EP0343038A1 - Oberflächenreinigungsverfahren mit transportiertem Plasma - Google Patents

Oberflächenreinigungsverfahren mit transportiertem Plasma Download PDF

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Publication number
EP0343038A1
EP0343038A1 EP89401297A EP89401297A EP0343038A1 EP 0343038 A1 EP0343038 A1 EP 0343038A1 EP 89401297 A EP89401297 A EP 89401297A EP 89401297 A EP89401297 A EP 89401297A EP 0343038 A1 EP0343038 A1 EP 0343038A1
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EP
European Patent Office
Prior art keywords
plasma
fluorinated
mixture
cleaning
nitrogen
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Withdrawn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
EP89401297A
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English (en)
French (fr)
Inventor
Odile Dessaux
Brigitte Mutel
Daniel Szurminski
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Prestations De Services Sps Ste
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Prestations De Services Sps Ste
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Filing date
Publication date
Application filed by Prestations De Services Sps Ste filed Critical Prestations De Services Sps Ste
Publication of EP0343038A1 publication Critical patent/EP0343038A1/de
Withdrawn legal-status Critical Current

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    • 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

Definitions

  • the present invention relates to surface cleaning of objects, for example the pickling of metal surfaces by removing oils or greases which cover them in whole or in part, for example the cleaning of ceramic objects or optical fibers based of glass, this list not being limiting.
  • the present invention relates more particularly to the treatment of such objects with a view to cleaning their surface with a plasma.
  • a plasma is given to various media containing simultaneously neutral particles - atoms or molecules - positive ions and electrons.
  • a plasma can be produced artificially by carrying a gas at high temperature or by subjecting it to an intense electric field.
  • Type I plasma commonly called plasma without any other qualifier
  • plasma is a highly ionized medium, in which a very high temperature prevails, and which is in thermodynamic equilibrium. It is obtained for example using a plasma torch type material. Its temperature is around 10,000 to 15,000 ° K. The surface cleaning of objects with type I plasmas is obtained by the destructive action due to high temperatures. These plasmas being confined in the restricted volume of the discharge, only small surfaces can be treated. A plasma of this type is described in US Pat. No. 4,555,303.
  • Type II plasma commonly called cold plasma
  • Cold plasma is a poorly ionized medium. Its temperature is lower, since it is less than 1000 ° K. It is however poorly defined because the environment is in strong thermodynamic imbalance. Cold plasma is obtained in electrical discharges with or without electrodes, in a gas under low pressure, less than 100 mbar, for example in electrical discharges, microwave or high frequency discharges. A plasma of this type is described in Patent FR.2.368.308.
  • Type III plasma will be called in the remainder of this text deferred plasma; in scientific literature, it is sometimes referred to as "activated gas” or "post-luminescence" when the plasma gas is nitrogen.
  • the deferred plasma is obtained by dynamic expansion of a cold plasma outside the discharge. This expansion can be carried out in very large volumes, of the order of several cubic meters. It is generally formed at pressures below 100 mbar but can be obtained up to pressures above atmospheric pressure. It is an environment in a state of very strong thermodynamic non-equilibrium, where the average temperature is that of the ambient atmosphere, for example 298 ° K.
  • Deferred plasma is known in the treatment of plastic surfaces, in particular by European patent applications No. 84.101.926.8 and 84.101.935.9, with a view to increasing the bonding power of said surfaces, resulting in particular in an increase in wettability, characterized by a decrease in the angle of contact of water on the surface of the material.
  • European patent applications No. 84.101.926.8 and 84.101.935.9 with a view to increasing the bonding power of said surfaces, resulting in particular in an increase in wettability, characterized by a decrease in the angle of contact of water on the surface of the material.
  • no particular applications of deferred plasmas are known.
  • deferred plasma has a cleaning action on the surface of certain objects which are not themselves altered. or modified by said plasma, in particular objects made of stainless steel, ceramic, procelaine, glass.
  • pollutants such as oils, fats, organic materials, deposited on the surface of said objects were degraded when subjected to the action of a delayed plasma for a given time. This time is a function of the pressure prevailing in the plasma expansion chamber and the surface condition of the object. This degradation occurs even when the plasma temperature is close to ambient temperature.
  • the delayed plasmas used in the context of the invention involve pure or mixed gases, in particular argon, dioxygen (O2), dinitrogen (N2) and even air, called plasma gas.
  • the plasmagenic medium is a mixture of gases, comprising in a proportion at most equal to 10%, a fluorinated or chlorinated compound. It has in fact been observed that the presence of such a gas has an amplifying effect on the action of cleaning the delayed plasma.
  • the fluorinated compound is in particular chosen from nitrogen trifluoride (NF3), carbon tetrafluoride (CF4), sulfur hexafluoride (SF6) or fluorine (F2).
  • the chlorinated compound is in particular chosen from nitrogen trichloride (NCl3), carbon tetrachloride (CCl4), trichloromethane (CHCl3), dichloromethane (CH2Cl2) or chlorine (Cl2).
  • the preferred composition of the plasma medium is as follows: dioxygen 75%, dinitrogen 23.5% and nitrogen trifluoride 1.5% for a pressure of 12 mbar.
  • the treatment time necessary for the complete cleaning of the surface of the object is of the order of 1 to 15 minutes if said surface is smooth; it is around 90 to 100 minutes if the surface is granite. This time is sufficient to carry out the complete degradation of all the polluting materials deposited on the surface of the object, whatever the shape of the object and even if the polluting materials would be located in indentations or interior cavities.
  • FIG. 1 is a schematic view of said installation
  • Figure 2 is a schematic view of a large capacity expansion chamber.
  • the cleaning installation of the invention comprises a plasma generator 1.
  • This is a microwave generator, operating at a frequency of 2450 MHz and delivering a variable, adjustable power, up to 1500 W.
  • a coupler 2 of parallelepiped shape, which allows a very good adaptation, thanks to the piston 11, to the screws 12, and to an inner iris not shown in the figure.
  • This coupler is described with precision in J. Phys.E.Sc.inst.16-1983 pages 1160-1161.
  • the quartz tube 3 has a diameter of 15 mm.
  • the plasma produced in tube 3 is type II cold plasma.
  • the tube 3 is connected to three gas bottles 13, 14, 15: respectively nitrogen, oxygen and nitrogen trifluoride in the preferred composition of the invention .
  • the tube 3 further comprises a gauge 4 for measuring the pressure.
  • the other end of the tube 3, on the right in the figure, is connected to the expansion chamber 7 by means of the male 6 and female 19 spherical connections.
  • This chamber 7 is moreover connected, by means of the male 20 and female spherical connections. 21, to a trap 8 containing a copper sponge and to a second liquid nitrogen trap 9 placed in series after the first trap 8, and connected to a vacuum pump not shown.
  • the vacuum pump has a flow rate of 35 m3 / h at atmospheric pressure.
  • the spherical connections make it possible to interchange the expansion chambers according to the volume of the objects to be cleaned.
  • the expansion chamber 7, shown in Figure 1 has a capacity of 2.5 l, it is suitable for objects of small dimensions, for example pliers or other hand tools.
  • the expansion chamber 7, shown in FIG. 2 which has a capacity of 125 l.
  • This chamber is composed of two separate parts, which can be separated to allow the introduction of the object or objects to be cleaned, each part being equipped with closing means capable of preserving the tightness of the expansion chamber 7 once the object or objects were introduced there.
  • the cleaning operation consists in introducing into the expansion chamber 7 the soiled tool 10 to be cleaned, in connecting the chamber 7 by its spherical connections 19 and 20 on the one hand to the tube 3 and on the other hand to the traps 8 and 9, to supply the tube 3 with one and / or the other of the gases, in the desirable proportion by acting on the regulators 16,17,18, and to create the cold plasma in the tube 3 by actuating the generator 1 and by adjusting the coupler 2.
  • the cold plasma, generated in the tube 3 is dynamically, by the gas flow which crosses the tube 3, transferred into the expansion chamber 7. There, the deferred plasma attacks the materials organic, oils or greases staining the surface of the tool.
  • the tool 10 must be kept in the activated gas flow for a sufficient time so that all the surface materials are degraded and are themselves evacuated from the chamber 7 and retained by the two successive traps 8 and 9.
  • the optimal composition of the plasma gas is the following, at a total pressure of 12 mbar: oxygen (WHERE) 75% nitrogen (N2) 23.5% nitrogen trifluoride 1.5%
  • the microwave power introduced via the coupler 2 was less than 160W.
  • the nitrogen trifluoride promotes the pickling of surfaces, in particular stainless steel, by reducing the processing time required to remove pollutants.
  • the duration of the treatment was 15 min; for tools with a granite surface, 90 min were required.
  • the time required is much shorter, less than a minute and in some cases less than a second.
  • the invention is not limited to the embodiment which has just been described, but covers all its variants. What has been said for the stripping of metallic surfaces is also true for the cleaning of ceramic materials, porcelains, glass objects (in particular glass fibers), ceramic composites - glasses-metals. Similarly, it is possible, without departing from the invention, to modify the conditions for obtaining deferred plasma: pressure, power, volume of the expansion chamber, plasma generated by electrical discharge, microwave or high frequency. Finally, oils and fats are not the only pollutants degradable by deferred plasma, they can be inks, more generally organic materials, or even certain metallic deposits.

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  • Chemical & Material Sciences (AREA)
  • Metallurgy (AREA)
  • Physics & Mathematics (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Optics & Photonics (AREA)
  • Mechanical Engineering (AREA)
  • Organic Chemistry (AREA)
  • Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
  • Cleaning In General (AREA)
  • Drying Of Semiconductors (AREA)
  • Cleaning Or Drying Semiconductors (AREA)
  • Electrical Discharge Machining, Electrochemical Machining, And Combined Machining (AREA)
  • Polishing Bodies And Polishing Tools (AREA)
  • Detergent Compositions (AREA)
EP89401297A 1988-05-10 1989-05-10 Oberflächenreinigungsverfahren mit transportiertem Plasma Withdrawn EP0343038A1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR8806607 1988-05-10
FR8806607A FR2631258B1 (fr) 1988-05-10 1988-05-10 Procede de nettoyage en surface par plasma differe

Publications (1)

Publication Number Publication Date
EP0343038A1 true EP0343038A1 (de) 1989-11-23

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ID=9366376

Family Applications (1)

Application Number Title Priority Date Filing Date
EP89401297A Withdrawn EP0343038A1 (de) 1988-05-10 1989-05-10 Oberflächenreinigungsverfahren mit transportiertem Plasma

Country Status (7)

Country Link
EP (1) EP0343038A1 (de)
JP (1) JPH0252084A (de)
CN (1) CN1038036A (de)
DK (1) DK226989A (de)
FR (1) FR2631258B1 (de)
NO (1) NO173921C (de)
ZA (1) ZA893473B (de)

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0618017A1 (de) * 1993-03-30 1994-10-05 Bridgestone Corporation Methode zur Reinigung eines Vulkanisierform
FR2733437A1 (fr) * 1995-04-27 1996-10-31 Aubert Bruno Procede de separation d'elements chimiques par formation de composes volatils avec un gaz excite dans un plasma froid et dispositif de mise en oeuvre
FR2750348A1 (fr) * 1996-06-28 1998-01-02 Conte Procede pour augmenter l'anti-mouillabilite d'un corps, corps ainsi traite et ses applications
EP0924282A1 (de) * 1997-12-18 1999-06-23 Central Glass Company, Limited Gas zum Wegnehmen von Ablagerungen und ihre Verwendung
US6125859A (en) * 1997-03-05 2000-10-03 Applied Materials, Inc. Method for improved cleaning of substrate processing systems
WO2000078123A1 (en) * 1999-06-24 2000-12-28 Wisconsin Alumni Research Foundation Cold-plasma treatment of seeds to remove surface materials
EP0828618A4 (de) * 1995-06-02 2001-01-03 Univ Tennessee Res Corp Verfahren und vorrichtung zum reinigen von oberflächen mittels eines glimmentladungsplasmas unter atmosphärendruck
US6274058B1 (en) 1997-07-11 2001-08-14 Applied Materials, Inc. Remote plasma cleaning method for processing chambers
CN104148334A (zh) * 2014-07-02 2014-11-19 太仓华德石太工业设备有限公司 一种针对工业局部清洁的碳氢化合物/等离子体的清洁方法
DE102020131832A1 (de) 2020-12-01 2022-06-02 Universität Kassel, Körperschaft des öffentlichen Rechts Verfahren zur Herstellung von Gussformen oder Gusskernen

Families Citing this family (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2005036250A (ja) * 2003-07-16 2005-02-10 Matsushita Electric Ind Co Ltd スパッタ装置
US20110108058A1 (en) * 2009-11-11 2011-05-12 Axcelis Technologies, Inc. Method and apparatus for cleaning residue from an ion source component
CN101837357B (zh) * 2010-05-04 2011-10-05 宁波大学 一种等离子体清洗装置
JP2012152855A (ja) * 2011-01-26 2012-08-16 Osg Corp ダイヤモンド被膜または硬質炭素被膜の脱膜方法
CN104353643B (zh) * 2014-12-02 2017-07-25 上海华虹宏力半导体制造有限公司 一种减小超声波清洗器的维护系统及维护方法

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2368308A1 (fr) * 1976-10-19 1978-05-19 Kernforschungsanlage Juelich Procede et dispositif pour nettoyer des surfaces, notamment des surfaces metalliques
US4555303A (en) * 1984-10-02 1985-11-26 Motorola, Inc. Oxidation of material in high pressure oxygen plasma
WO1987002603A1 (en) * 1985-10-29 1987-05-07 Hughes Aircraft Company Method and apparatus for atomic beam irradiation

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2368308A1 (fr) * 1976-10-19 1978-05-19 Kernforschungsanlage Juelich Procede et dispositif pour nettoyer des surfaces, notamment des surfaces metalliques
US4555303A (en) * 1984-10-02 1985-11-26 Motorola, Inc. Oxidation of material in high pressure oxygen plasma
WO1987002603A1 (en) * 1985-10-29 1987-05-07 Hughes Aircraft Company Method and apparatus for atomic beam irradiation

Cited By (16)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0618017A1 (de) * 1993-03-30 1994-10-05 Bridgestone Corporation Methode zur Reinigung eines Vulkanisierform
FR2733437A1 (fr) * 1995-04-27 1996-10-31 Aubert Bruno Procede de separation d'elements chimiques par formation de composes volatils avec un gaz excite dans un plasma froid et dispositif de mise en oeuvre
EP0828618A4 (de) * 1995-06-02 2001-01-03 Univ Tennessee Res Corp Verfahren und vorrichtung zum reinigen von oberflächen mittels eines glimmentladungsplasmas unter atmosphärendruck
US6197234B1 (en) 1996-06-28 2001-03-06 Conte Sa Method for increasing the anti-wettability of a body
FR2750348A1 (fr) * 1996-06-28 1998-01-02 Conte Procede pour augmenter l'anti-mouillabilite d'un corps, corps ainsi traite et ses applications
EP0815937A1 (de) * 1996-06-28 1998-01-07 Conte S.A. Verfahren zum Erhöhen der Anti-Benetzbarkeit eines Körpers, Körper dementsprechend behandelt und Verwendung davon
US6125859A (en) * 1997-03-05 2000-10-03 Applied Materials, Inc. Method for improved cleaning of substrate processing systems
US6274058B1 (en) 1997-07-11 2001-08-14 Applied Materials, Inc. Remote plasma cleaning method for processing chambers
EP0924282A1 (de) * 1997-12-18 1999-06-23 Central Glass Company, Limited Gas zum Wegnehmen von Ablagerungen und ihre Verwendung
US6673262B1 (en) 1997-12-18 2004-01-06 Central Glass Company, Limited Gas for removing deposit and removal method using same
US7168436B2 (en) 1997-12-18 2007-01-30 Central Glass Company, Limited Gas for removing deposit and removal method using same
US7744769B2 (en) 1997-12-18 2010-06-29 Central Glass Company, Limited Gas for removing deposit and removal method using same
WO2000078123A1 (en) * 1999-06-24 2000-12-28 Wisconsin Alumni Research Foundation Cold-plasma treatment of seeds to remove surface materials
US6543460B1 (en) 1999-06-24 2003-04-08 Wisconsin Alumni Research Foundation Cold-plasma treatment of seeds to remove surface materials
CN104148334A (zh) * 2014-07-02 2014-11-19 太仓华德石太工业设备有限公司 一种针对工业局部清洁的碳氢化合物/等离子体的清洁方法
DE102020131832A1 (de) 2020-12-01 2022-06-02 Universität Kassel, Körperschaft des öffentlichen Rechts Verfahren zur Herstellung von Gussformen oder Gusskernen

Also Published As

Publication number Publication date
NO173921B (no) 1993-11-15
CN1038036A (zh) 1989-12-20
JPH0252084A (ja) 1990-02-21
NO891827L (no) 1989-11-13
DK226989D0 (da) 1989-05-09
FR2631258B1 (fr) 1991-04-05
ZA893473B (en) 1990-01-31
DK226989A (da) 1989-11-11
NO173921C (no) 1994-02-23
NO891827D0 (no) 1989-05-03
FR2631258A1 (fr) 1989-11-17

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