Classifications

• • 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
• • 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
• • 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 to 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.
• components made of platinum are used in the glass industry, which are mechanically loaded, 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.
• Forming at low temperatures allows cost-effective adaptation to individual requirements.
• the mechanical properties of dispersion-hardened platinum materials are not sufficiently good, or at least could be better, especially in such forming techniques.
• the components have too little service life for some applications or must be replaced more frequently than desired. This exchange is associated with high costs.
• a conversion at high temperatures (a so-called hot forming) is very expensive and difficult, since the machines required for this are very expensive.
• 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 volume body.
• 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 stage 0.
• 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 usual 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 transformation takes place at relatively low temperatures below the recrystallization temperature of the platinum composition, and includes, in particular, drawing, pressing, deep drawing, cold rolling, cold hammering and pressing It can preferably be provided that 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 Accordingly, 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 expansion 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 a 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 the cross-sectional area of the sheet or the thickness of the plate from the dispersion-hardened platinum composition is reduced by a maximum of 20%, more preferably by a maximum of 18% and most preferably by a maximum of 15% during cold working or during 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 most preferably by a maximum of 15%.
• a temperature treatment of the cold-formed volume is carried out, in which the cold-formed product is tempered 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 1 100 ° 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 inventive method may also be provided in the inventive method that several cold transformations are carried out successively and the cross-sectional area of the volume body is reduced by more than 20% by the cold forming, wherein in each individual cold forming the cross-sectional area of the volume body of the dispersion-hardened platinum composition by a maximum of 20 %, more preferably by a maximum of 18%, and more preferably by a maximum of 15%, and a temperature treatment of the cold-formed volume body is performed between each cold working, wherein the cold-formed 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 tempering steps is the same
• Cold forming and temperature treatments has the advantage that with the cold forming and temperature treatments, which are relatively easy and inexpensive, larger transformations can be realized without weakening the dispersion-hardened platinum composition, that is, without, for example, reducing the alloy's creep rupture strength even 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 complicated and therefore uneconomical in one step after the other forming and annealing steps. 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.
• 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.
• 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 of the present invention is a process for producing a product from a dispersion-hardened platinum composition, which is characterized in that, before providing the dispersion-hardened platinum composition, these consist of a composition of at least 70% by weight platinum and at most
• 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 process for producing a product from a dispersion-cured platinum composition can preferably be combined with the above-described process for processing and the embodiments of the same described as preferred herein.
• 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 of the dispersion-hardened platinum material at 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.
• a cylindrical volume body is to be understood according to the invention as meaning a straight cylindrical body, in particular a cylinder, or a cylinder-like body with a non-circular or round base area.
• the cylindrical volume body is in particular also a cuboid (thus a cylinder-like body with a rectangular base) with edge lengths in the range of 0.5 mm to 5 mm.
• the length of the cylindrical volume body is understood to be the longest extent.
• Direction of the length is the axis of the cylindrical volume body in the case of a wire or a pipe, and in the case of a metal sheet an extension in the plane of the metal sheet. Furthermore, a dispersion-hardened platinum material with the mechanical properties described above for a cylindrical volume body is the subject of the present invention.
• at least one at least partially oxidized non-noble metal selected from zirconium, cerium, scandium and yttrium includes.
• 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 mechanical weakening of cold-formed dispersion-hardened platinum compositions is caused by too great a number of strong defects, such as microcracks, delaminations of the particle / matrix interfaces and pores at grain boundaries, and these are at too high a degree of deformation Too large reduction of the cross-sectional area are due.
• 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 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 1 100 ° C for 1 h performed.
• 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.
• Example 3 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 1 150 ° C for 4 h. Thereafter, the sheet is rolled to 1, 92 mm and annealed at 1 150 ° C for 4 h. Then it is rolled to 1, 53 mm and again annealed for 4 h at 1 150 ° 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 for 4 h at 1 150 ° C after each rolling step ,
• 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 again annealed 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 1 150 ° C for 4 h. Thereafter, the sheet is rolled to 1, 92 mm and annealed at 1 150 ° C for 4 h. Then it is rolled to 1, 53 mm and again annealed for 4 h at 1 150 ° 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 for 4 h at 1 150 ° C after each rolling step ,
• the reduction in the cross-sectional area per rolling step is 20%.
• Example 8 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 rolled to 1.29 mm, then to 1.16 mm, then to 1.05 mm, then to 0.94 mm and then to 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 10 is essentially repeated, but after rolling to a final thickness of 0.85 mm, a final annealing is carried out at 1700 ° C for 1 h.
• 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 1 100 ° 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 forming) and then annealed at 1250 ° C for 4 h. Then 1, 02 mm rolled (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 forming) 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.
• Comparative Example 1 The semifinished product precursor 1 obtained according to the method set forth above with a thickness of about 2 mm is further processed according to a conventional method. For this purpose, the sheet is rolled directly to 1 mm and annealed at 1000 ° C. Then it is rolled to 0.85 mm and a
• Comparative Example 2 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. For this purpose, 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%. Comparative Example 3
• 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 the cross-sectional area per rolling step is 50%.
• Example 1 1> 100 h

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• 2013
  • 2013-12-06 DE DE102013225187.4A patent/DE102013225187B4/de active Active
• 2014
  • 2014-12-04 US US15/100,809 patent/US20160289808A1/en not_active Abandoned
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