DE19644153A1 - Multistage low pressure plasma cleaning process - Google Patents

Multistage low pressure plasma cleaning process

Info

Publication number
DE19644153A1
DE19644153A1 DE1996144153 DE19644153A DE19644153A1 DE 19644153 A1 DE19644153 A1 DE 19644153A1 DE 1996144153 DE1996144153 DE 1996144153 DE 19644153 A DE19644153 A DE 19644153A DE 19644153 A1 DE19644153 A1 DE 19644153A1
Authority
DE
Germany
Prior art keywords
carried out
hydrogen
oxygen
low pressure
pressure plasma
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Withdrawn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
DE1996144153
Other languages
German (de)
Inventor
Roland Dr Gesche
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.)
Individual
Original Assignee
Individual
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 Individual filed Critical Individual
Priority to DE1996144153 priority Critical patent/DE19644153A1/en
Publication of DE19644153A1 publication Critical patent/DE19644153A1/en
Withdrawn legal-status Critical Current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
    • C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G5/00—Cleaning or de-greasing metallic material by other methods; Apparatus for cleaning or de-greasing metallic material with organic solvents
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B08—CLEANING
    • B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B7/00—Cleaning by methods not provided for in a single other subclass or a single group in this subclass
    • B08B7/0035—Cleaning by methods not provided for in a single other subclass or a single group in this subclass by radiant energy, e.g. UV, laser, light beam or the like
    • 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
    • C23C14/02—Pretreatment of the material to be coated
    • C23C14/021—Cleaning or etching treatments
    • C23C14/022—Cleaning or etching treatments by means of bombardment with energetic particles or radiation
    • 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
    • C23C16/02—Pretreatment of the material to be coated
    • C23C16/0227—Pretreatment of the material to be coated by cleaning or etching
    • C23C16/0245—Pretreatment of the material to be coated by cleaning or etching by etching with a plasma
    • 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
    • C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
    • C23C4/02—Pretreatment of the material to be coated, e.g. for coating on selected surface areas
    • 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
    • C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C8/02—Pretreatment of the material to be coated

Abstract

In a process and arrangement for low pressure plasma treatment of parts, the process is carried out in several successive steps with different process parameters and process gases. Preferably, the process involves two or more of degreasing (preferably with oxygen or an oxygen-containing process gas), reducing (preferably with hydrogen or a hydrogen-containing process gas) and sputter etching (preferably with argon, another inert gas or an inert gas mixture). A coating or nitriding operation may be carried out immediately after the treatment, without breaking the vacuum.

Description

Gegenstand der Anmeldung, AnwendungsbereicheSubject of registration, areas of application

Die Anmeldung beschreibt eine Anordnung und ein Verfahren zur Reinigung, Ent­ fettung und Aktivierung von Teilen mittels einer Niederdruck-Gasentladung (Plasma). Die Reinigung und Entfettung von Teilen ist in der industriellen Praxis vielfältig erforderlich. Die unterschiedlichen Materialien, Verschmutzungen und An­ forderungen erfordern eine Anpassung der verwendeten Prozesse.The application describes an arrangement and a method for cleaning, ent greasing and activation of parts by means of a low pressure gas discharge (Plasma). The cleaning and degreasing of parts is in industrial practice manifold required. The different materials, soiling and type requirements require an adjustment of the processes used.

Stand der TechnikState of the art

Die Reinigung und Entfettung mittels Plasmaprozessen wird z. B in DE 42 28 551 C2, in DE 44 37 269 C1 oder in DE 42 28 551 A1 beschrieben. Es bestehen an ei­ nen solchen Prozeß unterschiedliche Anforderungen: Entfetten durch die Reaktion der Kohlenwasserstoffe in einem Sauerstoffplasma, Entfernen von Oxiden des Werkstückmaterials durch Reduzieren mit Wasserstoff, Verdampfen von organi­ schen Verunreinigungen durch die thermische Wirkung von Elektronen und Ionen, Sputtern der Oberfläche durch den Beschuß mit Ionen, vorzugsweise Argon- Inertgasionen. In den vorliegenden Arbeiten wird versucht, diese verschiedenen Wirkungen durch geeignete Gasgemische auszubalancieren. The cleaning and degreasing by means of plasma processes is e.g. B in DE 42 28 551 C2, described in DE 44 37 269 C1 or in DE 42 28 551 A1. There exist on egg Such a process has different requirements: degreasing through the reaction the hydrocarbons in an oxygen plasma, removing oxides of the Workpiece material by reducing with hydrogen, evaporation of organi pollution caused by the thermal effects of electrons and ions, Sputtering the surface by bombardment with ions, preferably argon Inert gas ions. The present work tries to differentiate these Balancing effects with suitable gas mixtures.  

Da jedoch die Werkstückmaterialien, die Verschmutzungen und die Anforderungen unterschiedlich sein können, führen Gasgemische o. g. Art zu Problemen. Die An­ passung der Mischungen führt zu immer neuen vorgemischten Prozeßgasen oder zu aufwendigen Mischeinrichtungen mit hohem Optimierungsaufwand. Weiterhin lassen sich gegensätzlich wirkende Prozesse (Oxidieren/Reduzieren) nur schwer gleichzeitig effektiv durchführen.However, since the workpiece materials, the contamination and the requirements can be different, lead gas mixtures o. g. Kind of problems. The An Matching the mixtures always leads to new premixed process gases or to complex mixing devices with high optimization effort. Farther opposing processes (oxidizing / reducing) are difficult perform effectively at the same time.

Aufgabenstellung für die vorliegende Anmeldung war es, ein neues Verfahren zur schaffen, das es erlaubt, auf einfache und effiziente Weise die unterschiedlichen Wirkungen der Plasmabehandlung auf die jeweilige Situation anzupassen.The task for the present application was to develop a new method create that allows the different in a simple and efficient way Adapting the effects of plasma treatment to the respective situation.

Beschreibung des VerfahrensDescription of the procedure

Die Aufgabenstellung wird erfindungsgemäß dadurch gelöst, daß die verschiedenen Wirkungen der Plasmabehandlung einzeln in aufeinanderfolgenden Prozeßschritten aktiviert werden. Dies ermöglicht es, jeden einzelnen Schritt übersichtlich und nahe­ zu ohne Wechselwirkung mit anderen Prozeßschritten zu optimieren.The task is solved according to the invention in that the different Effects of plasma treatment individually in successive process steps to be activated. This makes every single step clear and close to optimize without interacting with other process steps.

Für eine Reinigung bietet sich zum Beispiel folgender Ablauf an:
For example, the following procedure is suitable for cleaning:

  • 1. Entfetten mit Sauerstoff1. Degreasing with oxygen
  • 2. Reduzieren mit Wasserstoff2. Reduce with hydrogen
  • 3. Entfernen von anorganischen Verunreinigungen durch Sputterätzen mit Ar­ gon.3. Removal of inorganic contaminants by sputter etching with Ar gon.

Jeder dieser Schritte kann einfach einzeln optimiert werden. Zum Beispiel muß nicht mit einer erneuten Oxidation während der Reduktion gerechnet werden. Es können je nach Anforderung weitere Prozeßschritte mit den unterschiedlichsten Prozeßga­ sen eingeführt werden. Weiterhin ist es möglich, ohne Bruch des Vakuums und da­ mit ohne Beeinträchtigung der Oberfläche weitere Behandlungsschritte, zum Bei­ spiel zum Korrosionsschutz oder zur Beschichtung, durchzuführen.Each of these steps can easily be optimized individually. For example, does not have to re-oxidation during the reduction can be expected. It can Depending on requirements, further process steps with the most varied process ga be introduced. Furthermore, it is possible without breaking the vacuum and there with further treatment steps without impairing the surface game for corrosion protection or for coating.

Claims (6)

1. Verfahren und Anordnung zur Behandlung von Teilen mittels Niederdruckplas­ men, dadurch gekennzeichnet, daß der Prozeß in mehreren zeitlich aufeinan­ derfolgenden Stufen mit verschiedenen Prozeßparametern und Prozeßgasen durchgeführt wird.1. The method and arrangement for the treatment of parts by means of Niederdruckplas men, characterized in that the process is carried out in several temporally aufeinan the following stages with different process parameters and process gases. 2. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß der Prozeß aus mindestens zwei der folgenden Schritte besteht: Entfetten, Reduzieren, Sput­ terätzen.2. The method according to claim 1, characterized in that the process There are at least two of the following steps: degreasing, reducing, sput estimate. 3. Verfahren und Anordnung nach Anspruch 2, dadurch gekennzeichnet, daß der Entfettungsschritt mit Sauerstoff oder einem sauerstoffhaltigen Prozeßgas durchgeführt wird.3. The method and arrangement according to claim 2, characterized in that the Degreasing step with oxygen or an oxygen-containing process gas is carried out. 4. Verfahren und Anordnung nach Anspruch 2, dadurch gekennzeichnet, daß der Reduzierschritt mit Wasserstoff oder einem wasserstoffhaltigem Prozeßgas durchgeführt wird.4. The method and arrangement according to claim 2, characterized in that the Reduction step with hydrogen or a hydrogen-containing process gas is carried out. 5. Verfahren und Anordnung nach Anspruch 2, dadurch gekennzeichnet, daß das Sputterätzen mit Argon, einem anderen Inertgas oder einer Mischung von Inertgasen durchgeführt wird. 5. The method and arrangement according to claim 2, characterized in that the Sputter etching with argon, another inert gas or a mixture of Inert gases is carried out.   6. Verfahren und Anordnung nach Anspruch 1, dadurch gekennzeichnet, daß im Anschluß an die Behandlung ohne Unterbrechung des Vakuums eine Be­ schichtung oder Nitrierung durchgeführt wird.6. The method and arrangement according to claim 1, characterized in that in Follow-up to treatment without interrupting the vacuum stratification or nitriding is carried out.
DE1996144153 1996-10-24 1996-10-24 Multistage low pressure plasma cleaning process Withdrawn DE19644153A1 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
DE1996144153 DE19644153A1 (en) 1996-10-24 1996-10-24 Multistage low pressure plasma cleaning process

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DE1996144153 DE19644153A1 (en) 1996-10-24 1996-10-24 Multistage low pressure plasma cleaning process

Publications (1)

Publication Number Publication Date
DE19644153A1 true DE19644153A1 (en) 1998-04-30

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2000050661A1 (en) * 1998-08-12 2000-08-31 Swagelok Company Low temperature case hardening processes
DE10024373A1 (en) * 2000-05-17 2001-11-29 Eupec Gmbh & Co Kg Coating process
EP1260602A1 (en) * 2001-05-23 2002-11-27 Sulzer Metco AG Process for producing a thermally insulating coating system on a metallic substrate
US6547888B1 (en) 2000-01-28 2003-04-15 Swagelok Company Modified low temperature case hardening processes
EP1477188A1 (en) * 2003-05-12 2004-11-17 Terolab Services Management SA Method for cleansing and bacterial decontamination of mechanical medical parts, and device therefor
WO2004098259A2 (en) * 2003-05-08 2004-11-18 Kolektor Group D.O.O. Plasma treatment for purifying copper or nickel
WO2007137557A2 (en) * 2006-05-30 2007-12-06 Schaeffler Kg Method for hardening running surfaces of roller bearing components
EP2309039A1 (en) * 2008-07-04 2011-04-13 Showa Denko K.K. Seed crystal for growth of silicon carbide single crystal, process for producing the same, and silicone carbide single crystal and process for producing the same

Cited By (17)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2000050661A1 (en) * 1998-08-12 2000-08-31 Swagelok Company Low temperature case hardening processes
US6547888B1 (en) 2000-01-28 2003-04-15 Swagelok Company Modified low temperature case hardening processes
DE10024373B4 (en) * 2000-05-17 2005-05-19 eupec Europäische Gesellschaft für Leistungshalbleiter mbH & Co. KG Method for coating
DE10024373A1 (en) * 2000-05-17 2001-11-29 Eupec Gmbh & Co Kg Coating process
EP1260602A1 (en) * 2001-05-23 2002-11-27 Sulzer Metco AG Process for producing a thermally insulating coating system on a metallic substrate
US8168261B2 (en) 2001-05-23 2012-05-01 Sulzer Metco A.G. Process for applying a heat shielding coating system on a metallic substrate
WO2004098259A2 (en) * 2003-05-08 2004-11-18 Kolektor Group D.O.O. Plasma treatment for purifying copper or nickel
WO2004098259A3 (en) * 2003-05-08 2005-02-24 Kolektor Group Doo Plasma treatment for purifying copper or nickel
EP1477188A1 (en) * 2003-05-12 2004-11-17 Terolab Services Management SA Method for cleansing and bacterial decontamination of mechanical medical parts, and device therefor
FR2854804A1 (en) * 2003-05-12 2004-11-19 Terolab Services Man Sa PROCESS FOR CLEANING AND BACTERIAL DECONTAMINATION OF MECHANICAL PARTS FOR MEDICAL USE, AND DEVICE FOR CARRYING OUT SAID METHOD
WO2007137557A2 (en) * 2006-05-30 2007-12-06 Schaeffler Kg Method for hardening running surfaces of roller bearing components
WO2007137557A3 (en) * 2006-05-30 2008-12-11 Schaeffler Kg Method for hardening running surfaces of roller bearing components
US8479396B2 (en) 2006-05-30 2013-07-09 Schaeffler Technologies AG & Co. KG Method for hardening running surfaces of roller bearing components
DE102006025008B4 (en) 2006-05-30 2022-09-15 Schaeffler Technologies AG & Co. KG Process for hardening running surfaces of roller bearing components
EP2309039A1 (en) * 2008-07-04 2011-04-13 Showa Denko K.K. Seed crystal for growth of silicon carbide single crystal, process for producing the same, and silicone carbide single crystal and process for producing the same
EP2309039A4 (en) * 2008-07-04 2011-11-16 Showa Denko Kk Seed crystal for growth of silicon carbide single crystal, process for producing the same, and silicone carbide single crystal and process for producing the same
CN102057084B (en) * 2008-07-04 2013-03-27 昭和电工株式会社 Seed crystal for growth of silicon carbide single crystal, process for producing the same, and silicone carbide single crystal and process for producing the same

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Legal Events

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