KR101831090B1 - Method for processing a dispersion-hardened platinum composition - Google Patents

Abstract

The present invention relates to a process for processing a dispersion-cured platinum composition, comprising the steps of: preparing a mixture of at least 70 wt.% Platinum, up to 29.95 wt.% Of other precious metals and 0.05 wt.% To 0.5 wt.% Of zirconium, cerium, scandium and yttrium Providing a three-dimensional shape of a dispersion-cured platinum composition comprising at least one partially oxidized noble metal; Forming a three-dimensional shape of the dispersion-cured platinum composition by cold forming, wherein the cross-sectional area of the three-dimensional shape produced by the dispersion-cured platinum composition during the cold forming is reduced by at most 20%; And then subjecting the cold-formed three-dimensional shaped body to a temperature treatment, wherein the cold-formed article is tempered at least at 1,100 ° C for at least one hour. The present invention also describes a method for producing a product made from a dispersion-cured platinum composition and a dispersion-cured platinum material obtainable according to the above-described processing method. Also disclosed is the use of dispersion-cured platinum materials.

Description

METHOD FOR PROCESSING A DISPERSION-HARDENED PLATINUM COMPOSITION [0001]

The present invention relates to a process for processing a dispersion-cured platinum composition. The present invention also describes a process for producing a product from a dispersion-cured platinum composition. The present invention also relates to the products obtainable from the process and to the use of the platinum compositions.

Molded bodies made of platinum are commonly used in high temperature processes where the material must have high corrosion resistance. For example, platinum parts exposed to mechanical loads, such as stirrers or glass fiber jet troughs, are used in the glass industry. However, when used as a material, platinum has a disadvantage of low mechanical strength at high temperatures. For this reason, dispersion-cured platinum compositions are generally used in the above-mentioned high temperature process.

The production and processing of these materials is known, for example, from 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.

The manufacture of components from a dispersion-cured platinum composition generally begins with the ingot being hot rolled. Next, the obtained semi-finished product can be cold-formed.

Low-temperature molding allows low-cost configuration to suit individual requirements. However, it has been found clearly that the mechanical properties of the dispersion-cured material are not yet good enough or at least better in the molding technology. Parts need to be either too short for some applications or replaced more frequently than desired. This replacement is associated with high cost. However, high temperature molding (so-called hot forming) is costly and difficult because of the complexity of the machines used for this purpose.

Therefore, an object of the present invention is to overcome the disadvantages of the prior art. And in particular, to provide a method for constructing a component made of a platinum composition to meet individual requirements at low cost while improving mechanical properties. At the same time, the parts thus obtained should have a long service life and should have as little wear and tear as possible. The method should also be easy to implement and low cost. In addition, the molded part should have good processing characteristics, particularly good welding characteristics.

SUMMARY OF THE INVENTION

At least one at least partially oxidized non-noble metal selected from at least 70% by weight of platinum, up to 29.95% by weight of other noble metals and zirconium, cerium, scandium and yttrium selected from zirconium, Providing a three-dimensional shape of the platinum composition;

C) cold-forming the dispersion-cured platinum composition, wherein the cross-sectional area of the three-dimensional shaped body made of the dispersion-cured platinum composition during the cold forming is reduced by at most 20%; And

Then subjecting the cold-formed three-dimensional shape to a temperature treatment, wherein the cold-formed article is tempered for at least 1 hour at a temperature of at least 1,100 ° C, whereby the dispersion-cured platinum composition is processed .

Within the scope of the present invention, the cross-sectional area should be understood as the surface area of the surface formed by the (imaginary) cross-section passing through the three-dimensional shape. The face defined by the cross-sectional area does not necessarily have to be positioned vertically or substantially perpendicular to the longest extension of the three-dimensional shaped body.

The weight percentage standards given above are 100% in total, and the weight of non-precious metal corresponds to the metal weight.

Precious or non-precious metals are preferably oxidized by oxygen at a level of at least 70%, preferably at least 90%. In this regard, preferably all the oxidation steps of the noble metal are considered so that up to 30 atomic%, in particular up to 10 atomic%, of the noble metals are present as metals, i.e. in the formal oxidation step 0.

Preferably, the dispersion-cured platinum composition comprises 0.05 to 0.5% by weight, particularly preferably 0.1 to 0.4% by weight, particularly preferably 0.15 to 0.3% by weight of at least partly oxidized ratio Contains precious metals.

The higher the fraction of noble metal oxide, the longer the life of the three-dimensional shaped body upon exposure to mechanical deformation. Having a non-noble metal oxide fraction with a low three-dimensional shape exhibits advantages associated with the machining properties of the three-dimensional shaped body, for example, the welding characteristics.

In the method according to the present invention, a three-dimensional shape is provided. In this context, the term 3D shape should be understood comprehensively. Preferably, the three-dimensional shaped body may appear in the form of sheet metal, tube or wire.

In this regard, the extension of the three-dimensional shape in three directions of the space is not particularly limited, but can be selected according to requirements. The sheet metal, tube or wire thus provided may have a thickness of from 0.1 mm to 10 mm, preferably from 0.3 mm to 5 mm. In this regard, the thickness means the minimum extension length of the three-dimensional shape. In the case of a wire, the thickness is a diameter. In the case of a tube, it is also called a wall thickness of the tube because of a difference between the outside radius and the inside radius.

Platinum compositions that can be used in accordance with the present invention include at least 70 wt% platinum and up to 29.95 wt% other precious metals. Thus, the composition may consist essentially of platinum and at least partially oxidized non-noble metals as noted above. Thus, the platinum material may be pure platinum, except for at least partially oxidized non-noble metal mixed and conventional impurities. In addition, the platinum composition may further comprise other noble metals, in which case the platinum composition is a platinum alloy.

According to the present invention, the other noble metals may be selected from ruthenium, rhodium, gold, palladium and iridium.

The provided three-dimensional shape is cold-formed according to the method according to the present invention. The term "cold forming" is known in the art world and is performed at relatively low temperatures below the recrystallization temperature of the platinum composition, and is particularly useful for cold rolling and compacting known as drawing, compression, deep drawing, hammering, . Molding involves extensive modification of the three-dimensional shape. Preferably, according to the present invention, at least 50%, particularly preferably at least 75%, particularly preferably at least 95%, of the volume of the three-dimensional shaped body can undergo deformation. According to this, when the three-dimensional shaped body is, for example, a sheet metal, preferably at least 50%, particularly preferably at least 75%, and particularly preferably at least 95% And / or pressure. In the case of sheet metal, the surface can be simplified to a plane perpendicular to the minimum extension length (thickness) of the three-dimensional shaped body. When the three-dimensional shaped body is, for example, a wire or a tube, preferably at least 50%, particularly preferably at least 75%, and particularly preferably at least 95%, of the length of the wire or tube is, for example, Exposed to force.

In the present invention, molding is essentially performed only to a relatively low degree during cold forming. The cross-sectional area of the three-dimensional shaped body made from the dispersion-cured platinum composition is reduced by at most 20%, particularly preferably by at most 18%, particularly preferably by at most 15%. These values are related to the maximum cross sectional area of the three-dimensional shape. In the case of a sheet metal that is rolled only in one direction, the reduction in cross-sectional area is determined, for example, from the thickness of the three-dimensional shaped body and the extension length not extended. In the case of a wire or tube, the cross sectional area reduction is determined from the change in diameter and / or wall thickness. Since the volume of the mold is not changed by molding, at least one cross-sectional area must be large during the molding process. For example, the length of the sheet metal, tube or wire will increase during the forming process and will also increase in surface area in the direction of increasing length. The direction in which the forming force acts is parallel or perpendicular to the plane defined by the cross-sectional area in particular.

According to a preferred embodiment, the cross-sectional area of the three-dimensional shaped body made of the dispersion-cured platinum composition is reduced by at least 5%, preferably by at least 8%, particularly preferably by at least 10% during cold forming.

It has been found clearly that the internal damage of the dispersion-cured three-dimensional shapes during forming and subsequent annealing, respectively, with respect to the reduction of the cross-sectional area of less than 5%, does not contribute significantly to creep strength improvement. The lower the change in cross-sectional area per molding step within the above-mentioned range, the better the creep strength improvement as compared to the molding process with respect to the cross sectional area reduction of 5% to 20%, preferably 8% to 18%, particularly preferably 10% .

According to the present invention, when the wire made from the dispersion-cured platinum composition is drawn or pressed during cold forming, the cross-sectional area is at most 20%, particularly preferably at most 18%, particularly preferably at most Sectional area or thickness during cold forming is reduced by up to 20%, particularly preferably by at most 18%, particularly preferably by at most 15%, when the sheet metal is rolled, drawn, pressed or compressed during cold forming, Or when the tube made of the dispersion-cured platinum composition is rolled, drawn or pressed during cold forming, the cross-sectional area is at most 20%, particularly preferably at most 18%, particularly preferably at most 15% %.

According to the present invention, microcracks or voids are not formed in the dispersion-cured platinum composition during cold forming at all or less than 100 microcracks per cubic millimeter and / or less than 1,000 voids are formed.

The three-dimensional shaped body is subjected to cold forming and then the cold-formed three-dimensional shaped body is subjected to temperature treatment, wherein the cold-formed article is tempered at least at 1,100 ° C for at least one hour. Said tempering may preferably take place over a period of at least 90 minutes, more preferably at least 120 minutes, particularly preferably at least 150 minutes, particularly preferably at least 180 minutes. The temperature at which the tempering is carried out may preferably be at least 1,200 ° C, particularly preferably at least 1,250 ° C, particularly preferably at least 1,300 ° C, and particularly preferably at least 1,400 ° C.

According to the present invention, the cold-formed three-dimensional shaped body can also be tempered during the temperature treatment for at least 1 hour at a temperature of at least 1,250 占 폚, preferably at a temperature of 1,400 占 폚 for 1 to 3 hours.

The longer the tempering process time and the higher the temperature at which the temperature treatment is performed, the better the mechanical properties of the cold-formed formed article. However, there is a concern that the improvement of the mechanical properties leads to saturation at some point and the growth of large particles, which causes the mechanical properties to decrease again. In addition, the cost of the method increases with the duration and tempering temperature. The minimum temperature of the tempering process is 1,100 ° C. The highest temperature of the tempering process is 20 [deg.] C below the melting point of each dispersion-cured platinum composition.

According to the present invention, it is possible to use temperature processing or temperature processing for the cold-formed three-dimensional shape to eliminate the defects of the three-dimensional shape.

Further, in the method according to the present invention, a plurality of cold forming processes can be sequentially performed and the cross-sectional area of the three-dimensional shaped body can be reduced by more than 20% by the cold forming process, wherein each individual cold forming process is a dispersion- The cross sectional area of the three-dimensional shaped body made of the platinum composition is reduced by at most 20%, particularly preferably by at most 18%, particularly preferably by at most 15%, and between each cold forming step, And the cold-formed article is tempered at least at 1,100 ° C for at least one hour.

In this connection, the term "during each cold forming step" means that the number of cold forming steps is equal to the number of tempering steps, preferably a temperature treatment at least at 1,100 ° C for at least one hour after each cold forming step It should be understood that.

Performing a number of cold forming and temperature treatments is relatively easy to carry out and can be carried out without undermining the dispersion-cured platinum composition by a simple cold forming process and temperature treatment, for example by reducing the creep strength of the alloy It is advantageous in that a much larger-scale molding process can be realized without the need for a mold. What is more surprising is that the creep strength is steadily improved as the number of forming and annealing steps increases.

According to a preferred embodiment of the present invention, in the case of a plurality of sequential cold forming processes, each individual cold forming process has a cross-sectional area of at least 5%, preferably at least 5%, of the three- 8%, particularly preferably at least 10%.

The forming step and subsequent annealing, which involve only a minimal reduction of the cross-sectional area of the dispersion-cured three-dimensional shape of less than 5% per forming step, do not contribute significantly to creep strength improvement. The lower the change in cross-sectional area per molding step in the above-mentioned range, the smaller the influence on the creep strength improvement as compared with the molding process relating to the sectional area reduction ratio of 5% to 20%. Moreover, having a plurality of sequential forming and annealing steps complicates the process and is therefore uneconomical. The greater the number of molding steps required to achieve the desired final dimensions of the dispersion-cured three-dimensional shape, the more likely it is. It is preferable to reach the final dimensions with a total of eight molding steps. The number of molding steps is a good trade-off between economic efficiency and improved mechanical properties.

Preferably, according to the invention, the cold-formed article is tempered at least at 1,550 ° C for at least 24 hours, at least 1,600 ° C for at least 12 hours, at least 1,650 ° C for at least one hour during the last temperature treatment after the last cold- Temperatures of from 1,690 ° C to 1,740 ° C can be tempered for at least 30 minutes.

This last step largely removes the few defects to be eliminated of the final form of the dispersion-cured platinum composition, so that the resulting product contains very high creep strength.

Any dispersion-cured platinum composition is suitable as a starting product for the process of the present invention. However, there is a surprising benefit from the use of semi-finished products, which are generally subjected to hot-forming processes. The dispersion-cured platinum composition can be formed by a hot forming process at a temperature of at least 800 캜, preferably at least 1,000 캜, particularly preferably at least 1,250 캜 before cold forming.

A further aspect of the present invention is a method for preparing a product from a dispersion-cured platinum composition, comprising providing a dispersion of at least 70% by weight platinum, up to 29.95% by weight of other precious metals and ruthenium, Preparing a composition of at least one non-noble metal selected from zirconium, cerium, scandium and yttrium at 0.05% by weight to 0.5% by weight and at least partially oxidizing the noble or non-noble metals to produce a dispersion-cured platinum composition .

Preferably, the noble metal or non-noble metal is converted to a metal oxide at a level of at least 70%, preferably at least 90%.

The treatment of the noble metal or noble metal may preferably be performed at a temperature of 600 ° C to 1,600 ° C in an oxidizing atmosphere, preferably 800 ° C to 1,000 ° C in an oxidizing atmosphere.

The method for producing a product made from the dispersion-cured platinum composition can preferably be combined with the above-described processing method and the embodiment of the method described herein as preferred.

Another aspect of the present invention is a dispersion-cured platinum material obtainable by a process and / or a process for producing a product from a dispersion-cured platinum composition. The gist of the present invention provides excellent mechanical properties in combination with excellent fabrication characteristics and / or simple manufacture at low cost.

According to the present invention, preferably, the cylindrical three-dimensional shaped body made of the dispersion-cured platinum material is capable of withstanding a tensile stress of 9 MPa in the longitudinal direction of the three-dimensional shaped body at a temperature of 1,600 DEG C for at least 40 hours without tearing, Preferably at least 50 hours without tearing, particularly preferably at least 100 hours without tearing, and / or having a rectangular cross section of 0.85 mm x 3.9 mm and a length of 140 mm and having a circular shape in an oven chamber at 1,650 ° C The sheet metal made of the dispersion-cured platinum material having a cross-sectional area of 2 mm and a spacing distance of 100 mm and disposed on two parallel-arranged cylindrical rods, , More preferably less than 14 mm, and more preferably less than 14 mm, after 40 hours when exposed, preferably less than 40 mm, preferably less than 30 mm, particularly preferably less than 20 mm, There.

According to the present invention, it is to be understood that the cylindrical three-dimensional shape is a shape such as a straight cylindrical shape, particularly a cylindrical shape, or a shape such as a cylinder having a non-circular or rounded bottom surface. In particular, the cylindrical three-dimensional shape is a rectangular parallelepiped having a corner length in the range of 0.5 mm to 5 mm (i.e., a shape similar to a cylinder having a rectangular bottom face).

It should be understood that the length of the cylindrical three-dimensional shape is the longest extension length. In the case of a wire or a tube, the longitudinal direction is the axis of the cylindrical three-dimensional shape, while in the case of sheet metal it is the direction of the extension from the surface of the sheet metal.

A dispersion-cured platinum material having the above-mentioned mechanical properties of a cylindrical three-dimensional shape is also a subject of the present invention.

According to the present invention, preferably, the dispersion-cured platinum material comprises at least one of at least one selected from zirconium, cerium, scandium and yttrium, in an amount of 0.05 to 0.4 wt%, particularly preferably 0.05 to 0.3 wt% And may include partially oxidized noble metals. According to this embodiment, it is possible to provide a material having particularly excellent mechanical properties and very good processing characteristics.

In a particular embodiment, the dispersion-cured platinum material may be sheet metal, tube or wire or a product formed from wire, tube and / or sheet metal.

It is another object of the present invention to provide a process for preparing a dispersion-cured platinum material which is obtainable or obtained through the process of the invention for producing a dispersion-cured platinum material or a product made from the process according to the invention and / It is intended for use in three-dimensional shaped glass industry or in laboratory equipment.

The present invention also allows for lower structural defects such as, for example, crystal lattice displacements introduced into a dispersion-cured platinum composition by keeping the cold forming degree low (up to 20% cross sectional area change) Lt; RTI ID = 0.0 > platinum < / RTI > composition is significantly higher than that of known methods for cold forming platinum compositions. If a wider range of forming is required, this can be accomplished by using the preceding hot forming process or a number of sequential, low-level cold forming processes, where the structural damage is eliminated through a temperature treatment between each cold forming process. In accordance with the insights gained in the scope of the present invention, the cold-formed dispersion-cured platinum compositions exhibit excellent properties such as microcracks caused by excessively high moldability and / or excessive cross-sectional area reduction, delamination of grain / It is mechanically weakened due to excessive major defects.

In particular, gentle low-level cold forming prevents internal cracks such as microcracks, particle / substrate boundary delamination and grain boundary voids that can not be solved at all or can be solved only by great effort. Microcracking due to molding and pores arising on grain boundaries are particularly damaging, especially since they impair the mechanical stability of the dispersed-cured platinum composition to a considerable extent. This damage can be prevented by using the method according to the present invention. Thus, the process of the present invention also claims as the first successful attempt to produce a dispersion-cured platinum composition with very high mechanical stability and good processing characteristics, especially welding properties.

Hereinafter, other exemplary embodiments of the present invention will be described based on some embodiments that do not limit the scope of the present invention.

The semi-finished precursor (1)

Preparation of semi-processed precursors with a sheet thickness of 2 mm through internal oxidation by Zr and Y

According to the method described in Example 1 of EP 1 964 938 A1, PtRh10 (an alloy made of 90 wt% Pt and 10 wt% Rh) and 2200 ppm of noble metals (1800 ppm Zr and 400 ppm Y) were cast. The ingot was mechanically and thermally treated as follows. The ingot was rolled to a sheet thickness of 2.2 mm, then recrystallized-annealed and then rolled to a sheet thickness of 2 mm. Next, the sheet metal was oxidized at 900 캜 for 18 days, followed by soft-annealing at 1400 캜 for 6 hours.

Semi-finished precursor (2)

Preparation of semi-processed precursors with a sheet thickness of 3 mm through internal oxidation by Zr and Y

According to the method described in Example 1 of EP 1 964 938 A1, PtRh10 (an alloy made of 90 wt% Pt and 10 wt% Rh) and 2200 ppm of noble metals (1800 ppm Zr and 400 ppm Y) were cast. The ingot was mechanically and thermally treated as follows. The ingot was rolled to a sheet thickness of 3.3 mm, then recrystallized-annealed and then rolled to a sheet thickness of 3 mm. Next, the sheet metal was oxidized at 900 ° C for 27 days, followed by soft-annealing at 1400 ° C for 6 hours.

Semi-finished precursor (3)

Preparation of semi-processed precursors with a sheet thickness of 3 mm through internal oxidation by Zr, Y and Sc

According to the method described in Example 1 of EP 1 964 938 A1, PtRh10 (an alloy made of 90 wt% Pt and 10 wt% Rh) and 2120 ppm of noble metals (1800 ppm Zr, 270 ppm Y and 50 ppm Sc) were cast. The ingot was mechanically and thermally treated as follows. The ingot was rolled to a sheet thickness of 3.3 mm, then recrystallized-annealed and then rolled to a sheet thickness of 3 mm. Next, the sheet metal was oxidized at 900 DEG C for 24 days, followed by soft-annealing at 1400 DEG C for 6 hours.

Example 1

Next, about 2 mm thick semi-finished precursor (1) obtained according to the procedure described above was further processed according to the invention into the following rolling and annealing steps.

The sheet metal was rolled to 1.7 mm and then annealed at 1,400 ° C for 4 hours. Next, the sheet metal was rolled to 1.4 mm and annealed at 1,400 ° C for 2 hours. The sheet metal was then rolled to 1.2 mm and annealed again at 1,400 ° C for 2 hours. Next, the sheet metal was rolled to 1 mm and annealed again at 1,400 ° C. The sheet metal was then rolled to a final thickness of 0.85 mm and finally annealed at 1,100 ° C for 1 hour. The cross sectional area reduction rate per rolling step was 20%.

Example 2

Example 1 was substantially repeated except that it was rolled to a final thickness of 0.85 mm and then finally annealed at 1,700 < 0 > C for 1 hour.

Example 3

Next, a semi-finished precursor (2) of about 3 mm thickness obtained according to the procedure described above was further processed according to the invention into the following rolling and annealing steps.

The sheet metal was rolled to 2.4 mm and then annealed at 1,150 占 폚 for 4 hours. Next, the sheet metal was rolled to 1.92 mm and annealed at 1,150 캜 for 4 hours. Next, the sheet metal was rolled to 1.53 mm and annealed again at 1,150 占 폚 for 4 hours. The rolling and annealing steps were repeated three times: the sheet metal was first rolled to 1.22 mm, then to 0.99 mm, then to 0.8 mm, and after each rolling step, annealing at 1,150 ° C for 4 hours. The cross sectional area reduction rate per rolling step was 20%.

Example 4

Next, a semi-finished precursor (2) of about 3 mm thickness obtained according to the procedure described above was further processed according to the invention into the following rolling and annealing steps.

The sheet metal was rolled to 2.4 mm and then annealed at 1,300 DEG C for 4 hours. Next, the sheet metal was rolled to 1.92 mm and annealed at 1,300 DEG C for 4 hours. The sheet metal was then rolled to 1.53 mm and annealed again at 1,300 DEG C for 4 hours. The rolling and annealing steps were repeated three times: the sheet metal was first rolled to 1.22 mm, then to 0.99 mm, then to 0.8 mm, and after each rolling step, annealing at 1,300 ° C for 4 hours. The cross sectional area reduction rate per rolling step was 20%.

Example 5

Next, a semi-finished precursor (2) of about 3 mm thickness obtained according to the procedure described above was further processed according to the invention into the following rolling and annealing steps.

The sheet metal was rolled to 2.4 mm and then annealed at 1,400 ° C for 4 hours. Next, the sheet metal was rolled to 1.92 mm and annealed at 1,400 DEG C for 4 hours. Next, the sheet metal was rolled to 1.53 mm and annealed again at 1,400 DEG C for 4 hours. The rolling and annealing steps were repeated three times: the sheet metal was first rolled to 1.22 mm, then to 0.99 mm, then to 0.8 mm, and after each rolling step, annealing at 1,400 ° C for 4 hours. The cross sectional area reduction rate per rolling step was 20%.

Example 6

Next, a semi-finished precursor (2) of about 3 mm thickness obtained according to the procedure described above was further processed according to the invention into the following rolling and annealing steps.

The sheet metal was rolled to 2.55 mm and then annealed at 1,400 ° C for 4 hours. Next, the sheet metal was rolled to 2.16 mm and annealed at 1,400 DEG C for 4 hours. The sheet metal was then rolled to 1.84 mm and annealed again at 1,400 ° C for 4 hours. Rolling and annealing steps in which the sheet metal is first rolled to 1.56 mm, then to 1.33 mm, then to 1.13 mm, then to 0.96 mm, then to 0.8 mm, and after each rolling step to anneal at 1,400 ° C for 4 hours Was repeated 5 times. The reduction rate of the cross-sectional area per rolling step was 15%.

Example 7

Next, a semi-finished precursor (3) of about 3 mm thickness obtained according to the procedure described above was further processed according to the invention into the following rolling and annealing steps.

The sheet metal was rolled to 2.4 mm and then annealed at 1,150 占 폚 for 4 hours. Next, the sheet metal was rolled to 1.92 mm and annealed at 1,150 캜 for 4 hours. Next, the sheet metal was rolled to 1.53 mm and annealed again at 1,150 占 폚 for 4 hours. The rolling and annealing steps were repeated three times: the sheet metal was first rolled to 1.22 mm, then to 0.99 mm, then to 0.8 mm, and after each rolling step, annealing at 1,150 ° C for 4 hours. The cross sectional area reduction rate per rolling step was 20%.

Example 8

Next, a semi-finished precursor (3) of about 3 mm thickness obtained according to the procedure described above was further processed according to the invention into the following rolling and annealing steps.

The sheet metal was rolled to 2.55 mm and then annealed at 1,400 ° C for 4 hours. Next, the sheet metal was rolled to 2.16 mm and annealed at 1,400 DEG C for 4 hours. The sheet metal was then rolled to 1.84 mm and annealed again at 1,400 ° C for 4 hours. Rolling and annealing steps in which the sheet metal is first rolled to 1.56 mm, then to 1.33 mm, then to 1.13 mm, then to 0.96 mm, then to 0.8 mm, and after each rolling step to anneal at 1,400 ° C for 4 hours Was repeated 5 times. The reduction rate of the cross-sectional area per rolling step was 15%.

Example 9

Next, a semi-finished precursor (3) of about 3 mm thickness obtained according to the procedure described above was further processed according to the invention into the following rolling and annealing steps.

The sheet metal was rolled to 2.7 mm and then annealed at 1,400 ° C for 4 hours. Next, the sheet metal was rolled to 2.43 mm and annealed at 1,400 DEG C for 4 hours. The sheet metal was then rolled to 2.19 mm and annealed again at 1,400 DEG C for 4 hours. Sheet metal is first rolled to 1.97 mm, then to 1.77 mm, then to 1.60 mm, then to 1.44 mm, then to 1.29 mm, then to 1.16 mm, then to 1.05 mm, then to 0.94 mm, then to 0.85 mm And rolling and annealing steps of annealing at 1,400 ° C for 4 hours after each rolling step were repeated nine times. The cross sectional area reduction rate per rolling step was 10%.

Example 10

Example 9 was substantially repeated except that it was rolled to a final thickness of 0.85 mm and then finally annealed at 1,700 < 0 > C for 1 hour.

Example 11

Next, a semi-finished precursor (3) of about 3 mm thickness obtained according to the procedure described above was further processed according to the invention into the following rolling and annealing steps.

The sheet metal was rolled at 1,100 DEG C (hot forming) to 1.5 mm and then annealed at 1,400 DEG C for 4 hours. Next, the sheet metal was rolled to 1.2 mm (first cold forming) and then annealed at 1,250 占 폚 for 4 hours. The sheet metal was then rolled down to 1.02 mm (second cold forming) and then annealed again at 1,250 占 폚 for 4 hours. The sheet metal is first rolled to 0.94 mm (third cold forming), then to 0.86 mm (fourth cold forming), then to 0.8 mm (fifth cold forming) and after each rolling step, Lt; / RTI > for 4 hours were repeated three times. During the hot forming step, the reduction rate of the cross-sectional area was 50%, and during the cold forming step, 20%, 15%, and then 8%, respectively.

Reference Example 1

Next, a semi-processed precursor (1) of about 2 mm thickness obtained according to the above procedure was further processed according to the conventional method. For this, the sheet metal was directly rolled up to 1 mm and annealed at 1,000 ° C. The sheet metal was then rolled to 0.85 mm and finally annealed at 1,000 DEG C for 1 hour.

Reference Example 2

Next, a semi-processed precursor (2) of about 3 mm thickness obtained according to the procedure described above was further processed according to the conventional method. For this, the sheet metal was rolled to 1.5 mm and annealed at 1,400 ° C for 4 hours. Next, the sheet metal was rolled to 0.8 mm. The cross sectional area reduction rate per rolling step was 50%.

Reference Example 3

Next, a semi-processed precursor (3) of about 3 mm thickness obtained according to the procedure described above was further processed according to the conventional method. For this, the sheet metal was rolled to 1.5 mm and annealed at 1,400 ° C for 4 hours. Next, the sheet metal was rolled to 0.8 mm. The cross sectional area reduction rate per rolling step was 50%.

The mechanical properties of the thus obtained platinum material

Creep strength according to rupture test:

In order to measure the creep strength, weights corresponding to the desired MPa unit load for a specific section were measured at a section of 0.85 mm x 3.9 mm and a length of 120 mm (Examples 1, 2, 9, 10 and Reference 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 Reference Examples 2 and 3). The sample was heated by an electric current and adjusted to a desired temperature by pyrometry measurement. The time until the sample ruptures was measured, which corresponds to the creep strength.

Creep strength up to rupture at 1,600 ℃ and 9 MPa load Reference Example 1 20 hours Reference Example 2 35 hours Reference Example 3 30 hours Example 1 50 hours Example 2 > 120 hours Example 3 > 100 hours Example 4 > 100 hours Example 5 > 100 hours Example 6 > 100 hours Example 7 > 100 hours Example 8 > 100 hours Example 9 > 100 hours Example 10 > 120 hours Example 11 > 100 hours

Creep strength value according to sagging test

The bending test is another method for evaluating the creep strength. To this end, a cross section of 0.85 mm x 10 mm and a length of 140 mm (Examples 1, 2, 9, 10 and Reference Example 1) or a cross section of 0.8 mm x 10 mm and a length of 140 mm (Examples 3, 5, 6, 7, 8, 11 and Reference Examples 2 and 3) was placed on two parallel ceramic rods spaced 100 mm apart and the middle portion of the sheet was exposed to a load of 30 g. Next, the sample batch structure was heated to 1,650 DEG C in a chamber oven and the flexure of the sample was measured after 40 hours.

Creep strength according to bending test Reference Example 1 Bend> 40 mm Reference Example 2 Flex 35 mm Reference Example 3 Bend 37 mm Example 1 Flex 18 mm Example 2 Flexibility <12 mm Example 3 Flex 18 mm Example 4 Flex 17 mm Example 5 Flex 18 mm Example 6 Flexion 16 mm Example 7 Flex 17 mm Example 8 Flex 17 mm Example 9 Flexion 16 mm Example 10 Flexure 10 mm Example 11 Flexion 16 mm

The embodiments described above demonstrate that the measures according to the invention can achieve a remarkable improvement in the mechanical properties and that this improvement can be further increased by a tempering step at temperatures above 1,100 DEG C, in particular above 1,500 DEG C.

The features of the invention disclosed in the foregoing description, the claims and the exemplary embodiments need to be solely and optionally combined to implement various implementations of the invention.

Claims (16)

At least 70% by weight of platinum, up to 29.95% by weight of other precious metals selected from ruthenium, rhodium, gold, palladium and iridium and 0.05 to 0.5% by weight of zirconium, cerium, scandium and yttrium Providing a three-dimensional shape of a dispersion-cured platinum composition comprising at least one at least partially oxidized noble metal;
Curing the dispersion-cured platinum composition by reducing the cross-sectional area of the three-dimensional shaped body made of the dispersion-cured platinum composition by as much as 20% during the cold forming; And
Subsequently subjecting the cold-formed three-dimensional shaped body to a temperature treatment, wherein the cold-formed article is tempered at least at 1,100 ° C for at least one hour
&Lt; / RTI &gt; characterized in that the process comprises the steps of: The method of claim 1, wherein the dispersion-cured platinum composition is formed by a hot forming process at a temperature of at least 800 ° C prior to the cold forming. The method according to any one of claims 1 to 3, wherein a plurality of cold forming processes are sequentially performed and the cross-sectional area of the three-dimensional shaped body is reduced by more than 20% by the plurality of cold forming processes, Sectional shape of the three-dimensional shaped body made of the platinum composition is reduced by at most 20%, and the cold-formed three-dimensional body is subjected to a temperature treatment between the respective cold-forming steps, RTI ID = 0.0 &gt; 1 hour. &Lt; / RTI &gt; 4. The method of claim 3, wherein the cold-formed article is tempered at least at 1,550 &lt; 0 &gt; C for at least 24 hours, tempered for at least 12 hours at least at 1,600 &Lt; RTI ID = 0.0 &gt; 1,690 &lt; / RTI &gt; to 1,740 &lt; 0 &gt; C for at least 30 minutes. 3. A method according to claim 1 or 2, wherein the wire made from the dispersion-cured platinum composition is pulled or pressed during cold forming to reduce the cross-sectional area by up to 20% during cold forming, Drawing or pressing or compressing the tube to reduce the cross-sectional area or thickness by as much as 20% during cold forming, or the tube made of the dispersion-cured platinum composition is rolled, drawn or pressed during cold forming, By weight. &Lt; / RTI &gt; 3. The method according to claim 1 or 2, wherein the cold forming is performed at a temperature of 500 DEG C or less. 3. The method according to claim 1 or 2, characterized in that temperature processing or temperature processes are used for the cold-formed three-dimensional shape to eliminate the defects of the three-dimensional shape. 3. The method of claim 1 or 2, wherein the cold-formed three-dimensional shaped body is tempered during a temperature treatment for at least one hour at a temperature of at least 1,250 占 폚. A process for preparing a product from a dispersion-cured platinum composition using the process according to claims 1 or 2, wherein at least 70% by weight of platinum, up to 29.95% by weight of platinum At least one noble metal selected from ruthenium, ruthenium, rhodium, gold, palladium and iridium and other precious metals and 0.05 to 0.5% by weight of ruthenium, zirconium, cerium, scandium and yttrium And at least partially oxidizing the noble metal or noble metals to produce a dispersion-cured platinum composition. The method according to claim 9, wherein the treatment of the noble metal or noble metal is performed at a temperature of 600 ° C to 1,600 ° C in an oxidizing atmosphere. A dispersion-cured platinum material characterized by being obtained through the process according to claims 1 or 2. 12. A method according to claim 11, characterized in that the cylindrical three-dimensional shaped body made of the dispersion-cured platinum material is capable of withstanding a tensile strain of 9 MPa in the longitudinal direction of the three-dimensional shaped body for at least 40 hours at a temperature of 1,600 DEG C without tear Dispersion-cured platinum material. 12. The method of claim 11, wherein the sheet metal, made of the dispersed-cured platinum material and having a rectangular cross-section of 0.85 mm x 3.9 mm and a length of 140 mm, has a circular cross-sectional area in the oven chamber of 1,650 & Placed on two parallelly arranged cylindrical rods having a diameter of 100 mm and a distance of 100 mm and sagging to less than 40 mm after 40 hours when the intermediate part of the sheet metal is exposed to a load of 30 g. Platinum material. The dispersion-cured platinum material according to claim 11, wherein the dispersion-cured platinum material is a sheet metal, a tube or a wire, or a product formed from at least one of wire, tube and sheet metal. 12. The dispersion-curable platinum material of claim 11, wherein the dispersion-cured platinum material comprises at least one at least partially oxidized non-noble metal selected from zirconium, cerium, scandium and yttrium, Cured platinum material. An apparatus for use in the glass industry or in a laboratory, comprising a dispersion-cured platinum material processed by the process according to claim 1.