EP0753599B2 - Method for producing corrosion and wear resistant protective coatings on iron based substrates - Google Patents

Method for producing corrosion and wear resistant protective coatings on iron based substrates Download PDF

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Publication number
EP0753599B2
EP0753599B2 EP96110790A EP96110790A EP0753599B2 EP 0753599 B2 EP0753599 B2 EP 0753599B2 EP 96110790 A EP96110790 A EP 96110790A EP 96110790 A EP96110790 A EP 96110790A EP 0753599 B2 EP0753599 B2 EP 0753599B2
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Prior art keywords
nitrogen
iron
carbon
oxidizing
process according
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EP96110790A
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German (de)
French (fr)
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EP0753599A1 (en
EP0753599B1 (en
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Steffen Dr. Hoppe
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Oerlikon Metaplas GmbH
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Metaplas Ionon Oberflaechenveredelungstechnik GmbH
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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
    • 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
    • C23C8/06—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 using gases
    • C23C8/34—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 using gases more than one element being applied in more than one step
    • 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
    • C23C8/06—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 using gases
    • C23C8/28—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 using gases more than one element being applied in one step
    • C23C8/30—Carbo-nitriding
    • C23C8/32—Carbo-nitriding of ferrous surfaces

Definitions

  • the invention relates to a method for generating of corrosion and wear protection layers on iron-based materials, near the surface Areas enriched with nitrogen, carbon as well as oxygen become.
  • nitride layer on aluminum or aluminum alloys it is from EP-A-0 158 271 known that the surface of the nitriding Material by means of a glow discharge with a Noble gas is activated as activation gas. This activation process serves to do so, by the ion bombardment the surface of the material to be nitrided this material surface of organic components, such as cleaning carbon and oils, so that in the subsequent nitriding process a permanent Connection of the nitriding layer with the aluminum material is possible.
  • the invention is based on the object Process for the production of corrosion and wear protection layers on iron-based materials on the one hand, the aforementioned disadvantages does not have and on the other hand, longer service life of thus treated materials allows.
  • the process is the oxidation in one Temperature range of 480 ° C to 520 ° C performed.
  • the activation of the material surface during the plasma-assisted vacuum method takes place advantageously by the bombardment of the material surface with nitrogen, hydrogen, carbon and oxygen ions.
  • the composition of a gas mixture to r generation the above-mentioned ions in the plasma can be defined and targeted changes in the Nitrocarburier suits formed compound layer be brought about, which in turn also on the subsequent oxidation step.
  • the normal pressure gas nitrocarburizing process and oxidizing and the plasma assisted vacuum process are executable in the same plant.
  • the iron base substances to be treated are first to the treatment temperature of about Heated to 500 ° C to 590 ° C and then in a Ammonia-nitrogen-carbon dioxide atmosphere the Nitrocarburierprozeß subjected to the enrichment from nitrogen and carbon to one from iron carbonitrides existing connection layer leads. After taking place under normal pressure Nitrocarburiervon the workpiece is at the temperature led the oxidation treatment. It can as well a cooling of the workpiece to room temperature respectively. For the following plasma-assisted Ion bombardment of the workpiece surface is the process room is evacuated. Likewise, besides this Evacuation with previous cooling of the workpiece to room temperature a simultaneous warming of the workpiece to the temperature of the oxidation treatment necessary.
  • the material is switched as a cathode, while, for example, the plant wall as Anode is connected.
  • the bonding layer formed so changed by heating, implantation and sputtering, that in the subsequent oxidation step a closed and uniform oxide layer in and on can form the bonding layer. Training the uniform oxide layer is thereby supported, that the plasma is during the activation process around the entire surface of the material formed.
  • the system with Nitrogen as inert gas flooded to normal pressure and the Material back to its treatment temperature of heated to about 480 ° C to 520 ° C.
  • water vapor for the oxidation process for generating a nitrogen-water vapor mixture directed to the plant. After completion of the oxidation process becomes the thus treated Material cooled under further nitrogen supply.

Abstract

The method concerns production of corrosion and wear resistant layers on ferrous material, according to which near-surface regions are enriched with nitrogen, carbon and oxygen. It is characterized by the following process steps: (a) carbonitration of the material to produce a connector layer consisting of iron carbonitrides; (b) activation of the material surface by a low-pressure plasma-assisted process; (c) oxidation of the material to produce a closed oxide layer. Also claimed is an appts. for implementation of the method in which processes at normal and low pressures can be carried out.

Description

Die Erfindung betrifft ein Verfahren zur Erzeugung von Korrosions- und Verschleißschutzschichten auf Eisenbasiswerkstoffen, bei dem oberflächennahe Bereiche mit Stickstoff, Kohlenstoff sowie Sauerstoff angereichert werden.The invention relates to a method for generating of corrosion and wear protection layers on iron-based materials, near the surface Areas enriched with nitrogen, carbon as well as oxygen become.

Seit Anfang der 80er Jahre ist es bekannt, daß das Korrosions- und Verschleißverhalten von Eisenbasiswerkstoffen durch die nachträgliche Oxidation von Nitridschichten deutlich verbessert werden kann. Besonders gute Ergebnisse wurden durch die Kombination der Verfahrensschritte Nitrocarburieren und anschließendes Oxidieren erreicht. Beide Verfahrensschritte können sowohl in gasförmigen als auch flüssigen Medien erfolgen. Die Aufgabe der nachträglichen Oxidation der Nitrierschichten besteht dabei in der Ausbildung einer geschlossenen Oxidschicht an der Oberfläche des Werkstoffs.Since the beginning of the 80s it is known that the corrosion and wear behavior of iron-based materials by the subsequent oxidation of Nitride layers can be significantly improved. Especially Good results were achieved by the combination the process steps nitrocarburizing and subsequent Oxidizing achieved. Both process steps can be both gaseous and liquid Media done. The task of the subsequent Oxidation of the nitriding layers is in the training a closed oxide layer on the surface of the material.

Obwohl des sehr effektiven Einsatzes einer Oxidation eine Vielzahl von kommerziell anwendbaren Technologien existieren, sind die bisher erreichten Kennwerte des Korrosionsverhaltes derart behandelter Werkstoffe für eine Vielzahl industrieller Anwendungen nicht ausreichend.Although the very effective use of a Oxidation a variety of commercially applicable Technologies exist, are the achieved so far Characteristics of the corrosion behavior treated in this way Materials for a variety of industrial applications unsatisfactory.

Nachteilig ist darüber hinaus, daß insbesondere der Einsatz von Salzbadverfahren sehr umweltbelastend ist und die solchermaßen erzeugten Oberflächen rauh sind, weshalb sie einer Zwischen- oder Nachbearbeitung unterzogen werden müssen.Another disadvantage is that in particular the use of Salzbadverfahren very polluting is and the surfaces thus produced are rough, which is why they are an intermediate or post-processing must be subjected.

Zur Ausbildung einer Nitridschicht auf Aluminium oder Aluminiumlegierungen ist es aus der EP-A-0 158 271 bekannt, daß die Oberfläche des zu nitrierenden Werkstoffs mittels einer Glimmentladung mit einem Edelgas als Aktivierungsgas aktiviert wird. Dieser Aktivierungsprozeß dient dabei dazu, durch den lonenbeschuß der Oberfläche des zu nitrierenden Werkstoffes diese Werkstoffoberfläche von organischen Komponenten, wie beispielsweise Kohlenstoff und Ölen zu reinigen, damit im nachfolgenden Nitrierprozeß eine dauerhafte Verbindung der Nitrierschicht mit dem Aluminiumwerkstoff möglich ist.For forming a nitride layer on aluminum or aluminum alloys it is from EP-A-0 158 271 known that the surface of the nitriding Material by means of a glow discharge with a Noble gas is activated as activation gas. This activation process serves to do so, by the ion bombardment the surface of the material to be nitrided this material surface of organic components, such as cleaning carbon and oils, so that in the subsequent nitriding process a permanent Connection of the nitriding layer with the aluminum material is possible.

Der Erfindung liegt die Aufgabe zugrunde, ein Verfahren zur Erzeugung von Korrosions- und Verschleißschutzschichten auf Eisenbasiswerkstoffen zu schaffen, das einerseits die voran genannten Nachteile nicht aufweist und andererseits höhere Standzeiten der solchermaßen behandelten Werkstoffe ermöglicht.The invention is based on the object Process for the production of corrosion and wear protection layers on iron-based materials on the one hand, the aforementioned disadvantages does not have and on the other hand, longer service life of thus treated materials allows.

Die verfahrensgemäße Lösung dieser Aufgabe durch die Erfindung ist gekennzeichnet durch die Verfahrensschritte:

  • a) Nitrocarburieren des Werkstoffs unter Normaldruck zur Bildung einer aus Eisenkarbonitriden bestehenden Verbindungsschicht;
  • b) Aktivieren der Oberfläche des Werkstoffs in einem plasmagestützten Unterdruckverfahren und
  • c) Oxidieren des Werkstoffs unter Normaldruck zur Bildung einer geschlossenen Oxidschicht.
    • The method according to the solution of this problem by the invention is characterized by the method steps:
  • a) nitrocarburizing the material under normal pressure to form a compound layer consisting of iron carbonitrides;
  • b) activating the surface of the material in a plasma assisted vacuum method and
  • c) oxidizing the material under normal pressure to form a closed oxide layer.

    • Bei diesem erfindungsgemäß ausgebildeten Verfahren werden in dem Verfahrensschritt Nitrocarburieren die oberflächennahen Bereiche mit Stickstoff und Kohlenstoff angereichert, um eine aus Eisenkarbonitriden bestehende Verbindungsschicht zu bilden. Überraschenderweise hat sich herausgestellt, daß das Korrosions- und Verschleißverhalten von Eisenbasiswerkstoffen deutlich verbessert werden kann, wenn die der Nitrocarburierung unterzogenen Werkstoffe vor der nachfolgenden Oxidation einem plasmagestützten Unterdruckverfahren unterzogen werden. Die durch den lonenbeschuß der Werkstoffoberfläche ablaufenden chemischen und physikalischen Wechselwirkungsreaktionen bewirken eine Aktivierung und gezielte Veränderung der oberflächennahen Bereiche der im Nitrocarburierschritt gebildeten Verbindungsschicht. Aufgrund dieses lonenbeschusses führt die Anreicherung der oberflächennahen Bereiche mit Sauerstoff beim Oxidieren zu einer geschlossenen und gleichmäßigen Oxidschicht auf der bestehenden Verbindungsschicht. Solchermaßen behandelte Eisenbasiswerkstoffe weisen bei normierten Korrosionstests (wie den Salz-Sprühnebel-Test nach DIN 500 21 SS) Standzeiten von bis zu 600 Stunden auf.In this inventively formed Methods are nitrocarburizing in the process step the near-surface areas with nitrogen and Carbon enriched to one of iron carbonitrides Form existing connection layer. Surprisingly it has been found that the corrosion and wear behavior of iron-based materials can be significantly improved if the the Nitrocarburizing materials before the subsequent oxidation of a plasma-assisted vacuum method be subjected. The by the Ion bombardment of the material surface running off chemical and physical interaction reactions cause activation and targeted change the near-surface areas in the Nitrocarburierschritt formed connecting layer. Because of this Ion bombardment leads to the enrichment of the near-surface Oxygen oxidizing areas to a closed and uniform oxide layer on the existing connection layer. thus Treated iron-based materials exhibit normalized Corrosion tests (such as the salt spray test according to DIN 500 21 SS) Service life of up to 600 hours on.

    Zur Erzeugung einer besonders effektiven Verbindungsschicht während des Nitrocarburierens werden durch Anreicherung von Stickstoff und Kohlenstoff in den oberflächennahen Bereichen die Eisenkarbonitride ε - Fe2 (N, C)1-x und/oder δ' - Fe4 (N, C)1-y gebildet.To produce a particularly effective bonding layer during nitrocarburizing, by enrichment of nitrogen and carbon in the near-surface regions, the iron carbonitrides ε - Fe 2 (N, C) 1-x and or δ '- Fe 4 (N, C) 1-y educated.

    Zur Bildung der geschlossenen und gleichmäßigen Oxidschicht hat es sich als besonders vorteilhaft erwiesen, daß zur Anreicherung der oberflächennahen Bereiche mit Sauerstoff die Oxidation in einem Stickstoff-Wasserdampf-Gemisch definierter Zusammensetzung durchgeführt wird. Gemäß einer bevorzugten Ausführungsform des Verfahrens wird die Oxidation in einem Temperaturbereich von 480°C bis 520°C durchgeführt.To form the closed and even Oxide layer has proven to be particularly advantageous proved that for the enrichment of the near-surface Areas of oxygen oxidation in a nitrogen-water vapor mixture defined composition is carried out. According to a preferred embodiment the process is the oxidation in one Temperature range of 480 ° C to 520 ° C performed.

    Die Aktivierung der Werkstoffoberfläche während des plasmagestützten Unterdruckverfahrens erfolgt vorteilhafterweise durch den Beschuß der Werkstoffoberfläche mit Stickstoff-, Wasserstoff-, Kohlenstoff- und Sauerstoffionen. Durch die geeignete Wahl der Zusammensetzung eines Gasgemisches zu r Erzeugung der voranstehend genannten Ionen im Plasma können definierte und gezielte Veränderungen der im Nitrocarburierschritt gebildeten Verbindungsschicht herbeigeführt werden, was sich wiederum auch auf den nachfolgenden Oxidationsschritt auswirkt.The activation of the material surface during the plasma-assisted vacuum method takes place advantageously by the bombardment of the material surface with nitrogen, hydrogen, carbon and oxygen ions. By the appropriate choice the composition of a gas mixture to r generation the above-mentioned ions in the plasma can be defined and targeted changes in the Nitrocarburierschritt formed compound layer be brought about, which in turn also on the subsequent oxidation step.

    Die Normaldruck-Gasverfahren Nitrocarburieren und Oxidieren und das plasmagestützte Unterdruckverfahren sind in der gleichen Anlage ausführbar.The normal pressure gas nitrocarburizing process and oxidizing and the plasma assisted vacuum process are executable in the same plant.

    Durch die Integration aller drei Verfahrensschritte läßt sich das erfindungsgemäße Verfahren trotz des zusätzlichen Verfahrensschrittes einfach und kostengünstig durchführen.By integrating all three process steps can the process of the invention despite the additional process step easily and inexpensively carry out.

    Der Ablauf des erfindungsgemäßen Verfahrens läßt sich schematisch wie folgt beschreiben:The course of the method according to the invention can be described schematically as follows:

    Die zu behandelnden Eisenbasisstoffe werden zunächst auf die Behandlungstemperatur von etwa 500°C bis 590°C erwärmt und anschließend in einer Ammoniak-Stickstoff-Kohlendioxid-Atmosphäre dem Nitrocarburierprozeß unterzogen, bei dem die Anreicherung von Stickstoff und Kohlenstoff zu einer aus Eisenkarbonitriden bestehenden Verbindungsschicht führt. Nach dem unter Normaldruck stattfindenden Nitrocarburierverfahren wird das Werkstück auf die Temperatur der Oxidationsbehandlung geführt. Es kann ebenso eine Abkühlung des Werkstückes auf Raumtemperatur erfolgen. Für den nachfolgenden plasmagestützten lonenbeschuß der Werkstückoberfläche wird der Prozeßraum evakuiert. Ebenso ist neben dieser Evakuierung bei vorheriger Abkühlung des Werkstükkes auf Raumtemperatur eine gleichzeitige Erwärmung des Werkstückes auf die Temperatur der Oxidationsbehandlung notwendig. Zur Erzeugung des aus Stickstoff-, Wasserstoff-, Kohlenstoff- und Sauerstoffionen gebildeten Plasmas wird der Werkstoff als Kathode geschaltet, während beispielsweise die Anlagenwand als Anode geschaltet ist. Durch die mit hoher kinetischer Energie auf die Oberfläche des Werkstoffes auftreffenden Ionen werden die oberflächennahen Bereiche der im Nitrocarburierschritt gebildeten Verbindungsschicht durch Erwärmung, Implantation und Sputtem so verändert, daß sich im nachfolgenden Oxidationsschritt eine geschlossene und gleichmäßige Oxidschicht in und auf der Verbindungsschicht ausbilden kann. Die Ausbildung der gleichmäßigen Oxidschicht wird dadurch unterstützt, daß sich das Plasma während des Aktivierungsprozesses um die gesamte Oberfläche des Werkstoffes ausbildet.The iron base substances to be treated are first to the treatment temperature of about Heated to 500 ° C to 590 ° C and then in a Ammonia-nitrogen-carbon dioxide atmosphere the Nitrocarburierprozeß subjected to the enrichment from nitrogen and carbon to one from iron carbonitrides existing connection layer leads. After taking place under normal pressure Nitrocarburierverfahren the workpiece is at the temperature led the oxidation treatment. It can as well a cooling of the workpiece to room temperature respectively. For the following plasma-assisted Ion bombardment of the workpiece surface is the process room is evacuated. Likewise, besides this Evacuation with previous cooling of the workpiece to room temperature a simultaneous warming of the workpiece to the temperature of the oxidation treatment necessary. To produce the nitrogen, Hydrogen, carbon and oxygen ions formed plasma, the material is switched as a cathode, while, for example, the plant wall as Anode is connected. By the ones with high kinetic Energy impinging on the surface of the material Ions are the near-surface areas of the in the nitrocarburizing step, the bonding layer formed so changed by heating, implantation and sputtering, that in the subsequent oxidation step a closed and uniform oxide layer in and on can form the bonding layer. Training the uniform oxide layer is thereby supported, that the plasma is during the activation process around the entire surface of the material formed.

    Nach dem Plasmaprozeß wird die Anlage mit Stickstoff als Inertgas auf Normaldruck geflutet und der Werkstoff wieder auf seine Behandlungstemperatur von ca. 480°C bis 520°C erwärmt. Zur Anreicherung der oberflächennahen Verbindungsschicht mit Sauerstoff wird anschließend für den Oxidationsprozeß Wasserdampf zur Erzeugung eines Stickstoff-Wasserdampf-Gemisches in die Anlage geleitet. Nach Beendigung des Oxidationsprozesses wird der solchermaßen behandelte Werkstoff unter weiterer Stickstoffzufuhr abgekühlt.After the plasma process, the system with Nitrogen as inert gas flooded to normal pressure and the Material back to its treatment temperature of heated to about 480 ° C to 520 ° C. To enrich the near-surface bonding layer with oxygen is then water vapor for the oxidation process for generating a nitrogen-water vapor mixture directed to the plant. After completion of the oxidation process becomes the thus treated Material cooled under further nitrogen supply.

    Claims (5)

    1. Process for producing corrosion and wear protection layers on iron-based materials, in which near-surface regions are enriched with nitrogen, carbon and oxygen, characterized by the following process steps:
      a) nitrocarbiding the material under normal pressure to form a bonding layer consisting of iron carbonitrides;
      b) activating the surface of the material in a plasma-enhanced vacuum process, and
      c) oxidizing the material under normal pressure to form a closed oxide layer.
    2. Process according to Claim 1, characterized in that the iron carbonitrides ε - Fe2(N,C)1-x and/or δ'-Fe4(N,C)1-y are formed during the nitrocarbiding.
    3. Process according to one of Claims 1 to 2, characterized in that the oxidizing is carried out in a nitrogen/water vapour mixture of defined composition.
    4. Process according to one of Claims 1 to 3, characterized in that the oxidizing is, in particular, carried out in a temperature range of from 480°C to 520°C.
    5. Process according to one of Claims 1 to 4, characterized in that the material surface is bombarded with nitrogen, hydrogen, carbon and oxygen ions during the activation.
    EP96110790A 1995-07-11 1996-07-04 Method for producing corrosion and wear resistant protective coatings on iron based substrates Expired - Lifetime EP0753599B2 (en)

    Applications Claiming Priority (2)

    Application Number Priority Date Filing Date Title
    DE19525182 1995-07-11
    DE19525182A DE19525182C2 (en) 1995-07-11 1995-07-11 Process for the production of corrosion and wear protection layers on iron-based materials

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    EP0753599A1 EP0753599A1 (en) 1997-01-15
    EP0753599B1 EP0753599B1 (en) 1999-04-07
    EP0753599B2 true EP0753599B2 (en) 2005-04-13

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    US (1) US5679411A (en)
    EP (1) EP0753599B2 (en)
    JP (1) JP3185015B2 (en)
    KR (1) KR100245361B1 (en)
    AT (1) ATE178659T1 (en)
    BR (1) BR9603031A (en)
    CA (1) CA2180927C (en)
    DE (2) DE19525182C2 (en)

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    Publication number Priority date Publication date Assignee Title
    DE102007046231A1 (en) 2007-09-26 2009-04-09 Rudolf Fuka Gmbh Traction sheave for ropes or belt, has hub and multiple annular disks, where each disk has traction surface in its outer radial area on one of axial front faces
    DE102011053253A1 (en) 2011-09-05 2013-03-07 Fritz Winter Eisengiesserei Gmbh & Co. Kg Disc, useful for a disc brake, comprises carrier part and friction ring carried by carrier part, where friction ring as one joint partner and carrier part as another joint partner are connected together by fasteners made of steel material

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    KR100245361B1 (en) 2000-03-02
    EP0753599A1 (en) 1997-01-15
    DE59601585D1 (en) 1999-05-12
    ATE178659T1 (en) 1999-04-15
    KR970006536A (en) 1997-02-21
    JP3185015B2 (en) 2001-07-09
    CA2180927A1 (en) 1997-01-12
    CA2180927C (en) 2006-10-03
    EP0753599B1 (en) 1999-04-07
    US5679411A (en) 1997-10-21
    DE19525182C2 (en) 1997-07-17
    BR9603031A (en) 1998-05-05
    DE19525182A1 (en) 1997-01-16
    JPH09104960A (en) 1997-04-22

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