EP1122330B1 - Procédé et utilisation d' un dispositif pour la carbonitruration de pièces métalliques - Google Patents

Procédé et utilisation d' un dispositif pour la carbonitruration de pièces métalliques Download PDF

Info

Publication number
EP1122330B1
EP1122330B1 EP20000102360 EP00102360A EP1122330B1 EP 1122330 B1 EP1122330 B1 EP 1122330B1 EP 20000102360 EP20000102360 EP 20000102360 EP 00102360 A EP00102360 A EP 00102360A EP 1122330 B1 EP1122330 B1 EP 1122330B1
Authority
EP
European Patent Office
Prior art keywords
hydrocarbons
reaction gas
coefficient
ammonia
volume
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.)
Expired - Lifetime
Application number
EP20000102360
Other languages
German (de)
English (en)
Other versions
EP1122330A1 (fr
Inventor
Wolfgang Lerche
Bernd Edenhofer
Michael Lohrmann
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.)
Ipsen International GmbH
Original Assignee
Ipsen International 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 Ipsen International GmbH filed Critical Ipsen International GmbH
Priority to AT00102360T priority Critical patent/ATE280847T1/de
Priority to DE50008409T priority patent/DE50008409D1/de
Priority to EP20000102360 priority patent/EP1122330B1/fr
Priority to US09/562,698 priority patent/US6406560B1/en
Publication of EP1122330A1 publication Critical patent/EP1122330A1/fr
Application granted granted Critical
Publication of EP1122330B1 publication Critical patent/EP1122330B1/fr
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

Links

Images

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
    • C23C8/28—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 according to the preamble of claim 1.
  • the invention further relates to the Use of a device for performing such a method.
  • the surface layer is enriched with nitrogen by the ammonia (NH 3 ) contained in a reaction gas at temperatures of generally over 500 ° C under the catalytic effect of the surface of the workpieces to be nitrided decays into nitrogen (N) and hydrogen (H).
  • the ammonia molecule is adsorbed and gradually degraded on the workpiece surface, whereby the required nitrogen is released in atomic form and is available for solution in iron and for the formation of iron nitride (Fe x N).
  • the surface layer is simultaneously enriched with carbon.
  • Atomic carbon (C) diffuses in an analogous manner through the workpiece surface into the surface layer.
  • connection layer which, when nitriding or nitrocarburizing, mainly consists of hexagonal ⁇ -nitride (Fe 2-3 N) and face-centered cubic ⁇ '-nitride (Fe 4 N).
  • connection layer which, when nitriding or nitrocarburizing, mainly consists of hexagonal ⁇ -nitride (Fe 2-3 N) and face-centered cubic ⁇ '-nitride (Fe 4 N).
  • the carbon index K C for a reaction gas with a composition of 50% by volume ammonia (NH 3 ) and 50% by volume endogas which is usually used for nitrocarburizing with regard to an optimized content of ⁇ -nitride, has values between 1, 5 and 2.5, if the proportion of ammonia reacted during nitrocarburizing in the gas atmosphere is between 15% by volume and 40% by volume.
  • the carbonization index K C is significantly lower for a reaction gas with a composition of 50% by volume NH 3 , 45% by volume N 2 and 5% by volume CO 2 .
  • nitrocarburizing is carried out with a proportion of carbon dioxide in the gas atmosphere between 0 vol.% And 7 vol.% And a proportion of ammonia between 0 vol.% And 40 vol.%
  • the carbonization index K C values between 0 and 0.5 on. Due to the by the formula: CO + H 2 O ⁇ CO 2 + H 2 described balance of the components carbon monoxide (CO), water vapor (H 2 O) D, carbon dioxide (CO 2) and hydrogen (H 2) in the gas atmosphere, the nitriding potential K N K C and the carburizing interdependent.
  • the carbonization index K C can only be changed to a limited extent with a predetermined nitriding index K N and can therefore only be used to a limited extent to influence workpiece properties.
  • a disadvantage is furthermore that the carburizing K C in the commonly used reaction gases has not sufficiently high values such that the influenced by the content of carbon in the bonding layer technical properties of metallic workpieces, such as wear resistance or corrosion resistance, not to the extent possible can be exploited.
  • the invention is based on the object of developing a method for the heat treatment of metallic workpieces in such a way that an improved wear and corrosion resistance of the treated workpieces can be achieved.
  • unsaturated hydrocarbons of the type C n H 2n preferably ethylene (C 2 H 4 ) or propylene (C 2 H 6 ).
  • saturated hydrocarbons of the type C n H 2n + 2 preferably ethane (C 2 H 6 ) or propane (C 3 H 8 ). This is because thermal splitting of the saturated hydrocarbons during the course of the process can result in the formation of unsaturated hydrocarbons.
  • the hydrocarbons can advantageously also be added only while they are kept at a certain temperature, preferably a nitriding temperature between 500 ° C. and 700 ° C. With regard to a process control optimized with regard to the required workpiece properties, it may also be expedient to add the hydrocarbons only at the end of the holding to the nitriding temperature.
  • a particularly advantageous procedure is also given when the hydrocarbons are added discontinuously, for example only at certain times, which enables a process-adapted procedure.
  • the invention according to the proposed limitation of the addition of hydrocarbons to a proportion of 3 vol.% To 25 vol.% Depending on the composition of the reaction gas offers the advantage that an increased separation of free carbon, which generally leads to undesired sooting, for example the interior of heat treatment furnaces , leads, is avoided.
  • a reaction gas with a composition of 95% by volume ammonia (NH 3 ) and 5% by volume propane (C 3 H 8 ) is proposed, which can also be produced economically.
  • 1 and 2 show the content of carbon w C and nitrogen w N of the connecting layer of two nitrocarburized workpiece samples as a function of the edge distance r of the connecting layer.
  • the identical workpiece samples of the steel grade 16 Mn Cr 5 material no. 1.7131 were heated to a nitriding temperature of approx. 580 ° C in an ammonia-containing gas atmosphere of a chamber furnace.
  • the volume flow of reaction gases G 1 , G 2 flowing through the chamber furnace was in each case approximately 4 m 3 / h. After approximately 180 minutes of nitrocarburizing, the samples were cooled to room temperature in a nitrogen atmosphere. The connection layer determined afterwards was approx. 16 ⁇ m - 18 ⁇ m.
  • the depth profiles of carbon differ considerably from one another.
  • the curve of the carbon content in the workpiece sample treated with the reaction gas G 2 lies considerably above the carbon content achieved with the reaction gas G 1 up to the middle of the connecting layer and only then takes a course that roughly matches this and is approximately parallel to the drop in the nitrogen content.
  • the course of the carbon content in FIGS. 1 and 2 thus confirms that the addition of propane in the reaction gas G 2 produces a higher carbon content in the connecting layer, which results from a higher carbon index K C of the reaction gas G 2 and not least to one leads to improved wear and corrosion resistance of the workpiece sample.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Solid-Phase Diffusion Into Metallic Material Surfaces (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Claims (6)

  1. Procédé destiné à la nitrocarburation de matériaux ferreux dans une atmosphère de gaz contenant de l'azote, dans lequel la teneur en azote et en carbone présente dans la couche superficielle de la couche de liaison des pièces traitées est réglée de façon ciblée par un choix approprié de l'indice de nitruration KN et de l'indice de carburation KC d'un gaz de réaction contenant de l'ammoniac,
       caractérisé en ce que,
       pendant l'ensemble du traitement thermique, ou pendant le maintien à la température de nitruration comprise entre 500 °C et 700 °C, des hydrocarbures sont ajoutés de façon supplémentaire au gaz de réaction à raison d'une proportion de 3 % en volume à 25 % en volume d'hydrocarbures pour la génération d'une atmosphère de nitrocarburation, et que le couplage entre l'indice de carburation KC et l'indice de nitruration KN est de ce fait supprimé pendant le traitement.
  2. Procédé selon la revendication 1, caractérisé en ce qu'il est ajouté des hydrocarbures insaturés du type CnH2n, de préférence de l'éthylène (C2H4) ou du propylène (C2H6), ou des hydrocarbures saturés du type CnH2n+2, de préférence de l'éthane (C2H6) ou du propane (C3H8).
  3. Procédé selon la revendication 1 ou 2, caractérisé en ce que les hydrocarbures ne sont ajoutés que vers la fin du maintien à la température de nitruration.
  4. Procédé selon l'une quelconque des revendications 1 à 3, caractérisé en ce que les hydrocarbures sont ajoutés en discontinu.
  5. Procédé selon l'une quelconque des revendications précédentes, caractérisé par un gaz de réaction d'une composition de 95 % en volume d'ammoniac (NH3) et de 5 % en volume de propane (C3H8).
  6. Utilisation d'un dispositif pour la mise en oeuvre du procédé selon l'une quelconque des revendications précédentes, constitué d'un four de traitement thermique comportant une enceinte étanche aux gaz pouvant être chauffée pour la nitrocarburation de pièces métalliques, et un dispositif pour l'ajout dosé d'ammoniac et d'hydrocarbures.
EP20000102360 2000-02-04 2000-02-04 Procédé et utilisation d' un dispositif pour la carbonitruration de pièces métalliques Expired - Lifetime EP1122330B1 (fr)

Priority Applications (4)

Application Number Priority Date Filing Date Title
AT00102360T ATE280847T1 (de) 2000-02-04 2000-02-04 Verfahren und verwendung einer vorrichtung zum nitrocarburieren von eisenwerkstoffen
DE50008409T DE50008409D1 (de) 2000-02-04 2000-02-04 Verfahren und Verwendung einer Vorrichtung zum Nitrocarburieren von Eisenwerkstoffen
EP20000102360 EP1122330B1 (fr) 2000-02-04 2000-02-04 Procédé et utilisation d' un dispositif pour la carbonitruration de pièces métalliques
US09/562,698 US6406560B1 (en) 2000-02-04 2000-04-28 Method for the thermal treatment of metal

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
EP20000102360 EP1122330B1 (fr) 2000-02-04 2000-02-04 Procédé et utilisation d' un dispositif pour la carbonitruration de pièces métalliques

Publications (2)

Publication Number Publication Date
EP1122330A1 EP1122330A1 (fr) 2001-08-08
EP1122330B1 true EP1122330B1 (fr) 2004-10-27

Family

ID=8167774

Family Applications (1)

Application Number Title Priority Date Filing Date
EP20000102360 Expired - Lifetime EP1122330B1 (fr) 2000-02-04 2000-02-04 Procédé et utilisation d' un dispositif pour la carbonitruration de pièces métalliques

Country Status (4)

Country Link
US (1) US6406560B1 (fr)
EP (1) EP1122330B1 (fr)
AT (1) ATE280847T1 (fr)
DE (1) DE50008409D1 (fr)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102732820A (zh) * 2011-04-10 2012-10-17 上海上大热处理有限公司 汽车刹车盘的气体氮碳共渗方法
DE102013226090A1 (de) 2013-12-16 2015-06-18 Robert Bosch Gmbh Verfahren zum Gasnitrocarburieren
DE102013226091A1 (de) 2013-12-16 2015-06-18 Robert Bosch Gmbh Zylindertrommel einer hydrostatischen Axialkolbenmaschine mit einer Verschleißschutzschicht

Families Citing this family (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7622197B2 (en) * 2006-11-20 2009-11-24 Ferroxy-Aled, Llc Seasoned ferrous cookware
DE102009038598B4 (de) * 2009-08-26 2017-06-22 Ipsen International Gmbh Verfahren und Vorrichtung zur Aufbereitung von Prozessgasen für Wärmebehandlungen von metallischen Werkstoffen/Werkstücken in Industrieöfen
CN103703274B (zh) * 2011-06-30 2016-10-26 罗伯特·博世有限公司 用于无级变速器传动带的柔性环及其制造方法
US9389155B1 (en) * 2013-03-12 2016-07-12 United Technologies Corporation Fatigue test specimen
WO2019205114A1 (fr) * 2018-04-28 2019-10-31 邢台三厦铸铁有限公司 Ustensile de cuisine en fonte et procédé de traitement de sa surface

Family Cites Families (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4496401A (en) * 1981-10-15 1985-01-29 Lucas Industries Corrosion resistant steel components and method of manufacture thereof
FR2524006B1 (fr) * 1982-03-23 1985-10-11 Air Liquide Procede de durcissement superficiel de pieces metalliques
US4547228A (en) * 1983-05-26 1985-10-15 Procedyne Corp. Surface treatment of metals
DE3718240C1 (de) * 1987-05-30 1988-01-14 Ewald Schwing Verfahren zur Waermebehandlung von metallischen Werkstuecken in einer gasdurchstroemten Wirbelschicht
DE3937699A1 (de) * 1989-11-13 1991-05-16 Thaelmann Schwermaschbau Veb Verfahren zum herstellen von (epsilon)-karbonitridschichten definierter zusammensetzung
DD297053A5 (de) * 1990-08-23 1992-01-02 Zi Fuer Festkoerperphysik Und Werkstofforschung Der Adw,De Verschleissfeste epsilon-eisenkarbinitridschicht auf kohlenstoffhaltigen staehlen und verfahren zu ihrer herstellung
DE4033706A1 (de) * 1990-10-24 1991-02-21 Hans Prof Dr Ing Berns Einsatzhaerten mit stickstoff zur verbesserung des korrosionswiderstandes martensitischer nichtrostender staehle
RU2048601C1 (ru) * 1993-12-20 1995-11-20 Рыжов Николай Михайлович Способ диагностики процесса химико-термической обработки сталей и сплавов в тлеющем разряде и устройство для его осуществления
DE19509614A1 (de) * 1995-03-21 1996-09-26 Hans Ruediger Dr Ing Hoffmann Regelung von Nitrier- und Nitrocarburieratmosphären
DE19719225C1 (de) * 1997-05-07 1998-08-06 Volker Dipl Ing Leverkus Verfahren zur Regelung einer Nitrier- bzw. Nitrocarburier-Atmosphäre sowie Vorrichtung zur Durchführung des Verfahrens

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102732820A (zh) * 2011-04-10 2012-10-17 上海上大热处理有限公司 汽车刹车盘的气体氮碳共渗方法
CN102732820B (zh) * 2011-04-10 2015-01-21 上海上大热处理有限公司 汽车刹车盘的气体氮碳共渗方法
DE102013226090A1 (de) 2013-12-16 2015-06-18 Robert Bosch Gmbh Verfahren zum Gasnitrocarburieren
DE102013226091A1 (de) 2013-12-16 2015-06-18 Robert Bosch Gmbh Zylindertrommel einer hydrostatischen Axialkolbenmaschine mit einer Verschleißschutzschicht
US9970093B2 (en) 2013-12-16 2018-05-15 Robert Bosch Gmbh Method for gas carbonitriding
US10281042B2 (en) 2013-12-16 2019-05-07 Robert Bosch Gmbh Cylinder drum of a hydrostatic axial piston machine having a wear-resistant layer

Also Published As

Publication number Publication date
US6406560B1 (en) 2002-06-18
DE50008409D1 (de) 2004-12-02
ATE280847T1 (de) 2004-11-15
EP1122330A1 (fr) 2001-08-08

Similar Documents

Publication Publication Date Title
DE3486037T2 (de) Korrosionsgeschuetzte werkstuecke aus stahl und verfahren zu ihrer herstellung.
DE69803389T2 (de) Verfahren zur behandlung von produkten aus austenitischem, rostfreiem stahl
DE69021658T2 (de) Verfahren zum Wärmebehandeln von Metallen.
EP1122330B1 (fr) Procédé et utilisation d' un dispositif pour la carbonitruration de pièces métalliques
DE2450879A1 (de) Verfahren zur waermebehandlung von eisenmetallen
DE2658174A1 (de) Verfahren zum nitrierhaerten martensitischer staehle
EP0049530A1 (fr) Procédé et dispositif pour carburer des pièces en acier
DE2135763B2 (de) Verfahren zur Behandlung von Eisen- und Stahlgegenständen zur Bildung einer Nitridschicht
DE2934930C2 (fr)
EP0662525B1 (fr) Procédé pour empêcher l'oxydation superficielle pendant la carburation des aciers
DE69902169T2 (de) Verfahren zum niederdrück-nitrocarburieren metallischer werkstücke
EP1122331B1 (fr) Procédé pour la nitruration et/ou carbonitruration d' acier fortement allié
EP0882811B1 (fr) Procédé de cémentation de pièces métalliques dans un four sous vide
DE1521450C3 (de) Atmosphäre für das !Carbonitrieren von Baustahl und Gußeisen bei niedrigen Temperaturen
DE3810892A1 (de) Verfahren zur nitrokarburierung und nitrierung von eisenhaltigen oberflaechen
EP1230415B1 (fr) Procede pour la nitro-carburation de pieces metalliques
DE19523956A1 (de) Verfahren zur Karburierungs- oder Karbonitrierungsbehandlung von Stählen
DE2109997C3 (de) Verfahren zum Oberflächeniegieren, insbesondere Inchromieren von Eisenwerkstoffen
DE2539722B2 (de) Verfahren zur thermischen Behandlung von Stahl in reduzierender und nicht entkohlender Atmosphäre
EP1050592A1 (fr) Procédé de traitement thermique de pièces métalliques
DE3937699A1 (de) Verfahren zum herstellen von (epsilon)-karbonitridschichten definierter zusammensetzung
WO2001055471A1 (fr) Procede de carbonitruration d'aciers a haute teneur en carbone et fortement allies
DE102019202101A1 (de) Verfahren zum Randschichthärten von Bauteilen aus nichtrostenden Stählen
DE758345C (de) Herstellung eines Gases fuer die Stahlzementation
DE2000060A1 (de) Verfahren zur Beschleunigung des Aufkohlens von Werkstuecken aus Stahl nach dem Generator-Traegergasverfahren

Legal Events

Date Code Title Description
PUAI Public reference made under article 153(3) epc to a published international application that has entered the european phase

Free format text: ORIGINAL CODE: 0009012

17P Request for examination filed

Effective date: 20000819

AK Designated contracting states

Kind code of ref document: A1

Designated state(s): AT CH DE FR GB IT LI

AX Request for extension of the european patent

Free format text: AL;LT;LV;MK;RO;SI

AKX Designation fees paid

Free format text: AT CH DE FR GB IT LI

17Q First examination report despatched

Effective date: 20020510

GRAP Despatch of communication of intention to grant a patent

Free format text: ORIGINAL CODE: EPIDOSNIGR1

GRAS Grant fee paid

Free format text: ORIGINAL CODE: EPIDOSNIGR3

GRAA (expected) grant

Free format text: ORIGINAL CODE: 0009210

AK Designated contracting states

Kind code of ref document: B1

Designated state(s): AT CH DE FR GB IT LI

REG Reference to a national code

Ref country code: GB

Ref legal event code: FG4D

Free format text: NOT ENGLISH

REG Reference to a national code

Ref country code: CH

Ref legal event code: EP

Ref country code: CH

Ref legal event code: NV

Representative=s name: E. BLUM & CO. PATENTANWAELTE

REF Corresponds to:

Ref document number: 50008409

Country of ref document: DE

Date of ref document: 20041202

Kind code of ref document: P

GBT Gb: translation of ep patent filed (gb section 77(6)(a)/1977)

Effective date: 20050207

ET Fr: translation filed
PLBE No opposition filed within time limit

Free format text: ORIGINAL CODE: 0009261

STAA Information on the status of an ep patent application or granted ep patent

Free format text: STATUS: NO OPPOSITION FILED WITHIN TIME LIMIT

26N No opposition filed

Effective date: 20050728

REG Reference to a national code

Ref country code: CH

Ref legal event code: PFA

Owner name: IPSEN INTERNATIONAL GMBH

Free format text: IPSEN INTERNATIONAL GMBH#FLUTSTRASSE 78#47533 KLEVE (DE) -TRANSFER TO- IPSEN INTERNATIONAL GMBH#FLUTSTRASSE 78#47533 KLEVE (DE)

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: CH

Payment date: 20140218

Year of fee payment: 15

Ref country code: DE

Payment date: 20140219

Year of fee payment: 15

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: AT

Payment date: 20140212

Year of fee payment: 15

Ref country code: IT

Payment date: 20140225

Year of fee payment: 15

Ref country code: FR

Payment date: 20140219

Year of fee payment: 15

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: GB

Payment date: 20140218

Year of fee payment: 15

REG Reference to a national code

Ref country code: DE

Ref legal event code: R119

Ref document number: 50008409

Country of ref document: DE

REG Reference to a national code

Ref country code: CH

Ref legal event code: PL

REG Reference to a national code

Ref country code: AT

Ref legal event code: MM01

Ref document number: 280847

Country of ref document: AT

Kind code of ref document: T

Effective date: 20150204

GBPC Gb: european patent ceased through non-payment of renewal fee

Effective date: 20150204

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: LI

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20150228

Ref country code: CH

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20150228

REG Reference to a national code

Ref country code: FR

Ref legal event code: ST

Effective date: 20151030

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: AT

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20150204

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: IT

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20150204

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: GB

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20150204

Ref country code: DE

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20150901

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: FR

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20150302