EP2726643A1 - Traitement de corps creux par plasma - Google Patents

Traitement de corps creux par plasma

Info

Publication number
EP2726643A1
EP2726643A1 EP12725436.5A EP12725436A EP2726643A1 EP 2726643 A1 EP2726643 A1 EP 2726643A1 EP 12725436 A EP12725436 A EP 12725436A EP 2726643 A1 EP2726643 A1 EP 2726643A1
Authority
EP
European Patent Office
Prior art keywords
plasma
hollow body
source
guide
process chamber
Prior art date
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Withdrawn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
EP12725436.5A
Other languages
German (de)
English (en)
Inventor
Stefan Nettesheim
Dariusz Korzec
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Relyon Plasma GmbH
Original Assignee
Reinhausen Plasma GmbH
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Reinhausen Plasma GmbH filed Critical Reinhausen Plasma GmbH
Publication of EP2726643A1 publication Critical patent/EP2726643A1/fr
Withdrawn legal-status Critical Current

Links

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
    • 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
    • C23C16/04—Coating on selected surface areas, e.g. using masks
    • C23C16/045—Coating cavities or hollow spaces, e.g. interior of tubes; Infiltration of porous substrates
    • 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
    • C23C16/448—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 generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials
    • C23C16/452—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 generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials by activating reactive gas streams before their introduction into the reaction chamber, e.g. by ionisation or addition of reactive species
    • 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
    • C23C16/515—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 using pulsed discharges
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/32—Gas-filled discharge tubes
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/32—Gas-filled discharge tubes
    • H01J37/32009—Arrangements for generation of plasma specially adapted for examination or treatment of objects, e.g. plasma sources
    • H01J37/32357—Generation remote from the workpiece, e.g. down-stream
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/32—Gas-filled discharge tubes
    • H01J37/32009—Arrangements for generation of plasma specially adapted for examination or treatment of objects, e.g. plasma sources
    • H01J37/32394—Treating interior parts of workpieces

Definitions

  • the present invention relates to an apparatus and a method for the plasma treatment of hollow bodies.
  • the invention is suitable for gentle plasma treatment of the inner surface of thermally sensitive hollow bodies such as plastic bottles.
  • the plasma treatment may consist, for example, of chemical activation, sterilization, purification or coating.
  • one or more hollow bodies are placed in a process chamber.
  • the process chamber is in fluid communication with at least one plasma source.
  • a suction device on the process chamber generates a negative pressure in the process chamber with respect to the plasma source, so that plasma can expand from the plasma source into the process chamber and the hollow body.
  • the invention is particularly suitable for the cleaning and further processing of bottles. If the bottles are to contain medicines or drinks intended for consumption, cleaning prior to filling must comply with strict hygiene criteria.
  • Plastic bottles such as PET have the advantage of being light and unbreakable.
  • glasses such as silicon dioxide
  • Multilayer systems combine the advantages of different materials. A prerequisite for this is a good adhesion between the layers, even under thermal, mechanical or chemical stress, as is the case with repeated cleaning cycles of refillable bottles.
  • a PET bottle can be provided from the inside with a glass layer and / or with a UH-absorbing layer.
  • Another example is the selective modification of the polymer structure on the inside surface of a plastic bottle.
  • the German patent application DE 1020080371 59 A1 describes a device for the treatment of hollow bodies comprising a Unterdruckbehand- treatment chamber and means for generating the plasma.
  • the plasma is in the Produced hollow body.
  • the energy required for plasma generation comes from an electric field between a U-shaped electrode outside the hollow body and a tubular electrode, which protrudes into the hollow body and also acts as a supply of a process gas into the hollow body.
  • International patent application WO 2005/099320 A2 discloses a method and a device for generating a low-pressure plasma, in which a plasma is sucked through a non-adjustable plasma nozzle through a negative pressure into a low-pressure chamber.
  • the invention also relates to various applications of low-pressure plasma for surface treatment, for surface coating or for treating gases.
  • European Patent EP 0 887 437 B1 discloses a method of depositing an adhesive coating on the surface of a substrate by plasma deposition. It involves forming an oxygen-containing plasma by a DC arc plasma generator, injecting a reactant gas into the plasma outside the plasma generator, directing the plasma into a vacuum chamber through a divergent nozzle injector connecting the plasma generator and the vacuum chamber. Thereby, reactive species formed from the oxygen and the reactant gas contacts the surface of the substrate for a sufficient period of time to form an adhesive coating.
  • the plasma generator is called a cascade-shaped arc plasma burner.
  • the mentioned layer systems include inter alia the silicon oxide deposition
  • HMDSO Hexamethyldisiloxane
  • US Patent US 5,853,815A discloses an apparatus for plasma assisted coating of flat substrates.
  • a static plasma expands from a plasma gun located inside a pressure chamber.
  • the plasma in the plasma gun a powder can be supplied by the plasma is changed and mixed with it to achieve a uniform distribution or coating on the workpiece to be machined.
  • International Patent Application WO 95/22413 A1 discloses methods and devices for creating inert or impermeable inner surfaces of vessels, in particular of plastic, as well as their coating with polymers.
  • the vessels to be treated are placed in a vacuum chamber.
  • One supply line for each process gas can be inserted into each vessel.
  • the process gas can be ignited within the vessels by applying a voltage between electrodes, which are outside of the vessels, or microwave irradiation to a plasma.
  • the voltage may be a DC voltage or a high frequency AC voltage.
  • one or more coating materials or process gases may be supplied to the process gas.
  • a sequence controller controls the process sequence of the coating process by driving vacuum valves to create a vacuum in the vacuum chamber, controlling process gas supply to the vessels, and finally driving a plasma generator connected to the electrodes. It is not described that the plasma is generated exclusively outside the vessel, nor by what means or measures it the vessel, in particular controlled, is supplied.
  • the invention has for its object to develop a device for efficient, gentle and complete cleaning and / or treatment of the inner surface of one or more hollow bodies.
  • the device according to the invention for the plasma treatment of hollow bodies comprises a process chamber for receiving at least one hollow body to be treated. Furthermore, it comprises at least one plasma source for generating a plasma.
  • An energy source supplies the plasma source with the necessary energy to plasma-process a process gas.
  • the energy source may be, for example, a voltage source, a radiation source (eg a microwave source) or a heat source.
  • At least one suction device adjusts a pressure difference between the plasma source and the process chamber.
  • the at least one plasma source is arranged outside the process chamber and is in fluid communication with it. About a control unit, the energy source is regulated so that a pulsating plasma can be generated.
  • each plasma guide carries a respective first metering unit for metering the influx of plasma into the respective hollow body.
  • Both the opening of the chamber, via which the plasma source is in fluid communication with it, and the outlet of the plasma guide can be designed as a nozzle or atomizer to mix the plasma and any substances contained therein homogeneously distributed and / or a directed To modulate plasma jet.
  • the plasma guide is preferably designed and arranged such that, when immersed in the hollow body, a circumferentially clear opening surface is formed along the opening of the hollow body.
  • This clear opening area thus establishes fluid communication of the hollow body with the process chamber. At the same time, it is a flow impedance for gas and / or plasma flowing out of the hollow body.
  • an overpressure in the hollow body can be set relative to the process chamber.
  • an overpressure in the hollow body can be set relative to the process chamber.
  • the outlet of the plasma guide can be suitably positioned.
  • the device according to the invention can be extended for coating or chemical treatment by a feed line to the inflow of a process material, which opens into the plasma guide.
  • the mouth of the supply line in the plasma guide can be designed as a nozzle or atomizer to distribute the process material evenly in the plasma.
  • the supply line to the inflow of the process material may be a second
  • the first and second metering units may also be controllable such that the influx of process material in time and amount is tunable to the influx of plasma.
  • the control unit required for this purpose can be, for example, a computer or microcontroller which activates the dosing devices coordinated with each other over time and in terms of quantity via an interface.
  • Some processes require the process material to be in a suitable state of aggregation, grain size or chemical state.
  • the tunable controller has the advantage that the process material can chemically react or be atomized completely with the plasma before contact with the inner surface of the hollow body.
  • the invention discloses a method for the plasma treatment of hollow bodies.
  • the device described above is suitable for this method. It is characterized by the following steps:
  • At least one hollow body is introduced and arranged in a process chamber.
  • a suction device sets a negative pressure in the process chamber with respect to at least one plasma source.
  • the parameter range in which the vacuum can be set depends on the effective pump power and the flow impedances.
  • the flow impedances include the opening of the process chamber, the first and second dosing unit, the plasma guide and its outlet, the hollow body and the clear opening area between the opening of the hollow body and the plasma guide. Then we generate a pulsed plasma in the plasma source.
  • the plasma can be advantageously ignited and generated at atmospheric pressure or higher.
  • This plasma is introduced into each hollow body by a respective plasma guide. Due to the negative pressure in the process chamber and thus also in the hollow body with respect to the plasma source, the plasma of higher pressure (in the plasma source) to a plasma of lower pressure (in the process chamber and the hollow body), also called low-pressure plasma.
  • the influx of plasma can be controlled via a metering unit in such a way that a pulsed plasma is uniformly distributed in each hollow body.
  • the effective heat output of the plasma can be regulated or adjusted to the hollow body.
  • a plasma source according to the invention can be supplied with energy from a voltage source.
  • the pulse of the plasma can additionally be modulated by the voltage source outputs voltage pulses.
  • the voltage pulses may be DC pulses having fixed or variable values for pulse duration, pulse interval and / or magnitude of the voltage.
  • the heat output, the thermal and / or electrostatic load can be adjusted by the plasma on the hollow body.
  • An extension of the method according to the invention provides to carry out a coating or chemical reaction with one or more constituents or reaction products of process gas and / or a process material, a polymerization or a preceding or subsequent cleaning of the inner surface of the hollow body with the plasma.
  • the invention particularly aims at hollow bodies, such as plastic bottles, which are intended for holding foods, drinks or medicines.
  • the downstream cleaning step must therefore clean the inner surface of the bottles of residual coating or polymerizing material and other contaminants in accordance with the relevant hygiene standards.
  • the process material can be introduced via a feed line leading into the plasma guide.
  • the first dosing unit and a second dosing unit for Dosing of the process material may be controlled to tune the flow of process material in time and amount to the influx of plasma.
  • a process gas may also be supplied at least temporarily between the pulses of plasma supplied by the hollow bodies. As a result, the heat generated by the plasma treatment is dissipated.
  • the inflow of the process gas for such cooling of the hollow body can be regulated via the first and / or second metering unit. Although reducing the flow of such a cooling gas reduces the cooling capacity, but allows the process at lower average pressure.
  • the process material can according to the invention consist of a carrier gas which carries an active substance in the form of vapor or mist or suspension.
  • the plasma can be adjusted so that the active substances are distributed and evaporated or sublimated in a targeted manner.
  • constituents of the active substance, the process gas or the hollow body can chemically react with one another. Which chemical reactions can take place can be adjusted by the nature of the plasma (eg plasma power, plasma pulsing, degree of ionization, gas, ion and electron temperature).
  • the nature of the plasma may be modulated by coordinately controlling the first metering unit and / or the control unit and the effective pumping power of the suction device.
  • HMDSO hexamethyldisiloxane
  • H 2 0 2 hydrogen peroxide
  • the carrier gas may for example consist of an oxygen-containing, hydrogen-containing or chemically inert gas mixture.
  • FIG. 1 shows a first sectional view through a device according to the invention and a hollow body to be treated
  • FIG. 2 shows a second sectional view through a device according to the invention and a hollow body to be treated.
  • FIG. 1 shows an embodiment of the device 1 according to the invention.
  • a process chamber 20 In a process chamber 20, at least one hollow body 50 to be treated is arranged.
  • a plasma source 10 is arranged outside the process chamber 20. It is in fluid communication with the process chamber 20 via an outlet 12.
  • the outlet 12 can also be designed as a nozzle.
  • the plasma source 10 Via a feed 11, the plasma source 10 can be supplied with a process gas gl.
  • An energy source 30 can ignite a plasma P by applying a voltage to an active electrode 31 against the common ground potential 32 of voltage source 30, plasma source 10 and process chamber 20 from the process gas.
  • the common ground potential 32 avoids electrostatic charging effects or parasitic currents and plasma ignitions.
  • the energy source 30 can output voltage pulses V (t) by means of a control unit 33, so that a pulsed plasma P is formed in the plasma source 10.
  • the process chamber 20 is in fluid communication with a drain device 60, so that a pressure difference Ap (a negative pressure) between the pressure p20 in the pressure chamber 20 against the pressure p10 in the plasma source 10 is generated.
  • the plasma P from the plasma source 10 can by a plasma guide 13 with a preferably designed as a nozzle outlet 14 flow into the hollow body 50 and expand. Due to the expansion, the supplied plasma P2 has a modulated nature with respect to the plasma P in the plasma source 10, in particular a lower pressure.
  • the influx of plasma P can be metered via a metering unit D1 of the plasma supply 1 3 time-precise or completely interrupted.
  • Plasma P2 process gas gl, process materials M or their reaction products can flow out into the process chamber 20 via an opening 52 of the hollow body 50. Due to the uniform expansion of plasma P2 into the hollow body 50 and the uniform outflow from him, the plasma P2 acts evenly on its inner surface 51st
  • a feed 40 for a process material M for coating, cleaning, sterilization, activation or polymerization of the inner surface 51 of the hollow body 50 opens into the plasma guide 13, downstream of the first dosing unit D1.
  • the process material can consist of a carrier gas g2 and an active substance A or an active substance mixture consist.
  • the mouth 41 of the feeder 40 may be designed as a nozzle or as an atomizer for the process material M.
  • a second dosing unit D2 controls the flow of process material M in time and amount.
  • the invention provides for the first and second metering units D1 and D2 and / or the control unit 33 of the voltage source 30 to be timed to one another.
  • the plasma P2 can be modulated (in particular pulsed) and the influx of process material M in time and quantity can be matched to the influx of plasma P2.
  • the plasma guide 13 protrudes through an opening 52 of the hollow body 50 so that the outlet 14 for plasma P2 is inside the hollow body 50. Its immersion depth is a parameter which is used to uniformly distribute plasma P2 over the inner surface 51 of the hollow body. pers 50 is set.
  • a hollow body 50 to be processed has a round opening 52; adapted to this round shape plasma guide 13 in the illustrated embodiment has a round cross-section.
  • the plasma guide 13 has a smaller outer diameter (d1 3) than an inner diameter (d52) of the opening 52 of the hollow body 50.
  • the plasma guide 13 is arranged concentrically to the opening 52 of the hollow body 50.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Plasma & Fusion (AREA)
  • Physics & Mathematics (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Vapour Deposition (AREA)
  • Apparatus For Disinfection Or Sterilisation (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)
  • Spectroscopy & Molecular Physics (AREA)

Abstract

La présente invention concerne un dispositif et un procédé de traitement de corps creux par plasma. L'invention s'applique en particulier au traitement ¨délicat par plasma de la surface intérieure de corps creux thermosensibles comme des bouteilles en matière plastique. Ledit traitement par plasma peut par exemple consister en activation chimique, en stérilisation, en nettoyage ou en revêtement En vue du traitement, un ou plusieurs corps creux sont placés dans une chambre de traitement. ladite chambre de traitement est en communication fluidique avec au moins une source de plasma. Un dispositif d'aspiration présent au niveau de la chambre de traitement produit une dépression dans ladite chambre de traitement par rapport à la source de plasma, de sorte que le plasma provenant de la source de plasma puisse être détendu depuis dans la chambre de traitement et les corps creux.
EP12725436.5A 2011-07-01 2012-06-04 Traitement de corps creux par plasma Withdrawn EP2726643A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102011107836 2011-07-01
PCT/EP2012/060497 WO2013004440A1 (fr) 2011-07-01 2012-06-04 Traitement de corps creux par plasma

Publications (1)

Publication Number Publication Date
EP2726643A1 true EP2726643A1 (fr) 2014-05-07

Family

ID=46208060

Family Applications (1)

Application Number Title Priority Date Filing Date
EP12725436.5A Withdrawn EP2726643A1 (fr) 2011-07-01 2012-06-04 Traitement de corps creux par plasma

Country Status (6)

Country Link
US (1) US20140102639A1 (fr)
EP (1) EP2726643A1 (fr)
JP (1) JP2014526116A (fr)
KR (1) KR20140053144A (fr)
CN (1) CN103649366A (fr)
WO (1) WO2013004440A1 (fr)

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Publication number Priority date Publication date Assignee Title
DE102012107282A1 (de) 2012-01-17 2013-07-18 Reinhausen Plasma Gmbh Vorrichtung und verfahren zur plasmabehandlung von oberflächen
MA40161B1 (fr) * 2014-09-30 2018-12-31 Plasco Energy Group Inc Système de plasma hors équilibre et procédé de raffinage de gaz de synthèse
DE102015121773B4 (de) * 2015-12-14 2019-10-24 Khs Gmbh Verfahren und Vorrichtung zur Plasmabehandlung von Behältern
DE102016101197A1 (de) * 2016-01-25 2017-07-27 Hella Kgaa Hueck & Co. Verfahren zum Oberflächenbeschichten eines Bauteils unter Vakuum und Vakuumbeschichtungsanlage hierzu
DE102016114292A1 (de) 2016-08-02 2018-02-08 Khs Corpoplast Gmbh Verfahren zum Beschichten von Kunststoffbehältern
CN110331385A (zh) * 2019-07-01 2019-10-15 大连理工大学 一种用于细管内壁镀膜的低温化学气相沉积装置
KR20220157958A (ko) * 2020-03-25 2022-11-29 산토리 홀딩스 가부시키가이샤 대기압 리모트 플라즈마 ｃｖｄ 장치, 피막 형성 방법 및 플라스틱병의 제조 방법

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US5308649A (en) * 1992-06-26 1994-05-03 Polar Materials, Inc. Methods for externally treating a container with application of internal bias gas
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Also Published As

Publication number Publication date
KR20140053144A (ko) 2014-05-07
WO2013004440A1 (fr) 2013-01-10
US20140102639A1 (en) 2014-04-17
CN103649366A (zh) 2014-03-19
JP2014526116A (ja) 2014-10-02

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