EP1246950A1 - Compacting and sintering steel powder - Google Patents

Compacting and sintering steel powder

Info

Publication number
EP1246950A1
EP1246950A1 EP00981941A EP00981941A EP1246950A1 EP 1246950 A1 EP1246950 A1 EP 1246950A1 EP 00981941 A EP00981941 A EP 00981941A EP 00981941 A EP00981941 A EP 00981941A EP 1246950 A1 EP1246950 A1 EP 1246950A1
Authority
EP
European Patent Office
Prior art keywords
mpa
compacting
sintering
temperature
treated
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.)
Granted
Application number
EP00981941A
Other languages
German (de)
French (fr)
Other versions
EP1246950B1 (en
Inventor
Hanna; WIŚNIEWSKA-WEINERT
Ewgienij Stepanowicz; Sewastianow
Michajlowicz Leszczynski Wolf
Aleksandr Anatolewicz; Stojanow
Jurij Jakowlewicz; Kuczma
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.)
Instytut Obrobki Plastycznej
Original Assignee
Instytut Obrobki Plastycznej
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 Instytut Obrobki Plastycznej filed Critical Instytut Obrobki Plastycznej
Publication of EP1246950A1 publication Critical patent/EP1246950A1/en
Application granted granted Critical
Publication of EP1246950B1 publication Critical patent/EP1246950B1/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C33/00Making ferrous alloys
    • C22C33/02Making ferrous alloys by powder metallurgy
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/12Both compacting and sintering
    • B22F3/16Both compacting and sintering in successive or repeated steps
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2998/00Supplementary information concerning processes or compositions relating to powder metallurgy
    • B22F2998/10Processes characterised by the sequence of their steps

Definitions

  • the invention concerns a method of getting shaped elements by pressing, sintering and cold-compacting of powder mixtures of steel with alloy additions, being used for production of machine parts, e.g. gears, bearings and others of high wear resistance and surface pressures.
  • a product from powder alloy steel is twice pressed and twice sintered at temperatures 800 °C and 1 150 °C.
  • Parts obtained by this method have insufficient strength parameters, in particular low bending strength.
  • Parts obtained by this method are characterized by low strength parameters, in particular low compressibility of ring products at radial action of a force.
  • Plastic forming of a presintered semi-final product follows forming and shift of dislocation through crystal lattice along definite surfaces and dislocation forces.
  • Plasticity of a sintered product, particularly density of a final product increases if, during first sintering, there is elimination of forming of factors inhibiting motion of dislocation shift, such as forming: a hard solution, fine-grained particles, secondary phases, etc.
  • the first sintering should be conducted in conditions of recrystallization annealing at temperature A c ⁇ .
  • Structure of die stampings from constructional steel powders is a mixture of separate components (if a matrix is iron powder with graphite additions) or an alloy ferrite (if a matrix is iron powder with alloy additions).
  • Optimum temperature of presintering should be from 720 °C to 730 °C. At this temperature, solubility of carbon in ⁇ -iron is about 0.03%, and after sintering in state of recrystallization annealing of a product, is characterized by low hardness coefficients as a result of lack of such consolidation factors as secondary phases, particle dispersability, etc.
  • interparticle contact points make a system of glide planes, which is used as a system of glide planes inside grains and particles at ambient (room) temperature. Gliding along interparticle connections takes place under outside presssure, what has an essential importance to the process of plastic strain.
  • Similar model can be called a model for staresuper dislocation" because it is based on an effective gliding along particle boundaries as a result of particular shift kind ofcrowdedspace contact lattice". This leads to additional, significant increase of sintered semi-final product palsticity, because it is known that metal material plasticity increases significantly if an additional mechanism of plastic strain, besides gliding at dislocation shift, is introduced into a process of plastic metal flow.
  • the essence of the invention concerning a method of getting shaped elements by pressing, sintering and compacting of powder mixtures of steel with alloy additions, consists in that a preformed element is treated with presintering. preferably in dissociated-ammonia atmosphere at temperature 700 - 750 °C, preferably 720 - 730 °C, during 20 - 40 min, preferably 30 min, and first compacting under pressure 700 - 800 MPa, preferably 750 MPa, and then second compacting with simultaneous calibration under pressure 900 - 1000 MPa, preferably 950 MPa, then final sintering at temperature 1100 - 1200 °C, preferably
  • Preformed semi-final product from powder mixtures of steel with alloy additions of brass, nickel, copper, and others is treated with presintering in dissociated-ammonia atmosphere at temperature 725 ⁇ 5 °C during 30 min, and treated with compacting under pressure 750 MPa. Then it is treated with second compacting under pressure 950 MPa and calibration, then final sintering at temperature 1 130 °C during 45 min.
  • Preformed semi-final product from powder mixtures of steel with alloy additions of brass, nickel, copper, and others is treated with presintering in dissociated-ammonia atmosphere at temperature 740 ⁇ 5 °C during 25 min, and first compacting under pressure 780 MPa. So prepared element is treated with second compacting under pressure 980 MPa and calibration, then final sintering at temperature 1 180 °C during 40 min.
  • Preformed semi-final product from powder mixtures of steel with alloy additions of brass, nickel, copper, and others is treated with presintering in dissociated-ammonia atmosphere at temperature 710 ⁇ 5 °C during 35 min, and first compacting under pressure 710 MPa, then it is treated with second compacting under pressure 910 MPa and calibration, then final sintering at temperature 1 100 °C during 50 min.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Powder Metallurgy (AREA)
  • Processing Of Stones Or Stones Resemblance Materials (AREA)
  • Mechanical Treatment Of Semiconductor (AREA)

Abstract

The invention concerns a method of getting shaped elements by pressing, sintering and cold-compacting of powder mixtures of steel with alloy additions, being used for production of machine parts, e.g. gears, bearings and others of high surface pressure strength and wear resistance. The method is characterized in that a preformed semi-final product is treated with presintering, preferably in dissociated-ammonia atmosphere at temperature 700 - 750 DEG C, preferably 720 - 730 DEG C during 20 - 40 min, preferably 30 min, and first compacting under pressure 700 - 800 MPa, preferably 750 MPa, and then second compacting with simultaneous calibration under pressure 900 - 1000 MPa, preferably 950 MPa, then is treated with final sintering at temperature 1100 - 1200 DEG C, preferably 1120 - 1150 DEG C, during 40 - 50 min, preferably 45 min.

Description

COMPACTING AND SINTERING STEEL POWDER
The invention concerns a method of getting shaped elements by pressing, sintering and cold-compacting of powder mixtures of steel with alloy additions, being used for production of machine parts, e.g. gears, bearings and others of high wear resistance and surface pressures.
In well-known solutions, constructional parts from powder mixtures with alloy additions are made by pressing and sintering at temperature 1 100 - 1 150 °C in a protective atmosphere. Products obtained by this method are characterized by high porosity up to 12% of volume and low compression strength.
In other method, a product from powder alloy steel is twice pressed and twice sintered at temperatures 800 °C and 1 150 °C.
In this solution, obtained products also do not get required high strength parameters.
There is also known a method of getting parts from powder mixtures of constructional steel with alloy additions, consisting in pressing, presintering at temperature 800 - 850 °C, strain of presintered semi-finished product and final sintering at temperature 1 120 - 1 180 °C in a protective atmosphere.
Parts obtained by this method have insufficient strength parameters, in particular low bending strength.
Moreover there is known a method of getting parts from metal powders with alloy additions, where pressing, presintering at temperature 650 °C, second pressing and second sintering at temperature 1150 °C are carried out.
Parts obtained by this method are characterized by low strength parameters, in particular low compressibility of ring products at radial action of a force.
Presented above methods of getting products of steel powder mixtures with alloy additions do not precise pressure values that are to act onto shaped part, as well as they do not specify exact time during which sintering should be performed, giving a very wide temperature range.
Compacting of powders in a closed pressing die under pressure is performed as a result of mutual shift and plastic strain of material particles. Their mutual wedging at some stage stops the mutual shift of particles. Further increasing of product densities under influence of press pressure force can take place thanks to deformation of particular particles. Intensive cold work of being pressed particles and further increasing pressing force are used to overcome outside friction forces at contact: powder material and a pressing tool. The result is to get high porosity after single pressing within limits from 15% to 20%.
Further increasing of product density can be obtained thanks to increasing of compact plasticity, which occurs during presintering at temperatures equal to annealing temperature of common metal. Process of presintering at annealing temperature increases powder material plasticity making possible to increase product density through its plastic strain.
Plastic forming of a presintered semi-final product, like for solid material, follows forming and shift of dislocation through crystal lattice along definite surfaces and dislocation forces. Plasticity of a sintered product, particularly density of a final product increases if, during first sintering, there is elimination of forming of factors inhibiting motion of dislocation shift, such as forming: a hard solution, fine-grained particles, secondary phases, etc.
That is why the first sintering should be conducted in conditions of recrystallization annealing at temperature Acι. Structure of die stampings from constructional steel powders is a mixture of separate components (if a matrix is iron powder with graphite additions) or an alloy ferrite (if a matrix is iron powder with alloy additions). Optimum temperature of presintering should be from 720 °C to 730 °C. At this temperature, solubility of carbon in α-iron is about 0.03%, and after sintering in state of recrystallization annealing of a product, is characterized by low hardness coefficients as a result of lack of such consolidation factors as secondary phases, particle dispersability, etc.
It is well-known that diffusion motion of iron atoms in carbon steels in state before transformation (in constructional steels, with admixture of Cr, Mo, Ni, Cu) at 720 °C - 730 °C is approximately of the same value as in a compound of γ-iron at
1 100 °C - 1200 °C. Incorrect, diffusion mobility of iron atoms in the range of temperatures 720 °C - 730 °C leads, at material sintering, to formation of powder interaction focuses, the concentration of which is determined by sintering time. The powder interaction focus may be generally defined by positions of atoms belonging to both powder particles, separated with interparticle boundaries - contact points. The powder interaction focus, defined by above definitions, is convergent with „space contact lattice", and its growth takes place not only as a result of shift of „space contact lattice" along boundary surfaces but also by approaching parameters of „space contact lattice" to matrix crystal lattice. If a solution of carbon and alloy additions in iron at 720 °C - 730 °C does not take place, then parameters of „space contact lattice" can be changed in wide range by changing time of sintering at above temperatures.
After determined time of sintering, interparticle contact points make a system of glide planes, which is used as a system of glide planes inside grains and particles at ambient (room) temperature. Gliding along interparticle connections takes place under outside presssure, what has an essential importance to the process of plastic strain. Similar model can be called a model for „super dislocation" because it is based on an effective gliding along particle boundaries as a result of particular shift kind of „space contact lattice". This leads to additional, significant increase of sintered semi-final product palsticity, because it is known that metal material plasticity increases significantly if an additional mechanism of plastic strain, besides gliding at dislocation shift, is introduced into a process of plastic metal flow.
Taking into account above-mentioned conditions, a method being a subject of the invention has been developed.
The essence of the invention, concerning a method of getting shaped elements by pressing, sintering and compacting of powder mixtures of steel with alloy additions, consists in that a preformed element is treated with presintering. preferably in dissociated-ammonia atmosphere at temperature 700 - 750 °C, preferably 720 - 730 °C, during 20 - 40 min, preferably 30 min, and first compacting under pressure 700 - 800 MPa, preferably 750 MPa, and then second compacting with simultaneous calibration under pressure 900 - 1000 MPa, preferably 950 MPa, then final sintering at temperature 1100 - 1200 °C, preferably
1 120 - 1 150 °C, during 40 - 50 min, preferably 45 min. Thanks to use of the method according to the invention, the following technical-and-operational effects were gained:
- high wear, crushing, shear and compressive strength of got product
- high yield point,
- density of got product above 7.6 g/cm3,
- low material flow coefficient, in the range 10"2 - 10"3 mm,
- decrease of production power consumption,
- possible use for products of optional shapes, optional application, especially for products of required high strength as gears, bearings, etc.
Subject of the invention is shown in the following exemplary embodiments:
Example I
Preformed semi-final product from powder mixtures of steel with alloy additions of brass, nickel, copper, and others is treated with presintering in dissociated-ammonia atmosphere at temperature 725±5 °C during 30 min, and treated with compacting under pressure 750 MPa. Then it is treated with second compacting under pressure 950 MPa and calibration, then final sintering at temperature 1 130 °C during 45 min.
Example II
Preformed semi-final product from powder mixtures of steel with alloy additions of brass, nickel, copper, and others is treated with presintering in dissociated-ammonia atmosphere at temperature 740±5 °C during 25 min, and first compacting under pressure 780 MPa. So prepared element is treated with second compacting under pressure 980 MPa and calibration, then final sintering at temperature 1 180 °C during 40 min.
Example III
Preformed semi-final product from powder mixtures of steel with alloy additions of brass, nickel, copper, and others is treated with presintering in dissociated-ammonia atmosphere at temperature 710±5 °C during 35 min, and first compacting under pressure 710 MPa, then it is treated with second compacting under pressure 910 MPa and calibration, then final sintering at temperature 1 100 °C during 50 min. In the enclosed table, the results of strength tests of parts made from powder mixtures of steel with alloy additions, made with the method according to the invention at different temperatures of the first sintering compared with standard sample made with hitherto method.

Claims

Claim
A method of getting shaped elements by sintering and pressing, of powder mixtures of steel with alloy additions, characterized in that a preformed semi-final product is treated with presintering, preferably in dissociated-ammonia atmosphere at temperature 700 - 750 °C, preferably 720 - 730 °C during 20 - 40 min, preferably 30 min, and first compacting under pressure 700 - 800 MPa, preferably 750 MPa, and then second compacting with simultaneous calibration under pressure 900 - 1000 MPa, preferably 950 MPa, then treated with final sintering at temperature 1 100 - 1200 °C, preferably 1120 - 1150 °C, during 40 - 50 min, preferably 45 min.
EP00981941A 1999-12-31 2000-12-14 Compacting and sintering steel powder Expired - Lifetime EP1246950B1 (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
PL33763799 1999-12-31
PL337637A PL191806B1 (en) 1999-12-31 1999-12-31 Method of obtaining shaped workpieces
PCT/PL2000/000098 WO2001049891A1 (en) 1999-12-31 2000-12-14 Compacting and sintering steel powder

Publications (2)

Publication Number Publication Date
EP1246950A1 true EP1246950A1 (en) 2002-10-09
EP1246950B1 EP1246950B1 (en) 2003-07-23

Family

ID=20075799

Family Applications (1)

Application Number Title Priority Date Filing Date
EP00981941A Expired - Lifetime EP1246950B1 (en) 1999-12-31 2000-12-14 Compacting and sintering steel powder

Country Status (5)

Country Link
EP (1) EP1246950B1 (en)
AT (1) ATE245715T1 (en)
DE (1) DE60004106T2 (en)
PL (1) PL191806B1 (en)
WO (1) WO2001049891A1 (en)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102004002714B3 (en) * 2004-01-19 2005-05-19 SCHWäBISCHE HüTTENWERKE GMBH To produce sintered components, of light metal alloys, the powder is compressed into a green compact to be give a low temperature sintering followed by further compression and high temperature sintering

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2648519B2 (en) * 1989-10-03 1997-09-03 日立粉末冶金株式会社 Method of manufacturing synchronizer hub
US5080712B1 (en) * 1990-05-16 1996-10-29 Hoeganaes Corp Optimized double press-double sinter powder metallurgy method
EP0934134A4 (en) * 1996-05-13 2003-07-30 Gkn Sinter Metals Inc Method for preparing high performance ferrous materials

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See references of WO0149891A1 *

Also Published As

Publication number Publication date
DE60004106T2 (en) 2004-04-22
PL191806B1 (en) 2006-07-31
PL337637A1 (en) 2001-07-02
ATE245715T1 (en) 2003-08-15
WO2001049891A1 (en) 2001-07-12
EP1246950B1 (en) 2003-07-23
DE60004106D1 (en) 2003-08-28

Similar Documents

Publication Publication Date Title
US5080712A (en) Optimized double press-double sinter powder metallurgy method
EP0331679B1 (en) High density sintered ferrous alloys
CN101124058B (en) Stainless steel powder
EP2207907B1 (en) Metallurgical powder composition and method of production
EP1844172B1 (en) Iron-based powder combination
JP2009203544A (en) Hard alloy material, production method, and tool and wear resistant member
EP2662167B1 (en) Hot pressed net or near net shape powder component
EP1246950B1 (en) Compacting and sintering steel powder
Romanski et al. Ball-milled Fe-Ni and Fe-Mn matrix powders for sintered diamond tools
Graham Wilson et al. The Preparation of Carbide-Enriched Tool Steels by Powder Metallurgy
US4603028A (en) Method of manufacturing sintered components
Wang Properties of high density powder forged iron based alloy
Kandavel et al. Experimental Investigations on Plastic Deformation and Densification Characteristics of P/M Fe–C–Cu–Mo Alloy Steels Under Cold Upsetting
KR0178578B1 (en) Method for manufacturing cementer carbides sintered body
Upadhyaya Processing and properties of sintered tool steels and cemented carbides
Sakamoto et al. Mechanical properties of high density sintered compacts obtained by cold-working
Kobayashi et al. Effect of small cold-reductions on mechanical properties of sintered steels
Borowiecka-Jamrozek Sintered FeCuRe Alloys Produced from Commercially Available Powders
JPH05156404A (en) High-strength sintered hard alloy
Zak-Szwed et al. IRON-BASE PM MATRIX ALLOYS FOR DIAMOND-IMPREGNATED TOOLS.
JPH0499805A (en) Complex hard sintered material having excellent wear resistance and melt-welding resistance and manufacture thereof
Azadbeh et al. The Influence of First Compaction on Properties and Microstructure of Double Pressed Cr-Mo Prealloyed Sintered Steel
Suzuki et al. Sinter hardening character of prealloyed 46 F 3 H steel powder
CN108486419A (en) A kind of preparation method of food-grade table knife
JPH0578712A (en) Production of sintered part

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

AK Designated contracting states

Kind code of ref document: A1

Designated state(s): AT BE CH CY DE DK ES FI FR GB GR IE IT LI LU MC NL PT SE TR

17P Request for examination filed

Effective date: 20020718

GRAH Despatch of communication of intention to grant a patent

Free format text: ORIGINAL CODE: EPIDOS IGRA

GRAH Despatch of communication of intention to grant a patent

Free format text: ORIGINAL CODE: EPIDOS IGRA

GRAA (expected) grant

Free format text: ORIGINAL CODE: 0009210

AK Designated contracting states

Designated state(s): AT BE CH CY DE DK ES FI FR GB GR IE IT LI LU MC NL PT SE TR

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 FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT;WARNING: LAPSES OF ITALIAN PATENTS WITH EFFECTIVE DATE BEFORE 2007 MAY HAVE OCCURRED AT ANY TIME BEFORE 2007. THE CORRECT EFFECTIVE DATE MAY BE DIFFERENT FROM THE ONE RECORDED.

Effective date: 20030723

Ref country code: TR

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20030723

Ref country code: FI

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20030723

Ref country code: AT

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20030723

Ref country code: CH

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20030723

Ref country code: FR

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20030723

Ref country code: BE

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20030723

Ref country code: LI

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20030723

Ref country code: NL

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20030723

REG Reference to a national code

Ref country code: GB

Ref legal event code: FG4D

REG Reference to a national code

Ref country code: CH

Ref legal event code: EP

REG Reference to a national code

Ref country code: IE

Ref legal event code: FG4D

REF Corresponds to:

Ref document number: 60004106

Country of ref document: DE

Date of ref document: 20030828

Kind code of ref document: P

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

Ref country code: SE

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20031023

Ref country code: GR

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20031023

Ref country code: DK

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20031023

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

Ref country code: ES

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20031103

NLV1 Nl: lapsed or annulled due to failure to fulfill the requirements of art. 29p and 29m of the patents act
PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: CY

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20031214

Ref country code: LU

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

Effective date: 20031214

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

Ref country code: IE

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

Effective date: 20031215

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

Ref country code: PT

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20031223

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

Ref country code: MC

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

Effective date: 20031231

REG Reference to a national code

Ref country code: CH

Ref legal event code: PL

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: 20040426

EN Fr: translation not filed
REG Reference to a national code

Ref country code: IE

Ref legal event code: MM4A

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: 20041214

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

Effective date: 20041214

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

Ref country code: DE

Payment date: 20151208

Year of fee payment: 16

REG Reference to a national code

Ref country code: DE

Ref legal event code: R119

Ref document number: 60004106

Country of ref document: DE

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

Ref country code: DE

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

Effective date: 20170701