A high-purity platinum material doped with trace substances and a preparation method thereof

Abstract

The present invention provides a high-purity platinum material doped with trace substances and a preparation method thereof, wherein the high-purity platinum material doped with trace substances comprises a pure platinum matrix and trace substances; the addition amount of the trace substances is 0.001 to 0.1% of the weight of the pure platinum matrix; the purity of the high-purity platinum material doped with trace substances is ≥99.95wt%. The high-purity platinum material doped with trace substances provided by the present invention has the advantages of low room temperature strength, easy processing, high temperature strength and long service life through the delicate addition of trace substances, and the purity of the platinum material can meet SM-Pt99.95.

Description

Technical Field

[0001] The invention belongs to the technical field of metal materials and relates to a method for preparing a platinum material, and in particular to a high-purity platinum material doped with trace substances and a method for preparing the same. Background Art

[0002] Platinum can be made into crucibles, stirrers, leak plates and other devices, and is a key material in the optical glass industry and glass fiber industry. Many materials have been developed at home and abroad to replace platinum-based alloys, but all have failed. First, the production temperature of optical glass and glass fiber is as high as 1200°C or above, and can reach up to 1650°C, which leads to the failure of many high-temperature alloys due to their inability to withstand high temperatures; secondly, the production of optical glass or glass fiber is highly corrosive, which leads to the failure of some high-temperature alloys due to their corrosion resistance; thirdly, glass production will be subject to certain external forces, which requires high-temperature alloys to have certain high-temperature creep strength.

[0003] In the current market, there are different types of platinum materials, but they can be mainly divided into two types. One is high-purity platinum, which is mainly used for thermocouple wires or disposable crucibles. Its high purity will not color the glass, but its high-temperature strength is extremely low. The other is reinforced platinum, which is used for leak plates, agitators, etc. It has higher room temperature and high-temperature strength, but it hardens quickly at room temperature and is not easy to perform complex processing.

[0004] At present, high-purity platinum materials have excellent processing properties. They can be drawn into 0.02mm φ filaments, or rolled into 0.05mm thick thin plates, or other complex special-shaped surfaces. However, their high-temperature strength is extremely poor. During use, the grains will grow rapidly and the strength will decrease rapidly, making it difficult to use for a long time in a high-temperature environment.

[0005] In order to make up for the shortcomings of high-purity platinum, people have studied and invented reinforced platinum. CN 111020275A discloses a method for preparing a zirconium dioxide dispersion-strengthened platinum material or a platinum-rhodium material, the preparation method comprising the following steps: (1) bottom casting vacuum smelting: adding a platinum ingot or a platinum-rhodium ingot and a metal zirconium into a bottom casting vacuum induction furnace for bottom casting vacuum smelting, wherein the content of the metal zirconium in the mixed material is 0.05wt% to 0.2wt%, the content of the metal rhodium in the platinum-rhodium ingot is 1wt% to 30wt%, and the rest is metal platinum, the vacuum degree of the bottom casting vacuum induction furnace is controlled at 0.1 to 12Pa, and alloy strips are obtained after bottom casting vacuum smelting; (2) slicing: cutting the alloy strip obtained in step (1) into alloy cylinders; (3) powdering: powdering the alloy cylinder obtained in step (2) with a pulse arc powder generator to obtain alloy powder; (4) drying: ) The alloy powder obtained in step (4) is placed in an oven for drying at a temperature of 180 to 250° C. and a drying time of 4 to 6 hours to obtain a dry powder; (5) Screening: The dry powder obtained in step (4) is screened, and the alloy powder with a mesh size less than 300 is retained, and the remaining dry powder is returned to step (3) for powder making, until the mesh size of the alloy powder obtained is less than 300 mesh; (6) Rough pressing: The alloy powder obtained in step (5) is added to a forming mold and roughly pressed with a hydraulic press to obtain a rough ingot; (7) Heat treatment: The rough ingot obtained in step (6) is placed in a furnace for heat treatment at a temperature of 1150 to 1300° C. and a time of 30 to 60 minutes; (8) Pressing: The heat-treated rough ingot is pressed with a hydraulic press to obtain a finished ZrO2 dispersion-strengthened platinum material or platinum-rhodium material.

[0006] CN 110983094A discloses a high-strength platinum material for resisting high-temperature deformation and a preparation method thereof. The platinum material is composed of platinum and a strengthening phase, wherein the strengthening phase is any one or more of zirconium oxide, yttrium oxide and titanium carbide particles dispersed in the platinum. The weight percentage of each component of the material is the strengthening phase component>0~≤0.4wt%, and platinum is the balance. The preparation method comprises the following steps: (1) batching; (2) liquid preparation: dissolving the platinum raw material with a strong oxidizing acid solution, adding sodium chloride with a mass fraction of 0.4-0.7 times the weight of the platinum and sodium hydroxide with a mass fraction of 5-20%, then adding deionized water to adjust the pH value to 7-9, adding a hydrated hydrazine reagent with a mass fraction of 50-90%, continuously and evenly stirring, and adding each component of the strengthening phase, stirring the solution from deep red to clear and colorless, precipitating, filtering, and repeatedly washing the precipitate with deionized water to obtain a wet powder of platinum wrapped with the strengthening phase; high temperature at 200~700℃ for 20~60min (3) sintering: the powder material of step (2) is screened, uniformly remixed, pressed at a pressure of 30-200 MPa for 10-30 min, and sintered at 1000-1300° C. to form a dense sintered body with a density of ≥99.5%; (4) molding: the sintered body obtained in step (3) is forged at 900-1300° C., the final forging temperature is 800-1100° C., cold rolled, and the single-pass deformation is ≤15% and the total deformation is ≤80% to obtain a dense material with full density, and machined to obtain a high-strength platinum material

[0007] Strengthened platinum prepared by the dispersion strengthening process has significant high-temperature strength and can serve for a long time below 1500°C. However, the improved room-temperature strength and hardening rate make the processing process difficult, and it is difficult to reach the processing limit of traditional pure platinum. In addition, the added dispersed phase content is high, which may affect the glass manufacturing process and is not suitable for the production of high-end optical glass. Summary of the invention

[0008] The purpose of the present invention is to provide a high-purity platinum material doped with trace substances and a preparation method thereof. The high-purity platinum material doped with trace substances has the advantages of low strength at room temperature and easy processing, sufficient high-temperature strength and long service life through the delicate addition of trace substances, and the purity of the platinum material can meet SM-Pt99.95.

[0009] In order to achieve the purpose of the invention, the present invention adopts the following technical solutions:

[0010] In a first aspect, the present invention provides a high-purity platinum material doped with a trace substance, wherein the high-purity platinum material doped with a trace substance comprises a pure platinum matrix and a trace substance;

[0011] The amount of the trace substance added is 0.001-0.1% of the weight of the pure platinum matrix, for example, it can be 0.001%, 0.005%, 0.01%, 0.05% or 0.1%, but is not limited to the listed values, and other values ​​not listed within the numerical range are also applicable.

[0012] The purity of the high-purity platinum material doped with trace substances is ≥99.95wt%.

[0013] The high-purity platinum material doped with trace substances of the present invention has the advantages of low strength at room temperature and easy processing, sufficient strength at high temperature and long service life through the delicate addition of trace substances, and the purity of the platinum material can meet SM-Pt99.95.

[0014] Generally speaking, the added elements generally have a certain solid solubility in the metal matrix, and precipitation will occur after the temperature drops, and there will be obvious dimples on the tensile fracture; however, the structure and performance of the platinum material provided by the present invention are very unique. At room temperature, the added elements are combined to form a highly dispersed distribution in the metal matrix and will not precipitate as a particle reinforcement phase, ensuring that the material has high toughness close to that of pure platinum.

[0015] The doping amount of the trace substance in the high-purity platinum material doped with trace substances described in the present invention is 0.001-0.1%. Too much doping amount will lead to a large amount of precipitation of dispersed phases, which will, on the one hand, cause a significant increase in the material work hardening rate and cause processing difficulties; on the other hand, it will cause welding cracks and create quality risks.

[0016] Preferably, the trace substance includes any one or a combination of at least two of B, CaB6, ZrB6 or TiB6, typical but non-limiting combinations include a combination of B and CaB6, a combination of CaB6, ZrB6 and TiB6, a combination of B and ZrB6, a combination of B and TiB6, or a combination of B, CaB6, ZrB6 and TiB6.

[0017] The trace substances described herein all contain the B element, which can be used as a trace additive element to form a unique combination with the matrix. It does not precipitate at room temperature, so that the material has the same easy processing properties as pure metal; at high temperatures, it forms submicron particles that are pinned in the crystals and grain boundaries, hindering dislocation movement and giving the material good high-temperature strength.

[0018] Preferably, the purity of the pure platinum matrix is ​​≥ 99.95wt%.

[0019] Preferably, the pure platinum metal includes sponge platinum and / or platinum ingot.

[0020] In a second aspect, the present invention provides a method for preparing a high-purity platinum material doped with trace substances as provided in the first aspect, the preparation method comprising the following steps:

[0021] (1) melting a pure platinum matrix in a reaction vessel, and then successively exhausting and refining to obtain liquid metal;

[0022] (2) mixing the trace substances and the liquid metal of step (1), keeping the temperature after casting, and then cooling to obtain an ingot;

[0023] (3) Extruding the ingot obtained in step (2) to obtain the high-purity platinum material doped with trace substances.

[0024] The preparation method of the present invention is to finally obtain the required platinum materials of different sizes through high-frequency melting, casting and heat preservation, medium-temperature extrusion, and subsequent processing. The invention adopts a unique process design and exquisite trace material addition to obtain a platinum material with low strength at room temperature and easy processing, sufficient high-temperature strength and long service life, and at the same time, the purity still meets SM-Pt99.95.

[0025] Preferably, the reaction vessel in step (1) comprises a smelting crucible.

[0026] Preferably, the material of the melting crucible includes any one of a yttria-stabilized zirconia crucible, a calcia-stabilized zirconia crucible, or a zirconia crucible.

[0027] Preferably, the pure platinum matrix in step (1) comprises sponge platinum and / or platinum ingots.

[0028] Preferably, the smelting temperature in step (1) is 1800-2000°C, for example, it can be 1800°C, 1850°C, 1900°C, 1950°C or 2000°C, but is not limited to the listed values, and other values ​​not listed within the numerical range are also applicable.

[0029] Preferably, the smelting time in step (1) is 20 to 30 min, for example, 20 min, 22 min, 24 min, 26 min, 28 min or 30 min, but is not limited to the listed values, and other values ​​not listed within the numerical range are also applicable.

[0030] Preferably, the exhaust time in step (1) is 20 to 30 minutes, for example, 20 minutes, 22 minutes, 24 minutes, 26 minutes, 28 minutes or 30 minutes, but is not limited to the listed values, and other values ​​not listed within the numerical range are also applicable.

[0031] Preferably, the refining time in step (1) is 5 to 10 minutes, for example, 5 minutes, 6 minutes, 7 minutes, 8 minutes, 9 minutes or 10 minutes, but is not limited to the listed values, and other values ​​not listed within the numerical range are also applicable.

[0032] Preferably, the refining temperature in step (1) is 2000-2050°C, for example, it can be 2000°C, 2010°C, 2020°C, 2030°C, 2040°C or 2050°C, but is not limited to the listed values, and other values ​​not listed within the numerical range are also applicable.

[0033] Preferably, the trace substances in step (2) include any one of B, CaB6, ZrB6, TiB6 or a combination of at least two thereof. Typical but non-limiting combinations include a combination of B and CaB6, a combination of CaB6, ZrB6 and TiB6, a combination of B and ZrB6, a combination of B and TiB6, or a combination of B, CaB6, ZrB6 and TiB6.

[0034] Preferably, the amount of the trace substance added in step (2) is 0.001-0.1% of the weight of the pure platinum matrix, for example, it can be 0.001%, 0.005%, 0.01%, 0.05% or 0.1%, but is not limited to the listed values, and other values ​​not listed within the numerical range are also applicable.

[0035] Preferably, the insulation temperature in step (2) is 1500-1650°C, for example, it can be 1500°C, 1540°C, 1580°C, 1620°C or 1650°C, but is not limited to the listed values, and other values ​​not listed within the numerical range are also applicable.

[0036] Preferably, the insulation time in step (2) is 20 to 60 minutes, for example, 20 minutes, 30 minutes, 40 minutes, 50 minutes or 60 minutes, but is not limited to the listed values, and other values ​​not listed within the numerical range are also applicable.

[0037] Preferably, the casting speed in step (2) is 700-800 g / s, for example, it can be 700 g / s, 720 g / s, 740 g / s, 760 g / s, 780 g / s or 800 g / s, but is not limited to the listed values, and other values ​​not listed within the numerical range are also applicable.

[0038] The insulation temperature after casting of the present invention is 1500-1650° C. If the insulation temperature is too high or too low, the dispersed additives will not be able to form submicron particles with uniform distribution that meet the requirements.

[0039] Preferably, the terminal temperature of the cooling in step (2) is 700-800°C, for example, it can be 700°C, 720°C, 740°C, 760°C, 780°C or 800°C, but is not limited to the listed values, and other values ​​not listed within the numerical range are also applicable.

[0040] Preferably, the extrusion temperature in step (3) is 700-800°C, for example, 700°C, 720°C, 740°C, 760°C, 780°C or 800°C, but is not limited to the listed values, and other values ​​not listed within the numerical range are also applicable.

[0041] Preferably, the extrusion discharge speed of the extrusion in step (3) is about 0.8 to 1.3 m / s, for example, it can be 0.8 m / s, 0.9 m / s, 1 m / s, 1.1 m / s, 1.2 m / s or 1.3 m / s, but is not limited to the listed values, and other values ​​not listed within the numerical range are also applicable.

[0042] Preferably, the extrusion pressure of the extrusion in step (3) is 180-250 MPa, for example, 180 MPa, 190 MPa, 210 MPa, 230 MPa or 250 MPa, but is not limited to the listed values, and other values ​​not listed within the numerical range are also applicable.

[0043] The extrusion pressure of the present invention is 180-250MPa. The extrusion process can be compared to "liquid phase sintering". The extrusion pressure will affect the various properties of the final product. Too high a pressure will cause extrusion defects in the material, while too low a pressure will not reach the target extrusion speed.

[0044] Preferably, step (3) further includes a post-processing process after the extrusion.

[0045] Preferably, the post-processing comprises drawing or rolling.

[0046] The present invention extrude the ingot in step (2) into round bars and / or square ingots of different sizes by extrusion, and then further processes them by drawing or rolling to obtain wires or plates of different sizes.

[0047] As a preferred technical solution of the present invention, the method for preparing the high-purity platinum material doped with trace substances provided in the second aspect of the present invention comprises the following steps:

[0048] (1) melting a pure platinum matrix in a melting crucible at a temperature of 1800 to 2000° C. for 20 to 30 minutes, then exhausting for 20 to 30 minutes and refining at a temperature of 2000 to 2050° C. for 5 to 10 minutes to obtain liquid metal;

[0049] (2) mixing the trace substances and the liquid metal of step (1), casting at a speed of 700-800 g / s, keeping the temperature at 1500-1650° C. for 20-60 min, and then cooling to 700-800° C. to obtain an ingot;

[0050] Wherein, the added amount of the trace substance is 0.001 to 0.1% of the weight of the pure platinum matrix;

[0051] (3) Extruding the ingot obtained in step (2) at a temperature of 700-800° C., an extrusion discharge speed of 0.8-1.3 m / s and a pressure of 180-250 MPa, and then drawing or rolling to obtain the high-purity platinum material doped with trace substances.

[0052] The numerical range described in the present invention not only includes the point values ​​listed above, but also includes any point values ​​between the above numerical ranges that are not listed. Due to space limitations and for the sake of simplicity, the present invention no longer exhaustively lists the specific point values ​​included in the range.

[0053] Compared with the prior art, the present invention has the following beneficial effects:

[0054] (1) The high-purity platinum material doped with trace substances provided by the present invention has the advantages of low strength at room temperature, easy processing, sufficient high-temperature strength and long service life, and the purity of the platinum material can meet SM-Pt99.95;

[0055] (2) The method for preparing a high-purity platinum material doped with trace substances provided by the present invention has a simple process and is suitable for industrial production;

[0056] (3) The method for preparing high-purity platinum materials doped with trace substances provided by the present invention is not only suitable for the preparation of platinum materials, but can also be used to prepare other metals or alloys such as gold, silver, iridium, and rhodium. BRIEF DESCRIPTION OF THE DRAWINGS

[0057] Figure 1 A tensile fracture morphology diagram of a platinum material is provided for Example 1 of the present invention;

[0058] Figure 2 A tensile fracture morphology diagram of a platinum material is provided for Comparative Example 2 of the present invention;

[0059] Figure 3 A high temperature creep fracture morphology diagram of a platinum material is provided for Example 1 of the present invention;

[0060] Figure 4 A high temperature creep fracture morphology of a platinum material is provided for Comparative Example 2 of the present invention;

[0061] Figure 5This is an internal morphology diagram of the platinum material provided in Example 1 of the present invention. DETAILED DESCRIPTION

[0062] The technical solution of the present invention is further described below in conjunction with the accompanying drawings and through specific implementation methods. It should be understood by those skilled in the art that the embodiments are only to help understand the present invention and should not be regarded as specific limitations of the present invention.

[0063] Example 1

[0064] This embodiment provides a high-purity platinum material doped with trace substances, wherein the high-purity platinum material doped with trace substances comprises a pure platinum matrix and trace substances;

[0065] The amount of the trace substance added is 0.021% of the weight of the pure platinum matrix;

[0066] The purity of the high-purity platinum material doped with trace substances is ≥99.95wt%.

[0067] The method for preparing the high-purity platinum material doped with trace substances comprises the following steps:

[0068] (1) 10 kg of pure platinum matrix with a purity meeting SM-Pt99.95 was smelted in a yttria-stabilized zirconia crucible at 1900°C for 25 minutes, and then vented for 30 minutes and refined at 2030°C for 6 minutes to obtain liquid metal;

[0069] (2) mixing 2.1 g of trace substance CaB6 and the liquid metal described in step (1), casting at a speed of 760 g / s, keeping the temperature at 1570° C. for 40 min, and then cooling to 750° C. to obtain an ingot;

[0070] (3) Extruding the ingot obtained in step (2) at a temperature of 750° C., an extrusion discharge speed of 1 m / s and a pressure of 190 MPa, and then drawing or rolling to obtain the high-purity platinum material doped with trace substances.

[0071] Example 2

[0072] This embodiment provides a high-purity platinum material doped with trace substances, wherein the high-purity platinum material doped with trace substances comprises a pure platinum matrix and trace substances;

[0073] The amount of the trace substance added is 0.04% of the weight of the pure platinum matrix;

[0074] The purity of the high-purity platinum material doped with trace substances is ≥99.95wt%.

[0075] The method for preparing the high-purity platinum material doped with trace substances comprises the following steps:

[0076] (1) 10 kg of pure platinum matrix with a purity meeting SM-Pt99.95 was melted in a calcium oxide stabilized zirconia crucible at 1950°C for 30 minutes, and then vented for 20 minutes and refined at 2000°C for 10 minutes to obtain liquid metal;

[0077] (2) mixing 4 g of trace substance B and the liquid metal of step (1), casting at a speed of 700 g / s, keeping the temperature at 1550° C. for 40 min, and then cooling to 700° C. to obtain an ingot;

[0078] (3) Extruding the ingot obtained in step (2) at a temperature of 7000° C., an extrusion discharge speed of 0.8 m / s and a pressure of 230 MPa, and then drawing or rolling to obtain the high-purity platinum material doped with trace substances.

[0079] Example 3

[0080] This embodiment provides a high-purity platinum material doped with trace substances, wherein the high-purity platinum material doped with trace substances comprises a pure platinum matrix and trace substances;

[0081] The amount of the trace substance added is 0.1% of the weight of the pure platinum matrix;

[0082] The purity of the high-purity platinum material doped with trace substances is ≥99.95wt%.

[0083] The method for preparing the high-purity platinum material doped with trace substances comprises the following steps:

[0084] (1) 10 kg of pure platinum matrix with a purity meeting SM-Pt99.95 was melted in a zirconia crucible at 2000°C for 20 minutes, and then vented for 30 minutes and refined at 2050°C for 5 minutes to obtain liquid metal;

[0085] (2) mixing 10 g of the trace substance ZrB6 and the liquid metal described in step (1), casting at a speed of 800 g / s, keeping the temperature at 1650° C. for 40 min, and then cooling to 800° C. to obtain an ingot;

[0086] (3) Extruding the ingot obtained in step (2) at a temperature of 800° C., an extrusion discharge speed of 1.3 m / s and a pressure of 250 MPa, and then drawing or rolling to obtain the high-purity platinum material doped with trace substances.

[0087] Example 4

[0088] This embodiment provides a high-purity platinum material doped with trace substances. The high-purity platinum material doped with trace substances is the same as that in Embodiment 1.

[0089] The method for preparing the high-purity platinum material doped with trace substances is different from that in Example 1 only in that:

[0090] In this embodiment, the insulation temperature after casting in step (2) is changed to 1610°C.

[0091] Example 5

[0092] This embodiment provides a high-purity platinum material doped with trace substances. The high-purity platinum material doped with trace substances is the same as that in Embodiment 1.

[0093] The method for preparing the high-purity platinum material doped with trace substances is different from that in Example 1 only in that:

[0094] In this embodiment, the insulation temperature after casting in step (2) is changed to 1480°C.

[0095] Example 6

[0096] This embodiment provides a high-purity platinum material doped with trace substances. The high-purity platinum material doped with trace substances is the same as that in Embodiment 1.

[0097] The method for preparing the high-purity platinum material doped with trace substances is different from that in Example 1 only in that:

[0098] In this embodiment, the casting temperature in step (2) is changed to 1680°C.

[0099] Example 7

[0100] This embodiment provides a high-purity platinum material doped with trace substances. The high-purity platinum material doped with trace substances is the same as that in Embodiment 1.

[0101] The method for preparing the high-purity platinum material doped with trace substances is different from that in Example 1 only in that:

[0102] In this embodiment, the extrusion pressure described in step (3) is changed to 160 MPa.

[0103] Example 8

[0104] This embodiment provides a high-purity platinum material doped with trace substances. The high-purity platinum material doped with trace substances is the same as that in Embodiment 1.

[0105] The method for preparing the high-purity platinum material doped with trace substances is different from that in Example 1 only in that:

[0106] In this embodiment, the extrusion pressure described in step (3) is changed to 260 MPa.

[0107] Example 9

[0108] This embodiment provides a high-purity platinum material doped with trace substances. The high-purity platinum material doped with trace substances is different from that of Embodiment 1 only in that:

[0109] In this embodiment, the added amount of the trace substance is changed to 0.001% of the weight of the pure platinum matrix.

[0110] The preparation method of the high-purity platinum material doped with trace substances is the same as that in Example 1.

[0111] Comparative Example 1

[0112] This comparative example provides a high-purity platinum material doped with trace substances, and the high-purity platinum material doped with trace substances is different from Example 1 only in that:

[0113] In this embodiment, the added amount of the trace substance is changed to 0.5% of the weight of the pure platinum matrix.

[0114] The preparation method of the high-purity platinum material doped with trace substances is the same as that in Example 1.

[0115] Comparative Example 2

[0116] This comparative example provides a common platinum material.

[0117] The common platinum material is a plate obtained by vacuum melting and conventional rolling of sponge platinum of SM / Pt-99.95 standard.

[0118] Comparative Example 3

[0119] This comparative example provides a reinforced platinum material, which is prepared according to the method described in CN 111020275A.

[0120] Performance testing:

[0121] The platinum materials provided in Examples 1-9 and Comparative Examples 1-3 were subjected to performance testing, and the performance testing included:

[0122] (1) Room temperature tensile test: The platinum material is drawn to obtain a φ0.5 mm wire and subjected to a room temperature tensile test to obtain the tensile strength and elongation of the wire;

[0123] (2) Creep test: The creep test was conducted at a temperature of 1400° C. and a load of 200 g to obtain the creep time of the wire;

[0124] (3) Spectral test: to obtain the purity of the silk material.

[0125] The above performance test results are shown in Table 1.

[0126] Table 1

[0127] Tensile strength / MPa Elongation / % Creep time / h Spectrum test Example 1 162 46 226 Compliant with SM-Pt99.95 Example 2 169 39 244 Compliant with SM-Pt99.95 Example 3 176 35 256 Compliant with SM-Pt99.95 Example 4 165 43 213 Compliant with SM-Pt99.95 Example 5 159 40 171 Compliant with SM-Pt99.95 Example 6 161 39 186 Compliant with SM-Pt99.95 Example 7 / / / Compliant with SM-Pt99.95 Example 8 163 24 150 Compliant with SM-Pt99.95 Example 9 151 41 5 Compliant with SM-Pt99.95 Comparative Example 1 191 12 21 / Comparative Example 2 150 40 2.0 Compliant with SM-Pt99.95 Comparative Example 3 350 20 ＞1000 Compliant with SM-Pt99.95

[0128] The tensile fracture morphologies of the platinum materials provided in Example 1 and Comparative Example 2 of the present invention during room temperature tensile testing are as follows: Figure 1 and Figure 2 As shown; the high temperature creep fracture morphology is as follows Figure 3 and Figure 4 As shown; the internal morphology of the platinum material provided in Example 1 is as Figure 5 It is knowable.

[0129] Depend on Figure 1 and Figure 2 It can be seen that the tensile fracture morphology of the platinum material provided by the present invention is basically the same as that of pure metal, which is the ductile fracture form of pure metal. Figure 5 It can be seen that there are a large number of submicron particles on the surface and inside of the platinum material provided in the present application.

[0130] Under high temperature conditions (>1200°C), due to the continuous effect of creep stress, the trace element combination in the material dissolves and aggregates along the stress direction, forming a submicron particle reinforcement structure at the grain boundary, which significantly enhances the strength of the matrix and prolongs the high temperature creep rupture time. The test results show that under the same load and temperature, the rupture time of the platinum material provided in Example 1 of the present invention is more than 10 times that of ordinary platinum.

[0131] In summary, the high-purity platinum material doped with trace substances provided by the present invention has the advantages of low strength at room temperature and easy processing, sufficient high-temperature strength and long service life through the exquisite addition of trace substances, and the purity of the platinum material can meet SM-Pt99.95.

[0132] The applicant declares that the present invention illustrates the detailed structural features of the present invention through the above-mentioned embodiments, but the present invention is not limited to the above-mentioned detailed structural features, that is, it does not mean that the present invention must rely on the above-mentioned detailed structural features to be implemented. Those skilled in the art should understand that any improvement of the present invention, equivalent replacement of the components selected by the present invention, addition of auxiliary components, selection of specific methods, etc., all fall within the protection scope and disclosure scope of the present invention.

[0133] The applicant declares that the present invention illustrates the detailed process flow of the present invention through the above-mentioned embodiments, but the present invention is not limited to the above-mentioned detailed process flow, that is, it does not mean that the present invention must rely on the above-mentioned detailed process flow to be implemented. Those skilled in the art should understand that any improvement of the present invention, equivalent replacement of various raw materials of the product of the present invention, addition of auxiliary components, selection of specific methods, etc., all fall within the protection scope and disclosure scope of the present invention.

Claims

1. A high-purity platinum material doped with trace substances, characterized in that: The high-purity platinum material doped with trace substances comprises a pure platinum matrix and trace substances; The added amount of the trace substance is 0.021-0.1% of the weight of the pure platinum matrix; the trace substance includes: ① ZrB6 and / or TiB6, ② a combination of B and ZrB6, ③ a combination of B and TiB6, ④ a combination of B, ZrB6 and TiB6, ⑤ a combination of CaB6 and ZrB6, ⑥ a combination of CaB6 and TiB6, ⑦ a combination of CaB6, ZrB6 and TiB6, or ⑧ a combination of B, CaB6, ZrB6 and TiB6. The purity of the high-purity platinum material doped with trace substances is ≥ 99.95wt%; The method for preparing the high-purity platinum material doped with trace substances comprises the following steps: (1) melting a pure platinum matrix in a reaction vessel, and then successively exhausting and refining to obtain liquid metal; (2) mixing the trace substances and the liquid metal of step (1), keeping the mixture warm for a period of time after casting, and then cooling the mixture to obtain an ingot; the keeping temperature is 1500-1650° C.; (3) Extruding the ingot obtained in step (2) to obtain the high-purity platinum material doped with trace substances; the extrusion pressure of the extrusion is 180 to 250 MPa.

2. The high-purity platinum material doped with trace substances according to claim 1, characterized in that: The purity of the pure platinum matrix is ​​≥99.95wt%.

3. The high-purity platinum material doped with trace substances according to claim 1, characterized in that: The pure platinum metal includes sponge platinum and / or platinum gold ingot.

4. A method for preparing a high-purity platinum material doped with trace substances as claimed in any one of claims 1 to 3, characterized in that: The preparation method comprises the following steps: (1) melting a pure platinum matrix in a reaction vessel, and then successively exhausting and refining to obtain liquid metal; (2) mixing the trace substances and the liquid metal of step (1), keeping the mixture warm for a period of time after casting, and then cooling the mixture to obtain an ingot; the keeping temperature is 1500-1650° C.; (3) Extruding the ingot obtained in step (2) to obtain the high-purity platinum material doped with trace substances; the extrusion pressure of the extrusion is 180 to 250 MPa.

5. The preparation method according to claim 4, characterized in that: The reaction vessel of step (1) comprises a smelting crucible.

6. The preparation method according to claim 5, characterized in that: The material of the melting crucible includes any one of a yttria-stabilized zirconia crucible, a calcia-stabilized zirconia crucible, or a zirconia crucible.

7. The preparation method according to claim 4, characterized in that: The pure platinum matrix in step (1) includes sponge platinum and / or platinum ingots.

8. The preparation method according to claim 4, characterized in that: The smelting temperature in step (1) is 1800-2000°C.

9. The preparation method according to claim 4, characterized in that: The smelting time in step (1) is 20 to 30 minutes.

10. The preparation method according to claim 4, characterized in that: The exhaust time in step (1) is 20 to 30 minutes.

11. The preparation method according to claim 4, characterized in that: The refining time in step (1) is 5 to 10 minutes.

12. The preparation method according to claim 4, characterized in that: The refining temperature in step (1) is 2000-2050°C.

13. The preparation method according to claim 4, characterized in that: The trace substances in step (2) include: ① ZrB6 and / or TiB6, ② a combination of B and ZrB6, ③ a combination of B and TiB6, ④ a combination of B, ZrB6 and TiB6, ⑤ a combination of CaB6 and ZrB6, ⑥ a combination of CaB6 and TiB6, ⑦ a combination of CaB6, ZrB6 and TiB6, or any one of a combination of B, CaB6, ZrB6 and TiB6.

14. The preparation method according to claim 5, characterized in that: The amount of the trace substance added in step (2) is 0.021 to 0.1% of the weight of the pure platinum substrate.

15. The preparation method according to claim 4, characterized in that: The insulation time in step (2) is 20 to 60 minutes.

16. The preparation method according to claim 4, characterized in that: The casting speed in step (2) is 700-800 g / s.

17. The preparation method according to claim 4, characterized in that: The terminal temperature of the cooling in step (2) is 700-800°C.

18. The preparation method according to claim 4, characterized in that: The extrusion temperature in step (3) is 700-800°C.

19. The preparation method according to claim 4, characterized in that: The extrusion discharge speed of the extrusion in step (3) is 0.8 to 1.3 m / s.

20. The preparation method according to claim 4, characterized in that: Step (3) also includes a post-processing process after the extrusion.

21. The preparation method according to claim 20, characterized in that: The post-processing includes drawing or rolling.

22. The preparation method according to any one of claims 4 to 21, characterized in that: The preparation method comprises the following steps: (1) melting a pure platinum matrix in a melting crucible at a temperature of 1800 to 2000° C. for 20 to 30 minutes, then exhausting for 20 to 30 minutes and refining at a temperature of 2000 to 2050° C. for 5 to 10 minutes to obtain liquid metal; (2) after mixing the trace substances and the liquid metal of step (1), casting at a speed of 700-800 g / s, keeping the temperature at 1500-1650° C. after casting, cooling to 700-800° C. after keeping the temperature for 20-60 min to obtain an ingot; Wherein, the added amount of the trace substance is 0.001 to 0.1% of the weight of the pure platinum matrix; (3) Extruding the ingot obtained in step (2) at a temperature of 700-800° C., an extrusion discharge speed of 0.8-1.3 m / s and a pressure of 180-250 MPa, and then drawing or rolling to obtain the high-purity platinum material doped with trace substances.

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