EP3077556B1 - Verfahren zur bearbeitung einer dispersionsgehärteten platinzusammensetzung - Google Patents
Verfahren zur bearbeitung einer dispersionsgehärteten platinzusammensetzung Download PDFInfo
- Publication number
- EP3077556B1 EP3077556B1 EP14812166.8A EP14812166A EP3077556B1 EP 3077556 B1 EP3077556 B1 EP 3077556B1 EP 14812166 A EP14812166 A EP 14812166A EP 3077556 B1 EP3077556 B1 EP 3077556B1
- Authority
- EP
- European Patent Office
- Prior art keywords
- dispersion
- temperature
- hardened platinum
- hardened
- cold forming
- 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.)
- Active
Links
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 title claims description 180
- 229910052697 platinum Inorganic materials 0.000 title claims description 91
- 239000000203 mixture Substances 0.000 title claims description 56
- 238000000034 method Methods 0.000 title claims description 53
- 238000011282 treatment Methods 0.000 title claims description 19
- 230000008569 process Effects 0.000 title claims description 13
- 238000005096 rolling process Methods 0.000 claims description 46
- 239000000463 material Substances 0.000 claims description 29
- 239000010970 precious metal Substances 0.000 claims description 14
- 229910052727 yttrium Inorganic materials 0.000 claims description 11
- 229910052726 zirconium Inorganic materials 0.000 claims description 10
- 229910052706 scandium Inorganic materials 0.000 claims description 9
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 8
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 8
- SIXSYDAISGFNSX-UHFFFAOYSA-N scandium atom Chemical compound [Sc] SIXSYDAISGFNSX-UHFFFAOYSA-N 0.000 claims description 8
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims description 8
- 229910052684 Cerium Inorganic materials 0.000 claims description 7
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 claims description 7
- 230000003647 oxidation Effects 0.000 claims description 7
- 238000007254 oxidation reaction Methods 0.000 claims description 7
- 238000012545 processing Methods 0.000 claims description 7
- 229910052703 rhodium Inorganic materials 0.000 claims description 7
- 239000010948 rhodium Substances 0.000 claims description 7
- 230000001590 oxidative effect Effects 0.000 claims description 6
- 238000005496 tempering Methods 0.000 claims description 6
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 claims description 5
- 238000003825 pressing Methods 0.000 claims description 5
- 229910052707 ruthenium Inorganic materials 0.000 claims description 5
- 230000007547 defect Effects 0.000 claims description 4
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 4
- 229910052737 gold Inorganic materials 0.000 claims description 4
- 239000010931 gold Substances 0.000 claims description 4
- 229910052741 iridium Inorganic materials 0.000 claims description 4
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 claims description 4
- 229910052763 palladium Inorganic materials 0.000 claims description 4
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 claims description 4
- 239000011521 glass Substances 0.000 claims description 3
- 238000000137 annealing Methods 0.000 description 30
- 229910000510 noble metal Inorganic materials 0.000 description 30
- 239000011265 semifinished product Substances 0.000 description 20
- 239000002243 precursor Substances 0.000 description 18
- 230000009467 reduction Effects 0.000 description 17
- 239000007787 solid Substances 0.000 description 15
- 230000000052 comparative effect Effects 0.000 description 13
- 239000000047 product Substances 0.000 description 13
- 238000005482 strain hardening Methods 0.000 description 11
- 238000001354 calcination Methods 0.000 description 8
- 230000006872 improvement Effects 0.000 description 8
- 239000011148 porous material Substances 0.000 description 5
- 229910045601 alloy Inorganic materials 0.000 description 4
- 239000000956 alloy Substances 0.000 description 4
- 230000008859 change Effects 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 150000004706 metal oxides Chemical class 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 238000001953 recrystallisation Methods 0.000 description 4
- 230000009466 transformation Effects 0.000 description 4
- 238000000844 transformation Methods 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- 238000007796 conventional method Methods 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 3
- 230000006978 adaptation Effects 0.000 description 2
- 230000006735 deficit Effects 0.000 description 2
- 230000032798 delamination Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 229910001260 Pt alloy Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000005097 cold rolling Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000007669 thermal treatment Methods 0.000 description 1
- 238000011144 upstream manufacturing Methods 0.000 description 1
- 230000003313 weakening effect Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/14—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of noble metals or alloys based thereon
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
- C22C1/1078—Alloys containing non-metals by internal oxidation of material in solid state
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/001—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides
- C22C32/0015—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides with only single oxides as main non-metallic constituents
- C22C32/0021—Matrix based on noble metals, Cu or alloys thereof
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C5/00—Alloys based on noble metals
- C22C5/04—Alloys based on a platinum group metal
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/24—After-treatment of workpieces or articles
- B22F2003/248—Thermal after-treatment
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
Definitions
- the invention relates to a method for processing a dispersion-hardened platinum composition. Further, the present invention describes a process for producing a product from a dispersion-hardened platinum composition. Furthermore, the present invention relates to a product obtainable from the methods set out above and the use of such platinum compositions.
- Platinum shaped bodies are frequently used in high-temperature processes in which the material must have high corrosion resistance.
- platinum components are used in the glass industry which are mechanically stressed, such as stirrers or glass fiber nozzle trays.
- a disadvantage of platinum as a material is its low mechanical strength at high temperatures. Therefore, dispersion hardened platinum compositions are generally used for the aforementioned high temperature processes.
- a billet is generally first produced which is hot-rolled.
- the resulting semi-finished product can then be cold-formed.
- the object of the invention is therefore to overcome the disadvantages of the prior art.
- the method should be a cost-effective adaptation of components of platinum compositions to individual needs while improving the mechanical Enable properties.
- the components obtained should show a long service life and the lowest possible wear.
- the method should be simple and inexpensive to carry out.
- the formed components should have a good processability, in particular weldability.
- the surface area of that surface is to be understood, which is formed at an (imaginary) section through the solid.
- the plane spanned by the cross-sectional area may or may not be perpendicular or substantially perpendicular to the longest extent of the solid.
- weight percentages set out above add up to 100%, the weight of the non-noble metals being based on the weight of metal.
- the non-noble metal or non-noble metals are at least 70%, preferably at least 90% oxidized with oxygen.
- all oxidation states of the non-noble metals are taken into account so that preferably at most 30 atomic%, particularly preferably at most 10 atomic% of the non-noble metal is present as metal, that is to say in the formal oxidation state 0.
- Solid bodies with low levels of non-noble metal oxides show advantages in terms of processability, for example weldability of the solid bodies.
- a solid is provided.
- the term solid is to be understood here comprehensively.
- a solid can be configured for example in the form of a sheet, a pipe or a wire.
- the sheets, tubes or wires provided may have a thickness in the range of 0.1 mm to 10 mm, preferably 0.3 to 5 mm.
- the thickness refers to the minimum extent of a solid.
- a wire this is the diameter and for a pipe, the difference between the outer and inner radius, which is also referred to as the wall thickness of the pipe.
- the platinum composition which can be used according to the invention comprises at least 70% by weight of platinum and a maximum of 29.95% by weight of other noble metals. Accordingly, the composition may consist essentially of platinum and the at least partially oxidized non-noble metals set forth above.
- the platinum material may therefore be pure platinum except for customary impurities, in which the at least partially oxidized non-noble metals are mixed in.
- the platinum composition may also comprise other precious metals, the platinum composition in this case being a platinum alloy.
- the other precious metals are selected from ruthenium, rhodium, gold, palladium and iridium.
- the provided solid is cold formed according to the inventive method.
- the term "cold working" is known in the art, which forming takes place at relatively low temperatures below the recrystallization temperature of the platinum composition, and particularly includes drawing, pressing, deep drawing, cold rolling, cold hammering and pressing.
- Deformation involves deformation of the bulk body over a large area.
- the volume body is subjected to deformation over at least 50%, more preferably over at least 75% and especially preferably over at least 95% of the volume.
- a sheet is preferably at least 50%, more preferably at least 75%, and more preferably at least 95% of the surface area of the sheet subjected to a force or pressure, for example, rolled.
- the surface can be simplified in relation to the surfaces, which is perpendicular to the minimum extent of the volume body (thickness).
- the solid is a wire or a tube, preferably at least 50%, more preferably at least 75%, and most preferably at least 95% of the length of the wire or tube is subjected to a force such as pulled.
- the cross-sectional area of the volume body of the dispersion-hardened platinum composition is reduced by a maximum of 20%, more preferably by a maximum of 18%, and especially preferably by a maximum of 15%.
- These values are related to the cross-sectional area of the volume, which is maximally reduced.
- the reduced cross-sectional area results, for example, from the thickness and the unstretched expansion of the solid.
- the reduction of the cross-sectional area results from the change of the diameter or the wall thickness.
- the volume of the body is not changed by the deformation, at least one cross-sectional area must be increased during a forming.
- the length will increase during forming, so that the surface becomes larger in the direction of increasing the length.
- the directions in which the deforming forces act in particular parallel or perpendicular to the plane, which is spanned by the cross-sectional area.
- the cross-sectional area of the volume body of the dispersion-hardened platinum composition is reduced by at least 5%, preferably reduced by at least 8%, and particularly preferably reduced by at least 10%.
- a wire is drawn or pressed, wherein in the cold forming the cross-sectional area of the wire from the dispersion-hardened platinum composition is reduced by a maximum of 20%, more preferably by a maximum of 18% and more preferably by a maximum of 15% or by cold forming a sheet is rolled, drawn, pressed or pressed, wherein in the cold forming, the cross-sectional area of the sheet or the thickness of the sheet of the dispersion-hardened platinum composition is reduced by a maximum of 20%, more preferably by a maximum of 18% and more preferably by a maximum of 15% or Cold forming a tube is rolled, drawn or pressed, wherein in the cold forming, the cross-sectional area of the tube of the dispersion-hardened platinum composition is reduced by a maximum of 20%, more preferably by a maximum of 18% and more preferably by a maximum of 15%.
- a temperature treatment of the cold-formed volume body is carried out, in which the cold-worked product is annealed at at least 1100 ° C for at least one hour.
- the annealing may preferably take place over a period of at least 90 minutes, preferably at least 120 minutes, more preferably at least 150 minutes, and especially preferably at least 180 minutes.
- the temperature at which the annealing is carried out may preferably be at least 1200 ° C, more preferably at least 1250 ° C, more preferably at least 1300 ° C, and most preferably at least 1400 ° C.
- the cold-formed solid is tempered at a temperature of at least 1250 ° C. for at least one hour, preferably at a temperature of 1400 ° C. for one to three hours.
- the costs of the process increase with the duration and the annealing temperature.
- the minimum temperature for the tempering process is 1100 ° C.
- the maximum temperature for the annealing process is 20 ° C below the melting temperature of the respective dispersion-hardened platinum composition.
- the temperature treatment or the temperature treatments of the cold-formed volume body are or will be used to heal defects of the bulk body.
- the cross-sectional area of the volume body is reduced by more than 20% due to the cold forming, the cross-sectional area of the volume body of the dispersion-hardened platinum composition being reduced by a maximum of 20% for each individual cold forming, more preferably at most 18% and more preferably at most 15% is reduced, and between each cold working, a temperature treatment of the cold-formed volume body is carried out at which the cold-worked product is annealed at at least 1100 ° C for at least one hour.
- each cold forming means that preferably after each cold forming a temperature treatment is carried out at at least 1100 ° C for at least one hour, so that the number of cold forming steps and the number of annealing steps is the same.
- the implementation of several cold forming and temperature treatments has the advantage that with the relatively easy and inexpensive to perform cold forming and temperature treatments and larger transformations are feasible without that the dispersion-hardened platinum composition is weakened, that is, without, for example, that the alloy is reduced in their creep strength , It has even been surprisingly found that the creep strength increasingly improves with increasing number of forming and annealing steps.
- the cross-sectional area of the volume body of the dispersion-hardened platinum composition is reduced by at least 5%, preferably reduced by at least 8%, and more preferably reduced by at least 10%.
- Forming steps involving only a minor reduction in the cross-sectional area of the dispersion-hardened bulk body of less than 5% per forming step and subsequent annealing do not significantly contribute to an improvement in creep rupture strength.
- the process is also consuming and therefore uneconomical. This is all the more the case, the greater the number of forming steps required in order to achieve the desired final dimension of the dispersion-hardened volume body.
- a number of 8 forming steps is preferred in order to obtain the desired final size. This number of forming steps is a good compromise between economy and improvement of mechanical properties.
- the cold worked product is annealed at at least 1550 ° C for at least 24 hours, at least 1600 ° C for at least 12 hours, at least 1650 ° C for at least one hour is annealed or at a temperature of 1690 ° C to 1740 ° C for at least 30 minutes.
- any dispersion-hardened platinum composition is suitable. Surprising advantages, however, result from the use of semi-finished products, which were generally subjected to hot working.
- the dispersion-hardened platinum composition may be hot worked at a temperature of at least 800 ° C prior to cold forming, preferably formed at a temperature of at least 1000 ° C, most preferably formed at a temperature of at least 1250 ° C.
- a further subject matter of the present invention is a process for producing a product from a dispersion-hardened platinum composition, which is characterized in that, prior to providing the dispersion-hardened platinum composition, it consists of a composition of at least 70% by weight of platinum and not more than 29.95% by weight. % of other noble metals, wherein the other precious metals are selected from ruthenium, rhodium, gold, palladium and iridium, and 0.05 wt .-% to 0.5 wt .-% of at least one non-noble metal selected from zirconium, cerium, scandium and Yttrium is prepared by at least partially oxidizing the non-noble metal or the non-noble metals.
- the non-noble metal or non-noble metals will be at least 70%, preferably at least 90%, reacted to metal oxides.
- a further subject matter of the present invention is a process for producing a product from a dispersion-hardened platinum composition, which is characterized in that, prior to providing the dispersion-hardened platinum composition, it consists of a composition of at least 70% by weight of platinum and not more than 29.95% by weight. % of other precious metals and from 0.05% to 0.5% by weight of at least one non-noble metal selected from ruthenium, zirconium, cerium, scandium and yttrium is prepared by at least partially oxidizing the non-noble metal or non-noble metals ,
- the non-noble metal or non-noble metals will be at least 70%, preferably at least 90%, reacted to metal oxides.
- the treatment of the non-noble metal or the non-noble metals may preferably be carried out at a temperature between 600 ° C and 1600 ° C in an oxidizing atmosphere, preferably between 800 ° C and 1000 ° C in an oxidizing atmosphere.
- the method of making a product from a dispersion-cured platinum composition may preferably be combined with the previously described method of processing and the embodiments of the invention described herein as preferred.
- a further subject of the present invention is a dispersion-hardened platinum material obtainable by a method for processing and / or a method for producing a product from a dispersion-hardened platinum composition.
- This article provides excellent mechanical properties in combination with excellent processability and low cost and inexpensive manufacturability.
- a cylindrical volume body of the dispersion-hardened platinum material withstands a tensile load of 9 MPa in the direction of the length of the volume at a temperature of 1600 ° C. for at least 40 hours without tearing, preferably withstands at least 50 hours without tearing, particularly preferably withstands at least 100 hours without tearing and / or that a sheet of the dispersion-hardened platinum material having a rectangular cross-section of 0.85 mm by 3.9 mm and a length of 140 mm, in a furnace chamber at 1650 ° C to two parallel cylindrical rods with a circular cross-section and 2 mm diameter are placed at a distance of 100 mm and the sheet in the middle with a weight of 30 g
- a dispersion-hardened platinum material with the mechanical properties described above for a cylindrical volume body is the subject of the present invention.
- the dispersion-hardened platinum material 0.05 wt .-% to 0.4 wt .-%, particularly preferably 0.05 wt .-% to 0.3 wt .-% of at least one at least partially oxidized non-noble metal selected from zirconium, cerium, scandium and yttrium.
- a material with excellent mechanical properties and very good processability can be provided by this embodiment.
- the dispersion-hardened platinum material may be a sheet, a tube or a wire or a product formed from a wire, tube and / or sheet.
- a further subject matter of the present invention is a use of a dispersion-hardened platinum material or of a reshaped volume body of a platinum composition obtainable or obtained by a method according to the invention for processing and / or with a method according to the invention for producing a product from a dispersion-hardened platinum composition the glass industry or equipment to be used in a laboratory.
- the invention is based on the surprising finding that it is possible by the low cold working (with at most 20% change in the cross-sectional area) to enter only such weak structural impairments, such as crystal lattice dislocations in the dispersion-hardened platinum composition that succeeds with the downstream temperature treatment, annealing them again to such an extent that the stability of the reformed platinum composition is significantly higher than in known methods for cold working dispersion-hardened platinum compositions. If stronger transformations are desired, they may be achieved either with an upstream hot working or a series of small cold forming operations are performed sequentially, with annealing of the structural degradation by a thermal treatment being performed between each cold working.
- the gentle, low cold forming internal damage such as microcracks, delaminations of the particle / matrix interfaces and pores are avoided on grain boundary surfaces, which can not be cured or only with great effort.
- Particularly damaging are microcracks and pores, which are formed by the deformation on the grain boundaries, since they particularly affect the mechanical stability of the dispersion-hardened platinum composition.
- the method according to the invention it is possible to avoid these impairments. This has made it possible for the first time to produce a dispersion-hardened platinum composition with very high mechanical stability and excellent processability, in particular weldability, which is likewise claimed according to the invention.
- Example 1 Based on the in EP 1 964 938 A1 In Example 1, a billet was cast with PtRh10 (alloy of 90 wt.% Pt and 10 wt.% Rh) and 2200 ppm of non-noble metals (1800 ppm Zr and 400 ppm Y). Subsequently, the ingot was treated mechanically and thermally. So this was rolled to a plate thickness of 2.2 mm, then recrystallization annealed and then rolled to a plate thickness of 2 mm. The sheet was then oxidized at 900 ° C for 18 days and then ductile annealed at 1400 ° C for 6 hours.
- Example 1 Based on the in EP 1 964 938 A1 In Example 1, a billet was cast with PtRh10 (alloy of 90 wt.% Pt and 10 wt.% Rh) and 2200 ppm of non-noble metals (1800 ppm Zr and 400 ppm Y). Subsequently, the ingot was treated mechanically and thermally. So this was rolled to a sheet thickness of 3.3 mm, then recrystallization annealed and then rolled to a plate thickness of 3 mm. The Sheet was then oxidized at 900 ° C for 27 days and then ductile annealed at 1400 ° C for 6 hours.
- Example 1 Based on the in EP 1 964 938 A1 In Example 1, a billet was cast with PtRh10 (alloy of 90 wt.% Pt and 10 wt.% Rh) and 2120 ppm of non-noble metals (1800 ppm Zr, 270 ppm Y and 50 ppm Sc). Subsequently, the ingot was treated mechanically and thermally. So this was rolled to a sheet thickness of 3.3 mm, then recrystallization annealed and then rolled to a plate thickness of 3 mm. The sheet was then oxidized at 900 ° C for 24 days and then ductile annealed at 1400 ° C for 6 hours.
- the semifinished product precursor 1 obtained according to the method set out above with a thickness of about 2 mm is further processed according to the invention after the following rolling and annealing steps.
- the sheet was rolled to 1.7 mm and then annealed at 1400 ° C for 4 h. Thereafter, the sheet is rolled to 1.4 mm and annealed at 1400 ° C for 2 h. Then, further rolled to 1.2 mm and annealed again at 1400 ° C for 2 h. Then it is rolled to 1 mm and annealed again at 1400 ° C. Then it is rolled to the final thickness of 0.85 mm and a final annealing at 1100 ° C for 1 h carried out.
- the reduction in the cross-sectional area per rolling step is 20%.
- Example 1 is essentially repeated, but after rolling to a final thickness of 0.85 mm, a final annealing at 1700 ° C for 1 h is performed.
- the semifinished product precursor 2 obtained according to the method set out above with a thickness of about 3 mm is further processed according to the invention after the following rolling and calcination steps.
- the sheet was rolled to 2.4 mm and then annealed at 1150 ° C for 4 h. Thereafter, the sheet is rolled to 1.92 mm and annealed at 1150 ° C for 4 h. Then it is rolled to 1.53 mm and again annealed for 4 h at 1150 ° C.
- the rolling and annealing steps are repeated 3 more times, rolling first to 1.22 mm, then to 0.99 mm and then to 0.8 mm and annealing after each rolling step for 4 h at 1150 ° C.
- the reduction in the cross-sectional area per rolling step is 20%.
- the semifinished product precursor 2 obtained according to the method set out above with a thickness of about 3 mm is further processed according to the invention after the following rolling and calcination steps.
- the sheet was rolled to 2.4 mm and then annealed at 1300 ° C for 4 h. Thereafter, the sheet is rolled to 1.92 mm and annealed at 1300 ° C for 4 h. Then it is rolled to 1.53 mm and annealed again for 4 h at 1300 ° C.
- the rolling and annealing steps are repeated 3 more times, rolling first to 1.22 mm, then to 0.99 mm and then to 0.8 mm and annealing after each rolling step for 4 h at 1300 ° C.
- the reduction in the cross-sectional area per rolling step is 20%.
- the semifinished product precursor 2 obtained according to the method set out above with a thickness of about 3 mm is further processed according to the invention after the following rolling and calcination steps.
- the sheet was rolled to 2.4 mm and then annealed at 1400 ° C for 4 h. Thereafter, the sheet is rolled to 1.92 mm and annealed at 1400 ° C for 4 h. Then it is rolled to 1.53 mm and again annealed for 4 h at 1400 ° C.
- the rolling and annealing steps are repeated 3 more times, rolling first to 1.22 mm, then to 0.99 mm and then to 0.8 mm and annealing after each rolling step for 4 h at 1400 ° C.
- the reduction in the cross-sectional area per rolling step is 20%.
- the semifinished product precursor 2 obtained according to the method set out above with a thickness of about 3 mm is further processed according to the invention after the following rolling and calcination steps.
- the sheet was rolled to 2.55 mm and then annealed at 1400 ° C for 4 h. Thereafter, the sheet is rolled to 2.16 mm and annealed at 1400 ° C for 4 h. Then it gets to 1.84 mm rolled and annealed again for 4 h at 1400 ° C.
- the rolling and annealing steps are repeated 5 more times, rolling first to 1.56 mm, then to 1.33 mm, then to 1.13 mm, then to 0.96 mm and then to 0.8 mm, and after each rolling step for 4 h at 1400 ° C is annealed.
- the reduction in cross-sectional area per rolling step is 15%.
- the semifinished product precursor 3 obtained according to the method set out above with a thickness of about 3 mm is further processed according to the invention after the following rolling and calcining steps.
- the sheet was rolled to 2.4 mm and then annealed at 1150 ° C for 4 h. Thereafter, the sheet is rolled to 1.92 mm and annealed at 1150 ° C for 4 h. Then it is rolled to 1.53 mm and again annealed for 4 h at 1150 ° C.
- the rolling and annealing steps are repeated 3 more times, rolling first to 1.22 mm, then to 0.99 mm and then to 0.8 mm and annealing after each rolling step for 4 h at 1150 ° C.
- the reduction in the cross-sectional area per rolling step is 20%.
- the semifinished product precursor 3 obtained according to the method set out above with a thickness of about 3 mm is further processed according to the invention after the following rolling and calcining steps.
- the sheet was rolled to 2.55 mm and then annealed at 1400 ° C for 4 h. Thereafter, the sheet is rolled to 2.16 mm and annealed at 1400 ° C for 4 h. Then it is rolled to 1.84 mm and again annealed for 4 h at 1400 ° C.
- the rolling and annealing steps are repeated 5 more times, rolling first to 1.56 mm, then to 1.33 mm, then to 1.13 mm, then to 0.96 mm and then to 0.8 mm, and after each rolling step for 4 h at 1400 ° C is annealed.
- the reduction in cross-sectional area per rolling step is 15%.
- the semifinished product precursor 3 obtained according to the method set out above with a thickness of about 3 mm is further processed according to the invention after the following rolling and calcining steps.
- the sheet was rolled to 2.7 mm and then annealed at 1400 ° C for 4 h. Thereafter, the sheet is rolled to 2.43 mm and annealed at 1400 ° C for 4 h. Then it is rolled to 2.19 mm and again annealed for 4 h at 1400 ° C.
- the rolling and annealing steps are repeated 9 more times, first at 1.97 mm, then at 1.77 mm, then at 1.60 mm, then at 1.44 mm, then 1.29 mm, then 1.16 mm, then 1.05 mm, then 0.94 mm and then 0.85 mm, and after each rolling step for 4 h at 1400 ° C is annealed.
- the reduction in the cross-sectional area per rolling step is 10%.
- Example 9 is essentially repeated, but after rolling to a final thickness of 0.85 mm, a final annealing at 1700 ° C for 1 h is performed.
- the semifinished product precursor 3 obtained according to the method set out above with a thickness of about 3 mm is further processed according to the invention after the following rolling and calcining steps.
- the sheet was rolled at 1100 ° C (hot working) to 1.5 mm and then annealed at 1400 ° C for 4 h. Thereafter, the sheet is rolled to 1.2 mm (1st cold working) and then annealed at 1250 ° C for 4 h. Then rolled 1.02 mm (2nd cold forming) and then again annealed at 1250 ° C for 4 h.
- the rolling and annealing steps are repeated 3 more times, rolling first to 0.94 mm (3rd cold working), then to 0.86 mm (4th cold working) and then to 0.8 mm (5th cold working), and after each rolling step for 4 h at 1250 ° C is annealed.
- the reduction in the cross-sectional area is 50% for the hot-forming step, 20% for the cold-forming steps, then 15% and then 8% each.
- the semifinished product precursor 1 obtained according to the method set out above with a thickness of about 2 mm is further processed according to a conventional method.
- the sheet is rolled directly to 1 mm and annealed at 1000 ° C. It is then rolled to 0.85 mm and a final annealing at 1000 ° C for 1 h carried out.
- the semifinished product precursor 2 obtained according to the method set out above with a thickness of about 3 mm is further processed according to a conventional method.
- the sheet is rolled to 1.5 mm and annealed at 1400 ° C for 4 h. Then it is rolled to 0.8 mm.
- the reduction in cross-sectional area per rolling step is 50%.
- the semifinished product precursor 3 obtained according to the method set out above with a thickness of about 3 mm is further processed according to a conventional method.
- the sheet is rolled to 1.5 mm and annealed at 1400 ° C for 4 h. Then it is rolled to 0.8 mm.
- the reduction in cross-sectional area per rolling step is 50%.
- Examples 1, 2, 9, 10 and Comparative Example 1 To measure the creep rupture strength is measured on a sheet sample with a cross section of 0.85 mm ⁇ 3.9 mm and a length of 120 mm (Examples 1, 2, 9, 10 and Comparative Example 1) or 0.8 mm x 3.9 mm and a length of 120 mm (Examples 3, 4, 5, 6, 7, 8, 11 and Comparative Examples 2 and 3) appended a weight corresponding to the desired load in MPa for said cross-section.
- the sample is brought to temperature by current flow and controlled by pyrometer measurement to the desired temperature.
- the time to break of the sample is determined and indicates the creep rupture strength.
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Catalysts (AREA)
- Manufacture Of Alloys Or Alloy Compounds (AREA)
- Powder Metallurgy (AREA)
- Heat Treatment Of Steel (AREA)
- Adornments (AREA)
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE102013225187.4A DE102013225187B4 (de) | 2013-12-06 | 2013-12-06 | Verfahren zur Bearbeitung einer dispersionsgehärteten Platinzusammensetzung |
PCT/EP2014/076600 WO2015082630A1 (de) | 2013-12-06 | 2014-12-04 | Verfahren zur bearbeitung einer dispersionsgehärteten platinzusammensetzung |
Publications (2)
Publication Number | Publication Date |
---|---|
EP3077556A1 EP3077556A1 (de) | 2016-10-12 |
EP3077556B1 true EP3077556B1 (de) | 2019-06-19 |
Family
ID=52101298
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP14812166.8A Active EP3077556B1 (de) | 2013-12-06 | 2014-12-04 | Verfahren zur bearbeitung einer dispersionsgehärteten platinzusammensetzung |
Country Status (7)
Country | Link |
---|---|
US (1) | US20160289808A1 (ko) |
EP (1) | EP3077556B1 (ko) |
JP (1) | JP6530402B2 (ko) |
KR (1) | KR101831090B1 (ko) |
CN (1) | CN105765092B (ko) |
DE (1) | DE102013225187B4 (ko) |
WO (1) | WO2015082630A1 (ko) |
Families Citing this family (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108165812B (zh) * | 2017-11-16 | 2019-09-24 | 重庆材料研究院有限公司 | 一种用于铂基器皿的弥散强化型材料及其制备方法和应用 |
EP3971311B1 (de) | 2020-09-17 | 2022-07-06 | Heraeus Deutschland GmbH & Co. KG | Verbesserte, dispersionsgehärtete edelmetalllegierung |
EP3978884B1 (de) | 2020-10-02 | 2024-05-29 | Heraeus Precious Metals GmbH & Co. KG | Draht mit platin-zusammensetzung zur kontaktierung von temperatursensoren |
EP4282526A1 (de) | 2022-05-25 | 2023-11-29 | Heraeus Deutschland GmbH & Co. KG | Katalysatornetz mit einem edelmetalldraht aus einer dispersionsverfestigten edelmetalllegierung |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB1280815A (en) | 1968-07-12 | 1972-07-05 | Johnson Matthey Co Ltd | Improvements in and relating to the dispersion strengthening of metals |
WO1981001013A1 (en) | 1979-10-04 | 1981-04-16 | Owens Corning Fiberglass Corp | Thermomechanical processing of dispersion-strengthened precious metal alloys |
EP1964938A1 (de) | 2007-02-14 | 2008-09-03 | W.C. Heraeus GmbH | Oxiddispersionsgehärteter, durch innere Oxidation hergestellter Pt, PtRh- oder PtAu-Werkstoff mit hohem Oxidanteil und guter Duktilität |
Family Cites Families (13)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US156A (en) * | 1837-03-30 | Improvement in machines for packing and pressing flour | ||
US2636819A (en) * | 1951-01-31 | 1953-04-28 | Baker & Co Inc | Grain stabilizing metals and alloys |
GB1340076A (en) | 1970-01-23 | 1973-12-05 | Johnson Matthey Co Ltd | Dispersion strengthening of platinum group metals platinum group metal based alloys gold and gold based alloys |
DE3030751A1 (de) | 1980-08-14 | 1982-03-18 | Degussa Ag, 6000 Frankfurt | Verfahren zur herstellung von halbzeugen aus dispersionsgehaertetem platin |
US4507156A (en) * | 1984-04-09 | 1985-03-26 | Owens-Corning Fiberglas Corporation | Creep resistant dispersion strengthened metals |
DE4417495C1 (de) | 1994-05-19 | 1995-09-28 | Schott Glaswerke | Verfahren zur Herstellung von mit Y¶2¶0¶3¶ dispersionsverfestigten Reinst-Platin-Werkstoffen, Halbzeugen und Blechen |
DE19714365A1 (de) * | 1997-04-08 | 1998-10-15 | Heraeus Gmbh W C | Dispersionsverfestiger Platin-Werkstoff, Verfahren zu seiner Herstellung und seine Verwendung |
US6569270B2 (en) * | 1997-07-11 | 2003-05-27 | Honeywell International Inc. | Process for producing a metal article |
DE19813988C1 (de) | 1998-03-28 | 1999-10-28 | Heraeus Gmbh W C | Verfahren zur Herstellung eines aus durch feinverteilte, kleine Teilchen aus Unedelmetalloxid dispersionsverfestigtem Platinwerkstoff bestehenden, geschweißten, insbesondere mindestens eine Innenwand aufweisenden Formkörpers, isnbesondere eines Rohres |
JP3778338B2 (ja) * | 2000-06-28 | 2006-05-24 | 田中貴金属工業株式会社 | 酸化物分散強化型白金材料の製造方法 |
DE10046456C2 (de) | 2000-09-18 | 2003-04-10 | Heraeus Gmbh W C | Durch feinverteilte, kleine Teilchen aus Unedelmetalloxid dispersionsverfestigter, goldfreier Platin-Werkstoff |
JP4136914B2 (ja) * | 2003-11-28 | 2008-08-20 | 田中貴金属工業株式会社 | 強化白金材料の製造方法 |
CN100500898C (zh) * | 2006-09-08 | 2009-06-17 | 国内贸易部物资再生利用研究所 | 一种强化铂材料及其制造方法 |
-
2013
- 2013-12-06 DE DE102013225187.4A patent/DE102013225187B4/de active Active
-
2014
- 2014-12-04 CN CN201480065977.XA patent/CN105765092B/zh active Active
- 2014-12-04 KR KR1020167017985A patent/KR101831090B1/ko active IP Right Grant
- 2014-12-04 US US15/100,809 patent/US20160289808A1/en not_active Abandoned
- 2014-12-04 WO PCT/EP2014/076600 patent/WO2015082630A1/de active Application Filing
- 2014-12-04 EP EP14812166.8A patent/EP3077556B1/de active Active
- 2014-12-04 JP JP2016536823A patent/JP6530402B2/ja active Active
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB1280815A (en) | 1968-07-12 | 1972-07-05 | Johnson Matthey Co Ltd | Improvements in and relating to the dispersion strengthening of metals |
WO1981001013A1 (en) | 1979-10-04 | 1981-04-16 | Owens Corning Fiberglass Corp | Thermomechanical processing of dispersion-strengthened precious metal alloys |
EP1964938A1 (de) | 2007-02-14 | 2008-09-03 | W.C. Heraeus GmbH | Oxiddispersionsgehärteter, durch innere Oxidation hergestellter Pt, PtRh- oder PtAu-Werkstoff mit hohem Oxidanteil und guter Duktilität |
US20100276646A1 (en) | 2007-02-14 | 2010-11-04 | W.C. Heraeus Gmbh | Pt or pt alloy materials hardened by oxide dispersion, produced by inner oxidation and having proportions of oxide and good ductility |
Non-Patent Citations (3)
Title |
---|
BERND FISCHER, ET AL: "Oxide Dispersion Hardened Platinum Alloys with Improved Strength at High Temperatures", 36TH INTERNATIONAL PRECIOUS METALS CONFERENCE, 9 June 2012 (2012-06-09), pages 1 - 32, XP055710438 |
DOMINIC MORRIS, ROB MCGRATH: "ZGS Platinum Materials for Improved Glass Manufacturing Equipment and Laboratory Ware", PLATINIUM METALS REVIEW., JOHNSON MATTHEY PLC, LONDON, GB, vol. 57, no. 3, 1 July 2013 (2013-07-01), LONDON, GB, pages 230 - 232, XP055710434, ISSN: 0032-1400, DOI: 10.1595/147106713X668901 |
YU N LOGINOV, ET AL: "Annealing Characteristics and Strain Resistance of 99.93 wt.% Platinum", PLATINUM METALS REVIEW, vol. 51, no. 4, 1 October 2007 (2007-10-01), pages 178 - 184, XP055710443 |
Also Published As
Publication number | Publication date |
---|---|
CN105765092B (zh) | 2018-10-19 |
DE102013225187B4 (de) | 2018-07-19 |
WO2015082630A1 (de) | 2015-06-11 |
EP3077556A1 (de) | 2016-10-12 |
KR101831090B1 (ko) | 2018-02-21 |
CN105765092A (zh) | 2016-07-13 |
US20160289808A1 (en) | 2016-10-06 |
JP2017502170A (ja) | 2017-01-19 |
DE102013225187A1 (de) | 2015-06-11 |
KR20160097249A (ko) | 2016-08-17 |
JP6530402B2 (ja) | 2019-06-12 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
EP3314031B1 (de) | Hochfestes und gut umformbares almg-band sowie verfahren zu seiner herstellung | |
EP2386663B1 (de) | Verfahren zur Herstellung eines Bauteiles und Bauteile aus einer Titan-Aluminium-Basislegierung | |
DE69511037T2 (de) | Verfahren zur Herstellung von Formgedächtnislegierungen mit hoher Umwandlungstemperatur | |
DE69108295T2 (de) | Verfahren zur Herstellung von korrosionsbeständigen nahtlosen Röhren aus Titanlegierung. | |
DE1558521C3 (de) | Verwendung einer Nickel Chrom Knetlegierung als superplastischer Werk stoff | |
EP2559779B1 (de) | Warmfeste Al-Cu-Mg-Ag-Legierung sowie Verfahren zur Herstellung eines Halbzeuges oder Produktes aus einer solchen Aluminiumlegierung | |
DE102004056582B4 (de) | Legierung auf der Basis von Titanaluminiden | |
EP2449145B1 (de) | AlMgSi-Band für Anwendungen mit hohen Umformungsanforderungen | |
EP3077556B1 (de) | Verfahren zur bearbeitung einer dispersionsgehärteten platinzusammensetzung | |
WO2013037919A1 (de) | HERSTELLVERFAHREN FÜR AlMgSi-ALUMINIUMBAND | |
DE112008001968T5 (de) | Bilden von Magnesiumlegierungen mit verbesserter Duktilität | |
EP2192202A1 (de) | Aluminiumband für lithographische Druckplattenträger mit hoher Biegewechselbeständigkeit | |
EP3259378A1 (de) | Verfahren zum herstellen eines strangs aus edelstahl sowie strang aus edelstahl | |
DE112020003615T5 (de) | Verfahren zur gemischten behandlung von magnesiumlegierungen (varianten) | |
EP1748088B1 (de) | Verfahren zur Herstellung eines Halbzeugs oder Bauteils von Fahrwerk- oder Strukturanwendungen im Kraftfahrzeug | |
DE1533497B1 (de) | Verfahren zur Verbesserung der mechanischen Eigenschaften von AlCuMg-Platten in deren kurzer Querrichtung | |
DE1290727B (de) | Verfahren zur Herstellung von Nioblegierungen hoher Festigkeit | |
WO2020007437A1 (de) | Aluminiumlegierung sowie überaltertes aluminiumlegierungsprodukt aus einer solchen legierung | |
DE4000270A1 (de) | Verfahren zum kaltverformen von unlegiertem titan | |
DE102019105598A1 (de) | Verfahren zur Herstellung eines Aluminiumbands mit hoher Festigkeit und hoher elektrischer Leitfähigkeit | |
EP2426228B1 (de) | Magnesiumblechhalbzeuge mit verbessertem Kaltumformvermögen | |
EP3763845B1 (de) | Magnesiumlegierung und verfahren zur herstellung derselben | |
WO2015144888A2 (de) | Hochumformbare, mittelfeste aluminiumlegierung zur herstellung von halbzeugen oder bauteilen von kraftfahrzeugen | |
EP4332260A1 (de) | Aushärtbaren aluminiumlegierung, metallband oder -blech aus dieser aluminiumlegierung, verfahren zur herstellung dieses metallbands oder -blechs und dessen verwendung bei einem superplastischen umformen | |
DE1533481C3 (de) | Verfahren zur Verbesserung der mechanischen Eigenschaften eines dispersionsgehärteten Metalls oder einer Legierung aus der Gruppe Kupfer und Edelmetalle |
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: 20160408 |
|
AK | Designated contracting states |
Kind code of ref document: A1 Designated state(s): AL AT BE BG CH CY CZ DE DK EE ES FI FR GB GR HR HU IE IS IT LI LT LU LV MC MK MT NL NO PL PT RO RS SE SI SK SM TR |
|
AX | Request for extension of the european patent |
Extension state: BA ME |
|
DAX | Request for extension of the european patent (deleted) | ||
STAA | Information on the status of an ep patent application or granted ep patent |
Free format text: STATUS: EXAMINATION IS IN PROGRESS |
|
17Q | First examination report despatched |
Effective date: 20170811 |
|
GRAP | Despatch of communication of intention to grant a patent |
Free format text: ORIGINAL CODE: EPIDOSNIGR1 |
|
STAA | Information on the status of an ep patent application or granted ep patent |
Free format text: STATUS: GRANT OF PATENT IS INTENDED |
|
INTG | Intention to grant announced |
Effective date: 20190307 |
|
GRAS | Grant fee paid |
Free format text: ORIGINAL CODE: EPIDOSNIGR3 |
|
GRAA | (expected) grant |
Free format text: ORIGINAL CODE: 0009210 |
|
STAA | Information on the status of an ep patent application or granted ep patent |
Free format text: STATUS: THE PATENT HAS BEEN GRANTED |
|
AK | Designated contracting states |
Kind code of ref document: B1 Designated state(s): AL AT BE BG CH CY CZ DE DK EE ES FI FR GB GR HR HU IE IS IT LI LT LU LV MC MK MT NL NO PL PT RO RS SE SI SK SM TR |
|
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 |
|
REG | Reference to a national code |
Ref country code: IE Ref legal event code: FG4D Free format text: LANGUAGE OF EP DOCUMENT: GERMAN |
|
REG | Reference to a national code |
Ref country code: DE Ref legal event code: R096 Ref document number: 502014012030 Country of ref document: DE |
|
REG | Reference to a national code |
Ref country code: AT Ref legal event code: REF Ref document number: 1145607 Country of ref document: AT Kind code of ref document: T Effective date: 20190715 |
|
REG | Reference to a national code |
Ref country code: NL Ref legal event code: MP Effective date: 20190619 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: NO 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: 20190919 Ref country code: AL 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: 20190619 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: 20190619 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: 20190619 Ref country code: HR 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: 20190619 Ref country code: LT 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: 20190619 |
|
REG | Reference to a national code |
Ref country code: LT Ref legal event code: MG4D |
|
REG | Reference to a national code |
Ref country code: DE Ref legal event code: R082 Ref document number: 502014012030 Country of ref document: DE Representative=s name: BRAND, NORMEN, DR. RER. NAT., DE Ref country code: DE Ref legal event code: R082 Ref document number: 502014012030 Country of ref document: DE Representative=s name: BRAND, NORMEN, DIPL.-CHEM. UNIV. DR. RER. NAT., DE |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
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: 20190920 Ref country code: BG 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: 20190919 Ref country code: RS 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: 20190619 Ref country code: LV 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: 20190619 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: RO 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: 20190619 Ref country code: SK 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: 20190619 Ref country code: CZ 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: 20190619 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: 20191021 Ref country code: EE 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: 20190619 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: 20190619 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: SM 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: 20190619 Ref country code: IS 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: 20191019 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: 20190619 |
|
REG | Reference to a national code |
Ref country code: DE Ref legal event code: R026 Ref document number: 502014012030 Country of ref document: DE |
|
PLBI | Opposition filed |
Free format text: ORIGINAL CODE: 0009260 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
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: 20190619 |
|
26 | Opposition filed |
Opponent name: JOHNSON MATTHEY PUBLIC LIMITED COMPANY Effective date: 20200317 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: PL 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: 20190619 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: 20190619 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: IS 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: 20200224 |
|
PLAX | Notice of opposition and request to file observation + time limit sent |
Free format text: ORIGINAL CODE: EPIDOSNOBS2 |
|
PG2D | Information on lapse in contracting state deleted |
Ref country code: IS |
|
REG | Reference to a national code |
Ref country code: CH Ref legal event code: PL |
|
REG | Reference to a national code |
Ref country code: BE Ref legal event code: MM Effective date: 20191231 |
|
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 FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20190619 Ref country code: SI 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: 20190619 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: LU Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20191204 Ref country code: IE Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20191204 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: BE Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20191231 Ref country code: LI Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20191231 Ref country code: CH Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20191231 |
|
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: 20190619 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: HU Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT; INVALID AB INITIO Effective date: 20141204 Ref country code: MT 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: 20190619 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: MK 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: 20190619 |
|
P01 | Opt-out of the competence of the unified patent court (upc) registered |
Effective date: 20230728 |
|
PGFP | Annual fee paid to national office [announced via postgrant information from national office to epo] |
Ref country code: GB Payment date: 20231220 Year of fee payment: 10 |
|
PGFP | Annual fee paid to national office [announced via postgrant information from national office to epo] |
Ref country code: IT Payment date: 20231228 Year of fee payment: 10 Ref country code: FR Payment date: 20231221 Year of fee payment: 10 Ref country code: DE Payment date: 20231214 Year of fee payment: 10 Ref country code: AT Payment date: 20231221 Year of fee payment: 10 |