Preparation method of oxide dispersion strengthened ODS nickel-based superalloy

By optimizing the mechanical alloying and discharge plasma sintering processes, the cold welding and uneven oxide distribution of ODS nickel-based high-temperature alloys are solved, and the preparation of high-performance ODS nickel-based high-temperature alloys is realized, which improves the mechanical properties and oxidation resistance of the alloys.

CN120555810APending Publication Date: 2025-08-29NORTHEASTERN UNIV AT QINHUANGDAO
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Patent Information

Application Number
CN202510783894.4
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-06-12
Publication Date
2025-08-29

AI Technical Summary

Technical Problem

The existing ODS nickel-based high-temperature alloy preparation process has problems such as insufficient cold welding and powder morphology control, as well as uneven oxide distribution, which affects the alloy performance.

Method used

By optimizing the mechanical alloying and discharge plasma sintering process, specifically including the optimization of ball milling time, process control agent addition amount and sintering temperature, combined with the uniform distribution of Y2O3 powder, an oxide dispersion-strengthening ODS nickel-based high-temperature alloy is prepared.

Benefits of technology

It significantly improves the mechanical properties and oxidation resistance of the alloy, the material is easy to operate, and the oxide particles are evenly distributed, improving the mechanical properties and thermal stability of the alloy.

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Patent Text Reader

Abstract

The invention relates to a preparation method of oxide dispersion strengthened (ODS) nickel-based superalloy, and belongs to the technical field of superalloy materials. The preparation method provided by the invention comprises the following steps: weighing a certain amount of third-generation novel nickel-based high-temperature alloy powder, fully mixing the third-generation novel nickel-based high-temperature alloy powder with Y2O3 powder, and packaging the mixture and grinding balls in a ball milling tank to obtain alloyed powder; and then the alloyed powder is subjected to spark plasma sintering forming, and the oxide dispersion strengthened nickel-based high-temperature alloy with excellent mechanical performance and oxidation resistance is prepared.
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Description

Technical Field

[0001] The present invention belongs to the technical field of high-temperature alloy materials, and in particular relates to a method for preparing an oxide dispersion strengthened (ODS) nickel-based high-temperature alloy. Background Art

[0002] Nickel-based superalloys are widely used in aerospace engines and nuclear power equipment due to their excellent high-temperature strength, creep resistance, and corrosion resistance. Traditional strengthening methods (such as solid solution strengthening and precipitation strengthening) have limitations in extreme environments. However, oxide dispersion strengthening (ODS) significantly improves alloy properties by introducing nano-oxide particles. By incorporating a high density of nano-sized oxide particles into the microstructure, forming a high density of dislocations and submicron grains, these alloys exhibit excellent room-temperature and high-temperature mechanical properties, thermal stability, and radiation resistance. ODS nickel-based alloys are considered to be ideal structural materials for the first wall of fourth-generation fission reactors, cladding for advanced fusion reactors, and accident-tolerant fuel rod cladding. While research on third-generation ODS nickel-based superalloys has made some progress, existing processes still suffer from issues such as insufficient cold welding and powder morphology control, as well as uneven oxide distribution. Therefore, optimization of key parameters in mechanical alloying and sintering (such as ball milling time, process control agent dosage, and sintering temperature) is necessary to promote the development and application of high-performance ODS alloys and fourth-generation nickel-based superalloys. Summary of the Invention

[0003] The purpose of the present invention is to provide a method for preparing a high-performance ODS nickel-based superalloy by optimizing the mechanical alloying and spark plasma sintering processes to address the shortcomings of the existing technology. The specific technical solution is as follows:

[0004] A method for preparing an oxide dispersion strengthened (ODS) nickel-based high-temperature alloy comprises the following steps: firstly weighing a certain amount of third-generation novel nickel-based high-temperature alloy powder, subjecting the alloy powder to a mechanical alloying treatment to obtain alloyed powder; and then forming the alloyed powder by spark plasma sintering to obtain an oxide dispersion strengthened nickel-based high-temperature alloy having excellent mechanical properties and oxidation resistance.

[0005] Furthermore, the third-generation new nickel-based high-temperature alloy powder composition is Co 17.50wt%-19.50wt%, Cr 12.00wt%-14.00wt%, Fe 6.50wt%-7.00wt%, Al 3.60wt%-4.00wt%, Ti 3.30wt%-3.70wt%, Mo 3.20wt%-3.60wt%, Ta 2.00wt%-2.50wt%, W 1.80wt%-2.40wt%, Nb0.70wt%-1.20wt%, Mn 0.10wt%-0.15wt%, Si 0.10wt%-0.20wt%, C 0.03wt%-0.07wt%, and the balance is Ni.

[0006] Furthermore, the mechanical alloying treatment is to fully mix the third-generation new nickel-based high-temperature alloy powder and Y2O3 powder and then encapsulate them together with grinding balls in a ball mill with a ball-to-material ratio of 10:1. Stainless steel grinding balls with diameters of 10 mm, 8 mm and 5 mm are used, with a mass ratio of 1:3:6, and anhydrous ethanol is added as a process control agent.

[0007] Furthermore, the mass ratio of the third-generation new nickel-based high-temperature alloy powder to the Y2O3 powder is 1000:6.

[0008] Furthermore, the particle size of the Y2O3 powder is 20nm-30nm.

[0009] Furthermore, the ball mill jar is vacuumed and fixed in a horizontal planetary ball mill, and intermittent ball milling is adopted; the rotation speed of the ball mill is 300 r / min-400 r / min, and the ball milling time is 0.5 h-36 h.

[0010] Furthermore, the mass fraction of the anhydrous ethanol is 0-20wt.%.

[0011] Furthermore, the spark plasma sintering molding is to dry the alloyed powder, place it in a mold, and sinter it using a spark plasma sintering method.

[0012] Furthermore, the spark plasma sintering temperature is 900° C.-1200° C., the sintering pressure is 50 MPa, and the holding time is 15 minutes.

[0013] Furthermore, the oxide dispersion strengthened nickel-based high-temperature alloy has a tensile strength in the range of 1400 MPa-1500 MPa and a yield strength in the range of 1300 MPa-1400 MPa.

[0014] The above solution of the present invention includes at least the following beneficial effects:

[0015] The above scheme of the present invention optimizes the parameters of mechanical alloying. Too short ball milling time will lead to excessively large particle size and segregation of chemical composition. Prolonging the ball milling time will significantly aggravate the cold welding phenomenon while refining the particles. The addition of process control agents can increase the lubricity of the grinding balls and particle surfaces, reduce the friction coefficient, and thus reduce the adhesion and agglomeration of powder particles during the mechanical alloying process, making the powder particles smaller and the surface smoother. Too little process control agent will lead to insufficient lubrication, and too much will cause mechanical alloying failure. The present invention effectively suppresses the cold welding phenomenon and refines the powder particles by combining and optimizing the above parameters, and Y2O3 is evenly distributed in the third-generation nickel-based high-temperature alloy powder; through oxide dispersion strengthening, the mechanical properties of the alloy are significantly improved; the conditions for preparing the material are relatively low and easy to operate. BRIEF DESCRIPTION OF THE DRAWINGS

[0016] Figure 1 Schematic diagram of the tensile specimen used in the mechanical property tests in the examples and comparative examples;

[0017] Figure 2 The SEM images of the powders obtained after drying in Examples 1, 2, and 3 are shown;

[0018] Figure 3 This is a microstructure diagram of the oxide dispersion strengthened nickel-based high-temperature alloy obtained after sintering in Example 2;

[0019] Figure 4 1 is a stress-strain curve of the oxide dispersion strengthened nickel-based high-temperature alloy obtained after sintering Examples 2 and 3 and Comparative Example 1;

[0020] Figure 5 Graph showing the ultimate tensile strength and elongation of the oxide dispersion strengthened nickel-based superalloy obtained after sintering Examples 2 and 3 and Comparative Example 1;

[0021] Figure 6 This is the oxidation weight gain curve obtained through the heat exposure experiment of Examples 2 and 3. DETAILED DESCRIPTION

[0022] The following will be combined with the embodiments of the present invention and the accompanying drawings to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the embodiments described are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative work are within the scope of protection of the present invention. The present invention is further described in detail below with reference to specific implementation cases. However, the scope of protection of the present invention is not limited by the specific implementation methods.

[0023] Example 1

[0024] A method for preparing an oxide dispersion strengthened (ODS) nickel-based high-temperature alloy comprises the following steps:

[0025] The third generation new nickel-based superalloy powder is fully mixed with Y2O3 powder accounting for 0.6% of the mass of the nickel-based superalloy powder and then packaged in a ball mill together with grinding balls. The composition of the third generation new nickel-based superalloy powder is Co17.68wt%, Cr13.42wt%, Fe 6.52wt%, Al 3.95wt%, Ti 3.35wt%, Mo 3.32wt%, Ta2.13wt%, W 1.82wt%, Nb 0.82wt%, Mn 0.14wt%, Si 0.13wt%, C The alloy powder MA-1 was obtained by evacuating the ball mill and then fixing it in a planetary ball mill and milling it at a speed of 300 r / min for 36 h. The obtained alloy powder MA-1 was placed in a drying oven for drying. The SEM image of the powder obtained after drying is shown in FIG. Figure 2 As shown in (a), the dried powder is placed in a mold for spark plasma sintering at a sintering temperature of 1050° C. and a sintering pressure of 50 MPa. The sintering is carried out for 15 minutes to obtain an oxide dispersion strengthened nickel-based high temperature alloy SPS-0%.

[0026] Tensile test

[0027] The tensile test was performed using an Mtest50 in-situ tension meter with a tensile rate of 0.1 mm / min. Bow-tie tensile specimens with dimensions of 20 mm × 3 mm × 2 mm were cut from the sintered specimens by electrospark machining. The dimensions of the tensile specimens were as follows: Figure 1 In order to ensure the accuracy of the tensile data, three tensile tests were performed on each heat-treated sample.

[0028] Heat exposure experiment

[0029] Oxidation tests were conducted on samples of sintered, oxide-dispersion-strengthened nickel-based superalloy. These samples were machined into 6 mm × 6 mm × 6 mm squares using wire-cut electrospark cutting (EDM) equipment. The surfaces were then ground with SiC sandpaper and cleaned in an ultrasonic cleaner using analytical-grade anhydrous ethanol. Isothermal oxidation tests were conducted in a muffle furnace at 900°C in air for 5, 15, 40, 70, 100, 200, and 500 hours. The samples were removed from the furnace at various oxidation intervals, and the mass gain was recorded using an electronic balance with an accuracy of 0.0001 g. Oxidation weight gain curves were then plotted.

[0030] Example 2

[0031] A method for preparing an oxide dispersion strengthened (ODS) nickel-based high-temperature alloy comprises the following steps:

[0032] The third generation new nickel-based superalloy powder is fully mixed with Y2O3 powder accounting for 0.6% of the mass of the nickel-based superalloy powder and then packaged in a ball mill together with grinding balls. The composition of the third generation new nickel-based superalloy powder is Co17.57wt%, Cr 13.38wt%, Fe 6.72wt%, Al 4.00wt%, Ti 3.37wt%, Mo 3.24wt%, Ta2.06wt%, W1.88wt%, Nb 0.75wt%, Mn 0.11wt%, Si 0.10wt%, C 0.04wt%, the balance being Ni; the ball-to-material ratio being 10:1, the grinding balls being stainless steel grinding balls with diameters of 10mm, 8mm and 5mm, respectively, with a mass ratio of 1:3:6, and 1wt% anhydrous ethanol being added as a process control agent, the ball milling jar being vacuumed, and then fixed in a planetary ball mill, and ball milled at a speed of 350r / min for 36h to obtain alloy powder MA-2; the alloy powder obtained in the step is placed in a drying oven for drying, and the SEM image of the powder obtained after drying is shown as follows Figure 2 (b) shown; the dried powder was placed in a mold for spark plasma sintering, the sintering temperature was 1050 ℃, the sintering pressure was 50MPa, and the temperature was kept for 15min to obtain an oxide dispersion-strengthened nickel-based superalloy SPS-1%, Figure 3 This is the microstructure diagram of the oxide dispersion strengthened nickel-based high-temperature alloy obtained after sintering. It can be seen from the figure that the structure after sintering is dense, has no obvious defects, has a small grain size, and has evenly distributed fine dispersed phases.

[0033] Tensile test

[0034] The tensile test was performed using an Mtest50 in-situ tension meter with a tensile rate of 0.1 mm / min. Bow-tie tensile specimens with dimensions of 20 mm × 3 mm × 2 mm were cut from the sintered specimens by electrospark machining. The dimensions of the tensile specimens were as follows: Figure 1 In order to ensure the accuracy of the tensile data, three tensile tests were performed on each heat-treated sample.

[0035] Heat exposure experiment

[0036] Oxidation tests were conducted on samples of sintered, oxide-dispersion-strengthened nickel-based superalloy. These samples were machined into 6 mm × 6 mm × 6 mm squares using wire-cut electrospark cutting (EDM) equipment. The surfaces were then ground with SiC sandpaper and cleaned in an ultrasonic cleaner using analytical-grade anhydrous ethanol. Isothermal oxidation tests were conducted in a muffle furnace at 900°C in air for 5, 15, 40, 70, 100, 200, and 500 hours. The samples were removed from the furnace at various oxidation intervals, and the mass gain was recorded using an electronic balance with an accuracy of 0.0001 g. Oxidation weight gain curves were then plotted.

[0037] Example 3

[0038] A method for preparing an oxide dispersion strengthened (ODS) nickel-based high-temperature alloy comprises the following steps:

[0039] The third generation new nickel-based superalloy powder is fully mixed with Y2O3 powder accounting for 0.6% of the mass of the nickel-based superalloy powder and then packaged in a ball mill together with grinding balls. The composition of the third generation new nickel-based superalloy powder is Co18.13wt%, Cr 12.84wt%, Fe 6.86wt%, Al 3.72wt%, Ti 3.47wt%, Mo 3.46wt%, Ta2.37wt%, W2.01wt%, Nb 0.89wt%, Mn 0.11wt%, Si 0.17wt%, C The ball-to-material ratio is 10:1, and the grinding balls are stainless steel grinding balls with diameters of 10 mm, 8 mm, and 5 mm, respectively, with a mass ratio of 1:3:6. 10 wt% anhydrous ethanol is added as a process control agent. The ball mill is vacuumed and then fixed in a planetary ball mill. The ball mill is milled at a speed of 400 r / min for 36 h to obtain alloy powder MA-3. The obtained alloy powder is placed in a drying oven for drying. The SEM image of the powder after drying is shown in FIG. Figure 2(c) As shown; the dried powder is placed in a mold for spark plasma sintering at a sintering temperature of 1050°C and a sintering pressure of 50 MPa, and the mixture is kept warm for 15 minutes to obtain an oxide dispersion strengthened nickel-based high temperature alloy SPS-10%.

[0040] Tensile test

[0041] The tensile test was performed using an Mtest50 in-situ tension meter with a tensile rate of 0.1 mm / min. Bow-tie tensile specimens with dimensions of 20 mm × 3 mm × 2 mm were cut from the sintered specimens by electrospark machining. The dimensions of the tensile specimens were as follows: Figure 1 In order to ensure the accuracy of the tensile data, three tensile tests were performed on each heat-treated sample.

[0042] Heat exposure experiment

[0043] The samples used for oxidation testing were taken from sintered oxide-dispersion-strengthened nickel-based superalloys and processed into 6mm×6mm×6mm squares using wire-cut electric discharge equipment. The surfaces were then ground with SiC sandpaper and cleaned with analytical-grade anhydrous ethanol in an ultrasonic cleaner. Isothermal oxidation tests were conducted in a muffle furnace at 900°C in an air atmosphere. The experimental times were set to 5h, 15h, 40h, 70h, 100h, 200h, and 500h. The samples were removed from the furnace at different oxidation intervals, and the mass gain was recorded using an electronic balance with an accuracy of 0.0001g. The oxidation weight gain curve was then plotted. Figure 6 The oxidation weight gain curves obtained from the heat exposure experiments of Examples 2 and 3 show that increasing the content of the process control agent can improve the oxidation resistance of the alloy.

[0044] Example 4

[0045] A method for preparing an oxide dispersion strengthened (ODS) nickel-based high-temperature alloy comprises the following steps:

[0046] The third generation new nickel-based superalloy powder is fully mixed with Y2O3 powder accounting for 0.6% of the mass of the nickel-based superalloy powder and then packaged in a ball mill together with grinding balls. The composition of the third generation new nickel-based superalloy powder is Co17.63wt%, Cr 12.74wt%, Fe 6.82wt%, Al 3.78wt%, Ti 3.65wt%, Mo 3.44wt%, Ta2.31wt%, W1.88wt%, Nb 0.73wt%, Mn 0.11wt%, Si 0.11wt%, C The raw materials are characterized by amorphous metal sintering, amorphous metal sintering, and amorphous metal sintering. The raw materials are characterized by amorphous metal sintering, amorphous metal sintering, and amorphous metal sintering. The raw materials are characterized by amorphous metal sintering, amorphous metal sintering, and amorphous metal sintering. The raw materials are characterized by amorphous metal sintering, amorphous metal sintering, and amorphous metal sintering. The raw materials are characterized by amorphous metal sintering, amorphous metal sintering, and amorphous metal sintering.

[0047] Tensile test

[0048] The tensile test was performed using an Mtest50 in-situ tension meter with a tensile rate of 0.1 mm / min. Bow-tie tensile specimens with dimensions of 20 mm × 3 mm × 2 mm were cut from the sintered specimens by electrospark machining. The dimensions of the tensile specimens were as follows: Figure 1 In order to ensure the accuracy of the tensile data, three tensile tests were performed on each heat-treated sample.

[0049] Heat exposure experiment

[0050] Oxidation tests were conducted on samples of sintered, oxide-dispersion-strengthened nickel-based superalloy. These samples were machined into 6 mm × 6 mm × 6 mm squares using wire-cut electrospark cutting (EDM) equipment. The surfaces were then ground with SiC sandpaper and cleaned in an ultrasonic cleaner using analytical-grade anhydrous ethanol. Isothermal oxidation tests were conducted in a muffle furnace at 900°C in air for 5, 15, 40, 70, 100, 200, and 500 hours. The samples were removed from the furnace at various oxidation intervals, and the mass gain was recorded using an electronic balance with an accuracy of 0.0001 g. Oxidation weight gain curves were then plotted.

[0051] Example 5

[0052] A method for preparing an oxide dispersion strengthened (ODS) nickel-based high-temperature alloy comprises the following steps:

[0053] The third generation new nickel-based superalloy powder is fully mixed with Y2O3 powder accounting for 0.6% of the mass of the nickel-based superalloy powder and then packaged in a ball mill together with grinding balls. The composition of the third generation new nickel-based superalloy powder is Co18.56wt%, Cr 12.93wt%, Fe 6.76wt%, Al 3.87wt%, Ti 3.45wt%, Mo 3.54wt%, Ta2.07wt%, W1.99wt%, Nb 0.82wt%, Mn 0.13wt%, Si 0.13wt%, C 0.06wt%, the balance is Ni; the ball-to-material ratio is 10:1, the grinding balls are stainless steel grinding balls with diameters of 10mm, 8mm and 5mm, respectively, with a mass ratio of 1:3:6, and 1wt% anhydrous ethanol is added as a process control agent, the ball mill is vacuumed, and then fixed in a planetary ball mill, and ball milled at a speed of 350r / min for 18h to obtain alloy powder; the obtained alloy powder is placed in a drying oven for drying; the dried powder is placed in a mold for spark plasma sintering, the sintering temperature is 900℃, the sintering pressure is 50MPa, and the heat preservation is carried out for 15min to obtain oxide dispersion strengthened nickel-based high-temperature alloy.

[0054] Tensile test

[0055] The tensile test was performed using an Mtest50 in-situ tension meter with a tensile rate of 0.1 mm / min. Bow-tie tensile specimens with dimensions of 20 mm × 3 mm × 2 mm were cut from the sintered specimens by electrospark machining. The dimensions of the tensile specimens were as follows: Figure 1 In order to ensure the accuracy of the tensile data, three tensile tests were performed on each heat-treated sample.

[0056] Heat exposure experiment

[0057] Oxidation tests were conducted on samples of sintered, oxide-dispersion-strengthened nickel-based superalloy. These samples were machined into 6 mm × 6 mm × 6 mm squares using wire-cut electrospark cutting (EDM) equipment. The surfaces were then ground with SiC sandpaper and cleaned in an ultrasonic cleaner using analytical-grade anhydrous ethanol. Isothermal oxidation tests were conducted in a muffle furnace at 900°C in air for 5, 15, 40, 70, 100, 200, and 500 hours. The samples were removed from the furnace at various oxidation intervals, and the mass gain was recorded using an electronic balance with an accuracy of 0.0001 g. Oxidation weight gain curves were then plotted.

[0058] Example 6

[0059] A method for preparing an oxide dispersion strengthened (ODS) nickel-based high-temperature alloy comprises the following steps:

[0060] The third generation new nickel-based superalloy powder is fully mixed with Y2O3 powder accounting for 0.6% of the mass of the nickel-based superalloy powder and then packaged in a ball mill together with grinding balls. The composition of the third generation new nickel-based superalloy powder is Co17.86wt%, Cr 12.76wt%, Fe 6.81wt%, Al 3.65wt%, Ti 3.37wt%, Mo 3.25wt%, Ta2.13wt%, W2.14wt%, Nb 0.86wt%, Mn 0.12wt%, Si 0.10wt%, C The invention discloses a method for preparing a nickel-based high-temperature alloy comprising the following steps: preparing the nickel-based high-temperature alloy by mixing the nickel-based high-temperature alloy with the nickel-based high-temperature alloy having an average nickel content of 0.06wt% and a nickel-based high-temperature alloy having an average nickel content of 0.06wt% and a nickel-based high-temperature alloy having a ball-to-material ratio of 10:1 and stainless steel grinding balls with diameters of 10, 8 and 5 mm, respectively, at a mass ratio of 1:3:6, and adding 1wt% anhydrous ethanol as a process control agent, and vacuumizing the ball mill, and then fixing the ball mill in a planetary ball mill and ball milling the ball mill at a speed of 350r / min for 0.5h to obtain an alloy powder; placing the obtained alloy powder in a drying oven for drying; placing the dried powder in a mold for spark plasma sintering at a sintering temperature of 1050°C and a sintering pressure of 50MPa for 15min to obtain an oxide dispersion strengthened nickel-based high-temperature alloy.

[0061] Tensile test

[0062] The tensile test was performed using an Mtest50 in-situ tension meter with a tensile rate of 0.1 mm / min. Bow-tie tensile specimens with dimensions of 20 mm × 3 mm × 2 mm were cut from the sintered specimens by electrospark machining. The dimensions of the tensile specimens were as follows: Figure 1 In order to ensure the accuracy of the tensile data, three tensile tests were performed on each heat-treated sample.

[0063] Heat exposure experiment

[0064] Oxidation tests were conducted on samples of sintered, oxide-dispersion-strengthened nickel-based superalloy. These samples were machined into 6 mm × 6 mm × 6 mm squares using wire-cut electrospark cutting (EDM) equipment. The surfaces were then ground with SiC sandpaper and cleaned in an ultrasonic cleaner using analytical-grade anhydrous ethanol. Isothermal oxidation tests were conducted in a muffle furnace at 900°C in air for 5, 15, 40, 70, 100, 200, and 500 hours. The samples were removed from the furnace at various oxidation intervals, and the mass gain was recorded using an electronic balance with an accuracy of 0.0001 g. Oxidation weight gain curves were then plotted.

[0065] Comparative Example 1

[0066] The third-generation new nickel-based high-temperature alloy powder was placed in a mold for spark plasma sintering. The powder composition was Co17.51wt%, Cr 13.74wt%, Fe 6.76wt%, Al 3.76wt%, Ti 3.46wt%, Mo 3.52wt%, Ta2.26wt%, W2.06wt%, Nb 0.82wt%, Mn 0.11wt%, Si 0.13wt%, C 0.03wt%, and the balance was Ni. The sintering temperature was 1200℃, the sintering pressure was 50MPa, and the temperature was kept for 15min to obtain the nickel-based high-temperature alloy Original alloy.

[0067] The tensile test was performed using an Mtest50 in-situ tension meter at a tensile rate of 0.1 mm / min. Bow-tie tensile specimens with dimensions of 20 mm × 3 mm × 2 mm were cut from the sintered specimens by electrospark machining. The dimensions of the tensile specimens were as follows: Figure 1 In order to ensure the accuracy of the tensile data, three tensile tests were performed on each heat-treated sample.

[0068] Figure 4 The stress-strain curves of the oxide dispersion-strengthened nickel-based high-temperature alloys obtained after sintering Examples 2 and 3 and Comparative Example 1 show that reducing the content of the process control agent can improve the strength of the alloy. However, the lower strength of Example 3 is attributed to the large-scale oxide generation caused by the excessive addition of the process control agent, which significantly increases the brittleness of the material.

[0069] Figure 5 The ultimate tensile strength and elongation diagram of the oxide dispersion strengthened nickel-based high-temperature alloy obtained after sintering Examples 2, 3 and Comparative Example 1. It can be seen from the figure that the alloy obtained in Comparative Example 1 has the best ductility. Analysis shows that this is because the high sintering temperature promotes tissue densification. Compared with Comparative Example 1, although the sintering temperature is lowered, Example 2 still maintains an ultimate tensile strength equivalent to that of the original alloy, and the yield strength is significantly increased. This illustrates the effectiveness of the oxide particles introduced by mechanical alloying and the key role of nano-oxide dispersion in improving alloy properties. An increase in the content of process control agents will lead to a decrease in the tensile strength and elongation of the alloy. Analysis shows that this is because a large amount of oxides are generated, resulting in increased brittleness of the material.

[0070] It is understood that the above embodiments are merely exemplary embodiments for illustrating the principles of the present invention, and the present invention is not limited thereto. Various modifications and improvements can be made in this field without departing from the spirit and essence of the present invention, and such modifications and improvements are also considered to be within the scope of protection of the present invention.

Claims

1. A method for preparing an oxide dispersion strengthened ODS nickel-based high-temperature alloy, characterized in that: The method comprises the following steps: firstly weighing a certain amount of third-generation new nickel-based high-temperature alloy powder, subjecting the alloy powder to mechanical alloying treatment to obtain alloyed powder; then forming the alloyed powder by spark plasma sintering to obtain an oxide dispersion-strengthened nickel-based high-temperature alloy with excellent mechanical properties and oxidation resistance.

2. The method for preparing an oxide dispersion strengthened ODS nickel-based high-temperature alloy according to claim 1, characterized in that: The third-generation new nickel-based high-temperature alloy powder has a composition of Co 17.50wt%-19.50wt%, Cr 12.00wt%-14.00wt%, Fe 6.50wt%-7.00wt%, Al 3.60wt%-4.00wt%, Ti 3.30wt%-3.70wt%, Mo 3.20wt%-3.60wt%, Ta 2.00wt%-2.50wt%, W 1.80wt%-2.40wt%, Nb 0.70wt%-1.20wt%, Mn 0.10wt%-0.15wt%, Si 0.10wt%-0.20wt%, C 0.03wt%-0.07wt%, and the balance is Ni.

3. The method for preparing an oxide dispersion strengthened ODS nickel-based high-temperature alloy according to claim 1, characterized in that: The mechanical alloying process involves fully mixing the third-generation new nickel-based high-temperature alloy powder and Y2O3 powder and then encapsulating the mixture together with grinding balls in a ball mill with a ball-to-material ratio of 10:

1. Stainless steel grinding balls with diameters of 10 mm, 8 mm, and 5 mm are used, with a mass ratio of 1:3:6, and anhydrous ethanol is added as a process control agent.

4. The method for preparing an oxide dispersion strengthened ODS nickel-based high-temperature alloy according to claim 3, characterized in that: The mass ratio of the third-generation new nickel-based high-temperature alloy powder to Y2O3 powder is 1000:

6.

5. The method for preparing an oxide dispersion strengthened ODS nickel-based high-temperature alloy according to claim 3, characterized in that: The particle size of the Y2O3 powder is 20nm-30nm.

6. The method for preparing an oxide dispersion strengthened (ODS) nickel-based high-temperature alloy according to claim 3, characterized in that: The ball mill jar is vacuumed and fixed in a horizontal planetary ball mill, and intermittent ball milling is adopted; the rotation speed of the ball mill is 300 rpm to 400 rpm, and the ball milling time is 0.5 h to 36 h.

7. The method for preparing an oxide dispersion strengthened (ODS) nickel-based high-temperature alloy according to claim 3, characterized in that: The mass fraction of the anhydrous ethanol is 0-20 wt.%.

8. The method for preparing an oxide dispersion strengthened (ODS) nickel-based high-temperature alloy according to claim 1, characterized in that: The spark plasma sintering molding is to dry the alloyed powder, place it in a mold, and sinter it using a spark plasma sintering method.

9. The method for preparing an oxide dispersion strengthened (ODS) nickel-based high-temperature alloy according to claim 8, characterized in that: The spark plasma sintering temperature is 900° C.-1200° C., the sintering pressure is 50 MPa, and the holding time is 15 minutes.

10. The method for preparing an oxide dispersion strengthened (ODS) nickel-based high-temperature alloy according to claim 1, characterized in that: The oxide dispersion strengthened nickel-based high-temperature alloy has a tensile strength ranging from 1400 MPa to 1500 MPa and a yield strength ranging from 1300 MPa to 1400 MPa.