EP3216883B1 - Iridium-platinlegierung, daraus hergestellter, maschinell bearbeiteter gegenstand und verfahren zu deren herstellung - Google Patents

Iridium-platinlegierung, daraus hergestellter, maschinell bearbeiteter gegenstand und verfahren zu deren herstellung Download PDF

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Publication number
EP3216883B1
EP3216883B1 EP16158893.4A EP16158893A EP3216883B1 EP 3216883 B1 EP3216883 B1 EP 3216883B1 EP 16158893 A EP16158893 A EP 16158893A EP 3216883 B1 EP3216883 B1 EP 3216883B1
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EP
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Prior art keywords
iridium
less
platinum alloy
forming
platinum
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EP16158893.4A
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English (en)
French (fr)
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EP3216883A1 (de
Inventor
Martin Schlott
Dirk Maier
Verena Wald
Nicole Staudt
Annette Lukas
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Heraeus Deutschland GmbH and Co KG
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Heraeus Deutschland GmbH and Co KG
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Priority to EP16158893.4A priority Critical patent/EP3216883B1/de
Priority to PCT/EP2017/054982 priority patent/WO2017153264A1/en
Priority to TW106106993A priority patent/TWI632242B/zh
Publication of EP3216883A1 publication Critical patent/EP3216883A1/de
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    • 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
    • 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

Definitions

  • WO 2011/034566 describes an item of jewelry made of a metal containing at least 75 wt% iridium.
  • US 2006/0270924 A1 describes an electrode for medical applications, comprising a base body which is coated by a porous Pt-Ir alloy.
  • shaped articles are prepared by machining (such as milling) from molded bodies made of a very hard and brittle material, the articles typically show surface defects. In particular along edges generated during the machining process, material may break off. However, for many applications, machined articles having such surface defects (e.g. edge defects) are not acceptable.
  • An object of the present invention is to provide an iridium-containing alloy which has improved workability and is suitable for preparing shaped articles by machining. If the structure of the shaped article contains edges, the number and size of defects along these edges (e.g. due to material that broke off) should be kept as low as possible.
  • the object is solved by an iridium-platinum alloy, which contains platinum in an amount of from 25 wt% to 45 wt%, the remainder being iridium and unavoidable impurities, and has an average grain width to height ratio of at least 5.
  • the shape of grains can be indicated by the grain width to height ratio. If the width to height ratio is close to 1, the grains have a relatively "round" shape, whereas a width to height ratio well above 1 indicates an elongated grain shape. In other words, the higher the aspect ratio is, the more elongated are the grains. Typically, if a material has been subjected to a recrystallization treatment, it contains a high amount of equiaxed grains or may even consist of such grains, i.e. grains having a width to height ratio of close to 1.
  • the alloy consists of iridium, platinum and unavoidable impurities.
  • iridium of high purity e.g. a purity of at least 99.9%, more preferably at least 99.99%)
  • platinum of high purity e.g. a purity of at least 99.9%, more preferably at least 99.99%)
  • the amount of unavoidable impurities in the final Ir-Pt alloy can be kept on a very low level.
  • the iridium-platinum alloy contains less than 200 wt-ppm rhodium.
  • the iridium-platinum alloy contains less than 200 wt-ppm rhodium, less than 150 wt-ppm copper, less than 100 wt-ppm calcium, less than 50 wt-ppm boron, and less than 100 wt-ppm iron.
  • the iridium-platinum alloy of the present invention is preferably prepared by a process wherein an Ir-Pt cast body is subjected to one or more forming steps such as rolling or forging. Accordingly, it is preferred that the iridium-platinum alloy is a formed iridium-platinum alloy, in particular a rolled or forged iridium-platinum alloy.
  • the formed iridium-platinum alloy can be a disc or a plate. However, other shapes are possible as well.
  • the present invention relates to a process for preparing the iridium-platinum alloy as described above, which comprises
  • the casting step (i) includes melting iridium and platinum metal in a furnace, e.g. an induction furnace, so as to prepare an iridium-platinum melt and then casting the melt into a mold.
  • the melt consists of iridium and platinum and unavoidable impurities.
  • the iridium-platinum melt contains the platinum in an amount of from 45 wt% to 25 wt%.
  • the mold is cooled, e.g. water-cooled. It can be preferred that the mold is made of a material having a high thermal conductivity, e.g. at least 200 W/(m*K) or at least 300 W/(m*K) at 20°C, such as copper.
  • a preferred mold is e.g. a water-cooled copper mold.
  • the pre-heating and the subsequent forming (e.g. rolling) steps are carried out under such conditions that the formed (e.g. rolled) iridium-platinum alloy finally obtained has a degree of recrystallisation of less than 30%.
  • the degree of recrystallization indicates the relative area (in %) of a microsection covered by the recrystallized equiaxed grains.
  • step (ii) which make sure that the formed (e.g. rolled) iridium-platinum alloy finally obtained has a degree of recrystallisation of less than 30%.
  • the forming (e.g. rolling) of the cast body can be carried out at a temperature which is sufficiently low so as to keep recrystallization on a very low level or is even below the recrystallization temperature.
  • one or more forming steps are at least partly carried out at a forming temperature above the recrystallization temperature, but the duration of these forming steps at a temperature above the recrystallization temperature is kept sufficiently short so as to avoid any substantial recrystallization.
  • step (ii) is a rolling, a forging, or a combination of both.
  • step (ii) comprises two or more forming steps, e.g. 6 to 30 forming steps, more preferably 10 to 26 forming steps.
  • each forming step is carried out at a forming rate of less than 4.0 s -1 , more preferably less than 3.0 s -1 , and/or a degree of forming of less than 10.0%, more preferably less than 8.0%.
  • step (ii) comprises two or more forming steps
  • the cast body is re-heated after at least one of these forming steps, so as to avoid that the iridium-platinum alloy cools down too much during the forming (e.g. rolling) treatment.
  • the iridium-platinum alloy is transferred from the forming (e.g. rolling) device to an oven, re-heated in the oven to a temperature which is, as explained above, preferably below the recrystallization temperature of the iridium-platinum alloy, and then re-transferred to the forming device so as to continue the forming treatment.
  • the re-heating time can vary over a broad range.
  • the present invention relates to a machined article which contains an the iridium-platinum alloy described above and has a density of at least 21.4 g/cm 3 .
  • At least 70 wt%, more preferably at least 80 wt%, even more preferably at least 90 wt% of the oscillating weight is made of the iridium-platinum alloy.
  • the oscillating weight consists of the iridium-platinum alloy.
  • the present invention relates to a process for preparing a machined article, which comprises
  • the microsection was taken perpendicular to the rolled surface and in (i.e. parallel to) the rolling direction.
  • the material was embedded under vacuum into an epoxy resin.
  • the surface to be analysed was ground and polished.
  • the wet grinding machine Labo-Pol-25 of Struers was used at 200 rpm in eight grinding steps (120, 320, 500, 800, 1200, 1500, 2400, and 4000). Polishing was carried out with the device LaboPol-5 of Struers (250 rpm) up to a fineness of 1 ⁇ m (diamond polishing paste). Subsequently, the samples were electrolytically etched with 20% KCN.
  • the average ratio of grain width to grain height of the samples was determined as follows: As already mentioned above, if the sample was rolled, the microsection was taken perpendicular to the rolled sample surface and parallel to the rolling direction. If two or more rolling steps were carried out on the sample surface and the rolling direction varied, the microsection was prepared in rolling direction of the final rolling step. On the microsection, at least two sub-sections were selected, each sub-section containing at least 40 grains. For each grain, its width (i.e. its maximum dimension in rolling direction) and its height (i.e. its maximum dimension perpendicular to the rolling direction) were determined using a light microscope (Olympus PMG3) with a scale bar. For each grain, the ratio of grain width to grain height was determined. Finally, from the ratio values of the individual grains, the average grain width to height ratio was determined as the arithmetic mean value.
  • a microsection was prepared as described above, i.e. perpendicular to the rolled sample surface and in rolling direction. On the microsection, at least two sub-sections were selected, each sub-section containing at least 40 grains. For each subsection, the relative area (in %) which was covered by recrystallized (i.e. equiaxed) grains was determined. The relative area covered by the recrystallized grains can be determined via image analysis software. As recrystallized grains, those were considered which have a grain width to height ratio of from 0.75 to 1.25. Finally, from the values of the sub-sections, the average degree of recrystallization was determined as the arithmetic mean value.
  • Hardness of the ground samples was determined under a load of HV1 using the device Zwick Roell ZH ⁇ .
  • the amount of impurities was determined by glow discharge lamp (GDL) using the device GD Profiler HR of Horiba-Jobin-Yvon. Sample excitation was effected by sputtering and an emission spectrum was obtained. By comparing the intensities of the emission lines to calibrated standards, the amounts of the impurities in the ppm-range was determined.
  • GDL glow discharge lamp
  • iridium-platinum alloys were prepared which differ in their average grain width to height ratios. From these Ir-Pt alloys, oscillating weights were prepared by milling and these machined articles were inspected for defects at their edges.
  • iridium (3N purity) and platinum (3N purity) for obtaining an Ir-Pt alloy having a Pt content of 40 wt% were melted under argon at 2200°C in an induction furnace using a ZrO 2 crucible.
  • the iridium-platinum melt was cast into a water-cooled copper mold. Upon solidification, an iridium-platinum cast body was obtained. The cast body was removed from the mold and casting wrinkles on its surface were removed by milling.
  • the cast body was pre-heated at 1200°C for 30 minutes in an oven under air atmosphere. Then, the pre-heated cast body was subjected to 19 rolling steps. After each rolling step, with the exception of the final rolling step, the cast body was transferred from the rolling machine to an oven, re-heated at a temperature of 1200°C for about 5 minutes, and then re-transferred to the rolling machine for carrying out the next rolling step.
  • Thickness of the cast body prior to the rolling treatment and after each rolling step as well as reduction in thickness (in mm and in %) and forming rates of each rolling step are listed below in Table 1.
  • Table 1 Forming rates and reduction in thickness Rolling step Thickness [mm] Reduction in thickness [mm] Reduction in thickness [%] Forming rate [1/s] 0 (i.e. prior to rolling) 12 0 0 1 11,4 0,6 5 1,34 2 10,6 0,8 7,02 1,64 3 9,25 0,6 5,66 1,52 4 8,50 0,75 7,50 1,82 16 3,7 0,3 7,50 2,88 17 3,5 0,2 5,41 2,52 18 3,3 0,2 5,71 2,66 19 3,1 0,2 6,06 2,83
  • Rotation speed of the roll was 22 rpm and roll radius was 155 mm.
  • the Ir/Pt40 alloy had an average grain width to height ratio of 12.5.
  • the number of pores was 0.01 per ⁇ m 2 . Pore size values were well below 5 ⁇ m. The degree of recrystallization was very low (well below 30%).
  • Impurities were present in low amounts: Rh ⁇ 200 wt-ppm, Cu ⁇ 150 wt-ppm, Ca ⁇ 100 wt-ppm, B ⁇ 50 wt-ppm, Fe ⁇ 100 ppm.
  • the sample had a hardness of 475 HV1 and a density of 22.0 g/cm 3 .
  • the cast body made of the Ir/Pt40 alloy was machined to a balance wheel by milling.
  • the edges of the milled article were inspected for defects having a size of > 10 ⁇ m. However, no defects were detected.
  • iridium (3N purity) and platinum (3N purity) for obtaining an Ir-Pt alloy having a Pt content of 40 wt% were melted under argon at 2200°C in an induction furnace using a ZrO 2 crucible.
  • the iridium-platinum melt was cast into a water-cooled copper mold. Upon solidification, an iridium-platinum cast body was obtained. The cast body was removed from the mold and casting wrinkles on its surface were removed by milling.
  • the cast body was heated at 1400°C for 30 minutes in an oven under air atmosphere. Then, the heated cast body was subjected to 19 rolling steps. After each rolling step, with the exception of the final rolling step, the cast body was re-heated at a temperature of 1400°C for about 4 minutes. Apart from the higher temperature, rolling conditions were identical to those of Inventive Example 1. Accordingly, thickness of the cast body prior to the rolling treatment and after each rolling step as well as reduction in thickness (in mm and in %) and forming rates of each rolling step were corresponding to those listed above in Table 1.
  • the Ir/Pt40 alloy of CE1 was a mixture of grains having a width to height ratio of close to 1 and slightly elongated grains having a width to height ratio of up to 5. Thus, the average grain width to height ratio was well below 5. The number of pores was 0.05 per ⁇ m 2 . A significant degree of recrystallization of more than 30% was detected.
  • impurities were present in low amounts: Rh ⁇ 200 wt-ppm, Cu ⁇ 150 wt-ppm, Ca ⁇ 100 wt-ppm, B ⁇ 50 wt-ppm, Fe ⁇ 100 ppm.
  • the sample of CE1 had a hardness of 485 HV1 and a density of 22.0 g/cm 3 .
  • the cast body made of the Ir/Pt40 alloy of CE1 was machined to a balance wheel by milling.
  • the edges of the milled article were inspected for defects having a size of > 10 ⁇ m. A significant number of such large size edge-located defects were detected.
  • Table 2 The results of Inventive Example 1 and Comparative Example 1 are summarized in Table 2.
  • Table 2 Properties of the samples of IE1 and CE1 Inventive Example 1 Comparative Example 1 Average grain width to height ratio 12.5 ⁇ 5 Number of pores/ ⁇ m 2 ) 0,01 0,05 Hardness (HV1) 475 485 Density (g/cm 3 ) 22,04 22,0 Number of large size (> 10 ⁇ m) edge-located defects in a milled article made of the Ir/Pt alloy 0 > 10
  • a molded body made of an iridium-platinum alloy having elongated grains can be machined to an article with a reduced number of surface defects.
  • the number and size of edge defects can be significantly reduced.

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  • 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)
  • Forging (AREA)
  • Powder Metallurgy (AREA)

Claims (14)

  1. Ididium-Platin-Legierung, die Platin in einer Menge von 25 Gew.-% bis 45 Gew.-% oder weniger enthält, wobei der Rest Iridium und unvermeidbare Verunreinigungen ist, und ein mittleres Verhältnis von Kornbreite zu -höhe von wenigstens 5 aufweist.
  2. Iridium-Platin-Legierung gemäß Anspruch 1, wobei das mittlere Verhältnis von Kornbreite zu -höhe in dem Bereich von 5 bis 25 liegt.
  3. Iridium-Platin-Legierung gemäß Anspruch 1 oder 2 mit einer mittleren Zahl von Poren pro µm2 von weniger als 0,04; und/oder mit einer Härte von 500 HV1 oder weniger, bevorzugter 480 HV1 oder weniger.
  4. Iridium-Platin-Legierung gemäß einem der vorstehenden Ansprüche, die weniger als 200 Gew.-ppm Rhodium, weniger als 150 Gew.-ppm Kupfer, weniger als 100 Gew.-ppm Calcium, weniger als 50 Gew.-ppm Bor und weniger als 100 Gew.-ppm Eisen enthält.
  5. Iridium-Platin-Legierung gemäß einem der vorstehenden Ansprüche, die eine gewalzte oder geschmiedete Iridium-Platin-Legierung ist, vorzugsweise mit der Form einer Scheibe oder Platte.
  6. Verfahren zur Herstellung der Iridium-Platin-Legierung gemäß einem der Ansprüche 1 bis 5, umfassend
    (i) Herstellen eines Gusskörpers aus einer Iridium-Platin-Schmelze, die aus Iridium, Platin und unvermeidbaren Verunreinigungen besteht,
    (ii) Vorheizen des Gusskörpers auf eine Temperatur Tp-h von 500 °C bis weniger als 1350 °C und Unterwerfen des vorgeheizten Gusskörpers an einen oder mehrere Formgebungsschritte, die bei einer Temperatur Tf von 500 °C bis weniger als 1350 °C durchgeführt werden, so dass die gebildete Iridium-Platin-Legierung einen Rekristallisationsgrad von weniger als 30 % aufweist.
  7. Verfahren gemäß Anspruch 6, wobei wenigstens der letzte Formgebungsschritt bei einer Formgebungstemperatur Tf durchgeführt wird, die unter der Rekristallisationstemperatur liegt; und/oder wobei Vorwärmen des Gusskörpers bei einer Temperatur Tp-h durchgeführt wird, die unter der Rekristallisationstemperatur liegt.
  8. Verfahren gemäß Anspruch 6 oder 7, wobei der Gusskörper bei einer Temperatur Tp-h von 800 °C bis weniger als 1300 °C, noch bevorzugter von 1000 °C bis weniger als 1250 °C, vorgewärmt wird; und der eine oder die mehreren Formgebungsschritte bei einer Temperatur Tf von 800 °C bis weniger als 1300 °C, noch bevorzugter von 1000 °C bis weniger als 1250 °C, durchgeführt werden.
  9. Verfahren gemäß einem der Ansprüche 6 bis 8, wobei die Formgebung von Schritt (ii) Walzen, Schmieden oder eine Kombination davon ist; und/oder Schritt (ii) einen oder mehrere Formgebungsschritte, bevorzugter von 6 bis 30 Formgebungsschritte, umfasst.
  10. Verfahren gemäß einem der Ansprüche 6 bis 9, wobei jeder Formgebungsschritt mit einer Formgebungsrate von weniger als 4,0 s-1, bevorzugter weniger als 3,0 s-1, und/oder einem Formgebungsgrad von weniger als 10,0 %, bevorzugter weniger als 8,0 %, durchgeführt wird.
  11. Bearbeiteter Gegenstand, der die Iridium-Platin-Legierung gemäß einem der Ansprüche 1 bis 5 enthält und eine Dichte von wenigstens 21,4 g/cm3 aufweist.
  12. Bearbeiteter Gegenstand gemäß Anspruch 11, der eine Schwungmasse ist.
  13. Bearbeiteter Gegenstand gemäß Anspruch 11 oder 12, wobei wenigstens 80 Gew.-%, bevorzugter wenigstens 90 Gew.-%, des bearbeiteten Gegenstands aus der Iridium-Platin-Legierung bestehen.
  14. Verfahren zur Herstellung eines bearbeiteten Gegenstands, umfassend
    - Herstellen einer Iridium-Platin-Legierung gemäß dem Verfahren gemäß einem der Ansprüche 6 bis 10,
    - Unterwerfen der Iridium-Platin-Legierung an Bearbeitung, insbesondere Fräsen.
EP16158893.4A 2016-03-07 2016-03-07 Iridium-platinlegierung, daraus hergestellter, maschinell bearbeiteter gegenstand und verfahren zu deren herstellung Active EP3216883B1 (de)

Priority Applications (3)

Application Number Priority Date Filing Date Title
EP16158893.4A EP3216883B1 (de) 2016-03-07 2016-03-07 Iridium-platinlegierung, daraus hergestellter, maschinell bearbeiteter gegenstand und verfahren zu deren herstellung
PCT/EP2017/054982 WO2017153264A1 (en) 2016-03-07 2017-03-03 Iridium-platinum alloy and machined article made thereof
TW106106993A TWI632242B (zh) 2016-03-07 2017-03-03 銥鉑合金及其製造之加工物件

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
EP16158893.4A EP3216883B1 (de) 2016-03-07 2016-03-07 Iridium-platinlegierung, daraus hergestellter, maschinell bearbeiteter gegenstand und verfahren zu deren herstellung

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EP3216883A1 EP3216883A1 (de) 2017-09-13
EP3216883B1 true EP3216883B1 (de) 2019-08-28

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EP (1) EP3216883B1 (de)
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WO (1) WO2017153264A1 (de)

Family Cites Families (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6982122B2 (en) 2003-12-15 2006-01-03 Ut-Battelle, Llc Ir-based alloys for ultra-high temperature applications
DE102005013066B4 (de) 2005-03-18 2008-11-20 W.C. Heraeus Gmbh Stimulationselektrode mit poröser Beschichtung, Verwendung und Herstellungsverfahren
DE102005038772B4 (de) * 2005-08-15 2013-04-18 Heraeus Materials Technology Gmbh & Co. Kg Draht aus oxiddispersionsgehärteten Pt-lr- und anderen Legierungen mit verbesserter Oberfläche für Zündkerzenelektroden
CN101483319B (zh) 2009-02-24 2012-05-23 昆明富尔诺林科技发展有限公司 一种火花塞电极材料和制造方法以及使用该电极材料的火花塞
DE102009031168A1 (de) 2009-06-29 2010-12-30 W.C. Heraeus Gmbh Festigkeitserhöhung von Iridium, Rhodium und ihren Legierungen
US20110061426A1 (en) 2009-09-16 2011-03-17 Michael Silver Jewelry made out of iridium and method of making jewelry out of iridium
JP6243275B2 (ja) * 2014-03-28 2017-12-06 田中貴金属工業株式会社 イリジウム又はイリジウム合金からなる金属線材

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
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WO2017153264A1 (en) 2017-09-14
TW201732045A (zh) 2017-09-16
EP3216883A1 (de) 2017-09-13
TWI632242B (zh) 2018-08-11

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