WO2012164050A1 - Dispositif et procédé de dépôt et/ou d'enlèvement d'un matériau au moyen d'un dépôt chimique en phase vapeur assisté par plasma/d'une gravure chimique sèche - Google Patents

Dispositif et procédé de dépôt et/ou d'enlèvement d'un matériau au moyen d'un dépôt chimique en phase vapeur assisté par plasma/d'une gravure chimique sèche Download PDF

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Publication number
WO2012164050A1
WO2012164050A1 PCT/EP2012/060318 EP2012060318W WO2012164050A1 WO 2012164050 A1 WO2012164050 A1 WO 2012164050A1 EP 2012060318 W EP2012060318 W EP 2012060318W WO 2012164050 A1 WO2012164050 A1 WO 2012164050A1
Authority
WO
WIPO (PCT)
Prior art keywords
workpiece
electrode
chamber
high frequency
feed points
Prior art date
Application number
PCT/EP2012/060318
Other languages
German (de)
English (en)
Inventor
Dirk REINER
Original Assignee
Surcoatec Ag
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 Surcoatec Ag filed Critical Surcoatec Ag
Publication of WO2012164050A1 publication Critical patent/WO2012164050A1/fr

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Classifications

    • 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
    • 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
    • H01J37/32082—Radio frequency generated discharge
    • 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
    • H01J37/32403—Treating multiple sides of workpieces, e.g. 3D workpieces
    • 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
    • H01J37/32577—Electrical connecting means

Definitions

  • the invention is based on a device for coating at least one
  • the device has a chamber containing a high-frequency electrode (RF electrode), a reference electrode and an electrically conductive
  • Workpiece holder includes and a circuit arrangement for feeding
  • High frequency in turn, at least one high-frequency generator and
  • High-frequency line paths is electrically connected to spatially separate feed points of the high-frequency electrode.
  • the invention further starts from a corresponding method for coating at least one surface area and / or for removing material from a surface area of an arbitrarily shaped workpiece by means of plasma-assisted chemical vapor deposition.
  • ion etching and plasma etching (CDE: Chemical Dry Etching) known.
  • CDE Chemical Dry Etching
  • a workpiece is placed in a vacuum chamber and fixed there.
  • the chamber is evacuated to a residual gas pressure in the high vacuum or ultrahigh vacuum range and an inert working gas admitted.
  • an RF field via an RF electrode arranged in the vacuum chamber, a low-pressure plasma is then ignited.
  • an ionized gas is generated, which contains a noteworthy proportion of fast-moving free charge carriers such as ions or electrons.
  • reaction gases are fed into the chamber, which in particular can contain carbon or silicon.
  • the electrons have such high energies that chemical reactions between the gas components and components of the surface of the workpiece are possible, which are not possible in thermal equilibrium.
  • layers are formed on the surface of the workpiece which, depending on the reaction gas, e.g. can consist of carbon or silicon oxide.
  • the reaction gas e.g. can consist of carbon or silicon oxide.
  • DLC diamond-like carbon coatings
  • ion etching and plasma etching are about removing material from the surface
  • the ions of the low-pressure plasma generated must have a certain minimum energy.
  • the acceleration of argon ions in high or ultra-high vacuum in the direction of the substrate to be machined, resulting in the impulse transmission of the In plasma etching, the etching is also carried out by a chemical reaction in which instead of pure argon, a reactive gas such as oxygen is supplied to the plasma.
  • the object of the present invention is to provide a device and a method for
  • the workpiece holder is electrically conductively connected to the high-frequency electrode having the plurality of feed points.
  • a device is a in the chamber
  • the reference electrode with the mostly constant electrical potential is - apart from electrical conduction via charge carriers of the plasma - electrically isolated from the workpiece.
  • Alternating field can be generated in the region of the workpiece. Due to the different feed points on the same RF electrode, an at least temporary formation of this plasma in inaccessible surface areas, such as cavities formed as recesses is achieved. Workpiece holder and RF electrode can also be integrally formed.
  • high-frequency generators RF or RF generators
  • RF or RF generators often have three or six different high-frequency outputs, so that a corresponding number of injection points on the
  • High frequency electrode is preferred.
  • the high-frequency electrode is formed flat.
  • the feed points are formed distributed over the corresponding area, so are arranged to each other objectionable.
  • the feed points are arranged linearly.
  • the feed points are arranged on an imaginary, over the surface centrally extending straight spaced from each other.
  • Circuit arrangement is arranged such that it can feed high frequency sequentially in the individual feed-points. This sequential feeding results in a temporal sequence of the feed-in location, in particular a feed-in cycle. If, for example, three linearly arranged feed points are provided, which are designated in succession from one side starting with a, b and c, the result is a preferred wiring in the sequence... B, c, b, a, b, ... in which there is a back and forth movement of the entry point with regard to the (imaginary) straight line.
  • a feed-in cycle If, for example, three linearly arranged feed points are provided, which are designated in succession from one side starting with a, b and c, the result is a preferred wiring in the sequence... B, c, b, a, b, ... in which there is a back and forth movement of the entry point with regard to the (imaginary) straight line.
  • Circuit arrangement at least one matching circuit part for impedance matching of the RF feed.
  • a matching circuit part is conventional
  • circuits are known, for example, as the circuit of a matching unit (or “match box"), the corresponding matching circuit part being associated with a specific HF electrode Trimming capacitor preferred embodiment of the invention, the circuit arrangement has one each
  • Circuit part are capacitively coupled. This coupling is in particular by means of RC elements, more preferably by means of series connections of resistors and
  • Capacitors realized.
  • the coupling can avoid harmful feedbacks via the respective non-active feed-in points. Such feedbacks would interfere with operation and could damage the circuitry.
  • High frequency electrode has. This results in several possibilities of electrical connection of the workpiece to the RF electrode.
  • the chamber has electrically conductive inner walls which form an interior of the chamber and at the same time form the reference electrode or at least form part of the reference electrode.
  • the arrangement of the electrodes consists only of the
  • Interior forming inner walls, which forms the reference electrode, and -elektrisch isolated thereof-the RF electrode in the interior.
  • the coating is carried out by means of a device mentioned above.
  • the surface area to be coated or the surface area in the material to be removed, a surface area in at least one cavity of the workpiece.
  • the invention thus encompasses the use of an abovementioned device for coating at least one surface area and / or for Removal of material from a surface area of a workpiece, in particular from a surface area in at least one cavity of the workpiece.
  • an alternating field with very high field strengths can be generated in the chamber, as is necessary for the formation of the cavity plasma.
  • An alternating field generated in this way has a sufficiently high penetration depth, so that even hollow bodies with large wall thicknesses can be penetrated and coated on the inside.
  • the workpiece itself does not have to function as an electrode and can therefore also consist of a non-metallic material.
  • the method comprises the following method steps:
  • a gas lance is preferred for workpieces designed as cavities
  • the gas lance protrudes preferably into the cavity of the Workpiece into it.
  • the hollow body to be coated is not earthed or provided with any other reference potential.
  • the workpiece may be formed in particular as a hollow body.
  • hollow bodies to be coated in principle all possible hollow bodies are possible, ie hollow bodies closed on one side (such as vessels, cans etc.) as well as tubular hollow bodies without bottom, such as e.g. Cannulas, bodies with a through-hole or tubes.
  • the latter hollow bodies must be closed with a lid or stopper on one side before coating.
  • the minimum distance between the outer wall of the workpiece and the inner wall of the chamber is 15 cm.
  • the maximum distance is, however, by the
  • the working gas is a gas selected from the group comprising argon, helium, hydrogen, oxygen or another noble gas.
  • reaction gas is a gas selected from the group containing oxygen.
  • Material removal is also referred to as plasma etching.
  • a reaction gas for this Oxygen is particularly suitable method, since the oxygen ions produced in the plasma are particularly heavy and therefore particularly effective in the accelerated state
  • the reaction gas is a gas selected from the group comprising hydrocarbon gases such as methane, ethane, ethene, ethyne, propane or silane gases such as tetramethylsilane or hexamethyldisiloxane are suitable for forming a DLC layer, the latter, for example, suitable for forming a SiCV layer.
  • DLC diamond-like carbon
  • the ratio of the two variants depends on the coating conditions. If the former predominates, the coating has graphite-like properties (low coefficient of friction), the latter predominate, the hardness and the transparency of the coating increase. Mixed coatings containing both variants often combine both advantages.
  • the plasma is preferably ignited by applying a high-frequency field with the following parameters:
  • the frequency is preferably in the range of 10 - 15 MHz. Particular preference is the frequency 13.56 MHz (RF, radio frequency).
  • Power (watts) area to be coated (m 2 ) x 1750.
  • the latter factor can be between 1500 and 2200 and is empirically determined in practice. A hollow body with an inner surface of 0.85 m 2 to be coated would therefore have to be coated with an energy of about 1500 watts.
  • the bias voltage which occurs under these circumstances is in the range of 0V, namely on all supply lines. Moreover, this value is independent of whether the hollow body to be coated is in electrically conductive contact with the high-frequency electrode or not.
  • the gas supply is regulated gas-specific and depending on the object and desired
  • Layer properties controlled in a range of 0-90 sccm It is preferably provided that the amount of reaction gas for the coating to be introduced amounts to 0.1 to 10 sccm reaction gas per 10 cm 2 of internal surface to be coated.
  • the unit sccm denotes standard cubic centimeters, ie the volume of the gas to be introduced in cubic centimeters per minute (minute volume).
  • a valve with a mass flow controller is used. At a given pressure of the gas supply so decides the opening state of the valve on the inflowing minute volume.
  • hydrocarbon gases the more gas is used, the harder the layer becomes, as the proportion of available carbon atoms increases.
  • silane gases on the other hand, the ratio of silane gas to oxygen determines the hardness of the layer.
  • the ratio is 100 sccm of HMDSO (hexamethyldisiloxane) to 400 sccm of oxygen. A reduction of the oxygen content, however, leads to softer layers.
  • the amount of the reaction gas to be introduced is 0.5-5 sccm of reaction gas per 10 cm 2 of internal surface to be coated.
  • the reaction gas is doped with one or more gases containing Si, N, F, B, O, Ag, Cu, V or Ti. These dopants can help to specifically influence the properties of the applied coating.
  • the doping of the reaction gas with a gas containing Si e.g.
  • Hexamthyldisiloxan to reduce friction even under wet conditions and to a higher thermal stability.
  • Doping with N, F, B, or O affects the surface tension, wettability, and hardness of the coating.
  • Doping with metals helps to affect the conductivity of the coating, while doping with Ag, Cu, V or Ti affects the biological behavior of the coating, particularly biocompatibility, e.g. is enormous important for implants.
  • a hollow body having an inner surface which is characterized in that the latter has been treated by a method according to one of the preceding claims, such that on the inner surface a
  • the coating can be, for example, a DLC, a TiOx or a SiO 2 bond direction.
  • this hollow body is a hollow body selected from the group comprising vessels, bottles, cans, cannulas, hollow needles, syringes, inner walls of cylinder or piston bores in internal combustion engines, inner sides of bearings, in particular ball or roller bearings.
  • FIG. 1 shows an apparatus 10 for coating at least one surface area and / or for removing material from at least one surface area of a workpiece 12 by means of plasma-assisted chemical vapor deposition PECVD or plasma etching (CDE).
  • the device 10 has a vacuum chamber designed as a chamber 14, which is shown in Fig. 1 in a sectional view.
  • the chamber 14 forms with its inner walls 16 an inner space 18 which can be evacuated.
  • a high-frequency electrode (HF electrode) 22 which is electrically insulated from the inner walls 16 by means of insulators 20 is arranged.
  • a workpiece holder 24 made of metal, on which in turn is held to be coated workpiece 12.
  • This workpiece 12 is formed as a hollow body with a recess formed as a blind hole 26 recess.
  • This cavity 26 is formed by a hard surface area 28 of the workpiece 12 formed by the inner wall of the hollow body.
  • the workpiece 12 is positioned spaced from the inner walls 16. Namely, the inner walls 16 at the same time form a reference electrode 29 of the device and carry as electrical reference potential e.g. Ground potential.
  • the device 10 further comprises a circuit arrangement 30 for feeding high-frequency signals or high-frequency voltage.
  • a circuit arrangement 30 for feeding high-frequency signals or high-frequency voltage.
  • Circuit arrangement 30 at least one high-frequency generator 32, at least one matching circuit part 34 for impedance matching in a matching unit ("match box") and a plurality of high-frequency line paths 36, 38, 40.
  • the high-frequency generator 32 is on the High-frequency line paths 36, 38, 40 at spatially separate feed points 42, 44, 46 (or a, b, c) of the high-frequency electrode 22 connected.
  • the individual high frequency paths 36, 38, 40 to the feed points 42, 44, 46th be controlled separately to produce a homogeneous alternating field with uniformly high field strengths in the entire chamber.
  • the high-frequency line paths 36, 38, 40 to the feed points 42, 44, 46 are capacitive in the region of the matching circuit part 34,
  • the circuit arrangement 30 is set up for feeding the high-frequency voltage in succession into the individual feed-in points 42, 44, 46 of the HF-electrode, in particular by means of RC elements (not shown).
  • Such a successive feeding of the high frequency into the individual feed points 42, 44, 46 of the HF electrode 22 produces a spatially varying plasma in the region of the workpiece 22.
  • This plasma also extends into the cavity 26 of the workpiece 12 or 12 formed as a hollow body even forms preferentially in this cavity.
  • Fig. 2 shows the rough circuit diagram of the circuit arrangement 30 with the
  • High frequency generator 32 one of the three matching circuit parts 34 with
  • Trim capacitors the interconnection of the three high-frequency line paths 36, 38, 40 and a supply line to the reference electrode 29, which is in the embodiment at ground potential (or neutral potential).
  • the capacitive coupling of the matching circuit parts 34 with each other is not shown, since only one matching circuit parts 34 is shown.

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  • Physics & Mathematics (AREA)
  • Engineering & Computer Science (AREA)
  • Plasma & Fusion (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Vapour Deposition (AREA)

Abstract

L'invention concerne un dispositif (10) de dépôt d'au moins une zone superficielle (28) et/ou d'enlèvement d'un matériau d'au moins une zone superficielle (28) d'une pièce de forme quelconque (22) au moyen d'un dépôt chimique en phase vapeur assisté par plasma. Ledit dispositif est doté d'une chambre (14) comportant une électrode haute fréquence (22), une électrode de référence (29) et un porte-pièce (24) électroconducteur et est doté également d'un circuit (30) destiné à injecter une haute fréquence et comportant au moins un générateur de haute fréquence (32) et des trajets de conduction haute fréquence (36, 38, 40). Le générateur de haute fréquence (32) est connecté à des points d'injection (42, 44, 46) spatialement séparés les uns des autres de l'électrode haute fréquence (22) par l'intermédiaire des trajets de conduction haute fréquence (36, 38, 40). L'électrode haute fréquence (22) est connectée de manière électroconductrice au porte-pièce (24) au moyen de la pluralité de points d'injection (42, 44, 46).
PCT/EP2012/060318 2011-05-31 2012-05-31 Dispositif et procédé de dépôt et/ou d'enlèvement d'un matériau au moyen d'un dépôt chimique en phase vapeur assisté par plasma/d'une gravure chimique sèche WO2012164050A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102011103706 2011-05-31
DE102011103706.7 2011-05-31

Publications (1)

Publication Number Publication Date
WO2012164050A1 true WO2012164050A1 (fr) 2012-12-06

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PCT/EP2012/060318 WO2012164050A1 (fr) 2011-05-31 2012-05-31 Dispositif et procédé de dépôt et/ou d'enlèvement d'un matériau au moyen d'un dépôt chimique en phase vapeur assisté par plasma/d'une gravure chimique sèche

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3821815A1 (de) * 1988-06-29 1990-01-04 Battelle Institut E V Vorrichtung zur beschichtung eines laenglichen innenraums eines hohlkoerpers mit einer diamantartigen, harten kohlenstoffbeschichtung mit hilfe eines plasmagestuetzten cvd-verfahrens
DE4242894A1 (de) * 1992-12-18 1994-06-23 Leybold Ag Vorrichtung zur Mehrfacheinspeisung von HF-Leistung in Kathodenkörpern
JPH08236294A (ja) * 1995-02-28 1996-09-13 Jeol Ltd 高周波プラズマ応用装置
US20040168770A1 (en) 2000-08-08 2004-09-02 Tokyo Electron Limited Method and apparatus for improved plasma processing uniformity
EP2041332B1 (fr) * 2006-07-12 2011-03-02 Stein, Ralf Procédé et dispositif de séparation chimique en phase gazeuse assistée par plasma sur la paroi intérieure d'un corps creux

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3821815A1 (de) * 1988-06-29 1990-01-04 Battelle Institut E V Vorrichtung zur beschichtung eines laenglichen innenraums eines hohlkoerpers mit einer diamantartigen, harten kohlenstoffbeschichtung mit hilfe eines plasmagestuetzten cvd-verfahrens
DE4242894A1 (de) * 1992-12-18 1994-06-23 Leybold Ag Vorrichtung zur Mehrfacheinspeisung von HF-Leistung in Kathodenkörpern
JPH08236294A (ja) * 1995-02-28 1996-09-13 Jeol Ltd 高周波プラズマ応用装置
US20040168770A1 (en) 2000-08-08 2004-09-02 Tokyo Electron Limited Method and apparatus for improved plasma processing uniformity
EP2041332B1 (fr) * 2006-07-12 2011-03-02 Stein, Ralf Procédé et dispositif de séparation chimique en phase gazeuse assistée par plasma sur la paroi intérieure d'un corps creux

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