Technique for novel high-temperature-resistant long-service-life strengthened platinum

Abstract

A technique for novel high-temperature-resistant long-service-life strengthened platinum, relating to the technical field of metal materials. By means of micro-alloy smelting, preparation of double powder, powder mixing and oxidation, ingot preparation under isostatic pressing, and hot and cold working, a required novel high-temperature-resistant long-service-life strengthened platinum sheet, bar or filament is finally prepared. By mixing micro-alloy powder with different particle sizes, and adjusting related parameters of the oxidation process, selective oxidation of micro-alloy components is achieved, and the purpose that a final product undergoes slow and continuous alloy phase re-oxidization during long-time use at a high-temperature to separate out second-phase particles is achieved; moreover, the second-phase particles separated out by reoxidation are at a nanoscale, so that the grain growth can be effectively inhibited, the high-temperature performance of a material is improved, and the product still has a long service life and a good use state at an extremely high temperature.

Description

A new high-temperature resistant and long-life reinforced platinum technology Technical Field

[0001] The present application relates to the field of metal material technology, and in particular to a novel high-temperature resistant and long-life reinforced platinum technology. Background Art

[0002] The high-end glass industry places stringent performance demands on platinum containers and channels. Generally, their operating temperatures range from 1300°C to 1600°C, with an expected service life of more than 18 months. Frequent addition of cold material during use can lead to significant thermal fatigue, while prolonged erosion of molten glass can cause wall thinning, flaking of reinforcement phases, and even toxic cracking due to certain elements. Consequently, the industry has long employed various strengthening mechanisms and process techniques in an effort to develop platinum materials that combine high-temperature resistance, erosion resistance, long life, and exceptional toughness.

[0003] CN 111519058 A discloses a method for preparing a dispersion-strengthened platinum-based alloy material by in-situ synthesis of nano-oxide particles. The method comprises the following steps: (1) heating and smelting; (2) atomizing and pulverizing; (3) oxidizing and sintering; and (4) forming and hot forging to obtain a finished dispersion-strengthened platinum-based alloy material, thereby simplifying the process and improving production efficiency.

[0004] CN 110983094A discloses a high-strength platinum material for resisting high-temperature deformation and a preparation method. The platinum material comprises 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 greater than 0 to less than 0.4% by weight, with platinum as the balance. The preparation method comprises the following steps: (1) batching; (2) liquid preparation; (3) sintering; and (4) forming to obtain the high-strength platinum material.

[0005] The above patent disclosures each propose a method for preparing mass-strengthened platinum materials, which achieve one or more of the characteristics of high temperature resistance, erosion resistance, long life, and toughness, but are still not comprehensive enough and face the dilemma of insufficient performance when applied.

[0006] Application Contents

[0007] In order to solve the problems existing in the prior art, the present application provides a method for preparing high-temperature resistant and long-life reinforced platinum.

[0008] This application adopts the following technical solutions:

[0009] A method for preparing high-temperature resistant and long-life reinforced platinum comprises the following steps:

[0010] (1) Microalloy smelting:

[0011] A dispersant and a pure platinum ingot are mixed according to weight percentage and placed in a vacuum induction furnace for smelting to obtain a uniformly mixed liquid alloy, which is then cast into a water-cooled copper mold at a constant speed to obtain a microalloy ingot with uniform composition and no segregation.

[0012] (2) Double powder preparation:

[0013] The microalloy ingot is hot forged into blanks, then rolled into thick plates, and then cut into metal particles. The particles are then put into a pulse arc powder making device for powder making. By adjusting different parameters of the pulse current, nano- and micron-sized microalloy powders are prepared respectively.

[0014] (3) Powder mixing and oxidation:

[0015] The nano-scale and micro-scale microalloy powders are mixed uniformly in proportion, placed in an oxidation furnace for oxidation sintering, and the oxidation degree and range of the microalloy powders in the furnace are controlled by adjusting the temperature curve, setting the oxygen flow rate and pressure, to obtain sintered pellets;

[0016] (4) Isostatic pressing ingots:

[0017] The sintered pellets after oxidation sintering are placed in a mold of a cold isostatic pressing equipment, and three levels of pressure, holding time and compensating pressure are set to press them into shape.

[0018] Preferably, in step (1), the dispersant is one or more pure metals selected from zirconium, yttrium, calcium, scandium, boron, lanthanum or titanium, or an alloy of one or more of zirconium, yttrium, calcium, scandium, boron, lanthanum or titanium and platinum, and the mass of the dispersant accounts for 0.01% to 0.6% of the total weight of the smelt.

[0019] Preferably, in step (1), the smelting vacuum is less than 20 Pa, the smelting temperature is 1800-2000° C., the smelting time is 1-2 hours, and the liquid alloy is uniformly poured into a water-cooled copper mold at a speed of 200-300 g / s.

[0020] Preferably, in step (2), the thickness of the thick plate is 3 mm, and the metal particles are 3×3 to 5×5 mm.

[0021] Preferably, in step (2), the pulse current frequency is 50 to 5000 Hz, and the intermittent period is 0.1 to 10 ms.

[0022] Preferably, in step (2), the particle size of the nano-scale powder is 20 to 100 nm, and the particle size of the micro-scale powder is 1 to 20 μm.

[0023] Preferably, in step (3), the powder mixing ratio is nanometer-scale powder: micrometer-scale powder = 1: (1-5).

[0024] Preferably, in step (3), the sintering oxidation time is 4 to 12 hours, the temperature is 250 to 1600° C., the oxygen pressure is 0.1 to 10 MPa, and the oxygen flow rate is 0.1 to 10 L / min.

[0025] Preferably, in step (4), the isostatic pressing level 3 pressure is 50-200 MPa, the holding time is 0.5-2.0 h, and the boosting pressure is 50-200 MPa.

[0026] Preferably, the method further comprises step (5):

[0027] (5) Hot and cold processing:

[0028] The pressed alloy ingots are processed into plates, bars or wires through hot forging, rolling, drawing and stamping.

[0029] This application starts with the microstructure of the material, mixes microalloy powders of different particle sizes, and then adjusts the relevant parameters of the oxidation process to achieve selective oxidation of the microalloy components, so as to achieve the purpose of slow and continuous reoxidation of the alloy phase to precipitate as second-phase particles during long-term use at high temperature in the final product. The reoxidation and precipitation of the second-phase particles are at the nanometer level, which can effectively inhibit grain growth and improve the high-temperature performance of the material, so that the product still has a long service life and good use status at extremely high temperatures, providing a new high-temperature resistant and long-life reinforced platinum technology.

[0030] This application uses the following innovative technologies:

[0031] On the one hand, the present application has prepared nano-scale (20-100nm) and micron-scale (1-20μm) microalloy powders respectively by controlling the process parameters. The conventional method of preparing nano-scale microalloy powder is mainly chemical precipitation or sol-gel method, which has a complex process flow, low output rate, and requires the use of a large amount of chemical reagents. The present application has successfully prepared nano-scale (20-100nm) microalloy powder by adjusting and transforming the relevant parameters and components of the pulse arc powder making equipment. The alloy itself reaches the nanoscale, and after oxidation, the alloy components are precipitated to become the second phase particles, and the corresponding scale is also nanoscale. According to the principle of dispersion strengthening, by introducing dispersed hard particles into the pure metal or alloy structure, the grains are refined and the dislocation movement is hindered, thereby causing a strengthening effect. Its strengthening mechanism can be simplified into the following three formulas:

[0032] (1)Hall Page formula

[0033] Where σ s is the yield strength of the material, and d is the average grain diameter of the polycrystal. Obviously, the finer the grains and the more grain boundaries there are, the greater the effect of hindering dislocation slip and the higher the yield strength.

[0034] (2) Orowan Mechanism

[0035] Where σ * is the critical shear stress, L is the distance between hard particles. It can be seen that the strengthening effect of the second phase particles is inversely proportional to the distance between particles. The smaller the distance between particles, the greater the yield strength of the material, that is, the greater the strengthening effect.

[0036] (3) Creep rate K = πσλ 3 D / 2kTd 2

[0037] Where K is the creep rate of the material, λ is the distance between hard particles, and d is the diameter of the hard particles. In this case, the creep rate of the dispersion-strengthened material is proportional to the λ of the dispersed particles. 3 / d 2 is proportional to , and λ and d have the following relationship:

[0038] Therefore, optimal strengthening effects can only be achieved by adopting appropriate dispersed particle content, distribution, and particle size. Currently, the most cutting-edge technology available in the industry is to control the second-phase particles to the nanometer scale or below, achieving breakthrough performance improvements. This application adopts this approach, using technical means to obtain nano-scale microalloy powders, which are then oxidized to precipitate second-phase particles of nanometer size and spacing. This effectively inhibits grain growth, hinders dislocation motion, and improves the material's high-temperature performance, ensuring a long service life and good performance even at extremely high temperatures.

[0039] On the other hand, platinum materials need to be used for a long time at high temperatures and face severe erosion, corrosion, and fatigue conditions during service. The performance of the original material alone is not enough. It is necessary to maintain or even provide higher performance in the case of thinning of the wall thickness and peeling of the reinforcement phase in the later stage of use to ensure the continued safe use of platinum equipment. To achieve this goal, the present application mixes nano-scale (20-100nm) and micron-scale (1-20μm) microalloy powders in a certain proportion and then performs oxidation sintering. During the process, the relevant parameters of the oxidation process are controlled to achieve selective oxidation of the microalloy components, so that the final product undergoes slow and continuous reoxidation of the alloy phase to precipitate as second-phase particles during long-term use at high temperature. The reoxidized and precipitated second-phase particles are at the nanometer level and are evenly distributed within the crystal and on the grain boundaries, further strengthening the matrix and compensating for the reduction in strength and toughness caused by thinning of the wall thickness and peeling of the reinforcement phase, so that the product can still provide sufficient performance guarantee after long-term use at extremely high temperatures.

[0040] The beneficial effects of this application are as follows:

[0041] By mixing microalloy powders of different particle sizes and then adjusting the relevant parameters of the oxidation process, selective oxidation of the microalloy components is achieved, so that the alloy phase slowly and continuously reoxidizes and precipitates into second-phase particles during long-term use at high temperatures in the final product. The reoxidized and precipitated second-phase particles are at the nanometer level, which can effectively inhibit grain growth and improve the high-temperature performance of the material, so that the product still has a long service life and good use status at extremely high temperatures.

[0042] The technical solution proposed in the examples of this application is applied to platinum by adding trace alloying elements to prepare a new type of high-temperature resistant, long-life reinforced platinum. However, after multiple tests, adjustments, and improvements based on the examples of this application, it can also be applied to materials such as gold, silver, rhodium, ruthenium, iridium, and other pure metals or their alloys. It has considerable application prospects. BRIEF DESCRIPTION OF THE DRAWINGS

[0043] The drawings described herein are used to provide a further understanding of the present application and constitute a part of the present application. The illustrative embodiments of the present application and their descriptions are used to explain the present application and do not constitute an improper limitation on the present application. In the drawings:

[0044] Figure 1 shows the prepared nanoscale (20-100 nm) microalloy powder.

[0045] FIG2 shows the prepared micron-sized (1-20 μm) microalloy powder.

[0046] Figure 3 shows the microstructural state of the unused new high-temperature resistant and long-life reinforced platinum.

[0047] Figure 4 shows the microstructural state of the new high-temperature resistant and long-life reinforced platinum after 100 days of use.

[0048] Figure 5 shows the microstructural state of the new high-temperature resistant and long-life reinforced platinum after 100 days of use.

[0049] Figure 6 shows the microstructure of the conventionally reinforced platinum after 206 days of use.

[0050] Figure 7 shows the microstructure of the new high-temperature resistant and long-life reinforced platinum after 413 days of use. DETAILED DESCRIPTION

[0051] To make the purpose, technical solutions, and advantages of this application more clear, the technical solutions of this application will be clearly and completely described below in conjunction with the specific embodiments of this application and the corresponding drawings. Obviously, the embodiments described are only part of the embodiments of this application, not all of them. Based on the embodiments in this application, all other embodiments obtained by ordinary technicians in this field without making creative efforts are within the scope of protection of this application.

[0052] Example 1

[0053] This embodiment provides a novel high-temperature resistant and long-life reinforced platinum, which comprises a pure platinum matrix and a dispersant;

[0054] The purity of the pure platinum substrate meets SM / Pt-99.95;

[0055] The amount of zirconium added as the dispersant is 0.3% of the weight of the pure platinum matrix;

[0056] The added amount of the dispersant single substance yttrium is 0.06% of the weight of the pure platinum matrix.

[0057] The preparation method of the novel high-temperature resistant and long-life reinforced platinum comprises the following steps:

[0058] 1) Microalloy smelting:

[0059] Take 10 kg of pure platinum ingot, 30 g of elemental zirconium, and 6 g of elemental yttrium, mix them and put them into a vacuum induction furnace for smelting. The vacuum degree is less than 20 Pa, the melting temperature is 1950°C, and the melting time is 1.5 hours to obtain a uniformly mixed liquid alloy. Then, it is cast into a water-cooled copper mold at a uniform speed of 270 g / s to obtain a microalloy ingot with uniform composition and no segregation.

[0060] 2) Double powder preparation:

[0061] The microalloy ingot was hot forged and then rolled into 3.0 mm thick plates, which were then cut into 3×3 mm metal particles. 5 kg of the metal particles were placed in a pulse arc powder making machine for powder making. The pulse current frequency was adjusted to 3900 Hz and the interval was 2.1 ms to produce nano-scale microalloy powder. The D 90 = 50nm; take another 5kg of metal particles into the pulse arc powder making equipment for powder making, adjust the pulse current frequency to 800Hz, the interval is 7.3ms, and obtain micron-sized microalloy powder, test its D 90 =15μm.

[0062] 3) Powder mixing and oxidation:

[0063] The nano- and micro-sized microalloy powders were uniformly mixed using a V-type powder mixer for 2 hours. After mixing, the powders were removed and placed in an oxidation furnace for oxidation sintering. The temperature curve and oxidation process were as follows: first, the temperature was raised to 350°C and maintained for 1 hour, during which the oxygen pressure was 0.5 MPa and the oxygen flow rate was 1 L / min; then, the temperature was raised to 900°C and maintained for 2 hours, during which the oxygen pressure was 2 MPa and the oxygen flow rate was 5 L / min; finally, the temperature was raised to 1300°C and maintained for 2 hours, during which the oxygen pressure was 2 MPa and the oxygen flow rate was 2 L / min, to obtain sintered pellets.

[0064] 4) Isostatic pressing ingots:

[0065] The sintered pellets after oxidation sintering are placed in a mold of a cold isostatic pressing device, and the third-level pressure is set to 200 MPa, the holding time is 2.0 h, and the supplementary pressure is 80 MPa, and pressed into shape.

[0066] 5) Hot and cold processing:

[0067] The pressed alloy ingots were heat treated at 1500°C for 30 minutes, then forged into billets. They were then cold rolled into 1.0mm thick plates. The processing rate was 8% per pass, and the total processing rate was 85% after two annealings. The intermediate annealing was performed at 1300°C for 20 minutes. Samples of the finished plates were then taken for high-temperature mechanical property testing.

[0068] Example 2

[0069] This embodiment provides a novel high-temperature resistant and long-life reinforced platinum, which comprises a pure platinum matrix and a dispersant;

[0070] The purity of the pure platinum substrate meets SM / Pt-99.95;

[0071] The amount of zirconium added as the dispersant is 0.3% of the weight of the pure platinum matrix;

[0072] The added amount of the dispersant single substance yttrium is 0.06% of the weight of the pure platinum matrix.

[0073] The preparation method of the novel high-temperature resistant and long-life reinforced platinum comprises the following steps:

[0074] 1) Microalloy smelting:

[0075] Take 10 kg of pure platinum ingot, 30 g of elemental zirconium, and 6 g of elemental yttrium, mix them and put them into a vacuum induction furnace for smelting. The vacuum degree is less than 20 Pa, the melting temperature is 1950°C, and the melting time is 1.5 hours to obtain a uniformly mixed liquid alloy. Then, it is cast into a water-cooled copper mold at a uniform speed of 270 g / s to obtain a microalloy ingot with uniform composition and no segregation.

[0076] 2) Double powder preparation:

[0077] The microalloy ingot was hot forged and then rolled into 3.0 mm thick plates, which were then cut into 3×3 mm metal particles. 5 kg of the metal particles were placed in a pulse arc powder making machine for powder making. The pulse current frequency was adjusted to 4500 Hz and the interval was 1.3 ms to produce nano-scale microalloy powder. The D 90=36nm; take another 5kg of metal particles into the pulse arc powder making equipment for powder making, adjust the pulse current frequency to 1200Hz, the interval is 5.1ms, and obtain micron-sized microalloy powder, test its D 90 =11μm.

[0078] 3) Powder mixing and oxidation:

[0079] The nano- and micro-sized microalloy powders were uniformly mixed using a V-type powder mixer for 2 hours. After mixing, the powders were removed and placed in an oxidation furnace for oxidation sintering. The temperature curve and oxidation process were as follows: first, the temperature was raised to 350°C and maintained for 1 hour, during which the oxygen pressure was 0.5 MPa and the oxygen flow rate was 1 L / min; then, the temperature was raised to 900°C and maintained for 2 hours, during which the oxygen pressure was 2 MPa and the oxygen flow rate was 5 L / min; finally, the temperature was raised to 1300°C and maintained for 2 hours, during which the oxygen pressure was 2 MPa and the oxygen flow rate was 2 L / min, to obtain sintered pellets.

[0080] 4) Isostatic pressing ingots:

[0081] The sintered pellets after oxidation sintering are placed in a mold of a cold isostatic pressing device, and the third-level pressure is set to 200 MPa, the holding time is 2.0 h, and the supplementary pressure is 80 MPa, and pressed into shape.

[0082] 5) Hot and cold processing:

[0083] The pressed alloy ingots were heat treated at 1500°C for 30 minutes, then forged into billets. They were then cold rolled into 1.0mm thick plates. The processing rate was 8% per pass, and the total processing rate was 85% after two annealings. The intermediate annealing was performed at 1300°C for 20 minutes. Samples of the finished plates were then taken for high-temperature mechanical property testing.

[0084] Example 3

[0085] This embodiment provides a novel high-temperature resistant and long-life reinforced platinum, which comprises a pure platinum matrix and a dispersant;

[0086] The purity of the pure platinum substrate meets SM / Pt-99.95;

[0087] The amount of zirconium added as the dispersant is 0.3% of the weight of the pure platinum matrix;

[0088] The added amount of the dispersant single substance yttrium is 0.06% of the weight of the pure platinum matrix.

[0089] The preparation method of the novel high-temperature resistant and long-life reinforced platinum comprises the following steps:

[0090] 1) Microalloy smelting:

[0091] Take 10 kg of pure platinum ingot, 30 g of elemental zirconium, and 6 g of elemental yttrium, mix them and put them into a vacuum induction furnace for smelting. The vacuum degree is less than 20 Pa, the melting temperature is 1950°C, and the melting time is 1.5 hours to obtain a uniformly mixed liquid alloy. Then, it is cast into a water-cooled copper mold at a uniform speed of 270 g / s to obtain a microalloy ingot with uniform composition and no segregation.

[0092] 2) Double powder preparation:

[0093] The microalloy ingot was hot forged and then rolled into 3.0 mm thick plates, which were then cut into 3×3 mm metal particles. 5 kg of the metal particles were placed in a pulse arc powder making machine for powder making. The pulse current frequency was adjusted to 3900 Hz and the interval was 2.1 ms to produce nano-scale microalloy powder. The D 90 = 50nm; take another 5kg of metal particles into the pulse arc powder making equipment for powder making, adjust the pulse current frequency to 800Hz, the interval is 7.3ms, and obtain micron-sized microalloy powder, test its D 90 =15μm.

[0094] 3) Powder mixing and oxidation:

[0095] The nano- and micro-sized microalloy powders were uniformly mixed using a V-type powder mixer for 2 hours. After mixing, the powders were taken out and placed in an oxidation furnace for oxidation sintering. The temperature curve and oxidation process were as follows: first, the temperature was raised to 450°C and maintained for 2 hours, during which the oxygen pressure was 0.9 MPa and the oxygen flow rate was 1.2 L / min; then, the temperature was raised to 1000°C and maintained for 1.5 hours, during which the oxygen pressure was 3 MPa and the oxygen flow rate was 7 L / min; finally, the temperature was raised to 1400°C and maintained for 1.5 hours, during which the oxygen pressure was 2.5 MPa and the oxygen flow rate was 1.0 L / min, to obtain sintered pellets.

[0096] 4) Isostatic pressing ingots:

[0097] The sintered pellets after oxidation sintering are placed in a mold of a cold isostatic pressing device, and the third-level pressure is set to 150 MPa, the holding time is 2.0 h, and the supplementary pressure is 100 MPa, and the pellets are pressed into shape.

[0098] 5) Hot and cold processing:

[0099] The pressed alloy ingots were heat treated at 1500°C for 30 minutes, then forged into billets. They were then cold rolled into 1.0 mm thick plates. The processing efficiency was 7% per pass, and the two annealing steps resulted in a total processing efficiency of 90%. The intermediate annealing step was heat treated at 1300°C for 20 minutes. Samples of the finished plates were then tested for high-temperature mechanical properties.

[0100] Example 4

[0101] This embodiment provides a novel high-temperature resistant and long-life reinforced platinum, which comprises a pure platinum matrix and a dispersant;

[0102] The purity of the pure platinum substrate meets SM / Pt-99.95;

[0103] The amount of zirconium added as the dispersant is 0.4% of the weight of the pure platinum matrix;

[0104] The added amount of the dispersant single substance yttrium is 0.1% of the weight of the pure platinum matrix.

[0105] The preparation method of the novel high-temperature resistant and long-life reinforced platinum comprises the following steps:

[0106] 1) Microalloy smelting:

[0107] Take 10 kg of pure platinum ingot, 40 g of elemental zirconium, and 10 g of elemental yttrium, mix them and put them into a vacuum induction furnace for smelting. The vacuum degree is less than 20 Pa, the melting temperature is 1950°C, and the melting time is 1.5 hours to obtain a uniformly mixed liquid alloy. Then, it is cast into a water-cooled copper mold at a uniform speed of 270 g / s to obtain a microalloy ingot with uniform composition and no segregation.

[0108] 2) Double powder preparation:

[0109] The microalloy ingot was hot forged and then rolled into 3.0 mm thick plates, which were then cut into 3×3 mm metal particles. 5 kg of the metal particles were placed in a pulse arc powder making machine for powder making. The pulse current frequency was adjusted to 3900 Hz and the interval was 2.1 ms to produce nano-scale microalloy powder. The D 90 = 50nm; take another 5kg of metal particles into the pulse arc powder making equipment for powder making, adjust the pulse current frequency to 800Hz, the interval is 7.3ms, and obtain micron-sized microalloy powder, test its D 90 =15μm.

[0110] 3) Powder mixing and oxidation:

[0111] The nano- and micro-sized microalloy powders were uniformly mixed using a V-type powder mixer for 2 hours. After mixing, the powders were removed and placed in an oxidation furnace for oxidation sintering. The temperature curve and oxidation process were as follows: first, the temperature was raised to 350°C and maintained for 1 hour, during which the oxygen pressure was 0.5 MPa and the oxygen flow rate was 1 L / min; then, the temperature was raised to 900°C and maintained for 2 hours, during which the oxygen pressure was 2 MPa and the oxygen flow rate was 5 L / min; finally, the temperature was raised to 1300°C and maintained for 2 hours, during which the oxygen pressure was 2 MPa and the oxygen flow rate was 2 L / min, to obtain sintered pellets.

[0112] 4) Isostatic pressing ingots:

[0113] The sintered pellets after oxidation sintering are placed in a mold of a cold isostatic pressing device, and the third-level pressure is set to 200 MPa, the holding time is 2.0 h, and the supplementary pressure is 80 MPa, and pressed into shape.

[0114] 5) Hot and cold processing:

[0115] The pressed alloy ingots were heat treated at 1500°C for 30 minutes, then forged into billets. They were then cold rolled into 1.0mm thick plates. The processing rate was 8% per pass, and the total processing rate was 85% after two annealings. The intermediate annealing was performed at 1300°C for 20 minutes. Samples of the finished plates were then taken for high-temperature mechanical property testing.

[0116] Example 5

[0117] This embodiment provides a novel high-temperature resistant and long-life reinforced platinum, which comprises a pure platinum matrix and a dispersant;

[0118] The purity of the pure platinum substrate meets SM / Pt-99.95;

[0119] The addition amount of the dispersant elemental scandium is 0.3% of the weight of the pure platinum matrix;

[0120] The added amount of the dispersant single substance yttrium is 0.1% of the weight of the pure platinum matrix.

[0121] The preparation method of the novel high-temperature resistant and long-life reinforced platinum comprises the following steps:

[0122] 1) Microalloy smelting:

[0123] Take 10 kg of pure platinum ingot, 30 g of elemental scandium, and 10 g of elemental yttrium, mix them and put them into a vacuum induction furnace for melting. The vacuum degree is less than 20 Pa, the melting temperature is 1950°C, and the melting time is 1.5 hours to obtain a uniformly mixed liquid alloy. Then, it is cast into a water-cooled copper mold at a uniform speed of 270 g / s to obtain a microalloy ingot with uniform composition and no segregation.

[0124] 2) Double powder preparation:

[0125] The microalloy ingot was hot forged and then rolled into 3.0 mm thick plates, which were then cut into 3×3 mm metal particles. 5 kg of the metal particles were placed in a pulse arc powder making machine for powder making. The pulse current frequency was adjusted to 3900 Hz and the interval was 2.1 ms to produce nano-scale microalloy powder. The D 90= 50nm; take another 5kg of metal particles into the pulse arc powder making equipment for powder making, adjust the pulse current frequency to 800Hz, the interval is 7.3ms, and obtain micron-sized microalloy powder, test its D 90 =15μm.

[0126] 3) Powder mixing and oxidation:

[0127] The nano- and micro-sized microalloy powders were uniformly mixed using a V-type powder mixer for 2 hours. After mixing, the powders were removed and placed in an oxidation furnace for oxidation sintering. The temperature curve and oxidation process were as follows: first, the temperature was raised to 350°C and maintained for 1 hour, during which the oxygen pressure was 0.5 MPa and the oxygen flow rate was 1 L / min; then, the temperature was raised to 900°C and maintained for 2 hours, during which the oxygen pressure was 2 MPa and the oxygen flow rate was 5 L / min; finally, the temperature was raised to 1300°C and maintained for 2 hours, during which the oxygen pressure was 2 MPa and the oxygen flow rate was 2 L / min, to obtain sintered pellets.

[0128] 4) Isostatic pressing ingots:

[0129] The sintered pellets after oxidation sintering are placed in a mold of a cold isostatic pressing device, and the third-level pressure is set to 200 MPa, the holding time is 2.0 h, and the supplementary pressure is 80 MPa, and pressed into shape.

[0130] 5) Hot and cold processing:

[0131] The pressed alloy ingots were heat treated at 1500°C for 30 minutes, then forged into billets. They were then cold rolled into 1.0mm thick plates. The processing rate was 8% per pass, and the total processing rate was 85% after two annealings. The intermediate annealing was performed at 1300°C for 20 minutes. Samples of the finished plates were then taken for high-temperature mechanical property testing.

[0132] Example 6

[0133] This embodiment provides a novel high-temperature resistant and long-life reinforced platinum, which comprises a pure platinum matrix and a dispersant;

[0134] The purity of the pure platinum substrate meets SM / Pt-99.95;

[0135] The amount of zirconium added as the dispersant is 0.3% of the weight of the pure platinum matrix;

[0136] The amount of yttrium added as the dispersant is 0.02% of the weight of the pure platinum matrix;

[0137] The added amount of the dispersant elemental boron is 0.01% of the weight of the pure platinum matrix.

[0138] The preparation method of the novel high-temperature resistant and long-life reinforced platinum comprises the following steps:

[0139] 1) Microalloy smelting:

[0140] Take 10kg of pure platinum ingot, 30g of elemental zirconium, 2g of elemental yttrium, and 1g of elemental boron, mix them and put them into a vacuum induction furnace for melting. The vacuum degree is less than 20Pa, the melting temperature is 1950℃, and the melting time is 1.5 hours to obtain a uniformly mixed liquid alloy, which is then cast into a water-cooled copper mold at a uniform speed of 270g / s to obtain a microalloy ingot with uniform composition and no segregation.

[0141] 2) Double powder preparation:

[0142] The microalloy ingot was hot forged and then rolled into 3.0 mm thick plates, which were then cut into 3×3 mm metal particles. 5 kg of the metal particles were placed in a pulse arc powder making machine for powder making. The pulse current frequency was adjusted to 3900 Hz and the interval was 2.1 ms to produce nano-scale microalloy powder. The D 90 = 50nm; take another 5kg of metal particles into the pulse arc powder making equipment for powder making, adjust the pulse current frequency to 800Hz, the interval is 7.3ms, and obtain micron-sized microalloy powder, test its D 90 =15μm.

[0143] 3) Powder mixing and oxidation:

[0144] The nano- and micro-sized microalloy powders were uniformly mixed using a V-type powder mixer for 2 hours. After mixing, the powders were removed and placed in an oxidation furnace for oxidation sintering. The temperature curve and oxidation process were as follows: first, the temperature was raised to 350°C and maintained for 1 hour, during which the oxygen pressure was 0.5 MPa and the oxygen flow rate was 1 L / min; then, the temperature was raised to 900°C and maintained for 2 hours, during which the oxygen pressure was 2 MPa and the oxygen flow rate was 5 L / min; finally, the temperature was raised to 1300°C and maintained for 2 hours, during which the oxygen pressure was 2 MPa and the oxygen flow rate was 2 L / min, to obtain sintered pellets.

[0145] 4) Isostatic pressing ingots:

[0146] The sintered pellets after oxidation sintering are placed in a mold of a cold isostatic pressing device, and the third-level pressure is set to 200 MPa, the holding time is 2.0 h, and the supplementary pressure is 80 MPa, and pressed into shape.

[0147] 5) Hot and cold processing:

[0148] The pressed alloy ingots were heat treated at 1500°C for 30 minutes, then forged into billets. They were then cold rolled into 1.0mm thick plates. The processing rate was 8% per pass, and the total processing rate was 85% after two annealings. The intermediate annealing was performed at 1300°C for 20 minutes. Samples of the finished plates were then taken for high-temperature mechanical property testing.

[0149] Comparative Example 1

[0150] This embodiment provides a method for preparing reinforced platinum with micron-sized powder, wherein the reinforced platinum with micron-sized powder comprises a pure platinum matrix and a dispersant;

[0151] The purity of the pure platinum substrate meets SM / Pt-99.95;

[0152] The amount of zirconium added as the dispersant is 0.3% of the weight of the pure platinum matrix;

[0153] The added amount of the dispersant single substance yttrium is 0.06% of the weight of the pure platinum matrix.

[0154] The preparation method of the novel high-temperature resistant and long-life reinforced platinum comprises the following steps:

[0155] 1) Microalloy smelting:

[0156] Take 10 kg of pure platinum ingot, 30 g of elemental zirconium, and 6 g of elemental yttrium, mix them and put them into a vacuum induction furnace for smelting. The vacuum degree is less than 20 Pa, the melting temperature is 1950°C, and the melting time is 1.5 hours to obtain a uniformly mixed liquid alloy. Then, it is cast into a water-cooled copper mold at a uniform speed of 270 g / s to obtain a microalloy ingot with uniform composition and no segregation.

[0157] 2) Powder preparation:

[0158] The microalloy ingot was hot forged and then rolled into 3.0mm thick plates, which were then cut into 3×3mm metal particles. All the metal particles were put into a pulse arc powder making machine for powder making. The pulse current frequency was adjusted to 800Hz and the interval was 7.3ms to obtain micron-sized microalloy powder. The D 90 =15μm.

[0159] 3) Powder mixing and oxidation:

[0160] The above-mentioned micron-sized powder is placed in an oxidation furnace for oxidation sintering. The temperature curve and oxidation process are as follows: first, the temperature is raised to 350°C and kept warm for 1 hour, during which the oxygen pressure is 0.5 MPa and the oxygen flow rate is 1 L / min; then the temperature is raised to 900°C and kept warm for 2 hours, during which the oxygen pressure is 2 MPa and the oxygen flow rate is 5 L / min; finally, the temperature is raised to 1300°C and kept warm for 2 hours, during which the oxygen pressure is 2 MPa and the oxygen flow rate is 2 L / min, to obtain sintered pellets.

[0161] 4) Isostatic pressing ingots:

[0162] The sintered pellets after oxidation sintering are placed in a mold of a cold isostatic pressing device, and the third-level pressure is set to 200 MPa, the holding time is 2.0 h, and the supplementary pressure is 80 MPa, and pressed into shape.

[0163] 5) Hot and cold processing:

[0164] The pressed alloy ingots were heat treated at 1400°C for 30 minutes, then forged into billets. They were then cold rolled into 1.0 mm thick plates. Each pass had a 10% processing ratio, and two annealing steps resulted in a total processing ratio of 90%. The intermediate annealing step was heat treated at 1300°C for 20 minutes. Samples of the finished plates were then taken for high-temperature mechanical property testing.

[0165] Comparative Example 2

[0166] This embodiment provides a method for preparing reinforced platinum with a nano-scale powder, wherein the nano-scale powder comprises a pure platinum matrix and a dispersant;

[0167] The purity of the pure platinum substrate meets SM / Pt-99.95;

[0168] The amount of zirconium added as the dispersant is 0.3% of the weight of the pure platinum matrix;

[0169] The added amount of the dispersant single substance yttrium is 0.06% of the weight of the pure platinum matrix.

[0170] The preparation method of the novel high-temperature resistant and long-life reinforced platinum comprises the following steps:

[0171] 1) Microalloy smelting:

[0172] Take 10 kg of pure platinum ingot, 30 g of elemental zirconium, and 6 g of elemental yttrium, mix them and put them into a vacuum induction furnace for smelting. The vacuum degree is less than 20 Pa, the melting temperature is 1950°C, and the melting time is 1.5 hours to obtain a uniformly mixed liquid alloy. Then, it is cast into a water-cooled copper mold at a uniform speed of 270 g / s to obtain a microalloy ingot with uniform composition and no segregation.

[0173] 2) Powder preparation:

[0174] The microalloy ingot was hot forged and then rolled into 3.0 mm thick plates, which were then cut into 3×3 mm metal particles. All the metal particles were put into a pulse arc powder making machine for powder making. The pulse current frequency was adjusted to 3900 Hz and the interval was 2.1 ms to obtain nano-scale microalloy powder. The D 90 =50nm.

[0175] 3) Powder mixing and oxidation:

[0176] The above-mentioned nano-scale powder is placed in an oxidation furnace for oxidation sintering. The temperature curve and oxidation process are as follows: first, the temperature is raised to 350°C and kept warm for 1 hour, during which the oxygen pressure is 0.5 MPa and the oxygen flow rate is 1 L / min; then the temperature is raised to 900°C and kept warm for 2 hours, during which the oxygen pressure is 2 MPa and the oxygen flow rate is 5 L / min; finally, the temperature is raised to 1300°C and kept warm for 2 hours, during which the oxygen pressure is 2 MPa and the oxygen flow rate is 2 L / min, to obtain sintered pellets.

[0177] 4) Isostatic pressing ingots:

[0178] The sintered pellets after oxidation sintering are placed in a mold of a cold isostatic pressing device, and the third-level pressure is set to 200 MPa, the holding time is 2.0 h, and the supplementary pressure is 80 MPa, and pressed into shape.

[0179] 5) Hot and cold processing:

[0180] The pressed alloy ingots were heat treated at 1500°C for 30 minutes, then forged into billets. They were then cold rolled into 1.0 mm thick plates. The processing rate was 5% per pass, and the total processing rate was 80% after two annealings. The intermediate annealing was performed at 1300°C for 20 minutes. Samples of the finished plates were then taken for high-temperature mechanical property testing.

[0181] Comparative Example 3

[0182] This embodiment provides a mixed fully oxidized reinforced platinum, wherein the mixed fully oxidized reinforced platinum comprises a pure platinum matrix and a dispersant;

[0183] The purity of the pure platinum substrate meets SM / Pt-99.95;

[0184] The amount of zirconium added as the dispersant is 0.3% of the weight of the pure platinum matrix;

[0185] The added amount of the dispersant single substance yttrium is 0.06% of the weight of the pure platinum matrix.

[0186] The preparation method of the novel high-temperature resistant and long-life reinforced platinum comprises the following steps:

[0187] 1) Microalloy smelting:

[0188] Take 10 kg of pure platinum ingot, 30 g of elemental zirconium, and 6 g of elemental yttrium, mix them and put them into a vacuum induction furnace for smelting. The vacuum degree is less than 20 Pa, the melting temperature is 1950°C, and the melting time is 1.5 hours to obtain a uniformly mixed liquid alloy. Then, it is cast into a water-cooled copper mold at a uniform speed of 270 g / s to obtain a microalloy ingot with uniform composition and no segregation.

[0189] 2) Powder preparation:

[0190] The microalloy ingot was hot forged and then rolled into 3.0 mm thick plates, which were then cut into 3×3 mm metal particles. 5 kg of the metal particles were placed in a pulse arc powder making machine for powder making. The pulse current frequency was adjusted to 3900 Hz and the interval was 2.1 ms to produce nano-scale microalloy powder. The D 90 = 50nm; take another 5kg of metal particles into the pulse arc powder making equipment for powder making, adjust the pulse current frequency to 800Hz, the interval is 7.3ms, and obtain micron-sized microalloy powder, test its D 90 =15μm.

[0191] 3) Powder mixing and oxidation:

[0192] The nano- and micro-sized microalloy powders were uniformly mixed using a V-type powder mixer for 2 hours. After mixing, the powders were removed and placed in an oxidation furnace for oxidation sintering. The temperature curve and oxidation process were as follows: first, the temperature was raised to 350°C and maintained for 1 hour, during which the oxygen pressure was 0.5 MPa and the oxygen flow rate was 1 L / min; then, the temperature was raised to 900°C and maintained for 5 hours, during which the oxygen pressure was 2 MPa and the oxygen flow rate was 9 L / min; finally, the temperature was raised to 1300°C and maintained for 4 hours, during which the oxygen pressure was 2 MPa and the oxygen flow rate was 2 L / min, to obtain sintered pellets.

[0193] 4) Isostatic pressing ingots:

[0194] The sintered pellets after oxidation sintering are placed in a mold of a cold isostatic pressing device, and the third-level pressure is set to 200 MPa, the holding time is 2.0 h, and the supplementary pressure is 80 MPa, and pressed into shape.

[0195] 5) Hot and cold processing:

[0196] The pressed alloy ingots were heat treated at 1500°C for 30 minutes, then forged into billets. They were then cold rolled into 1.0mm thick plates. The processing rate was 8% per pass, and the total processing rate was 85% after two annealings. The intermediate annealing was performed at 1300°C for 20 minutes. Samples of the finished plates were then taken for high-temperature mechanical property testing.

[0197] The above performance test results are shown in Table 1.

[0198] Table 1

[0199] The foregoing is merely an embodiment of the present application and is not intended to limit the present application. For those skilled in the art, the present application may have various changes and variations. Any modifications, equivalent replacements, improvements, etc. made within the spirit and principles of the present application should all be included within the scope of the claims of the present application.

Claims

1. A method for preparing high temperature resistant and long life reinforced platinum, characterized in that: The steps include: (1) Microalloy smelting: The dispersant and the pure platinum ingot are mixed according to weight percentage and placed in a vacuum induction furnace for smelting to obtain a uniformly mixed liquid alloy, which is then cast into a water-cooled copper mold at a uniform speed to obtain a microalloy ingot with uniform composition and no segregation; (2) Double powder preparation: The microalloy ingot is hot forged into a blank, then rolled into a thick plate, and then cut into metal particles, which are put into a pulse arc powder making device for powder making. Nano- and micro-level microalloy powders are prepared by adjusting different parameters of the pulse current. (3) Mixing and oxidation: The nano-scale and micro-scale micro-alloy powders are mixed evenly according to a certain proportion, and placed in an oxidation furnace for oxidation sintering. The oxidation degree and range of the micro-alloy powders in the furnace are controlled by adjusting the temperature curve, setting the oxygen flow rate and pressure, and obtaining sintered pellets. (4) Isostatic pressing ingots: The sintered pellets after oxidation sintering are placed in a cold isostatic pressing equipment mold, and three levels of pressure, holding time and supplementary pressure are set to press them into shape.

2. The preparation method according to claim 1, characterized in that: In step (1), the dispersant is one or more pure metals selected from zirconium, yttrium, calcium, scandium, boron, lanthanum or titanium, or an alloy of one or more of zirconium, yttrium, calcium, scandium, boron, lanthanum or titanium and platinum, and the mass of the dispersant accounts for 0.01% to 0.6% of the total weight of the smelting.

3. The preparation method according to claim 1, characterized in that: In step (1), the smelting vacuum degree is less than 20 Pa, the smelting temperature is 1800-2000° C., the smelting time is 1-2 hours, and the liquid alloy is uniformly cast into a water-cooled copper mold at a speed of 200-300 g / s.

4. The preparation method according to claim 1, characterized in that: In step (2), the thickness of the thick plate is 3 mm, and the metal particles are 3×3 to 5×5 mm.

5. The preparation method according to claim 1, characterized in that: In step (2), the pulse current frequency is 50 to 5000 Hz, and the interval is 0.1 to 10 ms.

6. The preparation method according to claim 1, characterized in that: In step (2), the particle size of the nano-scale powder is 20 to 100 nm, and the particle size of the micro-scale powder is 1 to 20 μm.

7. The preparation method according to claim 1, characterized in that: In step (3), the powder mixing ratio is nanometer-grade powder: micrometer-grade powder = 1: (1-5).

8. The preparation method according to claim 1, characterized in that: In step (3), the sintering oxidation time is 4 to 12 hours, the temperature is 250 to 1600° C., the oxygen pressure is 0.1 to 10 MPa, and the oxygen flow rate is 0.1 to 10 L / min.

9. The preparation method according to claim 1, characterized in that: In step (4), the isostatic pressing level 3 pressure is 50-200 MPa, the pressure holding time is 0.5-2.0 h, and the boost pressure is 50-200 MPa.

10. The preparation method according to claim 1, characterized in that: The method further comprises step (5): (5) Hot and cold processing: The pressed alloy ingots are processed into plates, bars or wires by hot forging, rolling, drawing and stamping.

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