WO2010069594A1 - Procédé et dispositif pour revêtir des objets au moyen d'un plasma basse pression - Google Patents

Procédé et dispositif pour revêtir des objets au moyen d'un plasma basse pression Download PDF

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Publication number
WO2010069594A1
WO2010069594A1 PCT/EP2009/009150 EP2009009150W WO2010069594A1 WO 2010069594 A1 WO2010069594 A1 WO 2010069594A1 EP 2009009150 W EP2009009150 W EP 2009009150W WO 2010069594 A1 WO2010069594 A1 WO 2010069594A1
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WO
WIPO (PCT)
Prior art keywords
plasma
zone
activation
activation zone
dissipation
Prior art date
Application number
PCT/EP2009/009150
Other languages
German (de)
English (en)
Inventor
Thomas Jung
Original Assignee
Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V.
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 Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. filed Critical Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V.
Publication of WO2010069594A1 publication Critical patent/WO2010069594A1/fr

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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
    • 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
    • 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
    • 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
    • H01J37/32431—Constructional details of the reactor
    • H01J37/32532—Electrodes
    • H01J37/32596—Hollow cathodes

Definitions

  • the present invention relates to a novel process for coating substrates, in which the vapor of a precursor in the form of a coating material is activated in an activation zone and guided towards the substrate, and the activation is carried out by a glow discharge plasma generated between the generated plasma, which forms a plasma zone, and the activation zone at least one dissipation zone for reducing the energy of the plasma is arranged.
  • precursors By activating gaseous precursors (precursors) in a low-pressure glow discharge, thin layers with technically useful properties can be produced.
  • precursors mostly low molecular weight hydrocarbons (for example methane or ethyne) are used and also organosilicon compounds, in particular tetramethylsilane (TMS) and hexamethyldisiloxane (HMDSO) or organometallic compounds.
  • TMS tetramethylsilane
  • HMDSO hexamethyldisiloxane
  • the layers produced contain carbon, hydrogen, silicon or certain metals as well as nitrogen or oxygen. With less high degree of crosslinking of the molecules in the layer, this is referred to as plasma polymer layers. Highly crosslinked carbon-rich layers are called DLC (diamond-like carbon).
  • a disadvantage of all these methods is that the precursor molecules are always decomposed by the action of the plasma into very small components. Accordingly, the resulting layers are extremely highly networked and essentially inorganic in nature. Although such layers are often very hard and chemically resistant, important properties but the precursor is often lost. For example, the ductility is very low (elongation at elongation of usually less than 1%, ie similar to a ceramic) and specific optical properties (eg the spectral absorption) change greatly.
  • the object of the invention is to provide a method and a device for producing from gaseous, liquid or solid precursors a layer on an object, referred to below as substrate, which has the molecules of the precursor in little or moderately altered, in particular not very fragmented Contains form so that essential properties of the precursor are retained and the layer has primarily organic or organosilicon character.
  • the vapor of the precursor be activated in at least one so-called activation zone by means of a plasma generated by at least one plasma electrode and forming at least one plasma zone. It is essential that at least one dissipation zone is interposed between the at least one plasma zone and the at least one activation zone in order to reduce the energy of the plasma. By this measure it is achieved that instead of a plasma only certain particles which are contained in or arise in a plasma are used. These are preferably free electrons.
  • the plasma is generated by a glow discharge, preferably by a hollow cathode glow discharge.
  • the plasma is essentially formed by free electrons and ions. The excitation for this can be done by DC voltage, pulsed DC voltage, low, medium or high frequency AC voltage or by micro waves.
  • DC or AC voltage applied to the plasma electrode and the counter electrode, e.g. the anode is applied is in the range of 20 V to 2000 V.
  • a glow discharge for generating the plasma consist in the fact that, in contrast to many other gas discharges, a glow discharge has a sufficiently high plasma density and, in contrast to the arc discharge, can expand very uniformly to a large volume, which is great for the uniform coating Surfaces is very important.
  • glow discharges can be switched on and off stably in a very short time, which is very advantageous for discontinuous coating processes, for example in the case of repeated coating of individual objects.
  • the plasma as described above forms at least one so-called plasma zone.
  • the free electrons which are in particular movable in the at least one plasma zone are now conducted into the activation zone via a so-called dissipation zone.
  • the purpose of the dissipation zone is that, as the free electrons pass through the dissipation zone, there is a decrease in energy.
  • the formation of the length of the dissipation zone can be such that, at the working pressure prevailing in the dissipation zone, the energy of the electrons in the following activation zone is substantially less than 8 eV, preferably less than 3 eV.
  • Another essential feature of the invention consists in the fact that this so-called dissipation zone is arranged and designed such that the free electrons passing through it are conducted directly into the at least one activation zone.
  • Activations in the invention are understood here as follows: formation of radicals, ionization, conversion into a chemical compound with high chemical reactivity. It is essential that it is possible by this method, from gaseous, liquid or solid precursors to produce a layer on the substrate containing the molecules of the precursor in little or moderately altered, in particular not highly fragmented form, so that essential properties of the precursor and the layer has primarily organic or organosilicon character.
  • the working pressure in the at least one activation zone is advantageously 0.01 to 100 mbar, preferably 0.1 to 10 mbar.
  • the electrons forming the plasma are guided essentially transversely to the direction of the precursor direction within the at least one activation zone.
  • the electrons forming the plasma can be guided within the at least one activation zone essentially parallel to the direction of the precursor device. This embodiment then has the advantage that the electrons can also be conducted in the same or opposite direction to the precursor flow, thereby producing intensive contact with the precursor vapor.
  • the vapor of the precursor which is guided through the activation zone in the direction of the substrate, is produced by bringing the precursor to a temperature at which it has a sufficient vapor pressure for a sufficiently rapid coating.
  • the percursor is heated in an evaporator.
  • Precursors from the groups of the alkanes, alkenes, alkynes, arenes, cycloalkanes, terpenes or silanes or compounds derived therefrom are suitable in the process according to the invention, as are precursors from the groups of the organic compounds which contain an inorganic radical.
  • the precursor vapor can also consist of several different precursor substances.
  • the process according to the invention also opens up the possibility of influencing the activation of the precursor vapor and the layer formation by introducing at least one reactive gas, which is introduced into the activation zone, for example hydrogen, oxygen or nitrogen.
  • a reactive gas can also be in the plasma zone, where it is then activated directly in the plasma and from where it then flows into the activation zone, are supplied. Further influencing the activation of the precursor grain and the layer formation can take place in that particles are removed by cathode sputtering from an electrode of the plasma zone and guided into the activation zone by means of gas flow.
  • a purge gas can be passed through the plasma zone in the direction of the activation zone which limits the diffusion of the precursor vapor into the plasma zone.
  • the surroundings of the anode can also be kept free from the precursor vapor by a purge gas.
  • the anode can be formed, for example, as a hollow anode.
  • the preferred purge gas is an inert gas, e.g. Argon, used.
  • the at least one dissipation zone and / or the activation zone and / or the plasma zone are delimited by a housing.
  • a housing encloses the activation zone has the advantage that a device is provided here can be used, which serves for heating, so that a reduction of the condensation of precursor vapor occurs.
  • An increase in the activation rate of the precursor vapor can also be achieved by supplying heat to the activation zone.
  • the anode disposed inside or at the edge of the activation zone to be heated by the incident electrons or by means of heating.
  • the method described above is particularly suitable for coating organic substrates, substrates of metal, glass, plastic, for the production of barrier layers, anti-corrosion layers, wear protection layers, scratch protection layers, in particular of plastic and for the production of organic layers with defined electrical conductivity and for the production of organic Layers with specific spectral absorptivity.
  • the invention further relates to a device for coating substrates with a coating material by means of a plasma in a vacuum chamber, wherein at least one plasma electrode, at least one counter electrode and at least one storage container for the precursor Be Schweizerungsma- material is arranged in the vacuum chamber.
  • the device according to the invention is particularly characterized in that the at least one storage vessel is designed and positioned such that the vapor of the precursor can be guided onto the substrate via at least one activation zone and the at least one plasma electrode specifies a plasma zone, wherein the at least one plasma zone is so designed and arranged that between the at least one activity administratungszone and the at least one plasma zone is present at least one dissipation zone.
  • An advantageous embodiment of the invention proposes for this purpose that the at least one dissipation zone and / or the at least one activation zone and / or the at least one plasma zone is enclosed by a housing. This then defines the corresponding zones, ie the at least one plasma zone, the at least one activation zone and the at least one dissipation zone.
  • the activation zone it is also possible for the activation zone to be delimited by a housing, which in addition also encloses the substrate in its extension.
  • the housing of the at least one activation zone is designed such that it ends in front of the substrate and has an outflow opening.
  • This outlet opening of the housing which delimits the at least one activation zone, may be e.g. be formed in the form of a slot for coating large-area substrates, preferably in conjunction with a mutually relative movement of the slot and the substrate.
  • the extent is 0.1 to 3 m, preferably 0.3 to 1 m.
  • the formation of the activation zone is carried out as a uniformly uniform region in one direction for the simultaneous coating of large areas, the direction being parallel or approximately parallel to the substrate surface.
  • the extent is also here 0.1 to 3 m, preferably 0.3 to 1 m.
  • the formation of the plasma zone, the dissipation zone and the activation zone can also be used as a uniformly uniform area in one direction for the same time. be provided coating of large areas, wherein the direction is parallel or approximately parallel to the substrate surface.
  • the expansion is 0.1 to 5 m, preferably 0.5 to 2 m.
  • the arrangement of several plasma zones and activation zones is also possible side by side in one direction, ie linear, or in two directions, ie flat, for the simultaneous and uniform coating of large areas.
  • the at least one plasma electrode is preferably formed as a hollow cathode.
  • the at least one plasma zone and the at least one dissipation zone may also have the form of a largely isotropic prism.
  • the at least one plasma and dissipation zone is approximately in the form of an anisotropic rectangle in a plane which is perpendicular to the main direction of movement of the electrons.
  • FIG. 2 shows the schematic structure of a device according to the invention, wherein here a housing is provided which simultaneously encloses the substrate, 3 shows an embodiment of the device according to the invention, in which case a hollow cathode is provided,
  • FIG. 4 shows a further embodiment according to the invention, in which the plasma zone is connected to the activation zone via an angle of dissipation zone,
  • FIG. 5 shows a device in which the electrons move in the activation zone substantially transversely to the flow direction of the precursor vapor.
  • a counter electrode 11 which is operated as an anode, is arranged relative to the activation zone 5 with respect to the dispersion zone 4 and has a planar shape, for example in the form of a plate, of parallel bars or a network.
  • the plasma electrodes 10 define a plasma zone 3 which is arranged in a plane with the dissipation zone 4.
  • the substrate is denoted by 1 and the coating produced by 2.
  • the electrons from the plasma of the glow discharge pass through the dissipation zone 4, where they release some of their energy by collisions with the gas particles and then traverse on their way to the anode 11 the activation zone 5, where they meet with the molecules of precursor vapor and thereby activate this vapor.
  • the precursor is denoted by 7 and the evaporator by 6.
  • the arrangement and design of the evaporator 6 is selected such that the vapor of the precursor 7 in the gasket leads to the substrate 1 through the activation zone 4.
  • the anode 11 is located on the side of the dissipation zone 4.
  • the electrons are moved in the dissipation zone 4 by the electric field formed by the plasma 3 and the anode 11 in the activation zone 5, where they interact with the molecules meet the precursor vapor and thereby activate this vapor.
  • the activation zone 5 and the dissipation zone 4 as well as the plasma zone 3 are surrounded by a housing 12. With 2, the coating is designated.
  • a preferably inert purging gas for example argon, can be introduced through the purging gas inlet 13, which impedes the propagation of the precursor vapor into these zones as a result of the flow that thereby arises in the region of the electrodes 10, 11 and the dissipation zone, thereby preventing these zones from undesired changes.
  • argon a preferably inert purging gas, for example argon
  • a reactive gas can additionally or alternatively be admitted, which is activated in the plasma zone 3, flows from there into the activation zone 5 and there advantageously influences the activation of the precursor vapor or chemically reacts with it.
  • the substrate 1 is located within the housing 12 of the activation zone 5 in an area of expanded cross-section. For all-round coating, the substrate 1 is rotated during the coating.
  • the plasma electrode 10 is formed as a hollow cathode.
  • a particularly high plasma density and correspondingly a large electron current can thus be generated towards the activation zone 5.
  • the anode 11 is here of the same type as the cathode 10. This simplifies the construction of the device. In addition, when applying an AC voltage anode 10 and cathode 11 can be reversed periodically. This achieves a particularly uniform activation. Furthermore, the generation of undesirable changes to the electrodes 10, 11, i. at the anode and cathode, such as deposits or material removal impeded and avoided excessive heating of the electrodes.
  • a purge gas and additionally or alternatively a reactive gas can be introduced through the purge gas inlets 13.
  • the cathode surface can be removed by ion sputtering in this device.
  • this cathode material is added to the precursor vapor in the form of atoms or clusters and thus also passes into the layer. This material can also cause chemical reactions in activation and in the Influence layer formation and thereby advantageously change the layer properties.
  • the apparatus of Figure 3 may be formed so that the plasma zones 3 and the dissipation zones 4 are in the form of a substantially isotropic prism, i. for example, with approximately circular or approximately square cross-section, wherein the prism axis perpendicular to the axis of the activation zone 5, which also has a substantially isotropic shape.
  • this device can also be designed such that the plasma zones 3 and the dissipation zones 4 have approximately the shape of a strongly anisotropic rectangle in a plane which is perpendicular to the main movement direction of the electrons.
  • the junction of dissipation zone 4 and activation zone 5 then has the shape of a slot.
  • the substrate-side outlet opening of the activation zone has the shape of a slot having a width of, for example, 0.5 cm or 4 cm and a length of, for example, 20 cm or 80 cm. It is therefore a line source with a length of 20 cm or 80 cm.
  • the drawing in FIG. 3 corresponds to a cross-sectional drawing, wherein the same cross-sectional drawing results in any parallel planes in the region of the linear extension of the device.
  • the anode 11 is also formed as a hollow electrode.
  • this form is advantageous because the electron flow in this case is relatively uniform on the electrode surface. sharing and avoiding excessive local warming.
  • the plasma zone 3 is arranged so that only a very small part of the photons produced in the plasma can reach the activation zone 5. As a result, unwanted photochemical reactions can be prevented.
  • this device has inflow openings 14 for a further vapor or a reactive gas, which is added to the precursor vapor 8 only after it has already left the activation zone.
  • the evaporator 6 has two chambers for precursors 7, which can be kept at different temperatures. This makes it possible to simultaneously evaporate two different precursors with given proportions.
  • FIG. 5 shows a device in which the electrons in the activation zone 5, unlike the devices according to FIGS. 1 to 4, do not move substantially transversely to the flow direction of the precursor vapor, but essentially parallel to the flow direction of the precursor vapor, specifically this directed against.
  • a longer path of the electrons through the activation zone 5 can be achieved and thus the probability of activating collisions can be increased.
  • anodes 10, 11 are also arranged on both sides or in a ring around the (cylindrical) activation zone 5.
  • the flushing of the anodes 11, which in turn are formed as hollow electrodes, is carried out by a purge gas, which does not flow through the anodes 11 itself. This makes it easier to design the anodes.
  • Plasma electrode 10 negative pole
  • anode 11 positive pole
  • Plasma of hollow cathode glow discharge activated and then precipitates on the substrate as a very solid layer.
  • the substrate is moved evenly and at a fixed distance laterally to the discharge opening of the activation zone, whereby it is coated over the entire surface after some time.
  • Plasma electrode Setting the pressure in the activation zone to 0.3 mbar.
  • Plasma of hollow cathode glow discharge activated and then precipitates on the substrate as a very dense barrier layer. 7.
  • the substrate is rotated evenly around its own axis.
  • the vacuum chamber is vented and the substrate removed.

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

Abstract

La présente invention concerne un nouveau procédé de revêtement de substrats, selon lequel la vapeur d'une matière de revêtement présente sous la forme d'un précurseur est activée dans une zone d'activation et guidée en direction du substrat. L'activation se fait par l'intermédiaire d'un plasma généré par décharge luminescente, au moins une zone de dissipation destinée à réduire l'énergie du plasma étant disposée entre le plasma généré, lequel forme une zone de plasma, et la zone d'activation.
PCT/EP2009/009150 2008-12-19 2009-12-18 Procédé et dispositif pour revêtir des objets au moyen d'un plasma basse pression WO2010069594A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102008064134.0 2008-12-19
DE102008064134.0A DE102008064134B4 (de) 2008-12-19 2008-12-19 Verfahren zur Beschichtung von Gegenständen mittels eines Niederdruckplasmas

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WO2010069594A1 true WO2010069594A1 (fr) 2010-06-24

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Cited By (5)

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Publication number Priority date Publication date Assignee Title
EP2431995A1 (fr) * 2010-09-17 2012-03-21 Asociacion de la Industria Navarra (AIN) Dispositif d'ionisation
WO2013045596A3 (fr) * 2011-09-29 2013-08-08 Morgan Advanced Materials Plc Matériaux inorganiques, procédés et appareil pour leur fabrication, et leurs utilisations
WO2014063970A3 (fr) * 2012-10-25 2014-07-24 Nitride Solutions, Inc. Matières stratifiées, procédés et appareil pour leur réalisation et leur utilisations
US9856577B2 (en) 2013-09-04 2018-01-02 Nitride Solutions, Inc. Bulk diffusion crystal growth of nitride crystal
US20180023185A1 (en) * 2014-10-20 2018-01-25 Universidade Federal De Santa Catarina Plasma Process and Reactor for the Thermochemical Treatment of the Surface of Metallic Pieces

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DE102010039939B4 (de) 2010-08-30 2015-01-08 Aktiebolaget Skf Verfahren zur Haftbeschichtung eines metallischen Substrats, Beschichtung für eine metallische Oberfläche und Verwendung des beschichteten Substrats als Dichtung

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Publication number Priority date Publication date Assignee Title
EP2431995A1 (fr) * 2010-09-17 2012-03-21 Asociacion de la Industria Navarra (AIN) Dispositif d'ionisation
WO2013045596A3 (fr) * 2011-09-29 2013-08-08 Morgan Advanced Materials Plc Matériaux inorganiques, procédés et appareil pour leur fabrication, et leurs utilisations
CN104040675A (zh) * 2011-09-29 2014-09-10 氮化物处理股份有限公司 无机材料、制作其的方法和装置、及其使用
JP2015501372A (ja) * 2011-09-29 2015-01-15 ナイトライド ソリューションズ インコーポレイテッド 無機材料、それを作製する方法及び装置、並びにその使用
WO2014063970A3 (fr) * 2012-10-25 2014-07-24 Nitride Solutions, Inc. Matières stratifiées, procédés et appareil pour leur réalisation et leur utilisations
US9856577B2 (en) 2013-09-04 2018-01-02 Nitride Solutions, Inc. Bulk diffusion crystal growth of nitride crystal
US20180023185A1 (en) * 2014-10-20 2018-01-25 Universidade Federal De Santa Catarina Plasma Process and Reactor for the Thermochemical Treatment of the Surface of Metallic Pieces

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DE102008064134B4 (de) 2016-07-21

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