A new high temperature resistant and long life reinforced platinum technology

Abstract

The present application discloses a novel high-temperature resistant and long-life reinforced platinum technology, which belongs to the field of metal material technology. It is finally prepared through microalloy smelting, dual powder preparation, powder mixing and oxidation, isostatic pressing of ingots, hot and cold processing to obtain the required novel high-temperature resistant and long-life reinforced platinum sheet, rod or wire. The present application achieves the selective oxidation of microalloy components by mixing microalloy powders of different particle sizes and then adjusting the relevant parameters of the oxidation process, so as to achieve the purpose of slow and continuous reoxidation and precipitation of alloy phase into second phase particles during the long-term use at high temperature in the final product, and the reoxidation precipitation into the second phase particles is 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.

Description

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 has very strict requirements on the performance of platinum containers and channels. Generally speaking, the operating temperature is between 1300 and 1600°C, and the service life is expected to be more than 18 months. Frequent addition of cold materials during use will cause great thermal fatigue. Long-term erosion of glass liquid will cause wall thickness reduction, strengthening phase peeling, and even some elements will cause poisoning cracking. Therefore, for a long time, the industry has applied various strengthening mechanisms and process methods in order to obtain a platinum material that has the characteristics of high temperature resistance, erosion resistance, long life, and strong 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 powdering; (3) oxidative 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 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; (3) sintering; and (4) molding 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 used.

[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] 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;

[0012] (2) Double powder preparation:

[0013] 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.

[0014] (3) Mixing and oxidation:

[0015] 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.

[0016] (4) Isostatic Pressing Ingots:

[0017] 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.

[0018] Preferably, in step (1), the dispersant is one or more pure metals selected from zirconium, yttrium, calcium, scandium, boron, lanthanum or titanium, or the dispersant is 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.

[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 cast 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 interval 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-sized powder: micrometer-sized 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 pressure 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 by hot forging, rolling, drawing and stamping.

[0029] The present 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 precipitation of the second phase particles has a size of nanometers, 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 a good use state 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 powders is mainly chemical precipitation or sol-gel method, which has a complex process flow, low yield, and requires the use of a large amount of chemical reagents. The present application has successfully prepared nano-scale (20-100nm) microalloy powders by adjusting and modifying 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, only by adopting appropriate dispersed particle content, distribution, and particle size can a better strengthening effect be achieved, and the most cutting-edge technical means currently available in the industry is to control the second phase particles at or below the nanometer level to achieve a breakthrough performance improvement. This application adopts this idea, and obtains nanometer-level microalloy powder through technical means, and then oxidizes it to precipitate second phase particles of nanometer size and spacing, which can effectively inhibit grain growth, hinder dislocation movement, and improve the high-temperature performance of the material, so that the product still has a long service life and a good use state 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 strengthening 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 micro-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 can be slowly and continuously reoxidized and precipitated as second-phase particles during long-term use at high temperatures, and the reoxidized precipitation is the second-phase particle size at the nanometer level, evenly distributed in the crystal and on the grain boundary, further strengthening the matrix, compensating for the reduction in strength and toughness caused by thinning of the wall thickness and peeling of the strengthening 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 can be achieved, so that the alloy phase can be slowly and continuously reoxidized and precipitated as second-phase particles during long-term use at high temperatures in the final product. The size of the reoxidized and precipitated second-phase particles is 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 a good use state at extremely high temperatures.

[0042] The technical solution proposed in the embodiment of the present application is applied to the preparation of a new type of high temperature resistant and long life reinforced platinum after adding trace alloy elements to platinum. However, after multiple tests, adjustments and improvements according to the embodiment of the present application, it can also be applied to gold, silver, rhodium, ruthenium, iridium pure metals or their alloys and other materials. It has certain 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 The invention relates to a prepared nano-scale (20-100 nm) microalloy powder.

[0045] Figure 2 The invention relates to a prepared micron-sized (1-20 μm) microalloy powder.

[0046] Figure 3 For the unused new high temperature long life reinforced platinum microstructure state.

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

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

[0049] Figure 6 This is the normal reinforced platinum phase structure state after 206 days of use.

[0050] Figure 7 It is a new type of high temperature resistant and long life reinforced platinum phase organization state after 413 days of use. DETAILED DESCRIPTION

[0051] In order to make the purpose, technical solution and advantages of the present application clearer, the technical solution of the present application will be clearly and completely described below in combination with the specific embodiments of the present application and the corresponding drawings. Obviously, the described embodiments are only part of the embodiments of the present application, not all of the embodiments. Based on the embodiments in the present application, all other embodiments obtained by ordinary technicians in this field without making creative work are within the scope of protection of the present application.

[0052] Example 1

[0053] This embodiment provides a novel high temperature resistant and long life reinforced platinum, wherein the novel high temperature resistant and long life reinforced platinum 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 10kg of pure platinum ingot, 30g of elemental zirconium and 6g of elemental yttrium, mix them and put them into a vacuum induction furnace for smelting. The vacuum degree is less than 20Pa, the smelting temperature is 1950℃, and the smelting 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.

[0060] 2) Double powder preparation:

[0061] The microalloy ingot was hot forged into a blank, then rolled into a 3.0 mm thick plate, and then cut into 3×3 mm metal particles. 5 kg of the metal particles were put into a pulse arc powder making device 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. Its D 90 =50nm; take another 5kg of metal particles and put them into the pulse arc powder making equipment for powder making, adjust the pulse current frequency to 800Hz, the interval to 7.3ms, and obtain micron-sized microalloy powder, and test its D 90 =15μm.

[0062] 3) Mixing and oxidation:

[0063] The nano-scale and micro-scale microalloy powders were mixed evenly using a V-type powder mixer for 2 hours. After the powder mixing was completed, the powder was 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 350°C, and the temperature was kept for 1 hour, during which the oxygen pressure was 0.5MPa and the oxygen flow rate was 1L / min; then the temperature was raised to 900°C, and the temperature was kept for 2 hours, during which the oxygen pressure was 2MPa and the oxygen flow rate was 5L / min; finally, the temperature was raised to 1300°C, and the temperature was kept for 2 hours, during which the oxygen pressure was 2MPa and the oxygen flow rate was 2L / min, to obtain sintered pellets.

[0064] 4) Isostatic pressing ingots:

[0065] The sintered pellets after oxidation sintering are placed into 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 to press them into shape.

[0066] 5) Hot and cold processing:

[0067] The pressed alloy ingots were heat treated at 1500℃ for 30min, forged into billets, and then cold rolled into 1.0mm thick plates. The pass processing rate was 8%, and the total processing rate was 85% after two annealings. The intermediate annealing condition was heat treated at 1300℃ for 20min. The finished plates were sampled for high temperature mechanical property testing.

[0068] Example 2

[0069] This embodiment provides a novel high temperature resistant and long life reinforced platinum, wherein the novel high temperature resistant and long life reinforced platinum 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 10kg of pure platinum ingot, 30g of elemental zirconium and 6g of elemental yttrium, mix them and put them into a vacuum induction furnace for smelting. The vacuum degree is less than 20Pa, the smelting temperature is 1950℃, and the smelting 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.

[0076] 2) Double powder preparation:

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

[0078] 3) Mixing and oxidation:

[0079] The nano-scale and micro-scale microalloy powders were mixed evenly using a V-type powder mixer for 2 hours. After the powder mixing was completed, the powder was 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 350°C, and the temperature was kept for 1 hour, during which the oxygen pressure was 0.5MPa and the oxygen flow rate was 1L / min; then the temperature was raised to 900°C, and the temperature was kept for 2 hours, during which the oxygen pressure was 2MPa and the oxygen flow rate was 5L / min; finally, the temperature was raised to 1300°C, and the temperature was kept for 2 hours, during which the oxygen pressure was 2MPa and the oxygen flow rate was 2L / min, to obtain sintered pellets.

[0080] 4) Isostatic pressing ingots:

[0081] The sintered pellets after oxidation sintering are placed into 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 to press them into shape.

[0082] 5) Hot and cold processing:

[0083] The pressed alloy ingots were heat treated at 1500℃ for 30min, forged into billets, and then cold rolled into 1.0mm thick plates. The pass processing rate was 8%, and the total processing rate was 85% after two annealings. The intermediate annealing condition was heat treated at 1300℃ for 20min. The finished plates were sampled for high temperature mechanical property testing.

[0084] Example 3

[0085] This embodiment provides a novel high temperature resistant and long life reinforced platinum, wherein the novel high temperature resistant and long life reinforced platinum 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 10kg of pure platinum ingot, 30g of elemental zirconium and 6g of elemental yttrium, mix them and put them into a vacuum induction furnace for smelting. The vacuum degree is less than 20Pa, the smelting temperature is 1950℃, and the smelting 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.

[0092] 2) Double powder preparation:

[0093] The microalloy ingot was hot forged into a blank, then rolled into a 3.0 mm thick plate, and then cut into 3×3 mm metal particles. 5 kg of the metal particles were put into a pulse arc powder making device 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. Its D 90 =50nm; take another 5kg of metal particles and put them into the pulse arc powder making equipment for powder making, adjust the pulse current frequency to 800Hz, the interval to 7.3ms, and obtain micron-sized microalloy powder, and test its D 90 =15μm.

[0094] 3) Mixing and oxidation:

[0095] The nano-scale and micro-scale microalloy powders were mixed evenly using a V-type powder mixer for 2 hours. After the powder mixing was completed, the powder was 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 kept for 2 hours, during which the oxygen pressure was 0.9MPa and the oxygen flow rate was 1.2L / min; then the temperature was raised to 1000°C and kept for 1.5 hours, during which the oxygen pressure was 3MPa and the oxygen flow rate was 7L / min; finally, the temperature was raised to 1400°C and kept for 1.5 hours, during which the oxygen pressure was 2.5MPa and the oxygen flow rate was 1.0L / min, to obtain sintered pellets.

[0096] 4) Isostatic pressing ingots:

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

[0098] 5) Hot and cold processing:

[0099] The pressed alloy ingots were heat treated at 1500℃ for 30min, then forged into blanks, and then cold rolled into 1.0mm thick plates. The pass processing rate was 7%, and the total processing rate was 90% after two annealings. The intermediate annealing condition was heat treated at 1300℃ for 20min. The finished plates were sampled for high temperature mechanical property testing.

[0100] Example 4

[0101] This embodiment provides a novel high temperature resistant and long life reinforced platinum, wherein the novel high temperature resistant and long life reinforced platinum 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 10kg of pure platinum ingot, 40g of elemental zirconium and 10g of elemental yttrium, mix them and put them into a vacuum induction furnace for smelting. 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.

[0108] 2) Double powder preparation:

[0109] The microalloy ingot was hot forged into a blank, then rolled into a 3.0 mm thick plate, and then cut into 3×3 mm metal particles. 5 kg of the metal particles were put into a pulse arc powder making device 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. Its D 90 =50nm; take another 5kg of metal particles and put them into the pulse arc powder making equipment for powder making, adjust the pulse current frequency to 800Hz, the interval to 7.3ms, and obtain micron-sized microalloy powder, and test its D 90 =15μm.

[0110] 3) Mixing and oxidation:

[0111] The nano-scale and micro-scale microalloy powders were mixed evenly using a V-type powder mixer for 2 hours. After the powder mixing was completed, the powder was 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 350°C, and the temperature was kept for 1 hour, during which the oxygen pressure was 0.5MPa and the oxygen flow rate was 1L / min; then the temperature was raised to 900°C, and the temperature was kept for 2 hours, during which the oxygen pressure was 2MPa and the oxygen flow rate was 5L / min; finally, the temperature was raised to 1300°C, and the temperature was kept for 2 hours, during which the oxygen pressure was 2MPa and the oxygen flow rate was 2L / min, to obtain sintered pellets.

[0112] 4) Isostatic pressing ingots:

[0113] The sintered pellets after oxidation sintering are placed into 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 to press them into shape.

[0114] 5) Hot and cold processing:

[0115] The pressed alloy ingots were heat treated at 1500℃ for 30min, forged into billets, and then cold rolled into 1.0mm thick plates. The pass processing rate was 8%, and the total processing rate was 85% after two annealings. The intermediate annealing condition was heat treated at 1300℃ for 20min. The finished plates were sampled for high temperature mechanical property testing.

[0116] Example 5

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

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

[0119] The added amount of the single substance scandium as the dispersant 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 10kg of pure platinum ingot, 30g of scandium and 10g of yttrium, mix them and put them into a vacuum induction furnace for smelting. 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. Then, it is 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.

[0124] 2) Double powder preparation:

[0125] The microalloy ingot was hot forged into a blank, then rolled into a 3.0 mm thick plate, and then cut into 3×3 mm metal particles. 5 kg of the metal particles were put into a pulse arc powder making device 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. Its D 90 =50nm; take another 5kg of metal particles and put them into the pulse arc powder making equipment for powder making, adjust the pulse current frequency to 800Hz, the interval to 7.3ms, and obtain micron-sized microalloy powder, and test its D 90 =15μm.

[0126] 3) Mixing and oxidation:

[0127] The nano-scale and micro-scale microalloy powders were mixed evenly using a V-type powder mixer for 2 hours. After the powder mixing was completed, the powder was 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 350°C, kept for 1 hour, during which the oxygen pressure was 0.5MPa and the oxygen flow rate was 1L / min, then the temperature was raised to 900°C, kept for 2 hours, during which the oxygen pressure was 2MPa and the oxygen flow rate was 5L / min; finally, the temperature was raised to 1300°C, kept for 2 hours, during which the oxygen pressure was 2MPa and the oxygen flow rate was 2L / min, and sintered pellets were obtained.

[0128] 4) Isostatic pressing ingots:

[0129] The sintered pellets after oxidation sintering are placed into 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 to press them into shape.

[0130] 5) Hot and cold processing:

[0131] The pressed alloy ingots were heat treated at 1500℃ for 30min, forged into billets, and then cold rolled into 1.0mm thick plates. The pass processing rate was 8%, and the total processing rate was 85% after two annealings. The intermediate annealing condition was heat treated at 1300℃ for 20min. The finished plates were sampled for high temperature mechanical property testing.

[0132] Example 6

[0133] This embodiment provides a novel high temperature resistant and long life reinforced platinum, wherein the novel high temperature resistant and long life reinforced platinum 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 added amount of the dispersant single substance yttrium 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 smelting. 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 into a blank, then rolled into a 3.0 mm thick plate, and then cut into 3×3 mm metal particles. 5 kg of the metal particles were put into a pulse arc powder making device 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. Its D 90 =50nm; take another 5kg of metal particles and put them into the pulse arc powder making equipment for powder making, adjust the pulse current frequency to 800Hz, the interval to 7.3ms, and obtain micron-sized microalloy powder, and test its D 90 =15μm.

[0143] 3) Mixing and oxidation:

[0144] The nano-scale and micro-scale microalloy powders were mixed evenly using a V-type powder mixer for 2 hours. After the powder mixing was completed, the powder was 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 350°C, and the temperature was kept for 1 hour, during which the oxygen pressure was 0.5MPa and the oxygen flow rate was 1L / min; then the temperature was raised to 900°C, and the temperature was kept for 2 hours, during which the oxygen pressure was 2MPa and the oxygen flow rate was 5L / min; finally, the temperature was raised to 1300°C, and the temperature was kept for 2 hours, during which the oxygen pressure was 2MPa and the oxygen flow rate was 2L / min, to obtain sintered pellets.

[0145] 4) Isostatic pressing ingots:

[0146] The sintered pellets after oxidation sintering are placed into 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 to press them into shape.

[0147] 5) Hot and cold processing:

[0148] The pressed alloy ingots were heat treated at 1500℃ for 30min, forged into billets, and then cold rolled into 1.0mm thick plates. The pass processing rate was 8%, and the total processing rate was 85% after two annealings. The intermediate annealing condition was heat treated at 1300℃ for 20min. The finished plates were sampled 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 includes 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 10kg of pure platinum ingot, 30g of elemental zirconium and 6g of elemental yttrium, mix them and put them into a vacuum induction furnace for smelting. The vacuum degree is less than 20Pa, the smelting temperature is 1950℃, and the smelting 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.

[0157] 2) Powder preparation:

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

[0159] 3) 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 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 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 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 into 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 to press them into shape.

[0163] 5) Hot and cold processing:

[0164] The pressed alloy ingots were heat treated at 1400℃ for 30min, forged into billets, and then cold rolled into 1.0mm thick plates. The pass processing rate was 10%, and the total processing rate was 90% after two annealings. The intermediate annealing condition was heat treated at 1300℃ for 20min. The finished plates were sampled for high temperature mechanical property testing.

[0165] Comparative Example 2

[0166] This embodiment provides a method for preparing reinforced platinum with nano-scale powder, wherein the nano-scale powder for preparing reinforced platinum includes 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 10kg of pure platinum ingot, 30g of elemental zirconium and 6g of elemental yttrium, mix them and put them into a vacuum induction furnace for smelting. The vacuum degree is less than 20Pa, the smelting temperature is 1950℃, and the smelting 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.

[0173] 2) Powder preparation:

[0174] The microalloy ingot was hot forged into a blank, then rolled into a 3.0 mm thick plate, and then cut into 3×3 mm metal particles. All the metal particles were put into a pulse arc powder making device 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) Mixing and oxidation:

[0176] The above-mentioned nanoscale 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 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 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 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 into 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 to press them into shape.

[0179] 5) Hot and cold processing:

[0180] The pressed alloy ingots were heat treated at 1500℃ for 30min, forged into billets, and then cold rolled into 1.0mm thick plates. The pass processing rate was 5%, and the total processing rate was 80% after two annealings. The intermediate annealing condition was heat treated at 1300℃ for 20min. The finished plates were sampled 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 includes 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 10kg of pure platinum ingot, 30g of elemental zirconium and 6g of elemental yttrium, mix them and put them into a vacuum induction furnace for smelting. The vacuum degree is less than 20Pa, the smelting temperature is 1950℃, and the smelting 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.

[0189] 2) Powder preparation:

[0190] The microalloy ingot was hot forged into a blank, then rolled into a 3.0 mm thick plate, and then cut into 3×3 mm metal particles. 5 kg of the metal particles were put into a pulse arc powder making device 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. Its D 90 =50nm; take another 5kg of metal particles and put them into the pulse arc powder making equipment for powder making, adjust the pulse current frequency to 800Hz, the interval to 7.3ms, and obtain micron-sized microalloy powder, and test its D 90 =15μm.

[0191] 3) Mixing and oxidation:

[0192] The nano-scale and micro-scale microalloy powders were mixed evenly using a V-type powder mixer for 2 hours. After the powder mixing was completed, the powder was 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 350°C and kept for 1 hour, during which the oxygen pressure was 0.5MPa and the oxygen flow rate was 1L / min; then the temperature was raised to 900°C and kept for 5 hours, during which the oxygen pressure was 2MPa and the oxygen flow rate was 9L / min; finally, the temperature was raised to 1300°C and kept for 4 hours, during which the oxygen pressure was 2MPa and the oxygen flow rate was 2L / min, to obtain sintered pellets.

[0193] 4) Isostatic pressing ingots:

[0194] The sintered pellets after oxidation sintering are placed into 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 to press them into shape.

[0195] 5) Hot and cold processing:

[0196] The pressed alloy ingots were heat treated at 1500℃ for 30min, forged into billets, and then cold rolled into 1.0mm thick plates. The pass processing rate was 8%, and the total processing rate was 85% after two annealings. The intermediate annealing condition was heat treated at 1300℃ for 20min. The finished plates were sampled for high temperature mechanical property testing.

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

[0198] Table 1

[0199]

[0200] The above is only 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 modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application should be included in 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, wherein the pulse current frequency is 50 to 5000 Hz, the interval is 0.1 to 10 ms, the nano-level powder particle size is 20 to 100 nm, and the micro-level powder particle size is 1 to 20 μm; (3) Mixing and oxidation: The nano-scale and micro-scale micro-alloy powders are uniformly mixed in a ratio of nano-scale powder: micro-scale powder = 1: (1-5), and placed in an oxidation furnace for oxidation sintering, and the oxidation degree and range of the micro-alloy powder in the furnace are controlled by adjusting the temperature curve, setting the oxygen flow rate and pressure, to obtain sintered pellets, wherein the sintering oxidation time is 4-12 hours, the temperature is 250-1600° C., the oxygen pressure is 0.1-10 MPa, and the oxygen flow rate is 0.1-10 L / min; (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 (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.

6. 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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