JP6530402B2 - Method of processing a dispersion strengthened platinum composition - Google Patents

Description

  The present invention relates to a method of processing a dispersion strengthened platinum composition. Furthermore, the present invention relates to a method of producing an article from a dispersion strengthened platinum composition. Furthermore, the invention relates to the products obtained by the above-mentioned method and the use of such platinum compositions.

  Compacts made of platinum are used in many ways in high temperature processes, in which case the material must exhibit high corrosion resistance. For example, members made of platinum that are mechanically loaded, such as eg stirrers or glass fiber bushings, are used in the glass industry. However, the disadvantage of platinum as a raw material is the low mechanical strength at high temperatures. Thus, in general, dispersion-strengthened platinum compositions are used for the high temperature processes described above.

  The preparation and processing of this material are known, for example, from the documents GB 1 340 076 A, GB 2 082 205 A, EP 0 683 240 A2, EP 1 188 844 A1 and EP 1 964 938 A1.

  Generally, first, a hot-rolled ingot is manufactured to manufacture a member made of a dispersion strengthened platinum composition. The resulting semi-finished product can subsequently be cold-formed.

  By means of low-temperature molding, individual settings can be adapted at low cost. However, it has been found that the mechanical properties of the dispersion strengthened platinum material are still not sufficiently good, or at least still have room for improvement, even in such forming techniques. These components may have to be replaced too frequently or more often than desired for some applications. This exchange is tied to high costs. However, forming at high temperatures (so-called hot forming) is very expensive and difficult, because the machines required for this are very expensive.

  The object of the present invention is therefore to overcome the drawbacks of the prior art. In particular, this method should allow for the low cost application of parts consisting of platinum compositions on an individual basis, while improving the mechanical properties. At the same time, the members obtained should exhibit long use times and show as low wear as possible. Furthermore, the method is preferably simple and inexpensive to implement. Furthermore, it is preferred that the shaped parts exhibit good processability, in particular weldability.

The subject of the present invention is the process:
• at least 70% by weight platinum and up to 29.95% by weight other noble metals and 0.05% by weight at least one at least partially oxidized base metal selected from zirconium, cerium, scandium and yttrium Preparing a Volumenkoerper of a dispersion-strengthened platinum composition having ~ 0.5 wt%;
Cold-forming the dispersion-strengthened platinum composition, and reducing the cross-sectional area of the bulk of the dispersion-strengthened platinum composition by up to 20% during this cold-forming; and Heat treatment, during which the cold-formed product is tempered at least 1100 ° C. for at least one hour, and is solved by a method of processing a dispersion strengthened platinum composition.

  The cross-sectional area in the sense of the present invention is taken to be the area of the surface formed upon (virtual) cutting of the volume. The plane emanating from this cross-section may or may not be perpendicular to the direction of greatest extension of the volume.

  The weight percentages mentioned above add up to 100%, in which case the weight of the base metal is based on the weight of the metal.

  Preferably, the one or more base metals are at least 70%, preferably at least 90%, oxidized by oxygen. In this case, preferably at most 30 at%, particularly preferably at most 10 at% of the base metal is present as metal, ie in the formal oxidation state 0, since all oxidation states of the base metal are taken into account.

  Preferably, in the dispersion-strengthened platinum composition, the at least partially oxidized base metal is 0.05% by weight to 0.5% by weight, particularly preferably 0.1% by weight to 0.4% by weight, in particular Preferably, 0.15% by mass to 0.3% by mass is included.

  The high proportion of base metal oxide improves the service life of this volume at mechanical loading. Volumes with a low proportion of base metal oxide show advantages with regard to the processability of the volume, for example weldability.

  In the method of the invention, a volume is provided. The concept of this volume is comprehensively interpreted in this case. Preferably, the volume may be configured, for example, in the form of a plate, a tube or a wire.

  The three-dimensional extent of the volume is not subject to any particular limitation in this case and can be selected according to requirements. Thus, for example, the prepared plate, tube or wire can have a thickness in the range of 0.1 mm to 10 mm, preferably 0.3 to 5 mm. This thickness here represents the smallest spread of the volume. In the case of a wire, this is the diameter, and in the case of a tube, the difference between the outer radius and the inner radius, which is also referred to as the wall thickness of the tube.

  Platinum compositions that can be used in the present invention comprise at least 70% by weight platinum and up to 29.95% by weight other noble metals. Thus, this composition consists mainly of platinum and the at least partially oxidized base metal mentioned above. The platinum material, except for the usual impurities, may be pure platinum, in which an at least partially oxidized base metal is incorporated. Furthermore, the platinum composition may comprise other noble metals, wherein the platinum composition is in this case a platinum alloy.

  In the case of the present invention, the other noble metals may be scheduled to be selected from ruthenium, rhodium, gold, palladium and iridium.

  The prepared volume is cold-formed by the method according to the invention. The concept of "cold forming" is known in the art, wherein the forming takes place at a relatively low temperature below the recrystallization temperature of the platinum composition and in particular drawing, compression, deep drawing, cold Includes rolling, cold forging and pressing. This shaping involves deformation over a large area of the volume. Preferably, this volume may be intended to be deformed over at least 50%, particularly preferably at least 75%, particularly preferably at least 95% of the volume. If this volume is, for example, a plate, preferably at least 50%, particularly preferably at least 75%, particularly preferably at least 95% of the surface of the plate is exposed to force or pressure, for example rolled . This surface can be simplified in the case of a wire and referenced to the plane perpendicular to the smallest extent (thickness) of the volume. If this volume is, for example, a wire or tube, preferably at least 50%, particularly preferably at least 75%, particularly preferably at least 95% of the length of the wire or tube is subjected to force, for example drawn Ru.

  In the present invention, it is important that relatively little shaping is performed during cold forming. Preferably, the cross-sectional area of the volume of the dispersion-strengthened platinum composition is reduced by at most 20%, particularly preferably at most 18%, particularly preferably at most 15%. This value relates to the cross-sectional area of the volume which is maximally reduced. In the case of plates which are only rolled in one direction, the reduced cross-sectional area results, for example, from the thickness of the volume as well as the unstretched spread. In the case of wire or tubing, the reduction in cross-sectional area results from changes in diameter or wall thickness. Since the volume of this volume does not change with shaping, at least one cross-sectional area has to be enlarged during this shaping. In the case of a plate, a tube or a wire, for example, since the length is increased during the forming, the area in the direction in which the length is increased is increased. The direction in which the deforming force acts is directed in particular in a direction parallel or perpendicular to the plane extending from the cross section.

  In the case of a preferred embodiment, in this cold-forming, the cross-sectional area of the volume of dispersion-strengthened platinum composition is reduced by at least 5%, preferably by at least 8%, particularly preferably by at least 10%. Is scheduled.

  It has been determined that internal damage of the dispersion-strengthened volume essentially does not contribute to the improvement of the creep resistance during forming and subsequent annealing with a reduction of the cross-sectional area of less than 5% each. The smaller the change of the cross-sectional area per one molding step within the above range, the reduction of the cross-sectional area is 5% to 20%, preferably 8% to 18%, particularly preferably 10% to 15%. Compared to molding, the effect on improving creep resistance is also less.

  Furthermore, the wire is drawn or compressed by cold forming, where the cross-sectional area of the wire made of the dispersion strengthened platinum composition by cold forming is at most 20%, preferably at most 18%, particularly preferably at most 15% Reduce or cold-roll the plate material by rolling, drawing, compression or pressing, where the cross-sectional area or the plate thickness of the plate material comprising the dispersion-strengthened platinum composition in the cold-forming is up to 20%, The tube is rolled, drawn or compressed preferably by up to 18%, particularly preferably up to 15%, or by cold forming, where the cross section of the tube consisting of the dispersion strengthened platinum composition in this cold forming is A reduction of at most 20%, preferably at most 18%, particularly preferably at most 15% may be planned.

  In the case of the present invention, cold forming does not produce microcracks or pores inside the dispersion strengthened platinum composition, or produces less than 100 microcracks and / or less than 1000 pores per cubic millimeter. It may be planned.

  After cold forming of the volume, heat treatment of the cold formed volume is carried out, wherein the cold formed product is tempered at at least 1100 ° C. for at least one hour. This tempering can take place over a period of preferably at least 90 minutes, in particular at least 120 minutes, particularly preferably at least 150 minutes, particularly preferably at least 180 minutes. The temperature at which this tempering is carried out can preferably be at least 1200 ° C., particularly preferably at least 1250 ° C., particularly preferably at least 1300 ° C., and very particularly preferably at least 1400 ° C.

  Further, during heat treatment of the cold-formed volume, it may be scheduled to temper at least 1 hour at a temperature of at least 1250 ° C., preferably 1 to 3 hours at a temperature of 1400 ° C. .

  The longer the tempering process and the higher the temperature at which the heat treatment is carried out, the better the mechanical properties of the cold-formed volume. However, at some point the improvement in mechanical properties is saturated and there is a risk of significant grain growth which again degrades the mechanical properties. Furthermore, the cost of this method increases with time and temperature. The minimum temperature for the tempering operation is 1100.degree. The maximum temperature for the tempering operation is 20 ° C. below the melting temperature of the respective dispersion strengthened platinum composition.

  Preferably, one or more heat treatments of the cold-formed volume may be intended to be applied to recover the defects of this volume.

  In the case of the process according to the invention, a plurality of cold forming operations are carried out successively from one another, and their cold forming reduces the cross-sectional area of the volume by more than 20%, in this case individual cold forming Reduce the cross-sectional area of the volume consisting of the dispersion-strengthened platinum composition by at most 20%, preferably at most 18%, particularly preferably at most 15%, and a cold-formed volume during each cold forming Heat treatment, and during this heat treatment it may be scheduled to temper the cold-formed product at at least 1100 ° C. for at least one hour.

  Here, “during each cold forming” preferably performs the heat treatment at least 1100 ° C. for at least one hour after each cold forming, so the number of cold forming steps and the number of tempering steps are the same Means to be.

  The practice of multiple cold forming and heat treatments does not weaken the dispersion-strengthened platinum composition, that is to say the alloy should for example be cold relatively easily and at low cost without reducing its creep resistance. It has an advantage that relatively large deformation can be realized also by inter-forming and heat treatment. On the contrary, it has surprisingly been found that the creep resistance is improved in the direction of increasing with increasing number of forming and tempering steps.

  In the case of a preferred embodiment of the present invention, the cross-sectional area of the volume consisting of the dispersion-strengthened platinum composition is reduced by at least 5%, preferably for each individual cold-forming, in successive cold-forming, preferably Is intended to be reduced by at least 8%, particularly preferably by at least 10%.

  A forming step comprising a slight reduction of less than 5% of the cross-sectional area of the dispersion-strengthened volume and the subsequent tempering per forming step does not essentially contribute to the improvement of the creep resistance. The smaller the change in cross-sectional area per molding step within the above range, the more the effect on improving the creep resistance compared to molding with a reduction of the cross-sectional area of 5% to 20%. It becomes slight. With multiple alternating molding and tempering steps, the method is more expensive and thus uneconomical. This is all the more true as the number of forming steps required to achieve the desired final dimensions of the dispersion strengthened volume is increased. In order to obtain the desired final dimensions, a number of eight molding steps is preferred. The number of deformation steps is a favorable compromise between economics and improved mechanical properties.

  Preferably, during the final heat treatment after final cold forming of the volume, the cold formed product is at least 15 hours at least 1550 ° C., at least 12 hours at 1600 ° C., at least 1 hour at 1650 ° C. Tempering can be scheduled for a time or for at least 30 minutes at a temperature of 1690 ° C. to 1749 ° C.

  By this last step, the simple defects to be recovered of the dispersion-strengthened platinum composition are substantially eliminated in its final form, and the product thus produced exhibits thereby very high creep resistance.

  All dispersion-strengthened platinum compositions are suitable as starting products for this processing method. However, surprising advantages generally result from the use of semifinished products exposed to hot forming. The dispersion strengthened platinum composition is formed by hot forming at a temperature of at least 800 ° C., preferably at a temperature of at least 1000 ° C., particularly preferably at a temperature of at least 1250 ° C., before cold forming be able to.

  Another subject of the invention is selected from ruthenium, zirconium, cerium, scandium and yttrium and at least 70% by weight of platinum and up to 29.95% by weight of other noble metals prior to the preparation of the dispersion-strengthened platinum composition. The dispersion-strengthened platinum composition is produced by at least partial oxidation of the one or more base metals from a composition consisting of 0.05% by weight to 0.5% by weight of at least one base metal. A method of producing a product comprising a dispersion strengthened platinum composition.

  Preferably, at least 70%, preferably at least 90% of the one or more base metals are reacted to the metal oxide.

  The treatment of the one or more base metals can be carried out preferably at a temperature of 600 ° C. to 1600 ° C. in an oxidizing atmosphere, preferably at a temperature of 800 ° C. to 1000 ° C. in an oxidizing atmosphere.

  The method of producing the product consisting of the dispersion strengthened platinum composition may preferably be combined with the above-mentioned processing method and its embodiments described as preferred therein.

  Another subject of the present invention is a dispersion-strengthened platinum material obtainable by a method of treatment and / or a method of manufacturing a product consisting of a dispersion-strengthened platinum composition. The subject matter provides excellent mechanical properties combined with excellent processability or low cost and effortless manufacturability.

  Preferably, the cylindrical volume of dispersion-strengthened platinum material withstands a tensile load of 9 MPa in the longitudinal direction of the volume at a temperature of 1600 ° C. for at least 40 hours without tearing, preferably tearing at least 50 hours. Plates with a rectangular cross section of 0.85 mm × 3.9 mm and a length of 140 mm consisting of a dispersion-strengthened platinum material, preferably withstanding for at least 100 hours and / or at least 100 hours without When mounted on two cylindrical bars arranged in parallel at 100 mm intervals and having a circular cross section with a diameter of 2 mm at 1650 ° C., and with a 30 g weight applied to the center of the plate The deflection after 40 hours is less than 40 mm, preferably less than 30 mm, particularly preferably less than 20 mm, still more preferably Deflection may be expected to be less than 14mm.

  In the context of the present invention, a cylindrical volume is understood to mean a shaped body resembling a straight cylindrical shape, in particular a shaped body resembling a cylindrical shape or a cylindrical shape with a non-round or non-round bottom. . Cylindrical volumes are also in particular also rectangular bodies with side lengths in the range 0.5 mm to 5 mm (ie shaped bodies resembling cylinders with a rectangular base).

  The length of a cylindrical volume is taken to be the longest extension. The direction of this length is, in the case of a wire or a tube, the axis of a cylindrical volume, and in the case of a plate, the spread of the plane of the plate.

  Furthermore, dispersion strengthened platinum materials having the mechanical properties described above for cylindrical volumes are the subject of the present invention.

  Preferably, the dispersion strengthened platinum material comprises 0.05% by weight to 0.4% by weight, particularly preferably at least one at least partially oxidized at least one base metal selected from zirconium, cerium, scandium and yttrium. 05 mass%-0.3 mass% may be scheduled to be included. According to this aspect, it is possible to provide a material having particularly excellent mechanical properties and extremely good processability.

  In particular embodiments, the dispersion-strengthened platinum material can be a sheet, tube or wire, or a product formed from a wire, tube and / or sheet.

  Another subject of the invention is obtained by the processing method according to the invention and / or by the manufacturing method according to the invention products from dispersion-strengthened platinum compositions, for equipment to be used in the glass industry or in the laboratory Or the use of a volume formed from the dispersion-strengthened platinum material or platinum composition obtained.

  The present invention again demonstrates the stability of the shaped platinum composition by a slight cold forming (with a change in cross-sectional area of up to 20%), with the subsequent heat treatment, the known cold of the dispersion-strengthened platinum composition. Based on the surprising finding that weak structural damage, such as introducing crystal lattice defects into the dispersion-strengthened platinum composition, can be achieved to such an extent that recovery can be achieved significantly higher than in the molding method. If stronger forming is desired, this forming can be achieved by preceding hot forming, or several slight cold formings may be carried out successively, where structurally during each cold forming. Damage recovery is performed by heat treatment. It has been found within the scope of the present invention that mechanical weakening of a cold-formed dispersion-strengthened platinum composition results in strong defects such as microcracks, exfoliation of particle / matrix interfaces and too many pores at grain boundaries. And caused by these defects was a too high degree of deformation or a too large reduction of the cross-sectional area.

  In particular, due to mild, slight cold forming, microcracks that can not or can not recover much even with great effort, such as exfoliation of the particle / matrix interface and pores at the grain interface. Internal damage is reduced. In particular, the microcracks and pores that form at the grain boundaries due to shaping are detrimental, as these in particular significantly impair the mechanical stability of the dispersion strengthened platinum composition. The control of this damage is achieved by the method according to the invention. Thus, for the first time it is successful to produce dispersion-strengthened platinum compositions having very high mechanical stability and excellent processability, in particular weldability, which dispersion-strengthened platinum compositions are likewise claimed by the present invention.

  Next, further examples of the present invention will be described using examples, but this is not a limitation of the present invention.

Semi-finished product precursor 1
Production of semi-finished product of 2 mm thickness by internal oxidation with Zr and Y
In accordance with the method described in Example 1 of EP 1 964 938 A1, an ingot having PtRh10 (an alloy consisting of 90% by weight of Pt and 10% by weight of Rh) and 2200 ppm of base metal (1800 ppm of Zr and 400 ppm of Y) was cast. Subsequently, the ingot was treated mechanically and thermally. Thus, the ingot was rolled to a thickness of 2.2 mm, then annealed for recrystallization and subsequently rolled to a pressure of 2 mm. The plate was then oxidized at 900 ° C. for 18 days and subsequently ductile annealed at 1400 ° C. for 6 hours.

Semi-finished product precursor 2
Production of semi-finished product with 3 mm thickness by internal oxidation with Zr and Y
In accordance with the method described in Example 1 of EP 1 964 938 A1, an ingot having PtRh10 (an alloy consisting of 90% by weight of Pt and 10% by weight of Rh) and 2200 ppm of base metal (1800 ppm of Zr and 400 ppm of Y) was cast. Subsequently, the ingot was treated mechanically and thermally. Thus, the ingot was rolled to a plate thickness of 3.3 mm, then annealed for recrystallization and subsequently rolled to a plate pressure of 3 mm. The plate was then oxidized at 900 ° C. for 27 days and subsequently ductile annealed at 1400 ° C. for 6 hours.

Semi-finished product precursor 3
Production of semi-finished product with 3 mm thickness by internal oxidation with Zr, Y and Sc
According to the method described in Example 1 of EP 1 964 938 A1, an ingot having PtRh10 (an alloy consisting of 90% by weight of Pt and 10% by weight of Rh) and 2120 ppm of base metal (1800 ppm of Zr, 270 ppm of Y and 50 ppm of Sc) was cast. Subsequently, the ingot was treated mechanically and thermally. Thus, the ingot was rolled to a plate thickness of 3.3 mm, then annealed for recrystallization and subsequently rolled to a plate pressure of 3 mm. The plate was then oxidized at 900 ° C. for 24 days and subsequently ductile annealed at 1400 ° C. for 6 hours.

Example 1
The semifinished product precursor 1 with a thickness of about 2 mm obtained by the above-mentioned method is further processed according to the present invention by the following rolling and annealing steps.

  The plate was rolled to 1.7 mm and subsequently annealed at 1400 ° C. for 4 hours. Thereafter, the plate is rolled to 1.4 mm and annealed at 1400 ° C. for 2 hours. Then, it is further rolled to 1.2 mm and annealed again at 1400 ° C. for 2 hours. It is then rolled to 1 mm and annealed again at 1400 ° C. Thereafter, it is rolled to a final thickness of 0.85 mm and a final annealing is carried out at 1100 ° C. for 1 hour. The reduction rate of the cross sectional area for each rolling process is 20%.

Example 2
Example 1 is repeated approximately, but after rolling to a final thickness of 0.85 mm, a final annealing is performed at 1700 ° C. for 1 hour.

Example 3
The semifinished product precursor 2 with a thickness of about 3 mm obtained by the above-mentioned method is further processed by the following rolling and annealing steps according to the present invention.

  The plate was rolled to 2.4 mm and subsequently annealed at 1150 ° C. for 4 hours. Thereafter, the plate is rolled to 1.92 mm and annealed at 1150 ° C. for 4 hours. Then, it is rolled to 1.53 mm and annealed again at 1150 ° C. for 4 hours. The rolling and annealing steps are repeated three more times, initially rolling to 1.22 mm, then to 0.99 mm and then to 0.8 mm and annealing at 1150 ° C. for 4 hours after each rolling step. The reduction rate of the cross sectional area for each rolling process is 20%.

Example 4
The semifinished product precursor 2 with a thickness of about 3 mm obtained by the above-mentioned method is further processed by the following rolling and annealing steps according to the present invention.

  The plate was rolled to 2.4 mm and subsequently annealed at 1300 ° C. for 4 hours. Thereafter, the plate is rolled to 1.92 mm and annealed at 1300 ° C. for 4 hours. Then, it is rolled to 1.53 mm and annealed again at 1300 ° C. for 4 hours. The rolling and annealing steps are repeated three more times, initially rolling to 1.22 mm, then to 0.99 mm and then to 0.8 mm and annealing at 1300 ° C. for 4 hours after each rolling step. The reduction rate of the cross sectional area for each rolling process is 20%.

Example 5
The semifinished product precursor 2 with a thickness of about 3 mm obtained by the above-mentioned method is further processed by the following rolling and annealing steps according to the present invention.

  The plate was rolled to 2.4 mm and subsequently annealed at 1400 ° C. for 4 hours. Thereafter, the plate is rolled to 1.92 mm and annealed at 1400 ° C. for 4 hours. Then, it is rolled to 1.53 mm and annealed again at 1400 ° C. for 4 hours. The rolling and annealing steps are repeated three more times, initially rolling to 1.22 mm, then to 0.99 mm and then to 0.8 mm and annealing at 1400 ° C. for 4 hours after each rolling step. The reduction rate of the cross sectional area for each rolling process is 20%.

Example 6
The semifinished product precursor 2 with a thickness of about 3 mm obtained by the above-mentioned method is further processed by the following rolling and annealing steps according to the present invention.

  The plate was rolled to 2.55 mm and subsequently annealed at 1400 ° C. for 4 hours. Thereafter, the plate is rolled to 2.16 mm and annealed at 1400 ° C. for 4 hours. It is then rolled to 1.84 mm and annealed again at 1400 ° C. for 4 hours. The rolling and annealing steps are repeated five more times, first rolling 1.56 mm, then 1.33 mm, then 1.13 mm, then 0.96 mm and then 0.8 mm, and after each rolling step 1400 Anneal at 4 ° C for 4 hours. The reduction rate of the cross sectional area for each rolling process is 15%.

Example 7
The semifinished product precursor 3 with a thickness of about 3 mm obtained by the above-mentioned method is further processed by the following rolling and annealing steps according to the present invention.

  The plate was rolled to 2.4 mm and subsequently annealed at 1150 ° C. for 4 hours. Thereafter, the plate is rolled to 1.92 mm and annealed at 1150 ° C. for 4 hours. Then, it is rolled to 1.53 mm and annealed again at 1150 ° C. for 4 hours. The rolling and annealing steps are repeated three more times, initially rolling to 1.22 mm, then to 0.99 mm and then to 0.8 mm and annealing at 1150 ° C. for 4 hours after each rolling step. The reduction rate of the cross sectional area for each rolling process is 20%.

Example 8
The semifinished product precursor 3 with a thickness of about 3 mm obtained by the above-mentioned method is further processed by the following rolling and annealing steps according to the present invention.

  The plate was rolled to 2.55 mm and subsequently annealed at 1400 ° C. for 4 hours. Thereafter, the plate is rolled to 2.16 mm and annealed at 1400 ° C. for 4 hours. It is then rolled to 1.84 mm and annealed again at 1400 ° C. for 4 hours. The rolling and annealing steps are repeated five more times, first rolling 1.56 mm, then 1.33 mm, then 1.13 mm, then 0.96 mm and then 0.8 mm, and after each rolling step 1400 Anneal at 4 ° C for 4 hours. The reduction rate of the cross sectional area for each rolling process is 15%.

Example 9
The semifinished product precursor 3 with a thickness of about 3 mm obtained by the above-mentioned method is further processed by the following rolling and annealing steps according to the present invention.

  The plate was rolled to 2.7 mm and subsequently annealed at 1400 ° C. for 4 hours. Thereafter, the plate is rolled to 2.43 mm and annealed at 1400 ° C. for 4 hours. It was then rolled to 2.19 mm and annealed again at 1400 ° C. for 4 hours. The rolling process and the annealing process are repeated nine more times, with 1.97 mm then 1.77 mm then 1.60 mm then 1.44 mm then 1.29 mm then 1.16 mm then 1.16 mm then 1.05 mm. It is then rolled to 0.94 mm and subsequently to 0.85 mm and annealed at 1400 ° C. for 4 hours after each rolling step. The reduction rate of the cross sectional area for each rolling process is 10%.

Example 10
Example 9 is largely repeated, but after rolling to a final thickness of 0.85 mm, a final annealing is carried out at 1700 ° C. for 1 hour.

Example 11
The semifinished product precursor 3 with a thickness of about 3 mm obtained by the above-mentioned method is further processed by the following rolling and annealing steps according to the present invention.

  This plate was rolled to 1.5 mm at 1100 ° C. (hot forming) and subsequently annealed at 1400 ° C. for 4 hours. Thereafter, the plate is rolled to 1.2 mm (first cold forming) and subsequently annealed at 1250 ° C. for 4 hours. It is then rolled to 1.02 mm (second cold forming) and subsequently annealed at 1250 ° C. for 4 hours. The rolling process and the annealing process are repeated three times, first at 0.94 mm (third cold forming), then at 0.86 mm (fourth cold forming), and then 0.8 mm (fifth Cold forming) and annealing for 4 hours at 1250 ° C. after each rolling step. The reduction rate of the cross sectional area is 50% in the hot forming step, 20% first in the cold forming step, then 15%, and then 8% respectively.

Comparative Example 1
The semifinished product precursor 1 with a thickness of about 2 mm obtained by the above-mentioned method is further processed by the usual method. Therefore, the plate is directly rolled to 1 mm and annealed at 1000 ° C. Thereafter, it is rolled to 0.85 mm and final annealing is performed at 1000 ° C. for 1 hour.

Comparative example 2
The semifinished product precursor 2 with a thickness of about 3 mm obtained by the above-mentioned method is further processed by the usual method. Therefore, this plate is rolled to 1.5 mm and annealed at 1400 ° C. for 4 hours. After that, it is rolled to 0.8 mm. The reduction rate of the cross sectional area for each rolling process is 50%.

Comparative example 3
The semifinished product precursor 3 with a thickness of about 3 mm obtained by the above-mentioned method is further processed by the usual method. Therefore, this plate is rolled to 1.5 mm and annealed at 1400 ° C. for 4 hours. After that, it is rolled to 0.8 mm. The reduction rate of the cross sectional area for each rolling process is 50%.

Mechanical Properties of Obtained Platinum Material Creep Resistance by Fracture Test For measurement of creep resistance, plate samples of 0.85 mm × 3.9 mm cross section and 120 mm length (Examples 1, 2, 9; 10 and Comparative Example 1) or to a plate sample (Examples 3, 4, 5, 6, 7, 8, 11 and Comparative Examples 2 and 3) having a cross section of 0.8 mm × 3.9 mm and a length of 120 mm, The weight corresponding to the desired load, indicated in MPa, is suspended for the above-mentioned cross section. The sample is heated by electrical current and regulated at the desired temperature by pyrometer measurement. Determine the time to failure of the sample and show creep resistance.

Table 1: Creep resistance to failure at loads of 600 ° C and 9MPa

Creep Resistance by Deflection Test Another method to evaluate creep resistance is deflection test. To this end, plate materials having a cross section of 0.85 mm × 10 mm and a length of 140 mm (Examples 1, 2, 9, 10 and Comparative Example 1) or a plate having a cross section of 0.8 mm × 10 mm and a length of 140 mm (Examples 3, 4, 5, 6, 7, 8, 11 and Comparative Examples 2 and 3) were placed on two parallel ceramic bars spaced 100 mm apart and loaded with a 30 g weight in the middle . The sample configuration was heated to 1650 ° C. in a chamber furnace and after 40 hours the deflection of the sample was measured.

Table 2: Creep resistance by deflection test

  The embodiments described above can achieve a surprising improvement in mechanical properties by means of the measures according to the invention, wherein this improvement is further enhanced by an annealing process at temperatures above 1100 ° C., in particular above 1500 ° C. Show what you can do.

  The features of the invention disclosed in the above specification, as well as in the claims and in the examples, either alone or in each case for the realization of the invention in the case of the various embodiments of the invention. It can also be important as a combination.

Claims (19)

Next step:
70 wt% even without platinum small and other precious metals up to 29.95% by weight, and zirconium, cerium, a base metal selected from scandium and yttrium, at least one at least partially oxidized Providing a volume of dispersion-strengthened platinum composition consisting of 0.05% to 0.5% by weight of a base metal, but containing normal impurities ,
Cold forming the volume of the dispersion strengthened platinum composition, wherein the cross section of the volume of the dispersion strengthened platinum composition is reduced by up to 20% during the cold forming, and subsequently
Heat treating the cold-formed volume, wherein during the heat treatment tempering the cold-formed volume at least at 1100 ° C. for at least 1 hour, dispersion-strengthened platinum composition How to work. Before the cold forming, the dispersion strengthened platinum composition, characterized and Turkey be molded at a temperature of at least 800 ° C. by hot forming method according to claim 1. The method of claim 1, wherein prior to the cold forming, the dispersion strengthened platinum composition is formed by hot forming at a temperature of at least 1250 ° C. A plurality of cold formings are carried out successively from one another, and the multiple cold formings reduce the cross-sectional area of the volume by more than 20%, wherein in the case of individual cold formings The cross-sectional area of the volume consisting of the dispersion-strengthened platinum composition is reduced by up to 20%, and the heat treatment of the cold-formed volume is carried out during each cold-forming, during the heat treatment the cold-forming volume 4. A method according to any one of the preceding claims, characterized in that the in-moulded volume is tempered at at least 1100 <0> C for at least 1 hour. During the final heat treatment after the last cold-forming of the volume , the cold-formed volume is at least 15 hours at least 15 hours and at least 16 hours at 16 days. and returning at least baked for 30 minutes at 1 hour baked back or temperature of 1690 ℃ ~1740 ℃, method according to any one of claims 1 to 4. The wire is drawn or compressed by cold forming, and the cross-sectional area of the wire made of the dispersion strengthened platinum composition is reduced by up to 20% by the cold forming, or the plate is rolled or drawn by cold forming. Process, compress or press, reduce the cross-sectional area of the plate made of the dispersion strengthened platinum composition by the cold forming or the thickness of the plate by up to 20%, or roll process the tube by cold forming The method according to any one of claims 1 to 5 , wherein, in the case of drawing processing or compression processing, the cross-sectional area of the pipe material made of the dispersion strengthened platinum composition is reduced by at most 20% by the cold forming. Method described. It said cold forming, which comprises carrying out at 500 ° C. below the temperature A method according to any one of claims 1 to 6. Said one or more heat treatment of the cold-shaped volume element, and wherein applying for recovery of a defect of the volume body A method according to any one of claims 1 to 7 . During heat treatment of the cold-formed volumetric body, and returning at least 1 hour baked at a temperature of at least 1250 ° C., the method according to any one of claims 1 to 8. 10. A method according to any one of the preceding claims, characterized in that during the heat treatment of the cold-formed volume, it is tempered at a temperature of at least 1400 <0> C for 1 to 3 hours. A method of producing a product comprising a dispersion-strengthened platinum composition according to any one of claims 1 to 10 , wherein at least 70% by weight of platinum and other noble metals are provided prior to the preparation of the dispersion-strengthened platinum composition. up 29.95 wt%, and ruthenium, zirconium, cerium, at least one base metal 0.05 wt% is selected from scandium and yttrium to 0.5 wt% Tona is, however contain the usual impurities A method of producing a product comprising a dispersion strengthened platinum composition, characterized in that said dispersion strengthened platinum composition is produced from a good composition by at least partial oxidation of said one or more base metals. The one or more at least partial oxidation of the base metal, characterized by the TURMERIC line in an oxidizing atmosphere at a temperature of 600 ° C. to 1600 ° C., The method of claim 11. The method according to claim 11, characterized in that at least partial oxidation of the one or more base metals is performed at a temperature of 800 ° C to 1000 ° C under an oxidizing atmosphere. At least 70% by weight of platinum and up to 29.95% by weight of other noble metals, and 0.05% by weight of at least one base metal selected from zirconium, cerium, scandium and yttrium, at least partially oxidized A dispersion-strengthened platinum material consisting of ̃0.5% by mass, but may contain normal impurities ,
The cylindrical volume of the dispersion-strengthened platinum material withstands at least 40 hours under a tensile load of 9 MPa in the longitudinal direction of the volume at a temperature of 1600 ° C. and / or the dispersion-strengthened platinum material A plate of rectangular cross section of 0.85 mm × 3.9 mm and having a length of 140 mm consisting of two circular cross sections of 2 circular cross sections arranged in parallel at a distance of 100 mm at 1650 ° C. in the furnace chamber. A dispersion-strengthened platinum material , characterized in that the deflection after 40 hours is less than 40 mm when placed on a cylindrical rod of a diameter of 50 mm and the center of the plate is loaded with a 30 g weight . The dispersion-strengthened platinum material is characterized plate, or a tube or wire, or wire, to be formed from the tubing and / or sheet material, dispersion strengthened platinum material according to claim 14. The dispersion strengthened platinum material is characterized in that it contains 0.05% by mass to 0.3% by mass of an at least partially oxidized at least one base metal selected from zirconium, cerium, scandium and yttrium. The dispersion strengthened platinum material according to claim 14 or 15 . The cylindrical volume of said dispersion strengthened platinum material is characterized in that it withstands at a temperature of 1600 ° C. with a tensile load of 9 MPa in the lengthwise direction of said volume for at least 100 hours without tearing. 16. Dispersion-strengthened platinum material according to any one of the preceding claims. A 0.85 mm × 3.9 mm rectangular cross-section plate having a length of 140 mm, made of the dispersion-strengthened platinum material, is a circular plate in which the plate material is arranged in parallel at an interval of 100 mm at 1650 ° C. in a furnace chamber. It is characterized in that the deflection after 40 hours is less than 20 mm when it is placed on a cylindrical rod of transverse cross section and a diameter of 2 mm and the center of the plate is loaded with a weight of 30 g, The dispersion strengthened platinum material according to any one of claims 14 to 17. For devices to be used in or laboratory in the glass industry, use of dispersion-strengthened platinum materials according to any one of claims 14 to 18.