition device for thin tube inner wall plated film according to claim 1, feature exist In the insulating materials includes polytetrafluoroethylene (PTFE), oxide ceramics, quartz glass.
4. a kind of low temperature chemical vapor deposition device for thin tube inner wall plated film according to claim 1, feature exist In, the discharge tube (3) material include quartz, glass and ceramic tube etc., internal diameter between 1~100mm, length 10~ Between 1000mm.
5. a kind of low temperature chemical vapor deposition device for thin tube inner wall plated film according to claim 1, feature exist In the vacuum displacement control device (8) includes driving shaft, is transmitted axis, interior magnet rotor, outer magnet rotor and isolating seal Set, vacuum displacement control device (8) are connect by isolating seal therein set with vacuum chamber (9) upper surface；The driving shaft and Outer magnet rotor is set to vacuum chamber (9) outside, is connected to the motor, and axis, the interior magnet rotor of being transmitted is internal set on vacuum chamber (9), Axis is wherein transmitted to connect with tubule container (6)；Motor drives outer magnet rotor to rotate by driving shaft, is generated by permanent magnet Magneticaction is transmitted motion to and is transmitted on the interior magnet rotor that axis is connected, and realizes the purpose of power transmitting, and then realize Tubule container (6) is mobile.
CN201910586736.4A 2019-07-01 2019-07-01 A kind of low temperature chemical vapor deposition device for thin tube inner wall plated film Withdrawn CN110331385A (en)

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CN201910586736.4A CN110331385A (en) 2019-07-01 2019-07-01 A kind of low temperature chemical vapor deposition device for thin tube inner wall plated film

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Application Number Priority Date Filing Date Title
CN201910586736.4A CN110331385A (en) 2019-07-01 2019-07-01 A kind of low temperature chemical vapor deposition device for thin tube inner wall plated film

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2024060293A1 (en) * 2022-09-20 2024-03-28 湖南千山制药机械股份有限公司 Vacuum outer plating module and integrated forming machine for plastic ampoule

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2006124739A (en) * 2004-10-27 2006-05-18 Toppan Printing Co Ltd Film deposition apparatus by plasma cvd method
CN103649366A (en) * 2011-07-01 2014-03-19 莱茵豪森等离子有限公司 Plasma treatment of hollow bodies
CN205710908U (en) * 2016-04-18 2016-11-23 北京大学 A kind of for the device at lumen wall spraying TiO2 nano coating

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2006124739A (en) * 2004-10-27 2006-05-18 Toppan Printing Co Ltd Film deposition apparatus by plasma cvd method
CN103649366A (en) * 2011-07-01 2014-03-19 莱茵豪森等离子有限公司 Plasma treatment of hollow bodies
CN205710908U (en) * 2016-04-18 2016-11-23 北京大学 A kind of for the device at lumen wall spraying TiO2 nano coating

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2024060293A1 (en) * 2022-09-20 2024-03-28 湖南千山制药机械股份有限公司 Vacuum outer plating module and integrated forming machine for plastic ampoule

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Application publication date: 20191015

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