EP2425035A1 - Procédé et dispositif pour l'enduction à vitesse élevée par évaporation à haute pression - Google Patents

Procédé et dispositif pour l'enduction à vitesse élevée par évaporation à haute pression

Info

Publication number
EP2425035A1
EP2425035A1 EP10716336A EP10716336A EP2425035A1 EP 2425035 A1 EP2425035 A1 EP 2425035A1 EP 10716336 A EP10716336 A EP 10716336A EP 10716336 A EP10716336 A EP 10716336A EP 2425035 A1 EP2425035 A1 EP 2425035A1
Authority
EP
European Patent Office
Prior art keywords
coating
substrate
vapor
evaporator
evaporator source
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Withdrawn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
EP10716336A
Other languages
German (de)
English (en)
Inventor
Werner Prusseit
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.)
Theva Duennschichttechnik GmbH
Original Assignee
Theva Duennschichttechnik 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 Theva Duennschichttechnik GmbH filed Critical Theva Duennschichttechnik GmbH
Publication of EP2425035A1 publication Critical patent/EP2425035A1/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Withdrawn legal-status Critical Current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
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24—Vacuum evaporation
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—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
    • 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
    • C23C16/4485—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 evaporation without using carrier gas in contact with the source material

Definitions

  • the invention encompasses a process for the continuous or pulsed high rate coating of substrates and describes exemplary devices how this process can be implemented.
  • the process represents a form of vacuum deposition which allows very high deposition rates with high layer thickness homogeneity and material yield.
  • coating materials have high chemical reactivity, which allows them to react with atmospheric constituents such as oxygen and water so that they can only be deposited under suitable high vacuum conditions to prevent at least partial oxidation.
  • These materials generally include the elements of the first three main groups of the periodic table, of which aluminum and magnesium are of particularly high technical importance.
  • transition metals of the subgroups or rare earths have a very high affinity for oxygen and have a very high reduction potential in atomic form.
  • inorganic and organic chemical compounds that chemically react and change on contact with oxygen, water vapor or other oxygen-containing agents.
  • the coating material is so strongly heated by energy input that it passes into the vapor phase. According to the state of the art, the heating can take place, for example, by thermal contact with a heated crucible, direct current flow, radiation, induction or an electron beam or arc.
  • the vapor spreads in a high vacuum ( ⁇ 10 "3 Pa) ballistic, since it hardly comes to collision processes with the residual gas due to the large free path.
  • the effective coating rate R at the substrate is inversely proportional to the square of the distance d to the source, ie R oc d ⁇ 2 .
  • the flow is already in the Knudsen flow region and, due to the velocity distribution directed into the upper half-space and the collisions of the vapor molecules, a jet effect occurs the vapor distribution additionally bundles, so that n> 4 is observed.
  • the angular distribution and the requirement for layer thickness homogeneity within a tolerable fluctuation range define the usable angle range. Together with the substrate size, this is followed by the minimum distance that must be maintained between source and substrate. Any material which evaporates into the unacceptable angular range is lost to the coating, reduces the yield and represents an undesirable contamination. The requirement for homogeneity thus runs counter to the high deposition rate and material yield.
  • Coating material which is not initially directed to the substrate surface, backscattered back into the coating area and thus the loss rate is kept low.
  • the space in front of the substrate is designed so that a high vapor pressure can build up, so that the mean free path becomes significantly smaller than the geometric dimensions of the coating chamber and intensive scattering leads to the homogenization of the directional distribution in the vapor.
  • vapor pressures of> 10 Pa and thus average free path lengths in the millimeter range are typically sought. This can be achieved at least briefly by pulsed evaporation of a desired amount of material.
  • the published patent application DE 1 621 271 relates to a process for surface metallization of a body by condensation of a metal vaporized in a vacuum.
  • the invention relates to a process for producing a vapor from a coating metal, the vapor being free of particles trapped in the coating metal.
  • US 4 022 928 discloses coating a surface with a perfluoropolyether compound. This prevents that vaporous material can settle on these surfaces in a vacuum.
  • the perfluoropolyether protective layer may be applied by evaporation, spraying or spin coating in vacuum or atmospheric conditions, or may be applied by a fluid or a thixotropic paste by means of, for example, a printing process.
  • EP 0 795 890 A2 discloses a sputtering device for reactive coatings of substrates, wherein the electrical power supplied to the sputtering electrode oscillates between two values.
  • the two power values are chosen such that, with the same reactive gas flow, the target of the sputtering electrode is in the metallic mode at the first power value, while it is in oxidic mode at the second power value.
  • DE 101 53 760 A1 relates to a process for the production of UV-absorbing transparent abrasion protective layers by vacuum coating, in which simultaneously or immediately successively at least one inorganic compound which forms layers with high abrasion resistance and an inorganic compound which forms layers with high UV Absorption, which are each deposited by reactive or partially reactive plasma-enhanced high-rate vapor deposition on a substrate.
  • this is achieved in that the coating takes place within a kind of pressure chamber in the high vacuum chamber.
  • the volume within this pressure chamber defines the coating space.
  • the apparatus for high rate evaporation in a high vacuum comprises a substantially closed coating space, which is fed by at least one evaporator source with the vapor of a coating material.
  • the coating space is at least one side through the to be coated - 4 -
  • the term "substantially closed” in this context therefore means that the total cross section of all openings of the coating chamber through which the steam escapes can amount to less than 10% of the coating surface of the substrate and all surfaces which are not to be coated must be made such in that the vapor can not condense on them and is scattered back into the coating space.
  • a steam generator which transfers the coating material from the solid or liquid state into the coating space
  • Possibilities for evaporation are well known in the art, eg heating by radiation, current flow, electric arc, electron beam or electromagnetic alternating fields
  • the heated walls constitute a hot half space in front of the substrate, whose radiation represents an additional heat input to the substrate. Therefore, it must be estimated in each case whether this heat input is tolerable or, if necessary, has to be dissipated via an active substrate cooling.
  • the more expedient and elegant solution to the problem is an anti-stick coating which prevents the condensation or adhesion of the coating material even at low temperatures.
  • Such anti-adhesion coatings are known, for example, from US Pat. No. 4,022,928.
  • PFPE long-chain perfluoropolyethers
  • the vapor pressure should be below 10 Pa.
  • all anti-adhesive coated surfaces are actively cooled.
  • the coating material condenses substantially only on the substrate surface, which is the only sink of material in the coating space without contaminating the walls. This ensures a very high material yield and low contamination of surrounding parts.
  • the loss of material corresponds to the area ratio of parasitically coated parts and openings to the substrate surface.
  • the dynamic vapor pressure profile in the coating chamber can be calculated classically as with any gas flow by material inflow (source) and outflow (condensation on the substrate).
  • the upper limit of the pressure in the coating room is given by the vapor pressure at the source temperature. This can easily be in the range of 10 - 100 Pa.
  • the condensation rate on the substrate naturally also depends on its temperature. Typically, the substrate is significantly colder than the evaporator source. As the rate of condensation increases exponentially with the temperature differential, the substrate is a very effective sink of material and, in effect, sucks the material out of the coating space like a sponge.
  • a vapor pressure level> 10 Pa can be maintained within the coating space for at least a short time, which is several orders of magnitude higher than that of the surrounding vacuum and enables extremely high vapor condensation rates> 100 nm / s on the substrate.
  • the entire amount of material required for the coating is vaporized.
  • These are particularly suitable, for example, arc discharges, electromagnetic high-frequency or laser pulses, or a modulated electron beam.
  • the coating material must be tracked in this case again and again. If the material source consists of a continuously operating effusion cell, it can be periodically opened and closed by a cover in order to realize timed operation. However, in this case, similar measures (heating, anti-stick coating) as in the chamber walls must be taken to prevent evaporation of the lid.
  • the method is a real high-vacuum coating, because the residual gas pressure in the system is less than 10 "3 Pa 1 Be Anlagenung ⁇ raum is filled during the coating phase with a relatively dense cloud of steam. Because of the frequent collisions of the vapor molecules with each other and with the walls, the original direction information is at Emission from the source is lost very rapidly and there is a largely isotropic directional distribution in the vapor, the layer thickness variations across the substrate surface are correspondingly lower, and within the coating space, diaphragms or screens can be used to guide the vapor and / or protect the substrate and / or For example, a screen can be used to prevent material on the direct line of sight from the source to the substrate (see Fig.
  • FIG. 1 Schematic structure of the arrangement for high-pressure evaporation
  • Fig. 2 high-pressure evaporator with shielding to hide the direct
  • Fig. 1 shows a schematic diagram of the high-pressure evaporator.
  • the coating space (1) is bounded by walls (2) and at least on one side by the substrate (4) to be coated.
  • This arrangement can be located within a high vacuum chamber which can be pumped down to a suitable background pressure ⁇ 10 -3 Pa by suitable pumps so that there are only traces of oxygen or water vapor in the chamber prior to coating
  • Connected to this is at least one evaporation source (3) which converts the coating material into the vapor phase All surfaces which are not to be coated must have a very low adhesion coefficient for the vapor.
  • the condensation can be prevented by tempering these surfaces so that the vapor pressure is higher there than in the coating space.
  • magnesium is to be deposited as a metal on a semiconductor substrate as an electrically conductive contacting layer.
  • the walls of the coating chamber (2) are held by means of heating elements (5) at a temperature above 550 0 C, while the temperature of the substrate does not rise above 250 0 C during the process.
  • the magnesium vapor separates virtually quantitatively on the substrate surface.
  • the walls are not coated.
  • most of the technically interesting metals such as aluminum, chromium, copper or precious metals have a vapor pressure> 10 Pa only at temperatures above 1000 ° C. In these cases, heating the walls is impractical. It is therefore advisable to reduce the coefficient of adhesion by an anti-adhesion coating. Suitable coatings exist - 9 -
  • the wall temperature control (5) can therefore also be cooling elements, e.g. act water-carrying lines.
  • the wall material (2) should in this case consist of a material that conducts the heat well. Preference is given to materials having a heat conduction coefficient ⁇ > 80 W / (m-K), such as aluminum, copper and alloys of these metals.
  • Apertures may be in any geometric shapes, e.g. be designed as perforated plates. Since they are not to be coated, they are like the chamber wall depending on the litigation with a heater or with an anti-adhesive layer and a cooling (not shown) provided.
  • the evaporation sources should preferably be located within the coating space or be connected directly to the coating space. In order to ensure long-term operation, these evaporators must either have a large volume of material, or be charged from the outside. Some preferred configurations are described below by way of example. 3 shows a commercially available, heated effusion cell with a limited material volume (7), which is flanged directly onto the coating space. It is kept at high temperature and releases the material with high vapor pressure. In order to realize a pulsed operation, the hot effusion cell (7) can be opened and closed with a cover (8). In order to avoid the coating of the lid, this must be kept as the chamber walls or umbrellas at high temperature or provided with an anti-adhesive layer. - 1 0 -
  • an arc evaporator (9), the electrodes of which can be tracked.
  • the coating material is introduced in the form of two wires or rods (10) through sockets in the chamber wall into the coating space, which are brought together close to a narrow slit.
  • a flashover is ignited at the base of which electrode material evaporates and thus generates a conductive gas channel. This allows a high current flow between the electrodes and the resulting arc ensures a uniform evaporation of the electrode material.
  • the electrodes (10) are tracked until the desired amount of material has been evaporated and the arc is extinguished, for example by interrupting the power supply or increasing the distance between the electrodes.
  • the material is selectively heated by the current flow at the tip of the electrodes and evaporated very efficiently.
  • FIG. Another exemplary arrangement is shown in FIG.
  • the coating material (11) is supplied through a bush in the wall of the coating room.
  • a power-controlled, high-energy laser or electron beam (12) is used, which is generated outside the coating space and is directed onto the coating material through the smallest possible opening in the chamber wall. In this arrangement too, pulsed operation is possible by modulating the beam power.
  • Another embodiment of the invention is an apparatus for high rate vapor deposition comprising a substantially closed coating space fed by at least one evaporator source with the vapor of a coating material, characterized in that a) the coating space is bounded at least on one side by the substrate b) the total cross section of all openings of the coating space is less than 10% of the coating area of the substrate, c) all surfaces which are not to be coated are such that the vapor on them can not condense d) and the effective condensation rate on the substrate > 10 ⁇ m / s device according to Example 1, characterized in that all surfaces on which the condensation of the steam is to be prevented, either suitably tempered or provided with an anti-stick coating device according to one of Examples 1 to 2, characterized in that the anti-adhesion coating consists of a perfluoropolyether whose vapor pressure at room temperature below 10 "5 Pa device according to one of Examples 1 to 3, characterized in that the provided with the anti-adhesive layer surfaces are actively cooled device according to one of Examples
  • Seconds preferably in less than ten seconds, for the - 1 2 -
  • Coating necessary amount of material is evaporated, so that a short-cycle operation is made possible.
  • Device according to one of Examples 1 to 7, characterized in that the evaporator contains a refillable material supply, which is evaporated by means of a power-controlled laser or electron beam.
  • a method for Hochratenampfampfung in a high vacuum characterized in that a) the coating takes place within a substantially closed coating space, which by at least one

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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)
  • General Chemical & Material Sciences (AREA)
  • Physical Vapour Deposition (AREA)

Abstract

L'invention décrit un procédé d'enduction sous vide avec des taux de précipitation très élevés avec homogénéité élevée de l'épaisseur de couche et rendement de matériau élevé et des dispositifs pour la réalisation de l'enduction. Afin de résoudre la contradiction existant avec l'évaporation sous vide classique entre l'homogénéité d'épaisseur de couche d'une part et le rendement en matériau et le taux d'enduction d'autre part, le substrat forme la délimitation d'un espace de revêtement sensiblement fermé, qui est alimenté par une source d'évaporation. Les parois de cet espace d'induction ainsi que toutes les surfaces qui ne doivent pas être enduites sont soit mises à température soit dotées d'une couche antiadhésive, de sorte que la vapeur ne peut pas se condenser dessus et est redispersée dans l'espace d'enduction. De ce fait, il s'établit une pression de vapeur très élevée dans l'espace d'enduction, qui entraîne un taux de condensation très élevé sur le substrat et une homogénéisation de l'épaisseur de couche. Comme le substrat est la seule surface sur laquelle la vapeur peut se condenser, il ne se perd guère de matériau et le rendement est extrêmement élevé. Le fonctionnement pulsé de la source d'évaporateur permet de réaliser une enduction à cycle court.
EP10716336A 2009-04-29 2010-04-27 Procédé et dispositif pour l'enduction à vitesse élevée par évaporation à haute pression Withdrawn EP2425035A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102009019146.1A DE102009019146B4 (de) 2009-04-29 2009-04-29 Verfahren und Vorrichtung zur Hochratenbeschichtung durch Hochdruckverdampfen
PCT/EP2010/055633 WO2010133426A1 (fr) 2009-04-29 2010-04-27 Procédé et dispositif pour l'enduction à vitesse élevée par évaporation à haute pression

Publications (1)

Publication Number Publication Date
EP2425035A1 true EP2425035A1 (fr) 2012-03-07

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ID=42309491

Family Applications (1)

Application Number Title Priority Date Filing Date
EP10716336A Withdrawn EP2425035A1 (fr) 2009-04-29 2010-04-27 Procédé et dispositif pour l'enduction à vitesse élevée par évaporation à haute pression

Country Status (6)

Country Link
US (1) US20120088038A1 (fr)
EP (1) EP2425035A1 (fr)
JP (1) JP2012525495A (fr)
CN (1) CN102421930B (fr)
DE (1) DE102009019146B4 (fr)
WO (1) WO2010133426A1 (fr)

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KR20140136594A (ko) * 2013-05-20 2014-12-01 삼성전자주식회사 배기 장치 및 이를 구비하는 박막 증착 설비
DE102013108411B4 (de) * 2013-08-05 2017-08-24 Von Ardenne Gmbh Durchlauf-Substratbehandlungsanlage
DE102013108403B4 (de) * 2013-08-05 2017-08-24 Von Ardenne Gmbh Durchlauf-Substratbehandlungsanlage
DE102013109663A1 (de) * 2013-09-04 2015-03-05 Fhr Anlagenbau Gmbh Bedampfungseinrichtung zum Beschichten flächenförmiger Substrate
US9857027B2 (en) * 2014-07-03 2018-01-02 Applied Materials, Inc. Apparatus and method for self-regulating fluid chemical delivery
CN104233228A (zh) * 2014-07-18 2014-12-24 许昌学院 一种全自动非接触式真空镀膜方法与设备
EP3786311A1 (fr) * 2019-08-30 2021-03-03 Theva Dünnschichttechnik GmbH Dispositif, procédé et système de revêtement d'un substrat, en particulier d'un conduite de bande supraconductive ainsi que conduite supraconductive revêtue

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Also Published As

Publication number Publication date
US20120088038A1 (en) 2012-04-12
WO2010133426A1 (fr) 2010-11-25
DE102009019146B4 (de) 2014-07-24
JP2012525495A (ja) 2012-10-22
CN102421930A (zh) 2012-04-18
DE102009019146A1 (de) 2010-11-11
CN102421930B (zh) 2014-02-12

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